Powell -Harpstead, Inc. - Records Collections

SDMS Document

101598 Powell -Harpstead, Inc.Professional Engineering and Environmental Services

JOHNSON & TOWERS, INC.

FIELD OPERATIONS PLAN

DECEMBER, 1992REVISED: MARCH 18, 1993

REVISED: DECEMBER 4, 1997

SECTION F - STANDARD OPERATING PROCEDURES

1313 West Chester PikeWest Chester, PA 19382610-430-7866Fax 610-430-7872 A Women's Business Enterprise 301094

2615 River Road Unit 2Cinnaminson.NJ 08077

609-786-7171Fax 609-786-7174

Powell - Harpstead, Inc.

STANDARD OPERATING PROCEDURES

REVISED: DECEMBER 4, 1997

301095

Powell - Harpstead, Inc.

SELECTED STANDARD OPERATING PROCEDURES

FIELD ACTIVITIES

TABLE OF CONTENTS

SECTION

EXISTING MONITORING WELL EVALUATION....... F-3

GROUNDWATER LEVEL MEASUREMENTS F-4

SAMPLING ..F-5

ANALYTICAL METHODS/SAMPLE CONTAINERS F-6

EQUIPMENT DECONTAMINATION. F-8

SAMPLE PACKAGING & SHIPPING.. F-10

FIELD pH/SPECIFIC CONDUCTANCE/TEMPERATURE MEASUREMENT F-12

OPERATIONAL PROCEDURES - HORD3A U-10 WATER CHECKER. F-13

OPERATIONAL PROCEDURES - HNu PID (101) ...F-15

OPERATIONAL PROCEDURES - DISSOLVED OXYGEN METER F-16

OPERATIONAL PROCEDURES - KIR-89 INTERFACE PROBE F-18

OPERATIONAL PROCEDURES - GEOPROBE MACRO-CORE ANDLARGE-BORE SAMPLING DEVICES ...F-19

301096

PROCEDURE F-3

EXISTING MONITORING WELL EVALUATION

Powell Environmental Services, Inc.REVISED; KARCH 18, 1993

301097

1. 0 OBJECTIVE

The following procedure is a general guideline for the evaluationof existing wells. The guidelines may be modified depending on theproject objectives. After completion of the evaluation, a judgmentmay be made as to the reliability and future usefulness of pastdata.

2.0 LIMITATIONS

These guidelines provide overall technical guidance only and may bemodified by specified requirement of project-specific plans formonitoring-well evaluation.

3.0 DEFINITIONS

None..

4.0 GUIDELINES

The following guidelines and procedures should be used whenconducting monitoring well evaluations:

• Record the identification and general location of themonitoring well, including approximate distance from the site

, and access to the well.

• Record the physical condition of the monitoring well includingthe following":

Existence and condition of the protective steel casing,cap, and lock, including casing diameter.Existence and condition of cement collar surrounding theprotective casing.Presence or absence of standing water or depressionsaround the casing.Presence of any electrical cable and its connections.

• . Before removing well cap, check for and disconnect any wires,cables, or electrical sources. Remove lock and open cap. Airmonitoring equipment should be used to detect the presence oforganic vapors in the monitoring well. The followinginformation should be recorded:

Cap function. .Physical characteristics of the inner casing or riser,including inner diameter and casing composition.Presence of grout between the inner and outer protectivecasing.Presence of an inner casing or riser cap including itsattachment to the casing and if vented.

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Presence of a submersible pump or dedicated bailer.Remove bailer and check the diameter, material, andcondition of the equipment.

Record height from top of protective casing with cap opento ground surface and to top of inner casing or riserpipe if it exists.

• Record initial static water level from top of casing using aninterface probe.

• Check depth of the well, if not obstructed, with a calibratedweighted line. Bounce the weight on the bottom to check forsediment. The weight will advance slowly if the well containssediments. Note any sediment or bentonite on the end of theweight when removed. Note any obstructions or discrepancywith field logs.

• Check alignment and plumbness of the well. This is criticalin deep wells where a vertical line-shaft turbine pump orsubmersible pump will be installed. A plummet smaller than

' the inner well diameter should be. lowered into the well notingany obstructions.

• Check the function of the well estimating.the time required, for future sampling. Estimate the hydraulic conductivity.

The extent and method of testing depend on project objectives,well depth and diameter, and estimated hydraulic conductivity.

Test methods would include rising head, falling head, and slugtests. Record recovery using a pressure transducer withrecorder or a water level indicator. Record pH, specificconductance, and temperature of groundwater removed ifinstrumentation is available. In clustered or nested wells,record water level in shallow wells while deeper wells aretested.

• After water level stability has been reached, check theintegrity of the bentonite seal by pouring several gallons ofwater around the outside of the casing. Monitor water levelsfor 10 minutes and note any increase. :

• Close well, secure lock, and decontaminate all equipment.

5.0 ATTACHMENTS

5.1 WELL-MONITORING DATA SHEET

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Project Name:.

Site Location:

Well Number:

Sampler: .

Well Depth:

Water Depth:

Casing Size:

Volume Bailed:

Recharge Wait:

Sample ID No.:

Depth Sampled:

Sample Method:

VacuumBailerPressureOther

Sample Temp:

WELL-MONITORING D7VTA SHEET

Preservation Method:.

Project Number:.

Assisted By:.

pH:SpecificConductance;

Observations & Comments:

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STANDARD OPERATING PROCEDURESi . • '

PROCEDURE F-4

GROUNDWATER LEVEL MEASUREMENTS

Pcvel] Environmental Services, Inc.REVISED: MARCH 18, 1993

301101

1.0 OBJECTIVE

The objective of these guidelines is to provide general referenceinformation and technical guidance on the measurement ofgroundwater levels.

2.0 LIMITATIONS

These guidelines give overall technical guidance only and should bemodified by specified requirements of project-specific plans formeasuring groundwater levels in wells.

Cascading water within a borehole can cause false readings withsome types of electrical sounding devices. Oil layers may alsocause problems in determining the true water level in well.

All water level measurements at a site should ideally be made onthe same day.

Groundwater contaminated by organic compounds may release toxicvapors into the airspace inside the wellpipe. The release of thisair when the well is initially opened is a health/safety hazardwhich must be considered.

3.0 DEFINITIONSf

Hydraulic head - Also piezometer head or where groundwaterpotential pressure is equal to atmosphericpressure.

Water table - A surface in an aquifer where groundwater isequal to atmospheric pressure.

Piezometric(potentiometric)surface - A surface which is defined by the levels to

which water will rise in cased wells whichpenetrate a confined or artesian aquifer.

4.0 GUIDELINES

4.1 GENERAL

In measuring groundwater levels, there should be a clearlyestablished reference point of known elevation, which is normallythe top of the inner well casing. The field notes recorded shouldclearly describe the reference used. To be useful, the referencepoint should be tied in with the USGS - Benchmark or a local datum.An arbitrary datum could be used for an isolated group of wells ifnecessary. All groundwater level measurements shall be made andrecorded to the nearest 0.05 foot. After the groundwater

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monitoring well has been installed or the cased borehole completedand left open for approximately one week, the initial depth to thewater should be measured and recorded. The date and time of thereading should also be .recorded. Information related toprecipitation should be included in the data. The depth of thegroundwater should be entered.

Appropriate remarks describing the history of the groundwatermonitoring well or open-cased borehole should be recorded alongwith the name of the individual who has read the groundwater

i monitoring well. .

Readings should be taken regularly, as required by the sitegeologist. Groundwater monitoring wells or open-cased boreholesthcit are subject to tidal fluctuations should be read inconjunction with a tidal chart; the frequency of such readingsshould be established by the site geologist.

4.2 SPECIFIC GROUNDWATER LEVEL MEASURING TECHNIQUES

There are several methods for determining water levels in boreholesand monitoring wells. Certain methods have particular advantagesand disadvantages depending upon the diameter of the borehole orcasing, groundwater quality, and hydraulic conductivity of theformation. A general guideline for obtaining static water levelsand changes in water levels during testing is presented along witha listing of various advantages and disadvantages of eachtechnique. An effective technique should be selected for theparticular site conditions by the on-site hydrogeologist.

Procedure

• Check operation of equipment above ground.

• Record well number, top of casing elevation and surfaceelevation if available. Water levels should be taken from topof the inner well casing or a reference point at the groundsurface for borehole measurements. The distance between thetop of the protective casing and inner casing should, berecorded.

• Record water level to the nearest 0.05 foot.

• Record the time and day of the measurement.

Chalked steel Line - Water level is measured by chalking a steelweighted tape and lowering it a known distance into the well orborehole. Water level is determined by subtracting the wettedchalked mark from the total length lowered into the hole.

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The tape should be withdrawn quickly from the well because waterhas a tendency to rise up the chalk due to capillary action. Apaste called "National Water Finder" may be used in place of chalk.The paste is spread on the tape the same way as the chalk, but thepart that gets wet turns red.

Popper or Bell Bounder - A bell or cup-shaped weight that is hollowon the bottom is attached to a measuring tape and lowered into thewell. A "plopping" or "popping" sound is made when the weightstrikes the surface of the water. • An accurate reading may bedetermined by lifting and lowering the weight in short strokes, andreading the tape when the weight barely strikes the water.

KIR-89 Interface Probe and Reel or Equivalent - When the InterfaceProbe is lowered down the well, the float switch will activate thelight and audible signal at the first fluid level. The float willdetect any fluid with a specific gravity of .75 or greater. As thestainless steel contacts touch water (a conductive fluid), thesteady light and the audible signals will begin to oscillate. Ifthe first fluid is not water, and therefore non-conductive, theemitted light and audible signals will be continuous.

There are a number of commercial electric sounders available, noneof which is entirely reliable. Especially when there is oil on thewater, high specific conductance, water cascading into the well, ora turbulent water surface in the well, measuring with an electricsounder may be difficult. Before lowering the probe into the well,the circuitry can be checked by dipping the probe in water andobserving the indicator. The probe should be lowered slowly intothe well. The electric tape is marked at the measuring point wherecontact with the water surface was indicated. The distance fromthe mark to the nearest tape band is measured and added to the bandreading to obtain the depth to water.

Float Recorder - A float or an electromechanically actuated water-seeking probe may be used to detect vertical changes of the watersurface in the hole. A recording chart drum is rotatedmechanically with a clock drive over a recording pen horizontallyacross the chart. To ensure continuous records, it should beinspected, maintained, and adjusted periodically.

Pressure Transducer - Pressure transducers measure the pressure ofwater on the transducer. The transducer is lowered into a well orborehole below the water. The transducer is wired into a recorderat the surface to record changes in water level with time. Therecorder digitizes the information and can transfer the informationto a computer for evaluation. The pressure transducer should beinitially calibrated with another water level measurement techniqueto ensure accuracy. This technique is very useful for hydraulicconductivity testing in highly permeable material where repeatedaccurate water level measurements are required in a very shortperiod of time.

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Borehole Geophysics - Water levels could be determined duringgeophysical logging of the borehole. Several logging techniqueswill indicate water level. One main technique is the spontaneouspotential log.

Bailer Line Method - Water levels during a bailing test of a wellcould be measured by marking and measuring the bailer line from thebottom of the bailer where water is encountered to the point evenwith the top of the casing. On the last bailing run of the test,the bailing line is marked again at the top of the casing where thebailer encounters water. This level would be recorded as the baildown level.

A Liquid-Level Data Sheet, shown in Section 5.1, should be filledout for each round of water level measurements at a site. Allpertinent data should be recorded as shown on the sheet. Theelevation of reference point is generally the elevation of the topof the inner well casing. The water level indicator reading is theactual reading on the measuring device. This measurement must besubtracted from the elevation above mean sea level of the referencepoint on the top of the inner well casing to obtain the elevationof the water level in the well. It is important, to note weatherconditions on the form, as changes in barometric pressure willaffect the water level within the well.

Liquids floating on the surface of the water depresses the waterlevel in the well. The depth to the floating liquid can bemeasured by the interface probe if it is a non-conducting liquidwith specific gravity greater than 0.75. The depth to productshould be recorded on the Liquid Level Data Sheet. If the liquidis a hydrocarbon (hereby referred to as product) the followingequation should be used to calculate the elevation of the water:

Adjusted water elevation = Casing elevation[ water depth - (product thicknesses x 0.85)]

Th(= depth to product, product thickness and adjusted waterelevation are to be recorded on the Liquid Level Data Sheet.

5.0 ATTACHMENTS

5.1 LIQUID-LEVEL DATA SHEET

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LIQUID LEVEL DATA SHEET

• CLIENT

LOCATION

RECORDED BY PROJECT NO.

WEATHER CONDITIONS

WELLNO.

CASINGELEV.

DEPTHTO

PRODUCT

WATERELEV.

PRODUCTTHICK-NESS

ADJUST.WATERLEVEL

REMARKS

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PROCEDURE F-5

SAMPLING

Powell Environmental Services, Inc.REVISED: MARCH 18, 1993

301107

1.0 OBJECTIVE •

The objective of these guidelines is to provide general referenceinformation on sampling.

2.0 LIMITATIONS

These guidelines are for information only and are not to. take precedenceover the requirements of project-specific plans for sampling.

Sampling -

Environmental Samples -

Ha2:ardous Samples -

Sampling Plan -

3.0 DEFINITIONS

The physical collection of a representativeportion of a population, universe, orenvironment.

Usually off-site samples with mid- or low-contaminant concentrations such as ambient,air, streams, grgundwater, leachates, ditches,soil, and sediments collected at a distancefrom direct sources of contaminants.

Samples of "raw" wastes, up to 100 percent byconcentration, such as those taken from drums,tanks, and other containers; from waste piles,spills, or on-site lagoons or ditches; andfrom contaminated soil in the immediatevicinity of waste storage or spill areas.

A detailed plan that covers the samplingobjectives and strategy.

4.0 GUIDELINES

These guidelines identify the sampling equipment, the sequence ofoperations, and the documents involved in physical sampling at or nearuncontrolled hazardous-substance sites. Reference is made to otherdescriptive or instructional documents as appropriate.

4.1 SAMPLING RESPONSIBILITIES

Project managers are responsible for ensuring that the project specificsampling procedures are followed, maintaining chain-of-custody, anddetermining that all sampling documents have been completed properly andare accounted for. Samplers are responsible for collecting samples,initiating chain-of-custody forms, and the necessary sample documents asrequired.

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4.2 SAMPLING EQUIPMENT

Typical equipment used for air, solids or liquid samples are summarizedin Section 5.1. In SOP F-6,. container and preservation requirements forsamples are presented.

4.3 SAMPLING METHODS

4.3.1 Environmental Samples

If initial site atmospheric hazard surveys have been conducted andlevels of personnel protection have been established, surveys fororganic/inorganic vapors, oxygen content and combustible gases must berepeated periodically, as specified in the sampling plan.

Surface Water

Collecting a representative sample from surface water may be difficult.Samples should be collected near the shore unless boats are feasible andpermitted. A small container or dipper attached to a pole is used toobtain the samples. Samples from various locations and depth should becomposited; otherwise, separate samples will have to be collected.Approximate sampling points should be identified on a sketch of thewater body. The following procedures are used:

• Record available information for the pond, stream, or other waterbody, such as its size, location, depth, and probable contents, inthe field logbook, on the chain-of-custody form, and on the samplelog sheet.

• Take samples near the shore of the water body and transfer them toappropriate bottles.

• Secure the lid of each sample bottle and attach a label containingsample identification, number, and date. Securely tape the lid tothe bottle; then date and initial the tape.

• Carefully pack samples. Place a custody-seal on the shippingpackage.

Groundwater

Monitoring Wells

A typical well sampling data sheet is presented in SOP F-3. Not all theinformation shown can be obtained at all wells. Critical, requiredinformation includes:

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Well locationsWell radius or diameter •Depth to water levelTotal well depthAmount of water in well

This information should be entered in the field logbook.

Wells must be bailed or pumped three to five well volumes beforesampling. Samples are taken after the well recharges to initial waterdepth. Wells that do not recharge within 24 hours will be sampled afterthe well recharges to a sufficient depth to provide an adequate volumeof sample for analysis. Care must be taken not to disturb sediment atthe bottom of the well when taking samples. The following proceduresare used: . .

• Measure the water level in the well using the KIR-89 or otherdevice and record the elevation at the top of the water surface.

• Determine the submerged casing volume, (standing water volume) inthe well from the following equation:

3.14 r2h

Where:

V = volumer = radiush = standing water height as determined from drilling

logs and actual measurement.(1 cf = 7.48 gallons)

For example, a 30 ft. drilled well with 5 ft. of screen has a 2 in.casing with a nominal inside diameter of 1.90 in. The standingwater level has been determined to be 10 ft. Therefore, thesubmerged casing volume (in cubic feet and gallons).

= [3.14(0.95)2110

. = 0.196 ft.3 or 1.47 gallons

With a manual bailer, remove three to five casing volumes of waterfrom the well. To avoid disturbing the sediment, do not insert thebailer to the bottom of the screen. (Note: If the casing sizeallows, the well may be pumped with a submersible electric pump orother device until the appropriate volume has been removed. Do notoverpump.)

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• When the well has recharged sufficiently, remove enough water tofill all sample bottles in accordance with SOP F-6. Addpreservatives where required. In the event that recovery time ofthe well is very slow (e.g., 24 hours) , attempts to collect samplesimmediately after bailing or pumping can be delayed until thefollowing day. If the well has been bailed early in the morning,sufficient water may be standing in the well by the day's end topermit sample collection. If the well is incapable of producing asufficient volume of sample at any time, take the largest quantityavailable and record in the field logbook.

• Label, tag, and number the sample bottle. Tape the lid on securelyand mark the tape with the date and the sampler's initials.

• Replace the well cap. Make sure the well is readily identifiableas the source of the samples.

• Pack the samples for shipping. Attach a custody seal to theshipping package as described above. Make sure that trafficreports and chain-of-custody forms are properly filled out andenclosed or attached. '

Hydrants or Pumped Wells .

Sampling from hydrants or pumped wells such as domestic wells requiresa modified procedure. The well must be flushed by running the water for15 minutes through the tap nearest the well. Take the sample from thecontinuously running tap after the 15 minute period.

Follow the steps above for entering information, packing, preserving,labeling, and marking.

The sampler to be used is dependent on the parameters, to be analyzed,soil type, depth of sample desired, and homogeneity of soil.

For loosely packed earth, appropriately cleaned stainless steel orteflon coated scoops, trowels, and waste pile samplers can be used tocollect representative samples. For densely packed soils or deep soilsamples, a soil auger or other techniques may be used.

• Use a soil auger for deep samples (6 to 12 in.) or a scoop ortrowel for surface samples. Remove debris, rocks, twigs, andvegetation before collecting 200 to 250g. Mark the location witha numbered stake if possible and locate sample points on a sketchof the site.

• Transfer 100 to 200g of the sample to a 250ml container. Attach alabel, identification number, and tag. Record all requiredinformation in the field logbook and on a sample log sheet asdescribed in Section 4.4.3, below.

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• Store the sampling device in a plastic bag until decontamination ordisposal.

• Tape the lid on the sample bottle securely and mark the tape withthe date and the sampler's initials. .

• Carefully pack the samples. Attach a custody seal to the shippingpackage. Make certain that chain-of-custody forms are properlyfilled out and enclosed or attached.

Sludges and Sediments

Sludge samples and sediments can usually be collected by bucket orlonghandled dipper. If the sludges or sediments are relatively dense,waste pile samplers or tiers may be used.

• Collect at least three small, equal sized samples for severalpoints along the sludge or sediment deposition area. If possible,mark the location with a numbered stake and locate sample points ona sketch of the site. Deposit sample portions in a clean, 1/2 gal.jar and composite.

• Sediments from large streams, lakes, and the like may be taken from« a boat.

• Transfer 100 to 200g of the composite sludges from the 1/2 gal. jarto a 250ml sample bottle. Attach identification label number andtag. Record all necessary information in the field logbook and onthe sample log sheet.

• Store the sampling device and jar in a plastic bag untildecontamination or disposal.

• Tape the lid on the sample bottle securely and mark the tape withthe date and the sample collector's initials. .

• . Pack the samples for shipping. Attach a custody seal to theshipping package. Make certain that chain-of-custody forms areproperly filled out and enclosed or attached.

4.3.2 Hazardous Samples

Air samples are rarely taken to determine a medium of high hazard level.In fact, site activities are usually suspended .if high ambient hazardoussubstance concentrations are detected by routine monitoring devices orif low oxygen levels are discovered.

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Surface Water

When collecting samples from medium- to high-hazard surface waters, suchas on-site lagoons or ponds, the steps outlined above for environmentalsampling should be followed. Added safety precautions, such aslifelines, are required.

Prisms —

Drum samples should be obtained through a free opening or through thebung hole whenever possible, using the procedure described below.Because drums may fail structurally, losing all or part of theircontents, caution must always be exercised when it is necessary to movedrums to gain access to them. The best approach is to sample, analyze,,and remove the most accessible drums before handling damaged, tipped, orburied drums. Remote-controlled bung wrenches are the best tools foropening drums.

Drums must be opened slowly and carefully. If the drum is bulgingbecause of inside pressure or vacuum, special precautions must bedeveloped.

Place disposable sampling equipment in the drum that was sampled beforeresealing it. Separately labeled drums may be used as receptacles forcontaminated sampling equipment as long as compatibility of the wastesis ensured.

The following procedures are used to obtain samples from drums:

• Record any markings, special drum conditions, and type of openingin the field logbook, on the sample log sheet, and later, on thechain-of-custody form. Note the general location on a sketch ofthe site.

• Stencil an identifying number on the drums and record in fieldlogbook. Consult the sampling plan for identifications.

• Make certain that the drum is on a firm base, preferably in a fullyupright position.

• Using a non-sparking bung wrench or a remote-controlled bungremover, carefully remove the bung and set it aside. Drums withtop lids and ring seals may be opened by carefully removing theseal and prying off the lid with a non-sparking tool. Set the lidand ring aside.

• Carefully insert the sampling tube (either metal, glass, orcompatible plastic) into the drum contents. Secure the upper endof the tube with the thumb or palm and withdraw the tube. (Note:If the sample is not free-flowing and is contained in a drum witha lid, the sample may be removed with a clean scoop or a smallshovel.)

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• Deliver 100 to 250ml of sample (the sampling plan will specify theamount) to a clean, wide-mouth, 500ml (1 pt.) glass sample jar. Ifthe sample is not free-flowing and is taken through a bung opening,repeated sampling may be necessary. Replace the bung or covercarefully.

• Place the used sampling tube, along with paper towels or waste ragsused to wipe up any spills, into an empty metal barrel forsubsequent disposal. If glass tubing has been used, it may bebroken and left inside the drum being sampled.

• Replace the cap on the sample jar; label, date, and number the jar.Record all information on the chain-of-custody form, sample logsheet, sample tag, and field logbook. The sample jar numbers anddates must match those recorded on all forms.

• Secure the sample container lid with heavy-duty tape. Date andsign the tape.

• Carefully pack samples. The finished package will be padlocked orcustody sealed for shipment to the laboratory. The preferredprocedure includes the use of a custody seal wrapped acrossfilament tape that is wrapped around the package at least twice.The custody seal (paper, plastic, or metal) is then folded over andstuck to itself so that the only access to the samples is by

, cutting the filament tape or breaking the seal to unwrap the tape.The seal is signed before the package is shipped.

The sampling of tanks is similar to the sampling of drums. Techniquesof sampling are the same, except sampling equipment may need to belonger to give a representative sample of deep tanks.

• Record the tank's condition, markings, opening or valve types, andapproximate size in gallons in the field logbook, on the chain-of-custody form, and on the sample log sheet. Note the tank locationon the site sketch.

• Attach an identification number to the tank using a stencil orweatherproof tag. Number succeeding tanks consecutively. .Recordthe numbers in the field logbook.

• Determine whether the tank contents are stratified by inserting along plastic or glass tube sampler, withdrawing it, and examiningthe tube contents.

• Samples of stratified contents may be taken with a bomb or weightedbottle sampler at each level. A segmented tube sampler may also beused if available. Deliver sampled contents, if stratified, toseparate 500ml glass sample jars.

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• Secure the jar lid and label, date, and number the jar as above.Securely tape the lid to the jar; date and initial the tape.

• Carefully pack samples. Custody-seal the shipping package asdescribed previously. . . .

• Decontaminate any non-disposable sampling equipment and dispose of—-- cleaning solvents and materials in a metal drum. Wipe up any

spills and place rags or paper towels in the metal drum for laterdisposal.

Solid Waste Piles

To obtain small discrete samples of homogeneous piles, use scoops ortrowels. Layered (non-homogeneous) piles require the use of tubesamplers or triers to obtain cross-sectional samples.

• Collect small, equal portions of the waste from several points ator near the surface of the pile. Use numbered stakes, if possible,to mark the sampling locations and indicate sampling points on the

• site sketch.

• Collect a waste sample totaling 100 to 200g and place it in a 250mlglass container. Attach a label, identification number, and tag.Record all the required information in the field logbook and on the

, sample log sheet.

• Store the sampling tool in a plastic bag until decontamination ordisposal.

• Tape the lid on the sample bottle securely and mark the tape withthe date and the sampler's initials.

• Pack samples for shipping. Attach a custody seal to the shippingpackage. Make sure that the traffic report and the chain-of-custody form are properly filled out and enclosed or attached.

For layered, non-homogeneous piles, grain samplers, sampling triers, orwaste pile samplers must be used to acquire a cross-section of the pile.The basic steps are listed below.

• Insert a sampler into the pile at a 0- to 45-degree angle from thehorizontal to minimize spillage.

• Rotate the sampler once or twice to cut a core of waste material.Rotate the grain sample inner tube to the open position and thenshake the sampler a few times to allow the material to enter theopen slits.

• Move the sampling device into position with slots upward (grainsampler closed) and slowly withdraw it from the pile.

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• Transfer 100 to 200g of sample into a 250ml container with the aidof a spatula or brush. Attach a label identification number andtag. Record all necessary information in the field logbook and onthe sample log sheet.

• Store the sampling device in a plastic bag until decontamination ordisposal.

• Tape the lid on the sample bottle securely and mark the tape withthe date and the sample collector's initials.

• Pack sample for shipping. Attach a custody seal to the shippingpackage. Make certain that the traffic report and chain-of-custodyform are properly filled out and enclosed or attached. •

Soils .

Guidelines for collecting hazardous soil samples are the same as thosefor collecting environmental soil samples.

Sludges and Sediments

Guidelines for collecting hazardous sludge and sediment samples are thesame as those for collecting environmental sludge and sediment samples.

4.4 SAMPLING DOCUMENTS AND RECORDS

This section identifies the various documents, forms, labels, and tagsthat sampling personnel will be required to use in the field.

Field logbook(s)Field data records " " - •• -Sample log sheetTable of contents for sample log sheet notebookOtherSample identification labels and/or tagsChain-of-custody formCustody seal . ;

There are additional forms of documentation that may need to bemaintained that are not standard in format. These forms are discussedseparately.

4.4.1 Field Logbook

A field logbook is a bound notebook with numbered pages in which allpertinent information about a field investigation (data, observations,phone calls, etc.) is entered. It is advised that one field logbook bemaintained per site. This logbook is issued by the Project Manager forthe life of the project. Logbooks may be issued to other fieldpersonnel (including those collecting samples). The Project Manager (orhis designee) numbers all logbooks and records their transfer to otherindividuals as necessary. All project logbooks are to be turned over tothe Project Manager and to a central file at the completion of theparticular field activity.

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4.4.2 Field Data Records

Field data records may include sample log sheets, tables of contents forsample log sheet notebooks, and any other data records that the ProjectManager or task leader may designate for use in field data collection.The exact forms used will depend on the scope of the project and thesituations presented.

4.4.3 Sample Log Sheet

A sample log sheet is used to record specified types of data whilesampling. The data recorded on these sheets is useful in describing thewaste source and the sample (if obtained) as well as pointing out anyproblems encountered during sampling.

4.4.4 Table of Contents for Sample Log Sheet Notebook

Entries are made in the table of contents form as the completed samplelog sheets are placed in a three-ring binder. This form remains in thenotebook at all times and will be provided by a CLP laboratory.

4.4.5 Labeling of Samples

Sample Label

A sample label must be attached to each bottle that contains a sample.The label must be attached to the bottle just before putting the sampleinto the bottle. In addition, the label should be covered with clearplastic tape to ensure that it does not peel off or become damaged. Thesample number is the number assigned to the waste source underinspection and any samples taken from iti A sample label will beprovided by a CLP laboratory.

4.4.6 Chain-of-Custody Form

The chain-of-cus.tody form accompanies and documents a sample or group ofsamples as it is transferred from person to person. Additionalprocedures regarding chain-of-custody are given in SOP F-10. The chain-of-custody will be provided by a CLP laboratory.

4.4.7 Custody Seal

A custody seal (Section 5.3) is a small paper label with black letteringon an adhesive backing. The custody seal is part of the chain-of-custody process and is used to prevent tampering with samples after theyhave been collected in the field. The custody seals will be provided bya CLP laboratory.

REV. 1993 Pa<3£ 10

301117

4.4.8 Non-standard Documentation

Photographs

When movies, slides, or photographs are taken of a site or anymonitoring location, they are numbered to correspond to field logbookentries. The name of the photographer, date, time, site location, sitedescription, and weather conditions are entered in the field logbook asthe photographs are taken. A series entry may be used for rapid-sequence photographs. The photographer is not required to record theaperture settings and shutter speeds for photographs taken within thenormal automatic exposure range. However, special lenses, films,filters, and other image-enhancement techniques must be noted in thefield.logbook. If possible, such techniques should be avoided, since,they can adversely affect the admissibility of photographs as evidence.Chain-of-custody procedures depend upon the subject matter, type offilm, and the processing it requires. Film used for aerial photography,confidential information, or criminal investigations require chain-of-custody procedures. Adequate logbook notations and receipts may be usedto account for routine film processing. Once developed, the slides orphotographic prints shall be serially numbered and labeled according tothe field logbook descriptions.

REV.1993 Page 11

301118

PROCEDURE F-6

ANALYTICAL METHODS/SAMPLE CONTAINERS

Powell Environmental Services/ Inc.REVISED: MARCH ie, 1993

301119

1.0 OBJECTIVE

The following procedure is a general guideline for the analyticalmethods incurring sample container and preservation requirements. Theguidelines may be modified depending on project objectives.

2.0 LIMITATIONS

These guidelines are provided primarily for New Jersey projects and areprovided for technical guidance only. They may be modified based ontechnical requirements and/or on a project specific basis.

3.0 DEFINITIONS .

A.0 GUIDELINES

These technical guidelines consist of a. copy of Appendix 2-1 of theField Sampling Procedures Manual (May, 1992).

REV.1993 Page 1

301120

FIELD SAMPLINGPROCEDURES MANUAL

State of New JerseyJIM FLORIDGOVERNOR

New Jersey Department of Environmental Protectionand Energy

SCOTT WEINER

COMMISSIONER

May 1.992

301121

APPENDIX 2-1

Analytical Methodology Reference Charts

The following Appendix was designed to present field sampling personnelwith information "at a glance" on sampling containers and fieldpreservation requirements. The following charts are organized by

( analytical methodolQ,gy, including the USEPA-Contract LaboratoryProgram, USEPA SW-846, 40 CFR part'136 (State approved NPDES) and 40CFR Parts 141 and 143 (National Primary and Secondary Drinking WaterRegulations). The analytical methodologies in 40 CFR Part 136.3

I 1 include the 600 series methods and 40 CFR Part 141 include the 500series methods. These test procedures are incorporated as they existon the day of approval and a notice of any change in these testprocedures will be published in the Federal Register.

In addition to providing field personnel with necessary samplinginformation, laboratory personnel will find these charts helpful inchoosing a particular analytical methodology for a specific matrix.QA/QC Personnel and those individuals involved with data validationwill find the section on holding times particularly useful in ensuringthe quality of analytical data.

Finally there are descriptions for sample container preparationrequirements which, when performed accurately, help ensure thatanalytical data generated from sample results is representative and isnot subject to contamination from sample containers.

mmediately 'following the charts is a list of footnotes with anexplanation of abbreviations contained therein. Following thefootnotes are a comparison of Contract Laboratory Program TargetCompound List (TCL), Target Analyte List (TAL), Priority Pollutant List(PPL - which includes the NPDES 40 CFR 122 Appendix D Table 2 and Table3) and SW-846 analytes which identify the particular compounds whichcan be analyzed using the various analytical methodologies.

Target Compound List/Target Analyte ListUSEPA SW-846 MethodologiesSafe Drinking Water Methodologies (including 500 Series)Clean Water Act NPDES (NJPDES) for Wastewater (including 600 series)Sludge using Sludge MethodologiesBiological using NJDEPE MethodologiesFootnotes.Analyte Compound List

The following EPA CLP methodologies have been used: for TCL organics - doc. # OLM01.8;for low detection of volatiles - doc. #. SAMLC01092; for TAL organics - doc..# ILM02.1;and for low detection inorganics - doc. # .SAMLCI1091.

301122

Analysis of TARGET CGKFC'JJTC LIST/TARGET ANALYSE LISTUsing USEPA-Contract Lab Program Methodologies for'Aqueous and Nonaqueous Samples

ParameterVolatile OrganicB

SampleContainer (1)Aqueous-G, blackphenolic plasticscrew cap,teflon-linedseptumNonaqueous-G,polypropylenecap, whiteteflon liner

ContainerVolumeAqueous -2 40 ml

' Nonaqueous120 ml

Preservation (2)Cool, 4 deg C,dark,0.08% Na2S2C>3if residual C12

MaximumHoldino Time*10 days

10 days

AnalyticalMethbdoloavUSEPA-CLPStatement ofWork forOrganicAnalysis, MultiMedia, MultiConcentration(Docj/OLKOl.8)

SampleContainerCleanina(3)

Base Neutral/AcidExtractable(Semivolatile)Organics

Aqueous-4-1 literglass amber

Nonaqueous-1-8 oz.glass

1000 ml Cool, 4 deg C,dark-

Pesticide/ PCB's As Above As Above As Above

ExtractionAqueouscontinuousliquid-liquidextraction mustbe startedwithin 5 daysNon-aqueous -10 daysAnalysis -40 days fromVTSR*OIMJ1.8

As Above

As Above (3)

u>oHMtoU)

* Validated time of sample receipt (at the laboratory)• ' . 2 5 ' . ' • ' - . '

26Analysis of TARGET COMPOUND LIST/TARGET ANALYTE LIST

"sing USEPA-Contract .Lab Program Methodologies for Aqueous and Nonagueous Samples

ParameterHigh Level VolatileOrganic WasteSamples

SampleContainer (I)Aqueous-G, blackphenolic plasticscrew cap,teflon-linedseptumNonagueous-Gpolypropylenecap, whiteteflon liner

ContainerVolume Preservation (21Aqueous - Cool, 4 deg C,40 ml dark,

Nonaqueous120 ml

MaximumHolding Time*Analysiscompletedwithin 40days ofVTSRAs Above .

AnalyticalMethodoloavUSEPA-iCLPStatement ofWork forOrganicAnalyeiB-MultiMedia, HighConcentration9/88

High Concentration As AboveExtractable OrganicWaste Samples

High Concentration As AboveAroclors andToxaphene samples

1000 ml Cool, 4 deg C,dark

As Above As Above

As Above

Hto * Validated time of sample receipt (at the laboratory)

Analysis of TARGET COMPOUND ilsT/'IAEGET AKALYTS LISTUsing USEPA-Cpntract Lab Program Methodologies for Aqueous and Nonaqueous Samples

Parameter,SampleContainer (1)

ContainerVolume Preservation (2)

MaximumHolding Time*

AnalyticalMethodology

SampleContainerCleaning

PolychloriniatedDibenzo-p-Dioxins(PCDDs) andDibenzofurans (PCDFs)

Low Level MetalsWater except Hgand Cuu(CN)2

As Above

Aqueous -Pbottle, P cap,liner

2000 ml1 pint

Aqueous -1000 ml

polyethlene

As Above None

Aqueous - HNO3to PH<2

178 days

USEPA-CLP (3)Statement ofWork forAnalysis ofPolychlorinatedDibenzo-p-Dioxins (PCDD)PolyohlorinatedDibenzofurans (PCDF)Multi-Modi, Multi-Concentration(DFLM01.1) 9/91

USEPA-CLP

SAMLCI1091

Hg As Above As Above As Above 26 daya As Above (3)

U)oHHN)

Validated time of sample receipt (at the laboratory)27

Parameter

28Analyais of TARGET COMPOUND LIST/TARGET ANALYTE LIST

Using USEPA-Contract Lab Program Methodologies for Aqueous and Nonaqueous Samples

SampleContainer (1)

ContainerVolume Preservation

Cyanide, totalamenable tochlorination

Total Nitrogen

Fluoride

Metals except Hg

As Above As Above Aqueous - 0.6gascorbic acid ifresidual C12>NaOH to pH>12,cool, 4 deg Cuntil analyzed,CaCO3 in presenceof sulfide

phenolic cap,polyethyleneliner

As Above As Above As Above

12 days

As Above

Aqueous -1 liter Pbottle, P cap,P linerNonaqueous -Flint Glassbottle, black

As Above

Aqueous -1000 ml

Nonaqueous4,8,16, or32 oz

H2SO4 to pH<2

4 deg C untilanalysis

Aqueous - HNC>3to pH<2

Nonaqueous - 4deg C untilanalysis

12 days

26 days

178 days

As Above

26 days

As Above

USEPA-tcLPStatement ofWork forInorganicAnalysis HultiMedia, MultiConcentration(DOC./ILM02.1*)

As Above

* Validated time of sample receipt (at the laboratory)

Analysis of TARGET COHPOUND LIST/TARGET ANALYTE LISTUsing USEPA-Contract Lab Program Methodologies for Aqueous and Nonaqueous Samples

Parameter

Cyanide

High Level Metalsexcept Hg

Low Level VolatileOrganics

SampleContainer (1}

As Above

Aqueous - Pbottle, P cap,P linerNonaqueous -Flint Glassbottle, blackphenolic cap,polyethyleneliner

As Above

Aqueous-G, blackphenolic

ContainerVolume

As Above

Aqueous -1000 ml

Nonaqueous4,8,16, or32 oz

As Above

Aqueous -3- 40 ml

MaximumPreservation (2^ Holdina Time*

Aqueous - 0.6g • . 12 daysascorbic acid ifresidual Cl2/NaOH to pH>12,cool, 4 deg Cuntil analyzedCaCO^ in presenceof sulfideNonaqueous Cool, 4deg C untilanalysedAqueous - HNO3 180 daysto pH<2

Nonaqueous - 4 As Abovedeg C untilanalysis

As Above . 26 days

Cool, 4 deg C, 10 daysdark,

AnalyticalMethodoloqv

As Above

USEPA-CLPStatement ofWork forHigh

Concent rar.ionInorganicAnalysis(Doc.#HCIN)

As Above

USEPA-CLP

SAMLC01092

plastic screwcap teflon-lined septum

1:1 HC1 to pH<2

* Validated time of sample receipt (at the laboratory)29

Parameter

30Analysis of TARGET COMPOUND LIST/TARGET ANALYTE LIST

Using USEPA-Contraet Lab Program Methodologies for Aqueous and Nonaqueoua Samples

Sample Container Maximum AnalyticalContainer (1) Volume Preservation 12) Holding Time* Hethodolocrv

Low Level Semi-volatile Organics

Amber G, TeflonLined Cap

Extraction -Continuousextractionmust bestartedwithin 5daysAnalysis -40 days fromstart ofextraction

USEPA-CLP (3)Statement ofWork for LowConcentrationHater for OrganicAnalysis(Doc./OLCOl.O) 9/90

Low Level Pesticides/PCBs Organics

Amber G, TeflonLined Cap

As Above A* Above (3)

* Validated time of sample receipt (at the laboratory)

Parameter

AnalyeiB of ORGAKIC and INORGANIC Compounds Using USEPA 8H-846 METHODOLOGIESfor Aqueous, Non-aqueous, and Waste Samples

SampleContainer

ContainerVolume Preservation (21

AnalyticalMethodoloov

Volatile G, wide mouth, 8 ozOrganics - teflon linerConcentratedWaste Samples

Volatile G vial, teflon 40 mlOrganics - lined septum capLiquid Samplesno residual Cl->

None 14 days

4 drops cone. As AboveHCl, cool, 4 deg C

SW-846, 3rd (5)edition, Vol1-B;GC-8010,8015,8020;GC/MS-8240

As Above (5)

VolatileOrganics -Liquid Samplesresidual

As Above

VolatileOrganics -Liquid Samplesfor Acrolein andAcrylonitrile

As Above

Collect sample in As Above4 oz Soil VOAcontainerprepreserved w/10%

Gently mix sampleand transfer to 40ml VOA vialprepreserved w/4drops cone. HCl,cool, 4 deg C

Adjust to pH 4-5,cool, 4 deg C

As Above

SW-846, 3rdedition, Vol1-B;GC-8030;GC/MS-8240

to'Holding time begins at time of sample collection.

32Analysis of ORGANIC and INORGANIC Compounds Using USEPA SW-846 METHODOLOGIES

for Aqueous, Ncn-aquscus, and Hants Samples

SampleParameter Container (1)

SampleContainer Maximum Analytical ContainerVolu me Preservation (21 Holding Time* Methodology Cleaning

VolatileOrganics -

G, wide mouth, 4 ozteflon liner

Cool 4 deg C As Above

Soil /SedimentsSludge

Sulfates

TotalOrganicCarbon

Phenols

P, G 100 ml(12)

G-Preferred P-If 100 mldetermined that (12)there is nocontributingorganiccontamination

G only 1 liter(12)

Cool, 4 deg C

Cool, 4 deg C,dark, HCl orH2SO4 to pH<2 •if analysis can'tbe done within 2hrs

Cool, 4 deg C,H2SO4 to pH<2

28 days

2 Hrs -unpre served' 28 days -preserved

28 days

SW-846, 3rd (5)edition, Vol {1-B; jGC-8010, \8015,8020;GC/MS-8240, 8260

SW-846, 3rd (6)edition, Vol1-C;9035,9036,9038

SW-846, 3rd (6)edition, Vol1-C; 9060

SW-846, 3rd (6)edition, Vol1-C;9065,9066,9067

UJoHHOJO

Totalrecoverableoil andgrease

G only, widemouth

1 liter Cool, 4 deg c

5 ml HCl, Cool 4deg C

Unpreserved-Few hrs

Preserved -28 days

SW-846, 3rdedition, Vol1-C; 9070

*Holding time begins at time of sample collection.

Analysis of ORGANIC and INORGANIC Compounds Using WSEPA SW-846 METHODOLOGIESfor Aqueous, Non-aqueous, and Waste Samples

SampleParameter Container (1)Oil and Ggrease forsludge

Total GPetroleumHydrocarbons

Total P, GColiform

Nitrate P, G

Chloride P, G

ContainerVolume1 liter(12)

1 liter .

1 liter(12)

Preservation {2\Cool, 4 deg CpH<2 HC1

Cool, 4 deg C

Cool, 4 deg C,Na2S203 ifresidual C12, EDTAif high in heavymetals

Cool, 4 deg C,

H2S04 to pH<2,(2 ml/L)

Cool, 4 deg C

MaximumHoldino Time*28 days

Aqueous7 daysNon-Aqueous28 daysGasolinein soil7 days

24 hrs -Unpreserved

28 days -preserved

28 days

AnalyticalMethodoloavSW-846, 3rdedition,Vol 1-C/9071Method 418.1(modifiedfor soil)

SW-846 3rdedition, Vol1-C; 9131,9132

SW 846, 3rdedition, Vol1-C; 9200

SH-846, 3rdedition, Vol

No plastictubing

1-C; 9250,9251, 9252

•Holding time begins at time of sample collection.33

34Analysis of ORGANIC and INORGANIC Compounds Using USEPA SW-846 METHODOLOGIES

for Aqueous. Non-aqueous, and Haste Samples

Sample ContainerParameter Container (1) Volume Preservation (2)Radium 228 P 1 liter Cool, 4 deg C

(12) preserve atlab withHN03 topH<2, holdfor minimumof 16 hrsbeforeanalysis, 6moB.

MaximumHoldina Time*Transport tolab within 5days ,

AnalyticalMethodolocrvSW-846, 3rdedition, Vol1-C; 9320

SampleContainerCleaning(6)

ExtractableOrganics -ConcentratedWaste Samples

G, wide mouthw/teflon liner

Extractable G, amber,Organice - w/teflon linerLiquid Samplesno residual

1 gallonor 2 1/2gallon

HNO3 to pH<2,suggested atsampling

Cool, 4 deg C

6 mo s

14 days

Extractiondays

SW-846, 3rd (5)edition, Vol1-B;

• GC-8080;GC/MS-8270

As Above (5)

Analysis -40 days fromextraction

COoHHWto

"Holding tine begins at time of sample collection.

Analysis of ORGANIC and INORGANIC Compounds Using USEPA SW-846 METHODOLOGIESfor Aqueous, Non-aqueous, and Haste Samples

ParameterSampleContainer

ContainerVolume Preservation (21

Maximum AnalyticalHolding Time* Methodology

Extractable G, amber,Organica- w/Teflon linerLiquid Samplesresidual Cl

Extractable G, wide mouth,Organics - w/Teflon linerSoilB/SediroentsSludges

Metalsexcept CrVI and Hg

1 gallonor 2 1/2gallon

600 ml

3 ml 10%Na2S2O3 pergallon, cool 4deg C

Cool 4 deg C

HN03 to pH<2

Extraction 7days

Analysis -40 days fromextraction14 days

As Above

6 mo s

As Above

SW-846, 3rdedition, Vol1-A; 7000aeries

Hg(Total)

P, 400 ml HNO3 to pH<2 28 days SW-846, 3rdedition, Vol1-A; 7470,7471

Cr VI P, G 400 ml Cool, 4 deg C 24 hrs SW-846, 3rdedition, Vol1-A; 7195,7196, 7197,7198

COoHI-JCOCO

'Holding time begins at time of sample collection.• ' . ' . • • - . ' • 3 5 ' . ' '•'.-

36Analysis of ORGANIC and INORQANIC Compounds^Using USEPA SH-B46 METHODOLOGIES

for Aqueous, "on-aqueous, and Waste Samples

Sample

Parameter

Cyanide,total andamenable tochlorination

TotalOrganicHalides(TOX)

SampleContainer (11

P i-t/ G

G, vials, teflonsepta. Amber G,teflon linedcap/foil lined

ContainerVolume

1 liter orlarger

250 ml

Preservation (2)

Cool, 4 deg,0.6g ascorbic acidNAOH to pH>12

Cool, 4 deg C,dark, I SO topH<2 , noheadspace

MaximumHoldina Time*

14 days

7 days

AnalyticalMethodoloav

SW-846, 3rdedition, Vol1-C,7195,7196,7197,7198

SW-846, 3rdedition, Vol1-C; 9020,9022

ContainerCleaninq

Sulfides P,

Polychlor-inatedDibenzo-p-Dioxin(PCDDs) andPolychlor-inatedDibenzofurans(PCDFs)

G, with widemouth w/teflonliner

1 liter Cool, 4 deg C,(12) add 4 drops zinc

acetate per 100 mlsample, NaOH topH>9

1 pint Cool, 4 deg C,dark

7 days

Extractedwithin 30days andanalyzedwithin 45days ofsampling

SW-846, 3rd (6)edition, Vol1-C; 9030

SW-846, 3rd (3)edition, Vol1-B; GC/MS- .8280

OJoHHU>

•Holding time begins at time of sample collection.

Analysis of Contaminants Using SAFE DRINKING WATER Methodologies (including 500 series) for Aqueous Samples

ContaminantsSampleContainer(11

ContainerVolume Preservation f 2

MICROBIOLOGY CONTAMINANTS

Total coliforms P,G 125 ml 0.008%if residual0.3 ml/125 ml15% EDTA if> 0.01 mg/1heavy metals,Cool, 4 deg C

30 hours

Plate Count

INORGANIC CONTAMINANTS AND NONTOIIC METALS

Alkalinity P,G 100 ml

Asbestos (30) As Above

Calcium As Above 100 ml

Cool, 4 deg C

As Above

Cone. HNOjto pH<2 (26)

14 days

6 months

* Holding time begins at time of sample collection37

40 CFP. 141

Fecal coliforms

EBcherichia coli

Heterotrophic

As Above

As Above (20)

As Above

As Above (9)

Chloride

Conductivity

Cyanide

Fluoride

Foaming agents

As Above

100 ml

500 ml

300 ml.

250 ml

Cool, 4 deg C

As Above

Cool, 4 deg C

Cool ,4 deg C

28 days

24 hours

As Above

14 days

1 month

48 hours

40CFR141,143

40 CFR 143

40. CFH 141

40CFR141,143

As Above

40 CFR 143

As Above

Analysis of Contaminants Using SAFE DRINKING HATER Methodologies (including 500 series) for Aqueous Samples

Contaminants

Nitratechlorinatednon-chlorinated

Nitrite

Orthophosphate(unf iltered)

Residue, Non-filterable (TDS)

Residue-totalfilterable (TSS)

Silica

Sulfate

Turbidity

ANALYZE IMMEDIATELY

Chlorine, residual

Chlorine Dioxide

Ozone, residual

Temperature

SampleContainer (11

P,GAs Above

As Above

G only

As Above

P only

As Above

ContainerVolume

250 mlAs Above

200 ml

100 ml

As Above

100 ml

Preservation (21

1 Cool, 4 deg CCone. H2SO4to pH<2

Cool, 4 deg C

As Above

Cool, 4 deg C

As Above

28 days14 days

48 hours

24 hours

7 days

As Above

28 days

48 hours

40 CFR 141As Above

As Above

40 CFR 143

40 CFR 141

40 CFR 143

As Above

(20)As Above

As Above

INORGANIC CONTAMINANTS

As Above

G, only

As Above

200 ml

1000 ml

As Above

15 minutes

As Above

40CFR141,143

40 CPRJ141

As Above

* Holding tine begins at time of sample collection

OJoHMOJ

Contaminants

INORGANIC CONTAMINANTS,

Aluminum, Total

Antimony, Total

Arsenic, Total

Barium, Total

Beryllium, Total

Cadmium, Total

Chromium, Total

Copper, Total

Iron, Total

Lead, Total

Manganese, Total

Mercury, Total

Nickel, Total

Selenium, Total

Silver, Total

Sodium, Total

Thallium, Total

Zinc, Total

SampleContainerfl)

TOIIC HETALS(26)

As Above

AB Above

As Above

AB Above

As Above

AB Above

As Above

AB Above

As Above

ContainerVolume

100 ml

As Above

"As Above

As Above

Preservation (2)

Cone HN03 to pH<2

As Above

MaximumHoldinq Time*

6 months

As Above

28 days

6 months

As Above

40 CFR 143

40 CFR 141

As Above

40CFR141,143

40 CFR 143

40 CFR 141

40 CFU 143

40 CF!U 141((

As Above

40CFR141,143(31)

40 CFR 141

As Above

40 CtR 143

SampleContainerCleanina

As Above

'As Above

As Above

* Holding time begins at tine of sample collection39

^ • ^ * a P B a* ^ *™' »B H

40Analysis of Contaminants Using SATE DRINKING HATER Methodologies (including 500 series) for Aqueous Samples

OJoHHCO00

Contaminants

ORGANIC CONTAMINANTS,

ChlorinatedHydrocarbons

Chlorophenoxys

Trihalomethanes-total (TTM)

Trihalomethanesmaximum potential

VolatileHalogenatedOrganic Compounds

VolatileOrganicCompounds

Sample ContainerContainer m Volume

EXCLUDING OC/MS

G, foil orTeflon linedcap

As Above

G, narrow 25 mlscrew cap (501.1)with PTFE- 40 mlfluordcarbon (501.2)faced siliconesepta cap liner

As Above 40 ml

Screw cap 40 ml -vials, 120 mlPTFE-facedsilicone septum

As Above As Above

Preservation^ 1

Cool at 4 deg CASAP aftercollection

As Above

2.5-3 mg/40 mlNa2S2O3or sodiumsulf ite

25 deg CNo reducingagent

1:1 HC1 to pH<2Cool, 4 deg Cuntil analysis

As Above

extraction;14 daysanalysis;40 days

extraction;7 daysanalysis;30 days

14 days

Hold 7 daysbeforeanalysis

14 days

As Above

AnalyticalMethodoloav

40 CFR 141SM16-509A

• ' . > ' .

40 CFR 1141:SM16-50|9B

40 CFR 141Method 501.1Method 501.2

As Above

ii -40 CFR 141Method 502.1.

40 CFR 141Method 502.2

SampleContainerCleaninq

Aa Above

As Above

Aa Above

* Holding tine begins at time of sample collection

Analysis of Contaminants Using SAFE DRINKING HATER Methodologies (including 500 series) for Aqueous Samples

ContaminantsSampleContainer?1)

ContainerVolume Preservation(21

Volatile Aromaticand UnsaturatedOrganic Compounds

EDB/DBCP

OrganohalidePesticides andCommercialPCB Products(Arochlors)

Di-2(ethylhexyl)adipateDi-2(cthylhexyl)phthalate

Nitrogen- andPhosphorus-ContainingPesticides

Screw capvials, PTFEfaced siliconeseptum

As Above

Borosilicatew/graduations,screw capslined withPTFE-fluorocarbonextracted withmethanolovernight

40-120 ml 1:1 HCl to pH<2Cool, 4 deg Cuntil analysis

40 ml Cool 4 deg C0.08% Na2S2C>3if residual C121:1 HCl to pH<2

As Above 3 mg Na2S2C«3or 7 uL Na2S2C«3(0.04 g/ml),Cool, 4 deg Cuntil analyzed

1-liter HgCl to produceconcentrationsof 10 mg/L,80 mg

if residual C12Cool 4 deg Caway from lightuntil extraction

14 days

28 days

If HeptachlorExtraction:7 daysAnalysis;40 daysIf noextractionanalysis14 days(28)

40 CFJ* 141Method 503.1

40 CFR 141Method 504

As Above

Extraction:disulfotonsulfoxide,diazinonpronamide,terbufos7 days;14 day extractholding tine(28)

40 CFR 141GC-Method 507

oHHWVO

Holding time begins at time of sample collection41

Contaminants

ChlorinatedPesticides

PCBs (Screening)

Chlorinated phenoxyAcids

N-MethylGarbamoyloximesCarbamates

Glyphosphate

Endothall

Diguat

Sample ContainerContainer (11 Volume

Borosilicate 1-literw/graduations ,screw capslined withPTFE-f luorocarbpnextracted withmethanolovernight

As Above As Above

G, screw cap 60 mlvials withPFTE-f acedsilicone

Preservation 21

HgCl to produceconcentration of10 mg/L. Sealbottle and shakevigorously for 1minute.Cool, 4 deg Cuntil extraction

Cool, 4 deg C

80 mg Na2S203if residual C12

1.8 ml»monochloroaceticacid buffer.80 mg Na2S2C>3if residual C12Cool, 4 deg C

Extraction:7 daysAnalysis:14 days afterextraction (28)

Extraction:7 daysAnalysis;30 days (28)

Extraction;14 daysAnalysis;28 days

28 days

40 CFR 141Method 508A

40 CFR 141Method 515.1

40 CFR. 141Methodf 531.1

40 CFE 141Method 548

40 CFR 141 'Method 549

SampleContainerCleanincr

Benzo { a ) pyrene 40 CFR 141Method 550Method 550.1

* Holding time begins at time of sample collection

Analysis of Contaminants Using SATE DRIMKINO WATER Methodologies (including 500 series) for Aqueous Samples

Contaminants

- SampleSample Container Maximum Analytical ContainerContainerfIj Volume Preservation/2V Holding Time* Methodology Cleaning

ORGANIC CONTAMINANTS,

TrihalomethaneB

2,3,7,8-TCDD(Dioxin)

PurgeableOrganicCompounds

OrganicCompounds

G, screw capTeflon facedsilicone septum

As Above

G, amberTeflon-linedscrew caps

RADIOCHEHISTRY CONTAMINANTS, RADIOACTIVITY

Gross Alpha fi Beta

Strontium 89,90

Radium-total

Radium-226

Radium-228

Ruthenium-106

CeBium-134

Cesium-137

As Above

25 ml 10 mg 28203 14 daysor sodiumsulf ite

60-120 ml if residual Clz 14 days25 mg ascorbic acid1:1 HC1 to pH <2Chill, 4 deg C

1-L or if residual Cl2 Extraction;1 quart 40-50 mg 7 days

soditJm araenite Analysis;or N32S2O3 30 daysif urichlorinated6 N HC1 to pH < 2

AND RADIONUCLIDES

Cone. HNOj orHC1 to pH 2

As Above

Cone HCl to pH 2

As Above

40 CFR 141GC/MS 501.3GC/MS (SIM)

40 CFR 141GC/MS-524.1CG/MSi-524.2

40 Cfk 141GC/MS-525.1rev. 3.0

40 CFR 141

As Above

A« Above

As Above

A> Above

As Above

* Holding time begins at tine of sample collection43

.•44Analysis of Contaminants Using SAFE DRINKING WATER Methodologies (including 500 series) for Aqueous Samples

Contaminants

Cobalt-60

Iodine-131

Tritium

Uranium

SampleContainer ( 1)

As Above

ContainerVolume Preservation (2 )

Cone. HNOj orHC1 to pH 2

As Above

Cone. HNOo

Maximum AnalyticalHoldina Time* Methodoloav

40 CFR 141

As Above•1

1As Above

As Above

Photon emmiters As Above'

RADON IN DRINKING WATER

Radon G withTeflon-linedseptum

or HCl to pH 2

AB Above

Cool, 4 deg C

As Above

23 NJR 1423N.J.A..C. 7:18

Analysis of Parameters Using CLEAN WATER ACT HPDES (NJFueS) Methodologies for W&STEWA'tKR Samples

Sample

Parameter

BIOLOGICAL PARAMETERS

Coliform (fecal)

Coliform (fecal)chlorine present

Coliform (total)

Coliform (total)chlorine present

Fecal streptococci

Enterococci

HeterotrophicPlate Count

Pseudomonasaeruginosa

INORGANIC PARAMETERS,

Acidity

Alkalinity

Ammonia (as N)

Biochemicalo oxygen demand^ (BODd

SampleContainer (1)

As Above

NUTRIENTS AND

As Above

ContainerVolume

125 ml

As Above

DEMANDS

100 ml

As Above

400 ml

1000 ml

Preservation ( 2 )

Cool, 4 deg C,0.008% Na2S2Ojif residual C12

As Above

Cool, 4 deg C

As Above

Cool, 4 deg C

6 hours

As Above

14 days

As Above

28 days

48 hours

AnalyticalMethodolocrv

40 CFR 136.3

As Above

SM17 9230 B;C

SM17 9215B>C;D

SM17 9213 E;F

40 dFR 136.3- . f '.As Above

As Jbove

As Above

ContaineCleaning

As Above

u^Holding time begins at time of sample collection

P a rameter

46Analysis of Parameters Using d-EAK WATER ACT HPDER (NJPDES) Methodologies for WASTEWATER Samples

SampleSample Container Maximum Analytical ContainerContainer (11 Volume Preservation(21 Holding Time* Methodology Cleaning

Boron-total P,G

Bromide P,G

Calcium-total As Above

Carbonaceous As Abovebiochemicaloxygen demand(CBOD5)

Chemical As Aboveoxygen demand(COD)

Chloride As Above

Color As Above

Cyanide-total As Above

Cyanide amenable As Aboveto chlorination

Flouride-total P

Hardness-total P»G

100 ml

1000 ml

As Above

500 ml

As Above

300 ml

100 ml

HNO3 to pH<2

None Required

HN03 to pH<2

Cool, 4 deg C

None Required

Cool, 4 deg C

Cool, 4 deg C,NaOH to pH>120.6g ascorbicacid ifresidual C12

As Above

None Required

HNO3 to pH<2 ,

6 months

28 days

6 months

48 hours

28 days

As Above

48 hours

sulfide absent14 daysaulf ide present24 hours (22)

As Above

28 days

6 months

40 CFR 136.3

As Above

As Amove

Aa Above

As Above

Kjeldahl nitrogen-total (as N)

Magnesium-total

As Above

H2SO4 to pH<2

500 ml Cool, 4 deg C, 28 daysH2SO4 to pH<2

100 ml HNO3 to pH<2 6 months

'Holding time begins at tine of sample collection

As Above

cAnalysis of Parameters Using CT.RRH WATER ACT KPDES (NJPDBS) Methodologies for HASTBM&XER Samples

SampleParameter Container (1)

Nitrate (as N) P,G

Nitrate-nitrite P,G(as N)

Nitrite

Oil and

(as N) As Above

grease G

ContainerVolume

100 ml

1000 ml

Preservation^!

Cool,H2S04

4 deg C

4 deg Cto pH<2

petroleum based

AnalyticalMethkxJoloov

CFR 136.3

SampleContainerCleanino

As Above

As Above-total recoverable

Organic carbon-total (TOC)

Organic nitrogen{as N) (29)

Orthophosphate(as P)

Oxygen-dissolved(Winkler)

Phenols

Phosphorus(elemental)

Phosphorus-total

Potassium-total

Residue-total

P,G 25 ml

HCl or H2SO4to pH<2

As Above

3 daysnon-petroleum24 hours

As Above As Above

'Holding time begins at time of sample collection47

As Above

G, bottleand top

G. only

As Above

300 ml

500 ml

100 ml

As Above

Filter immediately,Cool, 4 deg C

Fix on site andand store in dark

Cool, 4 deg C,H2S04 to pH<2

Cool , 4 deg C

Cool, 4 deg C,R2S04 to pH<2

HN03 to pH<2

Cool, 4 deg C

48 hours

8 hours

28 days

48 hours

28 day*

6 months

7 days

As Above

Km Above

As Above

-*• - 'Analysis

Parameter

Residue- filter able(TDS)

Residue, non-filterable (TSS)

Residue- sett leable

Residue- volatile

Salinity

Silica-dissolved

Sodium-total

Specificconductance

Sulfate (as SO4)

Sulfide (as S)

Surfacants

Tannin and lignin

Turbidity

of Parameters Using CLEAN WATER

SampleContainer (1)

As Above

ContainerVolume

100 ml

1 As Above

1000 ml

100 ml

500 ml

250 ml

100 ml

"•'"" ""48

ACT KPDES, (JJJPDES)

Preservation(21

Cool, 4 deg C

Aa Above

As Above

Cool, 4 deg C

HN03 to pH<2

Cool, 4 deg C

As Above

Cool, 4 deg C,add zincacetate plusNaOH to pH>9

Cool, 4 deg C

Methodologies for

7 days

As Above

48 hours

7 days

28 days

6 months

28 days

As Above

7 days

48 hours

28 days

48 hours

T """ f """"• ' t . " •;

WASTEWA:IER samples

AnalyticalMethodoloOT

40 CFR 136.3

As Above

SM17-2520 B;C

40 CFR 136.3

As Above

SM17-5550 B(•

40 CFJt 136.3i

As Above

*Holding time begins at time of sample collection

Analysis of Parameters Using CLEAN WATER ACT NPDES (NdrDES) Methodologies for WASTEHATER Samples

Parameter

ANALYZE IMMEDIATELY

Chlorine- totalresidual

Hydrogen ion (pH)

Oxygen -dissolved(probe)

Sulfite (as SO3)

Temperature

INORGANIC PARAMETERS

Aluminum- total

Antimony- total

Arsenic- total

Barium-total

Beryllium- total

Cadmium-total

Chromium VI-dissolved

Chromium-total

Cobalt-totalOJoH Copper-total

Sample ,Container ( 1

(<15 MINUTES),

As Above

G, Bottleand Top

As Above

, TOXIC METALS

As Above

Container^ Volume Preservation^!

AnalyticalMethodoloo r

INORGANIC PARAMETERS

200 ml

.300 ml

1000 ml

100 ml

As Above

200 ml

100 ml

As Above

-HNO3 to pH<2

As Above

As Above •

Cool, 4 deg C

HN03 to pH<2

As Above

Analyzeimmediately

As Above

6 months

As Above

24 hours

6 months

As Above

40 CFR 136.3

As Above

As Above{•V

As Above

50Analysis of Parameters Using CLEMJ HATER ACT MPDES (NJPPES) Methodologies for WASTEWATER Samples

Parameter

Gold-total

Iridium-total

Iron-total

Lead-total

Manganese-total

Mercury- total

Molybdenum-total

Nickel-total

Osmium-total

Palladium-total

Platinum-total

Rhodium-total

Ruthenium-total

Selenium-total

Silver-total

Thallium-total

Tin-total

Titanium-total

Vanadium-total

SampleContainer (

As Above

Aa Above

As Above

Container11 Volume

100 ml

As Above

Preservation^ 1

HNO3 to pH<2

HN03 to pH<2

As Above

HNO3 to pH<2

As Above

As AbdVe

As Above

As Above As Above

•Holding time begins at time of sample

6 months

As Above

28 days

6 months

As Above

Aa Above

As Above

collection

40 CFR 136.3

40 CFR 136.3• • t

As Abd>ve

IAs Above

As Above

Analysis of Parameters Using CLEAN WATER ACT HPDBS (NJPDES) Methodologies for WASTSWAlTS™ S&Siplss

Parameter

Zinc-total

ORGANIC PARAMETERS,

Purgeablehalocarbons

Purgeablearomatichydrocarbons

AcroleinAcrylonitrile

SampleContainer (11

EXCLUDING GC/MS

G, vialscrew cap withcenter holeTeflon-facedsilicons septum

As Above

ContainerVolume Preservation^!

100 ml HNO3 to pH<2

25 ml or Cool, 4 deg C,larger 0.008% Na2S2O3

if residual C12

As Above Cool, 4 deg C,0.008% Na2S2O3if residual C121:1 HCl to pH 2

Aa Above Cool, 4 deg C,0.008% Na2S2O3if residual C12pH 4-5 with.1:1 HCl ifsamples analyzedfor acrolein

MaximumHoldino Time*

6 months

14 daysGC-601

Without HCl7 dayswith HCl14 days

Samples for .acroleinwith no pHadjustment3 days;with pHadjustmentor not foracrolein14 days

40 CFR 136.3

40 CFR 136.3GC-602

40 CFR 136.3GC-603

As Above

Phenols

CJoHH>t>vo

amber glassor protectfrom light,screw caplined withTeflon (orfoil ifsample notcorrosive)

1 liter1 quart

Cool, 4 deg C,0.008%Na2S2O3 ifresidual C12

7 days untilextraction40 days afterextraction

40 CFR 136.3 As AboveGC-604

*Holding time begins at time of sample collection51

52Analysis of Parameters Using CLEAN WATER ACT HP DBS. (HJPDES) Methodologies for WASTEWAXER Samples

Parameter

Benzidinee

SampleContainer ( 1)

amber glassor protectfrom lightscrew caplined withTeflon (orfoil ifsample notcorrosive)

1 liter Cool, 4 deg C,0.008% Na2S2O3if residual C12store in darkH2S04 to pH 2-7if 1,2-diphenylhydrazine islikely to bepresent :pH to4.0 +/- 0.2

Extraction7 daysAnalysis7 daysafterextractionif storedunder inert(oxidant free)atmosphere

40 CFR 136.3HPLC-605

Phthalate esters As Above As Above Cool, 4 deg C 7 days untilextraction40 days afterextraction

40 CFR 136.3GC-606

As Above

Nitrosamines

OrganochlorinePesticides & PCBs

As Above

As Above 1 liter1 quart

As Above Cool, 4 deg C, As Abovestore in dark0.008? Na2S2C«3if residual C12for determination ofN-nitroBodiphenylamineNaOH or H2SO4 topH 7-10

Cool, 4 deg CNaOH/H2S04to pH 5-9 ifaldrin to bedetermined.0.008% Na2S2C>3if residual C12

OJoHHUlO

NitroaromaticBand isophorone

As Above As Above

Extraction72 hours w/opH adjustment7 days withpH adjustment40 days afterextraction

Cool, 4 deg C,dark 0.008%Na2S2C>3 ifresidual C12

*Holding time begins at time of sample collection

40 CFR 136.3GC-60t7

As Above

40 CFR 136.3GC-608

As Above

40 CPR 136.3GC-609

As Above

Analysis of Parameters Using CLEAN WATER ACT NPDES (NJPDES) Methodologies for WASTEWRTER Samples

U)oHHU1

Parameter

Polynucleararomatichydrocarbon

Haloethers

SampleContainer (I)

Amber glassor protectfrom lightscrew caplined withTeflon (orfoil ifsample notcorrosive)As Above

ContainerVolume Preservation 21

1 liter Cool, 4 deg C,dark 0.008%Na2S203 ifresidual C12

As Above As Above

MaximumHoldiha Time*

As Above

40 CFR 136.3HPLC-610

40 C1TR 136.3

SampleContainerCleanincr

As Above

ChlorinatedHydrocarbons

As Above

ORGANIC PARAMETERS, MASS SPECTROMETRY

2,3,7,8-Tetrachloro-dibenzo-p-dioxin (TCDD)

Purgeables[except benzenetolueneethyl benzene(32)]

Purgeables[benzenetolueneethylbenzene(32)

G, screw caplined withTeflon (orfoil if samplenot corrosive)amber glassor protectfrom light

G, Teflonfaced siliconeseptum, screwcap with holein center

As Above

As Above Cool, 4 deg C

1 liter Cool, 4 deg C,0.008%Na2S2O3 ifresidual C12

As Above

25 ml orlarger

As Above

As Above 14 days

Cool, 4 deg C,0.008% Na2S2O3if residual C121:1 HC1 to pH<2

Without HC17 daysWith HC114 days

•Holding time begins at time of sample collection' . 5 3 •

GC-611

40 CFR 136.3 As AboveGC 6.12

40 C?R 136.3 (13)GC/MI5-613

40 C,?R 136.3GC/M5-624

As Above

54Analysis of Parameters Using CLEAN WATER ACT KPDES. (N-JPDES) Methodologies for WASTKWATER Samples

Parameter

Volatile OrganicCompounds byIsotope DilutionGC/MS [benzene,toluene, ethylbenzene only(32))

SemivolatileOrganicCompounds byIsotope DilutionGC/MS

SampleContainer(IV

SampleContainer Maximum Analytical ContainerVolume Preservation^ 1 Holding Time* Methodology Cleaning

Base/Neutralsand Acids

Volatile OrganicCompounds byIsotope DilutionGC/MS [exceptbenzene, tolueneethyl benzene(32)]

G, screw cap 1 literlined with 1 quartTeflon (orfoil if samplenot corrosiveamber bottle orprotect from .light

G, Teflon- 25 ml tofaced silicone 40 mlseptum, screwcap with centerhole

Cool, 4 deg C,0.008%Na2S2O3 ifresidual C12

Cool, 0-4 deg C,0.008% Na2S2O3if residual Cl2/

7 days until 40 CFR 136extraction GC/MS-62540 days afterextraction

14 days 40 CFR .136GC/MS-j-1624

AB Above As Above

Amber glassor protectfrom lightTeflon linedcap (oraluminum foilif samplenon-corrosive)

1.1 literorgreater

Cool, 0-4 deg C,0.008%Na2S2O3 ifresidual C121:1 HCl to pH<2

Cool, 0-4 deg C,0.008%Na2S203 ifresidual C12

Without HCl7 daysWith HCl14 days

As Above

As above (4)

40 CFR 136GC/MS--162 5

HUlN) ^Holding time begins at time of sample collection

cAnalysis of Parameters Using CLEAN WATER ACT NPDES (NJPDES) Methodologies for HASTSTWATER Samples

Parameter

PESTICIDES TESTS

OrganochlorinePesticides & PCBs

SampleContainer (1)

Amber glassor protect

ContainerVolume

1 liter1 quart

Preservation f 2)

Cool, 4 deg CNaOH/H2SO4

Extraction72 hours w/o

AnalyticalMethbdoloav

40 CFR 136.3GC-608

AQUATIC TOXICITY

Dilution Water

Effluent

Teflon linedcap (oraluminum foilif samplenot corrosive)

wide mouthlead freeglass orunplasticizedplasticcontainer

Aa Above

to pH 5-9if aldrin to bedetermined add0.008% Na2S2O3if residual C12

30 liters none

pH adjustment7 days withpH adjustment40 days afterextraction

96 hours

15 liters <2hr: teat temp. 24 hours>2hr: Cool, 4 deg C

RADIOCHEMISTRY PARAMETERS, RADIOACTIVITY AND RADIONUCLIDES

N.J.A.C. (27)7:18™Subchapter 6

As Above (27)

OJoHHtnU)

Alpha-total

Alpha-counting error

Beta-total

Beta-counting error

Radium-total

Radium-226

As Above

HN03 to pH<2

As Above

Aa Above

As Above

6 months

As Above

• As Above

Aa Above

As Above

40 CFR 136.3

As Above

Aa Above

Aa Aoovei

Aa Above"i

As Above

Aa Above

Parameter

Analysis of Parameters Using CLEAN WATER ACT NPDES JNJPDES) Methodologies for WASTEWATER Samples

SampleSample Container Maximum Analytical ContainerContainer(1) Volume Preservation(2) Holding Time* Methodology Cleaning

RADON IN WASTEHATER

Radon P/G HNO3 to pH<2 6 months N.J.A.C. 7:18 (9)23 NJR 1423

U)oHHU1 •Holding time begins at time of sample collection

ANALYSIS OF PARAMETERS USING SLUDOE METHODOLOGIES FOR SLUDGE SAMPLES

oHHU!Ul

Parameter

METALS

Chromium VI

Mercury

Metals

ORGANIC COMPOUNDS

Extractables(includingphthalates,nitrosamines ,organochlorineoesticides. PCBs.

SampleContainer (1)

As Above

G, Teflon-lined cap

ContainerVolume

400 ml

500 ml

1000 ml

Preservation^)

Cool, 4 deg C

HNO3 to pH<2

As Above

Cool, 4 deg C0.008%Na2S2O;jif residual Cl2

48 hours

28 days

6 months

Extraction:7 daysAnalysis:30 days

SW-846

DEP 100

As Above

nitroaromatics,isophorone,polynucleararomatichydrocarbons,haloetherB,chlorinatedhydrocarbons andTCDD)

Extractables(phenols)

Purgeables(Halocarbonsand Aromatics

As Above As Above Cool, 4 deg CH2S04 to pH<20.008%

As Above As Above

G, Teflon-lined septum

if residual Cl2

Cool, 4 deg C0.008%

14 days 624s

if residual Cl2HC1 to pH<2

As Above

Parameter

58ANALYSIS OF PARAMETERS USING SLUDGE-METHODOLOGIES FOR SI.USCS SAMPLES

SampleContainerdl

ContainerVolume Preservation^)

AnalyticalMethddoloov

Purgeablee(Acrolein andAcrylonitrile

Pesticides

Residuetotal

Residue,volatile,ash

Ph'enols

Oil and Grease

G, Teflonlined septum

G, Teflon-lined cap

P,Gwide mouthair tight

As Above

P,Gwide mouth

As Above

1000 ml

Cool, 4 deg C0.008%

if residual C]

As Above

Cool, 4 deg C

As Above

14 days

Extraction:7 daysAnalysis;30 days

DEP 010

DEP 012

DEP 013

DEP 032

DEP 036

As Above

U)oHH(Jlcn Holding time begins at time of sample collection

Analysis of BIOLOGICAL Samples Using NJDEPE Methodologiesfor Freshwater, Esturine And Marine Samples

Sample

301157

SampleContaminant Container (UPHYTOPLANKTON

FRESHWATER

Species Composition

(live samples) P,G

(preserved) As Above

Chlorophyll a P,Gamber orfoil-covered

MARIKE AND ESTUARINE

Species Composition

(live samples) P/G

(preserved) As Above

Container MaximumVolume Preservation^) Holdina Time*

250 ml Cool, 4 deg C 24 hours

1000 ml 50 ml 1 monthneutralizedformalinStoreytransport indark, cool container

250 ml Cool, 4 deg C 48 hoursstore/transportin dark

250 ml Cool, 4 deg C 24 hours

1000 ml 10 ml or more 48 hoursLugol'a solutionto maintain weaktea color.Store/transportin dark, coolcontainer.

SM17: 10200EPA73:Plankton 3,4

As Above

SM17il0200HEPA731Plankton 5.2

SM17 110200EPA73:Plankton 3,4

As Above

Containe:Cleaning

As Above

60Analysis of BIOLOGICAL Samples Using NJDEPE Methodologies

for Freshwater, Esturing And Marine Samples

ContaminantP HYTOPLANKTON

SampleContainer (11

ContainerVolume Preservation^ 1

MARINE AND ESTUARINE

Chlorophyll a

ZOOPLANKTON

Freshwater

P,Gamber orfoil-covered

250 ml Cool, 4 deg CStore/transportin dark.

6,000 ml 300 ml

48 hours

1 month

SM17:10200HEPA73:Plankton 5.2

SM17: 10200

As Above

Marine 6 Estuary As Above As Above

neutralizedformalin.Store in coolcontainer

5% formalin(5 ml)neutralizedformalin/100ml tap water),store andtransport incool container

As Above

EPA73:iPlanktion 3,4

As Above As Above

PERIPEYTON

DIATOMETER SLIDES AND ROCK SCRAPINGS

Speciescomposition

120 ml jarpolyeeal cap

U)oHHUl00

N/A 5% formalin 1 month(5 mlneutralizedformalin/100ml tap water),store andtransportin coolcontainer

SM17: 10300EPA73:Periphyton 3

As Above

Analysis of BIOLOGICAL Samples Using NJDEPE Methodologiesfor Freshwater, Esturine And Marine Samples

ContaminantSampleContainer/1)

PERIPHYTON

Chlorophyll a As Above 30 ml 90%neutralizedacetone, cool0-4 deg C,store andtransport indark container.

Ash Free Weight 120 ml jarpolyseal cap

MACROINVERTEBRATES

Speciescomposition

P,G N/A

48 hours

90 % N/Aneutralizedacetone, cool0-4 deg C,store andtransport indark container

5% neutralized N/Aformalin (5 mlneutralizedformalin/100 mlsample water)

SM17: il0300EPA73r«Periphyton 3.2

SM17:10300EPA73:Plankton 5.1

As Above

SM17J .10500 An AboveEPA73iMacroinvertebrates4.0

* Holding time begins at time of sample collection61

FOOTNOTES

P = Plastic, hard or soft G = Glass, hard or soft

I Discard bottles which have chips, cracks and etched surfaces.B Bottle closures must be water tight. Microbiological sample

containers must resist sterilization and solvent action of water.

( Sterilization must"noT produce toxic materials or bacteriostaticor nutritive compounds. Presterilized plastic bags can be used fordrinking water total coliform samples.

IIIIII4i

= Sodium thiosulfate

HC1 = Hydrochloric acid

Cl2 = Chlorine

EDTA = Ethylenediaminetetraacetic acid tetrasodium salt

NaOH = Sodium hydroxide

neutralized formalin = 100% neutralized formalin with sodiumtetraborate to pH 7.0-7.3

3. USEPA Statement of Work for Sample Container Repository, 4/85,Attachment A

i • .4. Detergent wash. Tap water rinse. Distilled water rinse. Air dry.

Heat in oven at 105 degrees Celsius for one hour. Cool in areafree of organics.

5. SW-846, 3rd edition, Volume 1-B, Section 4.1.4

6. Sample container cleaning procedure not specified

7. Washed. Rinse with extraction solvent (Chlorofluorocarbon 113).

8. Detergent, hot water wash. Hot tap water rinse. Rinse three timeswith distilled and deionized (ASTM Type II) water (non-toxictubing material). Cover tops and necks of glass closure bottleswith aluminum foil or heavy craft paper. Sterilize in autoclave at121 degrees Celsius for 15 minutes or in hot air oven at 170degrees Celsius for two hours.

9. Detergent and tap water wash. 1:1 HNOs rinse. Tap water rinse.Distilled and deionized (ASTM Type II) water rinse. (Additionaloption: Chromic acid or NOCHROMIX rinse, thorough Distilled anddeionized (ASTM Type II) water rinse to remove all traces ofchromium. Do not use on plastic bottles.)

10. Chromium cleaning solution. Detergent wash, hot. Tap water rinse.Distilled water rinse. Drain dry. Muffle furnace, 400 degreesCelsius C 15-30 minutes. Seal and store free from dust.

301160

11. Detergent wash, hot. Hot tap water rinse. Drain dry. Mufflefurnace at 400 degrees Celsius for i5-30 minutes. Acetone rinsefollowed by hexane rinse may be substituted for muffle furnace.Store inverted or capped with foil.

12. Sample container volume is not specified in methodology. Volume isrecommended by NJDEPE-Bureau of 'Environmental Measurements andQuality Assurance. -.-'—..—.„,.

13. Washed, rinsed with acetone or methylene chloride and dried beforei use. •

14. Detergent wash, hot. Tap water rinse. Distilled and deionized(ASTM Type II) water rinse. Drain dry. Oven or muffle furnace at400 degrees Celsius for 1 hour. Acetone rinse may be substitutedfor heating. Store inverted or capped with foil in cleanenvironment.

15. Detergent wash, hot tap water rinse. Drain dry. Oven or mufflefurnace at 400 degrees Celsius for one hour. Acetone rinse. Storeinverted or capped with foil in a clean environment.

16. Detergent wash, tap water, distilled water or solvent rinse, airdry (where appropriate) in an oven.

17'. Rinse with last solvent used. Detergent' wash, hot. Tap waterrinse. Reagent water rinse,. Drain dry. Oven or muffle furnace at450 degrees. Celsius for 1 hour. Acetone rinse may be substitutedfor heating. Store inverted or aluminum foil capped in cleanenvironment.

18. Detergent wash, rinse with tap and distilled water, dry at 105.degrees Celsius for 1 hour before use.

19. Detergent wash, distilled water rinse. Optional treatment withhydrochloric acid (1+9).

20. Warm detergent solution wash, thorough rinse in tap and distilledwater.

21. optionally, all samples may be tested with lead acetate paperbefore pH adjustment in order to determine if sulfide is present.If sulfide is present, it can be removed by the addition ofcadmium nitrate powder until a negative spot test is obtained. Thesample is filtered and the NaOH is added to pH>12.

22. Samples should be filtered immediately on site before addingpreservative for dissolved metals.

23. Thoroughly rinse with last solvent used. Hot water and detergentwash, thorough rinsing with dilute acid, tap and reagent water.Drain dry. Heat in oven or muffle furnace at 400 degrees Celsiusfor 1 hour. Thorough rinsing with acetone may be substituted for

301161

Iheating. Seal and store in clean environment. Store inverted orcapped with aluminum foil.

Rinse with water or last solvent used. Detergent wash, tap rinse,redistilled acetone rinse, pesticide quality hexane rinse. Heat inmuffle furnace at 400-500 degrees Celsius for 30 minutes toovernight. Store inverted or cover with aluminum foil.

25. Detergent wash, rinse in diTute HCl and then distilled water.Rinse with redistilled acetone rinse, pesticide quality hexanerinse. Heat in muffle furnace at 400-500 degrees Celsius for 30minutes to overnight. Store inverted or cover with aluminum foil.

26. If HNOs cannot be used because of shipping restrictions, samplesmay be inititally preserved by icing and immediately shipping tothe laboratory. Upon receipt in the laboratory, the sample must beacidified with cone. HNOj to pH<2. At time of analysis, samplecontainer should be thoroughly rinsed with 1:1 HNOs; washingsshould be added to sample.

27. Cleaning of all chambers and equipment shall be in accordance with,the following procedures:

As soon after breaking down a test as is practical, rinse with,acetone to remove organic compounds and then rinse twice withlaboratory grade freshwater; and secondly, soak and wash with a.'warm synthetic detergent/laboratory grade freshwater solution, and.then rinse with 50 degrees Cels*ius or warmer laboratory gradewater;.and

Finally, rinse with a fresh 5% hydrochloric or nitric acidsolution, for the removal of metals and bases, and then rinseagain with 50 degrees Celsius or warmer laboratory gradefreshwater.

28. NJDEPE recommended holding time for sample extraction andanalysis.

29. No test; calculated as total Kjeldahl Nitrogen minus AmmoniaNitrogen .

30. Proposed under Safe Drinking Water Act - size of communitydependent.

31. CFR 141 is under final rule to change from CFR 143.

32. Evidence indicates that some aromatic compounds, notably benzene,toluene and ethylbenzene are succeptble to rapid biodegradationunder certain environmental conditions. Refrigeration alone maynot be adequate to preserve these compounds in wastewaters formore than seven days. For this reason, a separate sample should becollected, acidified, and analyzed when these aromatics are to bedetermined.

iIIIIIPIIIIII

301162

Analyte Comparison List

1. Target Compound List (TCL) and Target Analyte List (TAL) from theUSEPA Contract Laboratory Program

2. Priority Pollutant List (PPL)from the Clean Water Act3. SW-846 Methodology list from the RCRA program

VOIATILES AND SEMIVOLATILES

Compounds ~**~~' TCL PPfr SW-8461. Acenaphthene x x x2. Acenaphthylene x x x3. Acetone x x4. Acrolein x x5. Acrylonitrile x x6. Anthracene . x x x7. Benzo(a)anthracene . x x x8. Benzo(a)pyrene x x x9. Benzene x X x10. Benzidine x x11. Benzo-(b)-fluoranthene x x x1?..' Benzo-(ghi)perylene x X x13. Benzo-(k)-fluoranthene x x x14.' Benzoic acid x x15. Benzyl alcohol x x16. Bis(2-chloroethoxy)-methane x x x17. Bis(2-Chloroethyl)-ether x x x18. Bis (2-chloroisopropyl)-either x x x19. Bis(2-ethylhexyl)-phthalate x x x20. Bromoform ' . . x x x21. • Bromodichloromethane x x x2 2 . Bromomethane x x x .23. 4-Bromophehylphenyiether x x x24. 2-Butanohe x x2.5. Butyl benzylphthalate x x x26. Carbon disulfide x x27. Carbon tetrachloride x x x28. 4-Chloro-3-methylphenol (P-Chloro-m-Cresol) x x x29. 4-Chloroaniline x x3 0 . Chlorobenzene x x x3 1 . chloroethane x x x3 2 . Chloromethane x x x33. Chlorodibromomethane x x34. 2-Chloroethylvinyl ether x x3 5 . Chloroform . ' x x x36. 2-Chloronapthalene x x x37. 2-Chlorophenol x x x3 8 . 4-Chlorophenylphenyl ether x x x3 9 . Chrysene . x x x40. Di-n-Butylphthalate x x x4 1 . Di-n-Octylphthalate x x x4 2 . Dibenz(a ,h)anthracene x x x43. Dibenzofuran x x44. 1,2-Dichlorobenzene x x x

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Compounds TCL PPL45. 1,3-Dichlorobenzene x - x x46. 1,4-Dichlorobenzene x x x47. 3,3-Dichlorobenzidine x x x48. l,l-Dichloroethane x x x49. 1,2-Dichloroethane x x x50. 1,1-Dichloroethylene x x x51. 1,2-Dichloroethylene (total) x52. trans-l,2-dichloroethylene .--— ^ x x53. 2,4-Dichlorophenol x x x54. 1,2-Dichlorppropane . x x x55. cis-1, 3-Dichloropropylene x x x56. trans-1, 3-Dichloropropylene x x x57. Diethylphthalate x x x58 . Dimethylphthalate x x x59. 2,4-Dimethylphenol x x x60. 4 , 6-Dinitro-2-methylphenol x x x61. , 2,4-Dinitrophenol x x x62. 2,4-Dinitrotoluene x x x63. 2, 6-Dinitrotoluene . x x x64. 1, 2-Diphenylhydrazine x x65. Ethylberizene x x x66. Fluoranthene x x x67. Fluorene x x x68. Hexachlorobenzene x x x69. Hexachlorobutadlene x x x70. ' Hexachlorocyclopentadiene x x x71. Hexachloroethane • X x x721. 2-Hexanone x x73. Indeno(l,2, 3-cd)pyrene x x x74,. Isophorone x x x75. Methylene Chloride x x x76. 4-Methyl-2-pentanone x x77. 2-Methylnaphthalene x x7«. 2-Methylphenol . x79. 4-Methylphenol ; X80. N-Nitrosodipropylamine x x x81. N-Nitrosodimethylamine x x82. N-Nitrosodiphenylamine . x x x83. Naphthalene x x x.84. 2-Nitroaniline x x8.'5. 3-Nitroaniline x x86. 4-Nitroaniline x x87. Nitrobenzene x x x88. 2-Nitrophenol x • x x89. 4-Nitrophenol x x x90. Pentachlorophenol x x x91. Phenanthrene x x x92 . Phenol x x x93. Pyrene x x x94 . Styrene x x95. l, 1, 2,2-Tetrachloroethane x x x96. Tetrachloroethylene x x x97. Toluene x x x

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Compounds TCL PPL SW-84698. Total Xylenes x *99. 1,2,4-Trichlorobenzene x x x100. 1,1, l-Trichloroethane x x x101. 1,1,2 Trichloroethane x x x102 . Trichloroethylene x x x103. 2>4,5-Trichlorophenol x x104. 2,4,6-Trichlorophenol x x x1Q5, Vinyl acetate x x106. Vinyl chloride ..... — "^ x x x

Pesticides/PCBs

107. Aldrin X x x108., Dieldrin x x x109., Chlordane x x110 . Alpha-chlordane x111. Gamma-chlordane x112. 4 , 4 '-DDT X X X113. 4, 4 '-ODD XX X114. 4, 4 '-DDE X x115. Endosulfan I x x x116. Endosulfan II x x x117. Endosulfan sulfate x x x118. Endrih x x x119. Endrin aldehyde . • x x120. Heptachlor x x x121. Heptachlor expoxide x x x122. Methoxychlor ' x x123. Endrin ketone x x124. BHC (Alpha) x x X125. B H C (Beta) X X X12(5. BHC (Gamma) (Lindane) x x x127. BHC (Delta) x x x128. Toxaphene x x x129. P C B 1242 X X X130. P C B 1254 . X X X131. P C B 1221 • X X X132. PCB 1232 x x x

133. P C B 1248 X X X134. P C B 1260 X X X135. P C B 1016 X X X

Dioxir)

136. 2,3,7,8-Tetrachlorodibenzo-p-dioxin (2 ,3 ,7 ,8-TCDD)x x x

Metals

EEL SW-846137. Aluminum x x138. Antimony . x . x x139. Arsenic x x x140. Barium x x

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Metals (con't)

II1IIII

141.142.143.144.145.146.147.148.149.150.151.152.153.154.155.156.157.158.159.

IIIIII4i

160,161.162,163,164,165,166167

169,170,

171.172,173,174,175,176177,

BerylliumCadmiumCalciumChromiumCobalt-CopperIronLead .MagnesiumManganeseMercuryNickelPotassiumSeleniumSilverSodiumThalliumVanadiumZinc

SW-846 Analytes not on the TCL

Phenols and Organic Acids

2-sec-Butyl-4, 6-dinitrophenol (DNBP)Cresol (methyl phenols)2-Cyclohexyl-4, 6-dinitrophenol2 , 6-Dichlorophenol4 , 6-Dinitro-o-cresol2 -Methyl-4, 6-dinitrophenolTetrachlorophenolsTrichlorophenols

Phthalate Esters

Benzyl butylphthalate

Nitroaroroatics and Cyclic Ketones

TAL PPL SW-B46XXXXXXXXXXXXXXXXXXX

XXXXXXXXXX

DinitrobenzeneNaphthaguinone

Polyaromatic Hydrocarbons

Benzo(j)fluorantheneDibenz(a,h)acridineDibenz(a,j)cridine7H-Dibenzo(c,g)carbazoleDibenzo(a,e)pyreneDibenzo(a,h)pyreneDibenzo(a,i)pyrene

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Polyaromatic Hydrocarbons (con't)

178. 3-Methylcholanthrene

Chlorinated Hydrocarbons

179. Benzotrichloride180. Benzyl chloride181. Dichlorobenzenes182. Dichlororaethylbenzenes (Dichlorotoluenes)183. Hexachlorocyclohexane184. Pentachlorohexane185. Tetrachlorobenzenes186. Trichlorobenzenes

Base Neutrals

187. Acetophenone

1 188. Aniline189. 4-Aminobiphenyl190. l-Chloronaphthalene191. 2-Chloronaphthalene

I 192. Dibenz(a,j)acridine• 193. p-Dimethylaminoazobenzene

194. 7 ,12-Dimethylbenz(a)anthracene

1 195. a,a-Dimethylphethylamine19'6. Diphenylamine197. Ethyl methanesulfonate (198. 2-Fluorobiphenyl199. .3-Methylcholanthrene200. Methyl methanesulfonate201. 1-Naphthylamine

• 202. 2-Naphthylamine203. N-Nitroso-di-n-butylamine-204. N-Nitrosopiperidine205. Pentachlorobenzene206. Phenacetin207. 2-Picoline208. Pronamide209. 1,2,4,5-Tetrachlorobenzene210. Toxaphene

Organophosphorous Pesticides

211. Azinphos methyl212. Bolst (Sulprofos)213. Chlorpyrifos214. Coumaphos215. Demeton216. Diazinon217. Dichlorvos218. Dimethoate219. Disulfoton220. EPN

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Oraanophorous Pesticides (con't)

221 i Ethoprop222. Fensulfothion223. Fenthion224. Malathion225. Merphos226. Mevinphos227. Monochrctcphast228. Naled '229. Parathion230. Parathion metp231. Phorate232. Ronnel233. Stirophos (TeMfflscvinphos)234. Sulfptepp235. TEPP236. Tokuthion237. Trichloronate

OaaBSJEJorine Pesticides and PCBs

238. Kepone

Herbicides

239. ' 2,4-D240. 2,4-DB241. 2,4, 5-T242. 2,4,5-TP243. Dalapon244. Dicamba245. Dichloroprop246. Dinoseb247. MCPA248. MCPP

Volatiles

249. Benzyl chloriife250. Bromobenzene251. Chloracetaldelps252. Chloral253. i-Chlorohexane254. Chloromethylmelp^Sher255. Chlorotoluene256. DibromochlorpitffitoB..257. Dibomomethane258. Dichlorodif luoas259. Dichlorometham260. 1, 1, 2 , 2-Tetra«3fesaa-thane261. 1, 1, l,2-TetracSfflB55ethane262. Trichlorof luoaa263. Trichloropropass;

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Non-haloqenated Vol^tiles

264. Acrylamide265. Diethyl ether266. Ethanol •267. Methylethylketone (MEK) (2-butanone)268. Methylisobutylketone(MIBK)269. Paraldehyde (trimer of acetaldehyde)

J - ...... -— - •' • - .. ..... •Acetonitrile. Acrolein. Acrilonitrile

•'. ,i 270. Acetonitrile

Volatiles

1 271. Broiriochloromethane272. 4-Bromofluorobenzene273. l,4-Dichloro-2-butane

1 274. 1,l-Dichloroethane27!5. trans-l,2-Dichloroethane27(5. cis-1,3-Dichloropropene277. trans-1,3-Dichloropropene

I 273. 1,4-Difluorobenzene• 779. F.thvl methacrvlate279. Ethyl methacrylate

280. lodomethane281. Trichloroethene282. 1,2,3-Trichloropropane

Herbicide's, by Method 8150

283. -Chlorobenzilate284. 2-chloroethyl-2-{4-(1,1-dimethyl)-phenoxy}-l-methyl-ethyl ester

TCL that are not PPL

Volatiles and Seroivolatiles Pesticides/PCBs Metals

Acetone Alpha-chlordane AluminumBe;nzoic acid Gamma-chlordane BariumBemzyl alchohol Methoxychlor Calcium2--Butanone Endrin Ketone VanadiumCarbon disulfide Cobalt4-Chloroaniline IronDibenzofuran Magnesium1, 2-Dichloroethylene (total) Maganese2-Hexanone Potassium4-Methyl-2-pentanone Sodium2-Methylnaphthalene2-Methylphenol4-MethyIphenol2-Nitroaniline3-Nitroaniline4-NitroanilineStyrene

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TCL that are not PPL (con't)

•Total Xylenes2,4,5-TrichlorophenolVinyl acetate

PPL that are not TCL

Volatiles and 's-emivolatiles ^^

AcroleinAcrylonitrileBenzidine2-Chloroethylvinyl ethertrans-1,2-dichloroethylene1,2-DiphenyIhydrazineN-Nitrosodimethylamine

SW-846 that are not PPL

Volatiles and Semivolatiles

AcetoneBenzbic acidBenzyl alcohol2-ButanoneCarbo'n disulfide4-Chloroaniline *2-Hexanone4-Methyl-2-petanone2-MethyInaphtha1ene2-N.itroaniline3-Nitroaniline4-NitroanilineStyreneTotal Xylenes2,4,5-TrichlorophenolVinyl acetate

PPL that are not SW-846

Volatiles and SeTrdvolatiles

Chlorodibromoroethane

TCL that are not SW-846

Volatiles and Semivolatiles

Chlorodibromomethane1,2-Dichloroethylene (total)2-Methylphenol4-Methylphenol

Pesticides/PCBs

ChlordaneEndrin aldehyde

Inorganics

Asbestos

Pesticides/PCBs

4,4'-DDEMethoxychlorEndrin ketorieDibenzofuran

Metals

AluminumBariumCalciumIronMagnesiumManganesePotassiumSodiumVanadium

Pesticides/PCBs

Alpha-chlordaneGamma-chlordane

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REFERENCES

American Public Health Assoc. and American Water Works Assoc. Standard Methods for the Examination of Water and WasteWater, 13-17th eds., Washington, D.C., 1980.

American Society for Testing and Materials, Annual Boole of ASTM Standards. Water and Environment a 1 Technology.Philadelphia, Pa, ASTM, 1985.

Berth, O.S. and B.J. Mason, Soil Sampling Quality Assurance and the Importance of Exploratory Study. ACS Symposia*Siries 267, Environmental Sampling for Hazardous Waste, ACS Publications. American Chemical Society, Wash.,D.C., 1984.

Borgianini, S.A. and M.S. Zackouski, "Field Decontamination Requirements to Assure the Quality of EnvironmentalMeasurements at Hazardous Waste Sites", in Proceedings of the Fourth Annual Hazardous Materials ManagementConference. Atlantic City, NJ, June 1986.

Brown, K.W., D.S. Berth, and B.J. Mason, Quality Assurance Audits of Field Sampling Activities. Presented at:Management of Uncontrolled Hazardous Waste Sites Conference, Washington,*D.C., Oct. 1984.

Hazardous Waste Engineering Research Laboratory, Guide for Decontamination of Buildings. Structures and Equipment atSuoerfund Sites. Cincinnati, OH, US Government Printing Office, EPA-600/2-85-02B, 1985.

Lowry, William et al, "A Field Audit Program to Ensure the Duality of Environmental Measurements'1, in Proceedings ofthe Third Annual Symposium on Solid Waste Testing end Quality Assurance Volime II. Washington D.C., July 1986.

iStevenson, T.J., Design of a Quality Assurance Program for the Assessment of Ground Water Contamination. Presented

nt: NUUA Conference on Ground Water Management? Orlando, FU., Oct. 1984.

USEPA, Biological Field and laboratory Methods for Measuring the Quality of Surface Water and Effluents. EnvironmentalMonitoring and Support Laboratory, Washington, D.C., US Governing Printing Office, EPA-670/4-73-001, 1973.

USEPA, Handbook for Analytical Quality Control in Water and Wastewater Laboratories. Environmental Monitoring andSupport Laboratory, Washington, D.C., US Government Printing Office, EPA-600/4-79-019, 1979.

USEPA, Handbook for Sampling and Sample Preservation of Water and Wastewater. Environmental Monitoring and SupportLaboratory, .Cincinnati, OH, US Government Printing Office, EPA-600/4-82-029, 1982. .

USEPA., Methods for Chemical Analysis of Water and Wastes. Environmental Monitoring and Support Laboratory,Cincimati, OH, US Government Printing Office, EPA-600/4-79-020. 1983. .

301171

PROCEDURE P-8

EQUIPMENT DECONTAMINATION

Powell Environmental Services/ Inc.REVISED: MARCH 18, 1993

301172

1.0 OBJECTIVE

The following procedure is a general guideline for decontamination offield and sampling equipment.

2.0 LIMITATIONS

._. These guidelines provide overall technical guidance and may be modifiedby specific project requirements.

3.0 DEFINITIONS

Decontamination - The process of neutralization, washing,rinsing, and removing exposed outer surfacesof equipment and personal protective clothingto minimize the potential for contaminationmigration.

Cross Contamination - The transfer of contaminants from their knownor suspected location into a non-contaminatedarea; a term usually applied to samplingactivities.

4.0 PROCEDURES

4,.:i RESPONSIBILITIES

The Site Manager is responsible for determining the type ofdecontamination facility to be used on-site, the solutions to beemployed, and the methodologies to be used in determining theeffectiveness of the decontamination approach. The Site Manager isassisted by the field team leader and site safety officer. On-site, thefield team leader is responsible for implementing the decontaminationplan by providing materials and staff members. The field team leaderoversees the decontamination process and provides verification of theeffectiveness of the procedures. The decontamination plan should bepresented or referenced in the Field Sampling Plan (FSP) and QualityAssurance Project Plan (QAPP).

4.2 AVOIDANCE

Numerous procedures are used in decontaminating people and objects. Themost effective procedure is contamination avoidance, that is, the use ofprocedures or materials to minimize or eliminate the potential forcontact with contaminants. Personal protection gear and standardoperating procedures are used to protect workers; other techniquesinclude encasing instruments and equipment in disposable outer wrappings(plastic sheeting), using disposable sampling devices, or isolating thecontaminants.

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4.3 METHODS -

Decontaminating procedures include flushing with water or othersolvents; using pressure or steam jets; heating, flaming, or bakingitems; scraping, rubbing, or grinding away1 or, most simply, disposingof the item after determining that the cost in time and staff necessaryfor decontamination is not acceptable, or that decontamination would notbs effective. .... . ... ,.„,„,„

Sampling Equipment

Any equipment that will be used to collect samples, such as stainlesssteel bailers, stainless steel ladles and stainless steel trowels willbe decontaminated at an upwind location on the site, following theprocedures described below:

The required decontamination procedure for all sampling equipment is asfollows:

Wash and scrub with low phosphate detergentTap water rinseRinse with 10% HNO3 ultrapureTap water rinseA methanol followed by hexane rinse (solvents must be pesticidegrade or better)

«, Thorough rinse with deionized demonstrated analyte free water(volume of water used during this rinse must be at least 5 timesthe volume of solvent used in above step)

• .Air dry• Wrap in aluminum foil for transport

Tap water may be used from any municipal water treatment system. Theuse of an untreated potable water supply is not an acceptablesubstitute. If metal samples are not being collected, the 10% nitricacid (HNO3) rinse may be omitted, and conversely, if organic samples arenot being taken, the solvent rinse may be omitted.

At the end of each day, the wash and rinse water will be drained .intodrums or the tanker used to collect purged groundwater for properdisposal. Non-interfering containers such as those made of glass,Teflon or stainless steel will be used to transport the hexane.

Field Instrumentation

The Interface Probe may be decontaminated before being used in each wellby following the procedures described below:

• Wash probe and cable with Alconox detergent and tap water• Rinse with distilled water. Allow water to drain into tub• Allow instrument to air dry• Place instrument into plastic bag

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301174

The wash and rinse water will be disposed of as described above.

Other field instrumentation will be cleaned as per manufacturer'sinstructions. Probes such as those used in pH and conductivity meterswill be rinsed after each use with deionized water.

4.4 RECORDS••-- — • - - .-2T . " - • - " . -

The QAPP and Field Sampling Plan document the decontamination approach.The use of equipment cleaning blanks, decontamination rinse blanks, andother quality control procedures serves to document the effectiveness ofthe cleaning before and the decontamination after working on-site. Thefield team leader typically furnishes documentation of equipmentdecontamination for those items leaving the site. In some instances,such as decontaminating a drill rig normally used by a subcontractor forwater well installation, the Site Manager may need to arrange forlaboratory testing of wipe samples before documenting the "cleanliness"1

of a piece of equipment.

5.0 ATTACHMENTS

5.1 DOCUMENTATION OF EQUIPMENT DECONTAMINATION

5.2 NJDEPE FIELD SAMPLING PROCEDURES MANUAL (MAY, 1992)CHAPTER 2 - SECTION C

REV.1993 . Page 3

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POWELL ENVIRONMENTAL SERVICES, INC.

DOCUMENTATION OF EQUIPMENT DECONTAMINATION

Project No:

Project Name:

Site Location:

Site Manager:

The following items of (corporate-owned) (rental) equipment have beendecontaminated following the procedures detailed in the Field SamplingPlian dated ; , (as modified oh _)..Additional information on the procedures used is contained in (list sitelogs, work plans, photographs, etc. ; ) .

EquipmentNomenc1ature

Manufacturer'sSerial Number

Dates ofUse

Date ofDecon.

SIGNED:

DATE:(Technician)

(Site Manager/Field Team Leader)DATE:

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NJDEPE FIELD SAMPLING PROCEDURES MANUAL (MAY, 1992)

CHAPTER 2 - SECTION C

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301177

FIELD SAMPLINGPROCEDURES MANUAL

State of New JerseyJIM FLORIDGOVERNOR

New Jersey Department of Environmental Protectionand Energy

SCOTT WEINER

COMMISSIONER

May 1992

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I vehicles, custody sealed in shuttles or in-the presenceof authorized personnel.

C. DECONTAMINATIONEQUIPMENT

OF SAMPLING

An ifiportant aspect of quality control ••--is-- -thedecontamination of field sampling equipment.Improperly cleaned and prepared sampling equipment canlead to misinterpretation of environmental data due tointerference caused by cross-contamination.

The following sampling equipment cleaning procedures(ASTH 0-5088-90. "Decontamination of Equipment") arestandard requirements of the NJDEPE. Also included areprocedures for cleaning heavy equipment end disposal ofdecontamination fluids and drill cuttings. Exceptionto the following procedures may be evaluated andapproved by NJDEPE on a case-by-case basis ifjustifications to do so involving site specific issuesor conditions are presented and verified beforehand.

1. LABORATORY DECONTAMINATION

In . certain instances laboratory decontamination canserve as a viable alternative to field decontaminationwhen sampling a non-aqueous matrix. Some advantagesinclude: 1_) decontamination takes place in acontrolled environment; 2) reduced need to transport,handle or dispose cleaning solvents, acids or washwater; 3) more attention can'be focused upon samplingwith field decontamination labor reduced or eliminated;4) reduced probability, of cross-contamination due toimproperly field decontaminated equipment; and 5)laboratory documentation of cleaning procedures endmaterials used. Disadvantages may include: 1)relative cost to scope of sampling event; 2)constraints meeting demands in emergency situations;and '3) logistics.

While the option to use, or not use, laboratorydecontaminated field sampling equipment for non-aqueoussampling end certain aqueous sampling equipment exists(i.e., foot check valves, filtering equipment,stainless steel clamps, automatic wastewater compositesamplers), there is no option available when samplingground water with bailers. GROUND UATER SAMPLINGDEVICES are required to be laboratory cleaned, packagedand dedicated for exclusive use at one sample locationfor that day's sampling (see definition of "laboratorycleaned" in the glossary). Field decontamination of

bailers elevates the potential of cross-contaminationto unacceptable levels. The possibility ofcontaminating a clean well, is also of concern whenusing improperly cleaned sampling devices.

It is recommended .that extra sampling devices txiavailable on-site in the event problems occur whichprohibit the use of a particular instrument. Whensamples are returned to the laboratory, the bailers arealso returned so they can be cleaned and prepared forthe next samp I ing event. It is preferred that the labperforming the analysis be the same lab that preparedthe sampling equipment. This cannot always bearranged; therefore, make certain the laboratoryanalyzing the samples will accept samples collectedwith field equipment not prepared at their laboratory.Also, the cleaning procedure of the laboratorypreparing the sampling equipment must be in accordancewith NJDEPE requirements. The procedure for laboratorydecontamination of dedicated field sampling equipmentcan be found in Table 2-1.

After this procedure has been completed, the samplingdevice should be wrapped in cleaned and oven bakedaluminum foil (see Chapter 2 footnote #4) or equivalentmaterial and custody sealed for identification. Arecord should be kept of the date and time and thisinformation should be labeled on the sampling device.

Sampling equipment should remain in the wrappedmaterial until it is used in the field. It should behandled as little as possible prior to use anddisposable gloves must be worn at all times whenhandling cleaned sampling equipment. Samplingequipment must never be stored near solvents, gasoline,exhaust emissions, or other equipment and/or materialsthat may impact the integrity of prepared samplinginstruments. .

2. FIELD DECONTAMINATION

In the event that laboratory cleaning is not an optionor not feasible, a field cleaning procedure must beused in order to reduce the chances of cross-contamination between sample locations. Severalcriteria are used to judge whether fielddecontamination procedures are appropriate. These are:

- Large number of sample locations may be scheduled ina one-day sampling event.

- Matrix of sample: Dedicated sampling equipment isalways the preferred option for all matrices,however, it may not be practical for soil sampling

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I*IIIIIII

IIIIII4ii

equipment such as split spoons end hand augers.(Ground water sampling equipment must be laboratory'cleaned and dedicated to a sampling point per day ofsanpling.)

Episode logistics: It may be impractical to labclean and dedicate sanpling equipment in a short-term emergency situation because of time and

ivti constraints.

Selection of a location for a field equipmentdecontamination station is also important. It shouldbe located away from any on-site source ofcontamination so as not to adversely impact thedecontamination procedure and close enough to thesanpling teams to keep equipment handling to a minimum.The decontamination station must also be set up in sucha way as to not adversely impact a clean environment.

Utilization of several units of one type of samplerwill allow decontamination teams to rotate equipmentmore effectively. Tables 2-1 and 2-2 detail theprocedures for field decontamination of aqueous andnon-aqueous sampling equipment respectively.

The decontamination procedures (Tables 2-1 and 2-2)developed,by the MJDEPE, have the concurrence of USEPA,Region II Monitoring Management Branch and follow ASTMD-50WI-90 methods. • The first step, a detergent andwater wash, is to remove all visible paniculate matterand r«:sidual oilst and grease. (This may be preceded bya steam or high pressure water wash to facilitateresidual removal). This is followed by a generous tapwater rinse and a distilled and'deionized water rinseto remove the detergent. If aqueous sampling is to beperformed, the following additional steps must becompleted. An acid rinse, included if metals samplesare to be collected, provides a low pH media for tracemetals removal. It is followed by another distilledand deionized water rinse. If the sample is not to beanalyzed for metals, the acid rinse and water rinse canbe omitted. Next, a high purity solvent rinse isdesignated for trace organics removal. Acetone has beenchosen because it is an excellent solvent, miscible inwater and is not a targeted analyte in PriorityPollutant Analysis. If acetone is known to be acontaminant at a given site or Target Compound Listanalysis is to be performed, Hethanol or anothersolvent may be substituted on a case by case basis withapproval from NJDEPE. Note, methanol can not be usedwhen sampling gasoline and its' by products. Thesolvent must be allowed to evaporate and then a finaldistilled and deioniied water rinse is performed. Thisrinse removes any residual traces of the solvent.

All equipment utilized for sampling use must bedecontaminated using distilled and deioniied water.Through distillation, all ionized solids and a broadrange of organic constituents will be removed, thusmaking it an ideal solvent for use when sampling fororganic parameters. Deionized water is water that hasbeen effectively freed from any existing ionicimpurities. .Deionized water should be used when

ysampling fer incrganic psi sorters. The »se ofdistilled and deionized water, commonly available fromcommercial vendors, is acceptable provided that the lotnumber and the associated analysis is available uponrequest to the NJDEPE.'

Whenever sanpling, regardless of how equipment has beencleaned, always start sanpling in the area of the sitewith the lowest contaminant probability and proceed tothe areas of highest known or suspected contamination.Following this procedure will add another measure ofquality control keeping cross contaminationinterference to a minimum.

3. DECONTAMINATION OF PUMPS

When submersible pumps are used to evacuate stagnantground water in the well casing, they must be cleanedand flushed prior to and between each use. Thiscleaning process consists of an external laboratorygrade glassware detergent wash and tap water rinse, orsteam cleaning of pump casing, hose and cables,followed by a 20 gallon flush of potable water throughthe pump. This flushing can be accomplished by the useof a clean plastic overpack drum or a plastic garbagecan filled with potable water. This must be followedby a distilled and deionized rinse of the outside ofthe pump. For submersible pumps smaller than fourinches in diameter, the recommended number of gallonsrequired for flushing may be proportionately reduced(i.e. three inch - 15 gallons, two inch - 10 gallon!;).If the evacuation hose is not changed betweenlocations, it must also be decontaminated in the siimemanner as the pump. Exercise caution to avoid contactwith the pump casing and water in the drum while thepimp is running (do not use metal drums or garbagecans) to avoid electric shock. Always disconnect thepump from power source before handling. Surface pumps(centrifugal and diaphragm) used for well evacuationneed not be cleaned between well locations only if acheck valve is used. New ASTH drinking water grndepolyethylene tubing must be used for each well linddiscarded after use. The submersible pump and tubingshould always be placed on clean polyethylene sheetingto avoid contact with the ground surface. All tubingmust be rinsed/wiped with distilled and deionized water

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toIiiiiiiiiiiii

to remove any residual material before entering thewell (Refer to ASTM D-5088-90, "Decontamination of

Equipment").

4. DECONTAMINATION OF HEAVY EQUIPMENT

Other equipment and material associated with samplingepisodes are required to be cleaned prior to usage.StiKTs such •s._drJAAwJiigs,_^eJJ_c^smg, auger flights,and backhoes all present potential sources oTinterference to environmental samples. These itemsmay come in contact with the materials adjacent to thematrix being sampled or may be attached to actualsampling equipment which has been cleaned in accordancewith procedures set forth in Table 2-2. Heavyequipment may potentially retain contaminants fromother sources such as roadways or storage areas or havesoil material from previous job sites that have notbeen removed. For these reasons it is most importantthat these items be cleaned prior to usage during asite investigation (Refer to ASTH D-5088-90).

Two options are available to accomplish cleaning ofheavy equipment: steam cleaning and manual scrubbing.The use of a steam generator can remove visible debrisand has several advantages. Steam generators usingpotable water provide a high pressure medium which isvery effective for residuals removal. They are alsoefficient in terms of ease of handling and generate lowvolumes of wash solutions.

Potential disadvantages include the need for a fixed orportiible power source and they may not be costeffective for use on small pieces of equipment or forone day sampling events.

A second option involves manual scrubbing of equipmentusing a laboratory grade glassware detergent solutionfollowed by a thorough water rinse. This procedure canbe .as effective as steam cleaning or preferred insituations where steam cleaning fails to remove visiblematerials. Disadvantages to manual scrubbing are thatit is labor intensive and it generates large volumes ofwash and rinse solutions.

The following requirements for cleaning heavy equipmentshould be incorporated into Field Sampling - QualityAssurance Project Plans where applicable.

5. DECONTAMINATION OF BACKHOES/DRILL RIGS

These items should be thoroughly steam cleaned ormanually scrubbed upon initial arrival on-site andbetween drilling or excavation locations. After the

initial washing, cleaning may be reduced to those areasthat are in close proximity to materials being sampled.The backhoe bucket and extension ana should be cleanedbetween each individual sample depth and between eachtest pit excavation. Drill rig items'such as augerflight*, drill rods, and drill bits must be cleanedbetween sample locations. Even when Shelby tubes orsplit spoons are used to collect samples that will not_undergo chemical analysis, they must also be steancleanea~of~scrubbed~between-each-sample point (Refer—to—ASTN D-5088-90).

6. DECONTAMINATION OF MONITOR WELL CASING ANDSCREEN

Before installation, field cleaning of well casing mustconsist of a manual scrubbing to remove foreignmaterial and steam cleaning, inside end out, until alltraces of oil and grease, are removed. Specialattention to threaded joints may be necessary to removecutting oil or weld burn residues. The casing shouldthen be handled end stored in such a manner so as toprevent cross contamination prior to installation.

7. CLEANING LOCATION

It is preferred, given site specific conditions, thatcleaning of all heavy equipment take place in onecentral location on site. A designated area ordecontamination pad should be established to conductall cleaning and provisions for containment of washsolutions must be made. All equipment such as. drillrigs, backhoes, and other mobile equipment shouldreceive an initial cleaning prior to use at a site.The frequency of subsequent cleanings while on-sitewill depend on how the equipment is actually used inrelation to taking environmental samples. Unlessotherwise specified and approved, all wash/rinsesolutions should be collected and contained on-site.The actual fate of this material will be determinedafter review of analytical data generated from samplesand on site discharge impacts have been evaluated.

8. DISPOSAL OF DRILL CUTTINGS

During the routine course of site investigation, wherematerials are known (via field instrumentation orvisual observation) or suspected (historic information)to be contaminated, sampling activity (i.e., soilboring or installation of monitoring wells) willproduce waste intrinsic to the site. The dispositionof this materiel must be carried out in a manner suchas not to contribute further environmental degradationor pose a threat to public health or safety.

301181

This materiel may be disposed of on-site provided: 1)the surface soils in areas of disposal are 'known orexpected to be contaminated at levels above NJDEPE soiltandards in effect at that time; 2) the disposedoil/water will not erode/flow either off-site or on-

site onto uncontaminated areas; 3) no potential tocontaminate an uncontaminated aquifer exists, and; 4)the potential to create a health hazard to adjoiningproperty owners through airborne expofl.u jSjgjJ s non-existent. In addition, the requirements of the NewJersey Pollution Discharge Elimination System (NJPDES)must be followed for discharges to ground or surface

waters.

If any of the above conditions cannot be met on-site,the materials must be placed in containers (drums,rolloffi;, etc.) and stored in a secure area of the site(fenced or access by unauthorized persons prevented) ortransported to a central secured location. The need toperform analyses of the secured material will bedetermined by NJDEPE. The material will be retainedfor remediation or disposal in accordance withregulations as part of the selected site remedy.

When test pits are utilized for investigation, materialexcavated may be returned to the hole, but, excavationbelow the water table is not allowed. Holes producedfrom soil borings are to be grouted in accordance withNJDEPE's Water Monitoring Management Programregulations unless NJDEPE determines the material canbe returned to the hole. Holes not grouted will befilled with sufficient quantities of material to makeup for amount of soil sampled and account for settlingthus allowing the hole to return to natural grade.

When materials of a noncontaminated nature are to bedisposed of on-site, the following guidelines must beconsidered: 1) disposed cuttings, soil or water willnot erode or flow off-site; 2) disposed water will notflow through an area of contamination and therebyspread it to a clean area; or 3) NJDEPE approves thedisposal procedures.

Finally, at off-site (i.e. background) locations whereno contamination is expected, the primary considerationis the wish of the property owner. If acceptable tothe property owner, dr i l l cuttings and muds from wellinstallation may be raked into adjacent soils. If theproperty owner requests the unconteminated material beremoved from the site, it is to be properly containedend removed to the site under investigation anddisposed of or stored per decision of the NJDEPE. Ifdrill cuttings and/or development water are expected tobe contaminated, they are to b« removed Irom the off-

site location to a secure on-site location and retainedfor remediation or disposed of per applicableregulations.

9. DISPOSAL OF DEVELOPMENT. PURGE, PUMP TESTAND DECON WATERS

Similar to drill cuttings, an initial determinationwhether the** west* taters should be consideredcontaminated should be Bade by evaluating fieldinstrumentation reading* or by previous analyticalinformation. Additional field tests to assist in thatdetermination (e.g. pH, color, other physical orchemical characterizations) must be utilized to themaximum extent possible.

Essentially, water generated that is not considered tobe contaminated may be rc-applled directly to theground surface and permitted to percolate back into theground water system. Care should be taken, however, toavoid nuiscrice situations where the discharge may causeundue concern on • the part of property owners or thecommunity. in such, cases. It Is advisable to disposeof the water into a local stomwater or sanitary sewersystem, or collect and discharge the water slowly toavoid such a condition. Please note that alldischarges to surface water and/or the sanitary sewer

.are subject to the permit requirements contained in theNJPDES regulations.

Where the water is considered to be contaminated, thewater generated may be re-applied to the ground surfaceprovided all the following conditions are met:

1. The water is not permitted to migrate off-site.

2. There is no potential for contaminating apreviously uncontaminated aquifer (for example, thedischarge will not be permissible if a loweraquifer is being tested and is contaminated whilethe upper aquifer is not).

3. The discharge will not cause an increase to groundsurface soil contamination.

If the above conditions cannot be met, the water shallbe collected and secured at a single location(preferably the primary site under investigation).Collected water may be subsequently re-applied toground surface only if, based on analytical results,there ere indications that the above conditions can bemet. If not, arrangements for proper disposal must beaccomplished prior to the event.

301182

In addition to the above considerations, therequirements of the New Jersey Pollution DischargeElimination System (NJPDES) must be followed for alldischarges to ground water and stormuater. The NJPDESPrograr.) requires the issuance of a permit for thesedischarges.

It is preferable to complete discharges of development,purge, and decon waters at a single, known contaminatedarea ofi-site; "'""TKis- area will -be selected, bytfieNJDEPE. In cases where such an area cannot be located,as with contaminated well field projects, dischargeswill.occur as close to the well or sampling location asreasonably possible.

D. PROCEDURES FOR QUALITYAND QUALITY CONTROL (QA/QC)

ASSURANCE

OA/OC samples are intended to provide control over thecollection of environmental measurements and subsequentvalidation,, review, and interpretation of generatedanalytical data. The various types of blank samplescurrently used by the NJDEPE and related QA/QC concernssuch as packaging, handling, preparation and actualprocurement of samples from field locations arediscussed below.

The trip blank is used exclusively for volatile organicanalysis (aqueous sampling only) and its purpose is tomeasure possible cross contamination of samples duringshipf)ing to and from the site. The "tripTslank is neveropened and travels to the site vn'th the empty samplebottles and back from the site with the collectedsamples in an effort to simulate sample handlingconditions. Contaminated trip blanks may also indicateinadequate bottle cleaning or blank water ofquestionable quality.

The primary purpose of this type of blank is to detectadditional sources of contamination that mightpotentially influence contaminant values reported inactual samples both quantitatively and qualitatively.The following have been identified as potential sourcesof contamination.

Laboratory reagent waterSample containersCross contamination in shipment, bottle handling andstorage

- Arctient air or contact uith analyticalinstrumentation during preparation and analysis at

the laboratory- Laboratory reagent* used in analytical procedures

The purpose of a field blank it to place • mechanism ofcontrol on cample equipment handling, preparation,storage, and shipment. The field blank travels and isstored uith the samples bottles, and is alsorepresentative of bottle shipment effects on samplequality. By being opened in the field and transferredoye£\a cleaned sampling device (where applicable), the«—field blank is indicative of ambient conditions end/or.equipment conditions that may potentially affect thequality of the associated samples.

The primary purpose of this type of blank is to providean additional check on possible sources ofcontamination beyond that which is intended for tripblanks. A field blank serves a similar purpose as atrip blank regarding blank water quality and samplebottle preparation. However, Vt is primarily used toindicate potential contamination from ambient air aswell as from sampling instruments used to collect andtransfer samples from point of collection into samplecontainers (it may also be referred to as the fieldrinsate blank).

The following is a breakdown by matrix of blank samplerequirements.

1. NON-AQUEOUS MATRIX

a. Field Blanks

i. Description - The performance of field blanksrequires two (2) sets of identical bottles: one setfilled with demonstrated analyte free waterprovided by the laboratory performing the sampleanalysis, and one etipty set of bottles. Thebottles should also be identical to those providedfor aqueous sample collection. Note: Since fieldblanks ere aqueous, the lab must provide water Horvolatile analysis in (0 ml septum vials. Althoughfor soil VOA sample collection the lab may provide4 oz wide mouth bottles. At the field location, inen area suspected to be contaminated, the water ispassed from the full set of bottles through thededicated or field decontaminated samplingdevice(s) and into the empty set of bottles. Thiswill constitute identical bottle to bottletransfer. Field blanks must be preserved in theseme manner BS samples and only need to becollected and analysed for volatile organics whenvolatile organics constitute a parameter being

301183

STANDARD OPERATING PROCEDURESi

PROCEDURE F-10

SAMPLE PACKAGING & SHIPPING

301184

1.0 OBJECTIVE

This guideline provides instructions for sample packaging and shippingin accordance with United States Department of Transportation (DOT)regulations.

2.0 APPLICABILITYJ"" ------ ••"-•S!?-"-- - - - .... . . . . . . ' ,,, irrv ffOngr.-.

The guideline is applicable to samples taken from uncontrolled hazardoussubstance sites and transported to off-site laboratories for analysis.

Carrier -

n. o. s. -

n.o. i. -

3.0 DEFINITIONS

A person or firm engaged in the transportation ofpassengers or property.

Not otherwise specified.

Not otherwise indicated. .

Other regulated material..

DOT Classifications for Hazardous Materials - The followingclassifications, set forth by the DOT in the Code of Federal Regulations(49 CFR 173.2):r

• Radioactive material

• Poison A

• Flammable liquid

• Non-flammable gas

• Oxidizer

• Corrosive material (liquid)

• Poison B

• Corrosive material (solid) '

• Irritating material .

• Combustible liquid (in containers having capacities exceeding 110gal.)

• ORM-B

• ORM-A

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• Combustible liquid (in containers having capacities exceeding 110gal. or less)

• ORM-E

4.0 GUIDELINES

.Samples collected at uncontrolled, hazardous substance_f acilities usuallyhave to be; transported elsewhere for analysis. Samples must betransported to protect their integrity, as well as to protect againstany detrimental effects from leakage or breakage. Regulations forpackaging, marking, labeling, and shipping hazardous materials andwastes are promulgated by the United States Department ofTransportation, and described in the Code of Federal Regulations (49 CFR171 through 177, in particular I72.402h, Packages Containing Samples).

4.1 RESPONSIBILITIES

The Project Manager or Site Manager is responsible for determining thatsamples are properly packaged and shipped. Sampling personnel andshippers (if.used) are responsible for implementing the packaging andshipping requirements. The chain-of-custody procedures and requirementsare described in SOP F-5.

4.:! EQUIPMENTI

The following equipment is used in packaging and shipping samples:

• Sample bottles, provided by designated laboratory

• Polyethylene bags, 2 mil or thicker

• Metal paint cans, 1 gal.

• Packaging material: bubble pack, vermiculite or similar non-combustible packing material

• Picnic coolers or ice chests, preferably metal, capable ofwithstanding impact caused by a 4 ft. drop

4.3 PACKAGING, MARKING, AND LABELING METHODS

4.3.1 Environmental Samples

Packaging

Environmental samples can be packaged following the procedures forsamples classified as flammable liquids or flammable solids. See SOP F-5 for details on the collection of environmental samples. Marking,labeling, and shipping papers do not apply.

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Environmental samples can also be packaged without being placed insidemetal cans as required for flammable liquids. For 'example, samplecontainers properly identified and with a sealed lid can be enclosed insealed polyethylene bags and packed in metal picnic cooler-typecontainers. Sufficient non-combustible, absorbent cushioning materialsuch as "bubble pack" must be used to minimize the possibility of samplecontainer breakage. Ice or "blue ice" is added to low-concentrationsamples. To further reduce the possibility of leakage, the sample,container, and the sample bottles and absorbent material can be placedin a larger bag that is also sealed.

Marking and Labeling

A complete sample identification tag or label must be affixed to samplecontainers. The words "Environmental Sample" should be marked on theoutside container.

No DOT marking or labeling is required.

Shipping Papers

No DOT shipping papers are required for environmental samples. However,the appropriate chain-of-custody forms must be included with theshipment. •

Transportation

There are no DOT. restrictions on the mode of transportation forenvironmental samples.

4.3.2 Dnanalyzed Hazardous Waste site Samples, ExcludingThose from Closed Containers

The procedures to be used to pack, mark, and ship hazardous wastesamples are presented below. A checklist summarizing these procedureshas been developed and is provided in .Section 4.4. This checklistshould always be consulted prior to sample shipment to ensure that allsample-handling requirements are satisfied.

Packaging

Packaging procedures are as follows:

• Collect samples in accordance with the procedures given in SOP F-10of this manual. Allow sufficient ullage (approximately 10 percentby volume) so container is not liquid-full at 130 F. If a solidmaterial is being collected, the container plus contents shall notexceed 1 lb. net weight.

• Attach properly completed sample identification tag or a PowellEnvironmental Services, Inc. sample label to sample container.

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• Seal sample container and place in 2-mil-thick (or thicker)polyethylene bag (one sample per bag). Tags should be positionedto enable them to be read through bag.

• Place sealed bag inside a metal can with incombustible, absorbentcushioning material (e.g., vermiculite or earth) to preventbreakage (one bag per can). Pressure-close the can and use clips,tape-,- or other posi-tiy-e means to hold the lid securely., tightly,and effectively.

• Mark and label this container as indicated below.

• Place one or more metal cans (or a single 1-gal. bottle)fsurrounded by incombustible packaging material for stability duringtransport, into a strong outside container, such as a metal picniccooler or a fiberboard box.

• Mark and label the outside container and complete shipping papersas described below.

Use abbreviations only where specified. Place the following information(either hand-printed or on pre-printed labels) on a metal can (orbottle): laboratory name and address and "Flammable Liquid, n.o.s.11 (ifnot liquid, write "Flammable Solid, n.o.s.").* Place the followinglabels on the outside of the can (or bottle): "Cargo Aircraft Only" and"Flammable Liquid" or, if not liquid, "Flammable Solid". ("DangerousWhen Wet" label should be used if the solid has not been exposed to wetenvironment.)

(Note: If the cans are placed in an exterior container, both thatcontainer and the inside cans must have the same markings and labels asabove. "Laboratory Samples" and "THIS SIDE UP" OR "THIS END UP" shouldalso be marked on the top of the outside container, and upward-pointingarrows should be placed on all four sides of the exterior container.)

• Using "Flammable" does not convey the certain knowledge that a sampleis in fact flammable, or how flammable, but is intended to prescribe theclass of packaging in order to comply with DOT regulations, just beforeor just after the "Flammable Liquid, n.o.s." or "Flammable, Solid,n.o.s." description.

Shipping Papers

Complete the carrier-provided bill-of-lading and sign the certificationstatement. If carrier does not provide these documents, use standardindustry form, providing the following information in the order listed(one form may be used for more than one exterior container) : "FlammableLiquid, n.o.s." (or "Flammable Solid, n.o.s." as appropriate); "CarqoAircraft Only", "Limited Quantity" or "Ltd. Qty."; "Laboratory Samples";"New Weight _" or "Net Volume \ " of hazardous contents) , byitem, if more than one metal can is inside an exterior container. Thenet weight or net volume must be placed just before or just after the"Flammable Liquid", n.o.s." or "Flammable Solid', n.o.s." description.,

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301188

A chain-of-custody record form (see SOP F-5) must be properly executedand included in the exterior container.

Unless samples are driven to the laboratory, a team member mustaccompany shipping container(s) to the transport carrier and, ifrequired, open outside container(s) for freight inspection.

g °" -jT3ir3—Una-aa-l-yz-ed—Haaarao-ua- Waste_Site_SamplesL_Talcen -pgen*Closed Containers

Slightly different procedures apply to hazardous waste site samplestaken from closed containers. The procedures to be followed by sitepersonnel for packaging, marking, and labeling are presented below.Th£-.y are rarely used and are provided for information only.

This packaging, marking, labeling, and shipping methods provides themost extreme procedure for materials classes as Poison A (49 CFR173.328). In the absence of reliable data that exclude the possibilityof the presence of Poison A chemicals or compounds, these proceduresmust be followed.

Packaging

The following packaging procedures are to be used:

• Collect sample in polyethylene or glass container which is of anouter diameter narrower than the valve hole on a DOT spec. 3A1800or 3AA1800 metal cylinder. Fill sample container allowingsufficient ullage (approximately 10 percent by volume) so it willnot be liquid-full at 130 F. Seal sample container.

• Attach properly completed sample identification tag and EPA samplecontrol label to sample container.

• With a string or flexible wire attached to the neck of the samplecontainer, lower the container into a mass cylinder that has beenpartially filled with incombustible, absorbent, loose packagingmaterial (vermiculite or earth). Allow sufficient cushioningmaterial between the bottom and sides of the container and themetal cylinder to prevent breakage. After the cylinder is filledwith cushioning material, dip the ends of the string or wire intothe cylinder valve hole. Only one sample container may be placedin a metal cylinder.

• Replace valve, torque to 250 ft.-lb. (for 1-in. opening) andreplace valve protector on metal cylinder using Teflon tape.

• Mark and label cylinder as described below.

• One or more cylinders may be placed in a strong outside container.

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• Mark and label outside container and complete shipping papers asdescribed below.

The samples may not be transported by Federal Express Corporation (aircargo) or other common carrier aircraft, or by rented, non-governmentaircraft. (Samples may be shipped by ground transport or governmentaircraft.)

• •-.- —- --•- ;.-._:- ----- :- - .: ,— --- — --.- .. —- -j • - - :_ -^_ • ••—•r.ri.--- • -.- — -'--' Si**** ' _^ "'"~ •— ;

Use abbreviations only where specified. Place the following information(either hand-printed or on pre-printed labels) on the side of thecylinder, or on a tag wired to the cylinder valve protector: "PoisonousLiquid or Gas, n.o.s." * and the laboratory name and address. Place thelabel "Poisonous Gas" on the cylinder ("Poisonous Liquid" label notacceptable here, even if liquid).

(Note: If the metal cylinders are placed in an outside container, boththe container and cylinders inside must have the same markings andlabels as above. In addition, "Laboratory Sample" and "Inside Packagescomply with Prescribed Specifications" should be marked on the top ofthe outside container. "THIS SIDE UP" marking should be placed on theoutside container and upward-pointing arrows on four sides.)

* Using "Poisonous" does not convey the certain knowledge that a sampleis in fact poisonous, or how poisonous, but is intended to prescribethat class of packaging in order to comply with DOT regulations.

Shipping Papers

Complete the shipper-provided bill-of-lading and sign the certificationstatement. If carrier does not provide these documents', use^standardindustry form, providing the following information in the order listed(one form may be used for more than one exterior container; useabbreviation only as specified): "Poisonous Liquid, n.o.s."; "LimitedQuantity" or "Ltd. Qty.";, "Laboratory Samples"; "Net Weight _" or"Net Volume " (of hazardous contents), by cylinder if inside anexterior container. The net weight or net volume must be placed justbefore or just after the "Poisonous Liquid, n.o.s." marking.

A chain-of-custody record form must also be properly executed andincluded in the container or with the cylinder.

Unless the samples are driven to the laboratory, a team member willaccompany shipping containers to the transport carrier and, if required,open outside container(s) for freight inspection.

4.4 RECORDS

A shipping certification form must be completed for all samples to beshipped. The following procedures shall be followed:

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Packaging

• Check DOT 172.500 table for appropriate type of package forhazardous substance.

• Check for container integrity, especially the closure.

• Check for sufficient absorbent material in package. .

• Check for sample tags and log sheets for each sample.

Shipping Papers

• Check that entries contain only approved DOT abbreviations.

• Check that entries are in English.

• Check that hazardous material entries are specially marked todifferentiate them from any non-hazardous materials being sentusing same shipping paper.

• Be certain all hazardous classes are shown for multi-classmaterials.

• Check total amounts by weight, quantity, or other measure used.r .

• Check that any limited-quantity exemptions are so designated on theshipping paper.

• Offer driver proper placards for transporting vehicle.

'• Check that certification is signed by-shipper. —- --.--. __

• Make certain driver signs for shipment.

RCRA Manifest

• Check that approved state/federal manifests are prepared.

• Check that transporter has the following: valid EPA identificationnumber, valid driver's license, valid vehicle registration,insurance protection, and proper DOT labels for materials beingshipped.

• Check that destination address is correct.

• Check that driver knows where shipment is going.

• Check that driver is aware of emergency procedures for spills andaccidents.

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Make certain driver s»k for shipment.

Make certain one cpp f executed manifest and shipping document isretained by shipper-

S-0 ATTACHMENTS

None« -•-;

II " ' ' •

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I301192

PROCEDURE F-12

FIELD pH/SPECIFIC CONDUCTANCE/TEMPERATURE MEASUREMENT

301193

A. FIELD pH MEASUREMENT

1.0 OBJECTIVE

This guideline details the steps required to measure the pH of anaqueous sample while in the field using both a pH meter and pH paper.It is important to obtain---tf^-pfr-measurement soon after taking a sampleand thus avoid sample changes such as precipitation, temperaturefluctuation, or oxidation which can affect the pH of the sample.

2.0 APPLICABILITY

This; guideline is applicable to all aqueous samples such as potable wellwateir, monitoring well water, surface water, leachate, drummedwastewater, and other water samples.

3.0 DEFINITIONS

pH -- The negative logarithm (base 10) of the hydrogen ionactivity. The hydrogen ion activity is related to thehydrogen ion concentration, and, in relatively weaksolution, the two are nearly equal. Thus, for allpractical purposes, pH is a measure of the hydrogen ionconcentration.

ipH paper - Paper that turns different colors depending on the pH of

the solution to which it is exposed. Comparison withcolor standard supplied by the manufacturer will thengive an indication of the solution pH.

4.0 GUIDELINES

Measurement of pH is one of the most important and frequently used testsin water chemistry. Practically every phase of water supply andwastewater treatment such as acid-base neutralization, water softening,and corrosion control is pH dependent. Likewise, the pH of leachate canbe correlated with other chemical analyses to determine the probablesource of contamination. It is therefore important that reasonablyaccurate pH measurements be taken.

Two methods are given for pH measurement: the pH meter and pH indicatorpaper. To use the pH meter, the meter and electrode are standardized inpH 7 buffer and then immersed in the unknown sample to obtain a pHreading. No standardization is required when using pH paper. Theindicator paper is simply immersed in the sample, and then a colorcomparison is made.

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The project team leader is responsible for deciding when a pHmeasurement should be taken1

The field samplers are responsible for measuring the pH arid forrecording and reporting the results.

4.2 EQUIPMENT

The following equipment is needed for taking field pH measurements:

• HYDAC pH tester with combination polymer body, sealed reference pHelectrode or equivalent.

• pH indicator paper, such as Hydrion or Alkacid, to cover the pHrange 2 through 10.

4.3 CALIBRATION

Calibration procedures should be in accordance with those specified inthe operations manual of the meter.

4.4 FIELD PH MEASUREMENT

, 4.4.1 pH Meter

The; following procedure is used for measuring pH with a pH meter:

• ±mmerse the tip of the electrode in water overnight. If this isnot possible due to field conditions, immerse the electrode tip inwater for at least an hour before use.

• Rinse the electrode with demineralized water.

• Immerse the electrode in pH 7 buffer solution.

• Adjust the temperature compensator to the proper temperature.

• Adjust the pH meter to read 7.0 (Note: If the sample is known tohave a very acidic or alkaline pH, standardize the meter with pH 4or pH 10 buffer, respectively.)

• Remove the electrode from the buffer and rinse with demineralizedwater.

• Immerse the electrode in the unknown solution.

• Read and record the pH of the solution, after adjusting thetemperature compensator to the sample temperature.

• Rinse the electrodes with demineralized water.

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301195

• Keep the electrode immersed in water or moist with a-wet cottonballor replace cap when not in use.

4.4.2 Indicator Paper

The following procedure is used for measuring pH with pH indicatorpaper:

• Immerse a strip of indicator paper into the unknown solution.

• Remove the paper from the solution and compare-the color with theindicator colors given on the pH paper container.

• Record the pH. (Note: If the indicator paper is suspected ofbeing old or deteriorated, immerse it in pH 7 buffer and check thecolor that develops against the standards given.)

4.5 RECORDS

All results are to be recorded in the field logbook.

5.0 ATTACHMENTS

5.1 EQUIPMENT MANUAL - HYDAC #301353

, Included in Section 5.1 of SOP F-12-C (Temperature Measurement)

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B. SPECIFIC CONDUCTANCE MEASUREMENT

1.0 OBJECTIVE

This guideline details the steps required to measure the specificconductance of an aqueous sample while in the field. It is important toobtain a specific conductance measurement soon after taking a samplesince temperature changes, precipitation reactions, and absorption ofcarbon dioxide from the air all affect the specific conductance.

2.0 APPLICABILITY

This guideline is applicable to all aqueous samples such as potable wellwater, monitoring well water, surface water, leachate, drummedwastewater, and other water samples.

3.0 DEFINITIONS

Resistance - The inability of a substance to conduct acurrent. For metals and solutions, theresistance is defined by Ohm's Law, E = IR,where E is the potential difference, I is thecurrent, and R is the resistance.

Cpnductance - The reciprocal of the resistance, I/R.

Specific conductance - The conductance of a 1-cm cube of electrolyte.Conductivity and specific conductance are usedsynonymously; this SOP will use the term"specific conductance".

4.0 GUIDELINES

Conductivity is a numerical expression of the ability of a water sampleto carry an electric current. This value depends on the totalconcentration of the ionized substances dissolved in the water and thetemperature at which the measurement is made. The mobility of each ofthe various dissolved ions, their valences, and their actual andrelative concentrations effect conductivity.

An aqueous system containing ions will conduct an electric current. Ina direct-current field, the positive ions migrate toward the negativeelectrode, while the negatively charged ions migrate toward the positiveelectrode. Most inorganic acids, bases, and salts (such as hydrochloricacid, sodium carbonate, and sodium chloride) are relatively goodconductors.

Conversely, molecules of such organic compounds as sucrose and benzene,which do not dissociate in aqueous solution, conduct a current verypoorly, if at all.

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The Project Manager is responsible for deciding when a specificconductance measurement should be taken. Details will be given in thesampling plan for the site.

The field samplers are responsible for taking the conductancemeasurement and for reco»d4.ng and reporting the results.

4.2 EQUIPMENT •

The following equipment is needed for taking specific conductancemeasurements:

• HYDAC conductivity with combination polymer body sealed referencepH electrode or equivalent.

4.3 CALIBRATION

Calibration procedures should be in accordance with those specified inthe operations manual for the meter.

4.4 SPECIFIC CONDUCTANCE MEASUREMENT

The steps involved in taking specific conductance measurements arelisted below:

• Immerse the electrode in water overnight. If this is not possibledue to field conditions, immerse the electrode for at least an hourbefore use or keep moist with a wet cottonball.

• Rinse the cell with one or more portions of the sample to betested. ' .

• Immerse the electrode in the sample and measure the conductivity.

• Read and record the results. Adjust the temperature setting to thesample temperature.

If the specific conductance measurements become erratic or inspectionshows that any of the platinum black has flaked off the electrode,replatinization of the electrode is necessary. See the manufacturer'sinstruction for details.

Note that specific conductance is occasionally reported at temperaturesother than ambient.

4.5 RECORDS

All results are to be recorded in the field logbook.

5.0 ATTACHMENTS

Included in Section 5.1 of SOP F-12-C (Temperature Measurement)REV.1993 Page 5

301198

C. TEMPERATURE MEASUREMENT

1.0 OBJECTIVE

This guideline details the steps required to measure the temperature ofan aqueous solution while in the field using the temperature probe or-thermometer. It is impcirta-iyk to obtain a temperature measurement soonafter taking a sample and thus avoid changes in temperature of thesample.

2.0 APPLICABILITY

This guideline is applicable to all aqueous samples such as potable wellwater, monitoring well water, surface water, leachate, drummedwastewater, and other water samples.

3.0 DEFINITIONS

Temperature - The degree of hotness or coldness of a solution or body.

4 . 0 GUIDELINES

The purpose of temperature measurement is to document the consistency oftemperature. A change in temperature may indicate fluctuation in thesource of the solution.

Temperatures must also be measured to properly obtain pH andconductivity measurements.

4.:L RESPONSIBILITIES

Same as previous section. .

4.:> EQUIPMENT

The following equipment is needed for taking temperature measurements:

• HYDAC temperature with combination polymer body sealed referenceprobe or equivalent.

• A thermometer that is approved by the National Bureau of Standards.

4.3 CALIBRATION

To check the temperature instrument, both the probe and a thermometerthat is approved by the National Bureau of Standards is immersed intothe same beaker of water. Any differences in temperature are noted andrecorded in the field logbook.

REV.1993 Page 6

301199

4.4 TEMPERATURE MEASUREMENT

The steps involved in temperature measurements using the probe arelisted below:

• Fill sample cup 2/3 full. If the sample is hot boiling water,allow to cool to 160° F, or below.

• Slide the right hand function switch to TEMP and push the READbutton. If temperature reading is not stable, empty and refill cupseveral times to bring cup and sample to the same temperature.

• Read the temperature on the digital display panel.

4.5 RECORDS

All records are to be recorded in the field logbook.

5.0 ATTACHMENTS

REV.1993 Page 7

301200

EQUIPMENT MANUAL - HYDAC #301353

REV.1993 Page 8

301201

OJoHIOOM

Tes te r with cose. P/N 301353

(includes bat tery , P/N 905531)

pH electrode with BNC connector. P/N 102927

Standard Conductance Solution 1413 micromhosP/N 905770

Buffer Solution Kit

(includes buffer solutions 4, 7 and 10 pH; also

bottle of (distilled) woter for rinse, P/N 102953)

24 Month Warranty

ooI—«

CAMBRIDGE SCIENTIFIC INDUSTRIESMooie lodge Rood Combridge, Maryland 2)613

INSTRUCTION MANUALDIGITAL CONDUCTANCE, TEMPERATUREAND pH TESTER, CATALOG No. 301353

Parameters:Conductance 4 ranges

0 to 20 U /cm0 fo 200 U /cm0 to 2.000 U/cm0 to 20.000 U./cm

Integral sample cup

Accessible internal calibration potentiometerStandard solution available:

500 ml. Bottle of .01 Molar PotassiumChloride 1413 micromhos @ 77° F.

pH 0 to 14 rangeSlope and zero adjustments on face of unitExternal electrode (purchased separately)Buffer solution kit available, includes: .

Buffer solutions, 4, 7 and 10 pHBottle of (distilled) water for rinse

Temperature Otol60DFIntegral sample cup

Accuracy Conductivity ± 2% Full scale at 77°FTemperature ± 2°FpH ± .01 pH units at 77"F

Operating Instructions:

1. Rinse the inside of sample cup with liquid to bemeasured. (This is especially important if samples with a

wide range of conductivity or pH ore to be measured.)

2. Fill sample cup. (see Figure 1),

CAUTION: THE MAIN BODY IS NOT WATER-PROOF

(Do not subject unit to splashing water).

CAUTION: UNIT DESIGNED FOR AQUEOUS SOLUTIONS

3. Fill sample cup at least 2/3 full. If the sample is hot

boiler water, allow to cool to 160°F, or below.

4. Slide the right hand function switch to "TEMP" and push

the "READ" button. If temperature reading is not stable,

empty & refill cup several times to bring cup and sample

to the same temperature.

5. Read the temperature on the digital display panel and

adjust both temperature compensation knobs accord-

ingly.

6. If the approximate conductance is known, slide the left

hand range selector switch to the proper range.

Example: If you expect the sample to be around 2000

micromhos, slide the left hand selector switch to xlOOO.

7. Slide the right hand function switch to "COND" and

push the "READ" button.

8. Multiply the digital display reading by the factor

indicated by the position of the left hand range switch to

determine conductance.

Example: A display reading of 1.00 with the left hand

range selector switch indicc|ing xlOOO is:

1.00 x 1000 or 1000 U /cm

Note: If o single "1" appears on the left hand side of the

digital display, the sample conductance is higher than

the selected range. Slide the left hand (range) selector

switch in one step intervals until a 3 or A digit displayappears.

Conversely, if o decimal display appears (such as 0.11)

move the range selector switch to the left until a 3 or 4

digit number, 1.00 or larger, appears on the display.

This puts the unit in a range affording the best accuracy.

. Caution: A single "1" :always means that the

conductance is higher than the selected range.

9. Slide the right hand function selector switch to "pH".

10. Insert the pH cable connector onto the tester. Push on

and twist clockwise. .

11. Remove the tape from the plastic storage cap.

12. Remove the plastic storage cap slowly.

13. Place the pH electrode \n the sample cup or anynon-metallic container holding the remainder ol thesample to be measured. II you use the tester's samplecup, you will have to hold the electrode.

oHfooto

H. Press the "READ" button: pH value will appear on the

digital display.

15. Always obtain conductivity reading before placing pH

probe in sample cup. pH probes tend to carry contam-ination over into the sample.

CAUTION:The main body is not waterproof.

FIGURE 1

CONDUCTIVITY CALIBRATION

IHDVI.W FIGURE 2

(Adjuilm*nl)

(Not* Hot* it normally C0v«f *d by O blocV plug)

CALIBRATION

Temperature and Conductance ore factory calibrated.

You may check conductance accuracy with a solution .of

known conductance and recalibrate, if necessary.

See Figure 2. to recalibrate conductance, remove black

plug revealing the adjustment potentiometer screw.

Add standard solution to cup, discard and refill. Repeatprocedure until the digital display indicates the same

value twice in a row. Adjust the potentiometer until the

digital display indicates the known value of conduc-

tance. To increase the digital display reading, turn the

adjustment potentiometer screw counterclockwise (clock-

wise to decrease). '

To standardize the pH electrode and meter, place the pH

electrode in the 7.0 buffer bottle. Adjust the "ZERO"

potentiometer on the face of the tester so that the digital

display indicates 7.00.

Then place the pH electrode in the 4.0 or 10.0 buffer bottle

(depending on where you expect the actual measurement

to be). Adjust the "SLOPE" potentiometer on the face of the

tester so that the digital display indicates the value of the

buffer chosen.

NOTE: There is interaction between the "ZERO" and

"SLOPE" adjustments, so the procedure should be repeated

several times. ;

woH10OUl

DO NOT SUBJECT THE pH ELECTRODE TO FREEZINGTEMPERATURES!

It is good practice to rinse the electrode, in distilled waterwhen going (rom one buffer to another. When not in usethe cop should be kept on the electrode. Keeping the cottonin the cap moist will keep the electrode ready to use.Moisten the cotton frequently (once a week, usually).

Maintenance

Battery replacement

The battery is located behind the snap-off cover on thebottom of the tester. Use o small tool to pop out the cover.Replace battery with a 9 volt; on alkaline battery such asDurocell MN 1604. Replace the battery whenever "LOBAT" appears on the display.

Sample cup:

The carbon electrodes in the cup may be cleaned with amild abrasive, 400 grit or finer on the end of the flatsurface.

SPECIAL NOTE: To avoid ever having to resort to harshermethods of cleaning, when rinsing cup out with liquid to bemeasured, wipe cup with paper towel or Kleenex and rinseagain.

Wipe cup after every sample and rinse with tap water whenpossible.

Conductivity electrodes

Temperature-Sensor

Sample cup

Digital display

.^Temperature compensation

S*/ knobs

pH zero adjustment

pH slope adjustment

Read buttonRange selector

Function selector

ji—Conductivity CalibrationAdjustment

pH Electrode Connector

pH electrode

IIIIIII4II

HOW TO USE YOUR POLYMER BODY, SEALED REFERENCE COMBINATION p_H ELECTRODE

Your new polymer body combination electrode affords a unique ease of use. Because the pH bulbis recessed inside the polymer body, the electrode can be allowed to rest against the bottomof a'beaker without damaging the glass bulb. In many measurements this recessed bulb designeliminates the need for electrode holders and the electrode actually can be used as a stirringrod. The sealed reference design eliminates the need to add filling solutions, and minimizesreference dryout.

HELPFUL OPERATING TECHNIQUES

1. As shipped, the electrode tip is covered by a protective cap which serves both to keep thereference from drying and to prevent breakage. This cap is a snug fit and it contains apressure relief hole to facilitate removal and installation. As supplied, this hole iscovered by a piece of vinyl tape to retain moisture inside the cap. Before removingor reinstalling this cap, the tape must be removed to expose the pressure relief hole.

2. During shipment, the air pocket in the electrode's stem may move into the bulb area. Ifbubbles are seen in the bulb area, hold the electrode by its cap and shake downwards asis done with a clinical thermometer.

3. Vigorously stir the electrode in the sample, buffer or rinse solution. This action willbring solution to the electrode's surface more quickly and improve speed of response.

4. After exposure to a sample, buffer or rinse solution,, shake the electrode with a snapmotion to remove residual drops of solution. This action will minimize contaminationfrom carryover.

5. As a rinse solution, use a part of the next sample or buffer which is to be measured. Thisaction also will minimize contamination from carryover. \ '

6. When calibrating, use a buffer close in value to that expected from the sample. This actiowill minimize any span errors.

7. Keep buffers and samples at the same temperature. This action will eliminate the need tocorrect values for temperature effects. .

8. pH readings stabilize faster in some solutions than others; allow time for the reading tostabilize. In general, buffers provide stable readings in several seconds (tris bufferstake somewhat longer) while samples usually take longer.

9. Keep in mind that all pH electrodes "age" with time. Aging is characterized by shortenedspan and slower speed of response. The pH meter "slope" (span) control can be adjusted tocompensate for electrode span errors but will not affect speed of response. When theslope control can no longer be adjusted to compensate for the span errors, the electrodeshould be cleaned and/or reconditioned. If reconditioning does not restore performance,the electrode should be replaced.

. CALIBRATION

The frequency of calibration is a function of both the electrode and the pH meter. They shoulbe calibrated together with the calibration frequency determined by experience. The followingstep-wise procedure has been found useful:

1. Remove the vinyl tape from the electrode's protective cap to open the pressure relief holeand then remove and save the cap.

2. Vigorously stir the electrode in a rinse solution. :

3. Shake the electrode with a snap action to remove residual drop of solution.4. Vigorously stir the electrode in a 7.0 buffer and allow the electrode to rest against the

beaker1s side. . .5. Allow the reading to stabilize and use the pH meter zero adjustment to make the meter reac

the buffer value (remember to adjust to the buffer's pH value at the temperature of the• buffer).

6. Repeat steps 2 & 3.7. Vigorously stir the electrode in a second buffer whose value is near that expected from

the sample, and allow the electrode to rest against the beaker's side.8. Allow the reading to stabilize, and use the pH meter slope adjustment to make the meter

read the 'buffer value (remember to adjust to the buffer's pH value at the temperatureof the buffer).

9. Repeat steps 2 thru 5, and then repeat steps 2 & 3 and 7 & 8. It may be necessary towork back and forth between the two buffers several times to secure adjustments which donot require changing between buffers.

10. If the unit is in frequent use, with the same electrode, steps 7 & 8 (slope adjustment)need not be repeated more than once a day, but steps 2 thru 5 should be repeated foreach group of readings.

I 301206

iPERATION

erating steps are similar to calibration procedures and are as follows:

Remove the vinyl tape from the electrode's protective cap to open the pressure reliefhole and then remove and save the cap.Vigorously stir the electrode in a rinse solution.Shake the electrode with a snap action to remove residual drops of solution.Vigorously stir the electrode in the sample and allow the electrode to rest against thebeaker's wall. .. .. .Allow the reading to stabilize and then take the reading.Repeat these steps for each sample determination.Between readings, place the electrode in a beaker containing about 2 cm (1 inch) of distilled

" or tap water.

ELECTRODE STORAGE

When pH readings are made infrequently, for example, several days or weeks apart, the elec-trode can be stored simply by replacing its protective cap. Make certain that the cotton insidethe cap is wet (use distilled water), that the cap pressure relief hole is open and slowlyush the cap into position. Then, cover the hole in the cap's side with a piece of tape. Forery long term storage, taping the top of the cap to the electrode's body will provide addi-ional protection against water loss.

LECTRODE CLEANING

IIIIII

oating of the pH bulb can lead to erroneous readings including shortened span. The type ofcoating will determine the cleaning technique. Soft coatings can be removed by vigorousstirring or by use of a squirt bottle. Organic chemical or hard coatings should be chemically

•removed. In no case should the bulb be mechanically cleaned, because abrasion can lead to( permanent damage.

RECONDITIONING • ' ' . • ;

•When reconditioning is required due to electrode aging (see Helpful Operating Techniques,Part 9), the following chemical treatments should be tried. They are presented in the orderof the severity of their attack on the pH glass.

:OTE: .Use proper precautions when handling these hazardous chemicals.

1. Immerse the electrode tip in 0.1N HC1 for 15 seconds, rinse in tap water and thenimmerse tip in 0.1N NaOH for 15 seconds and rinse in tap water. Repeat this sequenceseveral times and then recheck electrode performance. If performance has not beenrestored, try Step 2.

2. Immerse the tip in a 20% solution of NH/F.HF (ammonium bifluoride) for 2 to 3 minutes,rinse in tap water and recheck performance. If performance has not been restored,try Step 3.

3. Immerse electrode tip in 10% HF for 10 to 15 seconds, rinse well in tap water, quicklyrinse in 5N HC1, rinse well in tap water and recheck performance. If performance hasnot been restored it is time to get a replacement electrode.

HI835-1

I 301207

PROCEDURE F-13

HAZCO SERVICES, INC.HORIBA MODEL U-10 WATER CHECKER

301208

H O R I B HModel U-10

Instrument Manual

HAZCO Services, Inc.

301209

301210

IMHHUCTION- MANUALfor

u-ioWESEQUALITY CHECKER

I: OCTOBER 1990

fefeed October 199T

HORIBA INSTRUMENTINCORPORATES

HORIBA INSTRUMENTS INC.17671 ARMSTRONGIRVINE INDUSTRIAL COMPLEXIRVINE, CALIFORNIA 92714TELEPHONE 714/250-4811

WATERQUALITY

CHECKER

301211

WARNING

The DO sensor contains a strong alkalinesolution. Should any of this solution comein contact with your clothing or skin, washit away immediately with plenty of water.

Be especially careful not to allow anyof the alkaline liquid in the DO sensor toget in your eyes.

301212

The U-10 Water Quality Checker isa state-of-the-art instrument forsimultaneous multiparameter,.___measurement of water quality. TheHORIBA U-10 measures six .different parameters of watersamples: pH, conductivity, turbidity,dissolved oxygen, temperature, andsalinity.

The U-10 is compact enough tobe held .in one hand while takingmeasurements. It has a large easy-

. to-read LCD readout.Measurements are taken simply byimmersing the probe right into thewater sample.

The U-10 is extremely versatile' and sophisticated, yet easy to use. .You will find it a valuable addition toon-site water control operations,whatever your needs-from testingfactory discharges to urbandrainage, river water, lake and

' marsh water, aquatic culture tanks,agricultural water supplies, and sea .water.

To get the most out of your U-10Water Quality Checker, please readand this Instruction Manual carefully..before you begin to takemeasurements.

Note that Horiba cannot be heldresponsible for any equipmentmalfunction or failure should theU-10 Water Quality Checker beoperated incorrectly or in a mannerother than specified in thisInstruction Manual.

Horiba's aim is to produce thebest possible equipment anddocumentation for our products. Wewelcome comments, questions, orsuggestions for improvementconcerning both our products andthe accompanying documentation,such as this Instruction Manual.

© Copyright 1991, Horiba, Ltd.No portion of this Instruction Manual.may be reproducedin any form without written permission from Horiba,Ltd.Note that the contents of this Instruction Manual aresubject to change without prior notice as designchanges are made on the instrument. First edition: July, 1991

301213

Section

IIIIII

Section 2

Section 3

CONTENTS

Getting StartedConfiguration of the U-10The Readout •The Keypad

• Setting up the U-10Inserting the DO sensorInserting the batteryAttaching the carrying strap

Making MeasurementsHow to make a measurement •Initial readoutSelect the parameter you wantshown on the readout •••

. Expanded readoutMeasuring fresh waterMeasuring salt waterAfter measurement:Cleaning and storing the U-10

Calibrating the U-10Auto-calibration procedureManual (2-point) calibration procedures

pH Calibration •1. Zero calibration • • • • •2. Span calibration •

COND Calibration—' •1. Zero calibration •2. Span calibration •

TURB Calibration1. Zero calibration •2. Span calibration

DO Calibration1. Zero calibration2. Span calibration

24688910

14151617

2023242425262829303131323333

I 301214

Section 4 Data Storage arid PrintoutStorage • • 36Recall • • • • • • 38Delete ••- '• • 40Printing out .••'.—•..•..••••. 41

Section 5 Daily Maintenance and TroubleshootingError codes • • • • • • • • • 44Normal probe maintenance • 47Replacing faulty sensors • • • • • 49Replacing a faulty probe •:••• 50

Section 6 Reference Materials .Conductivity • • • • • • 54Turbidity • • • 58Salinity ••• 60Temperature • • • • • • •• 60Dissolved-oxygen • • 61pH • • •••• • 63Specifications • • - • • • • • • 65Parts list • • 68

Unpacking the U-10 • 69Precautions when using the U-10 • • • • • 70

Contents of Tables

Table 1 Accuracy of expanded readout 15

Table 2 pH values of standard solutionsat various temperatures •• • • • • • • • ; • • 25

Table 3 Making the potassium chloridestandard solution •• •• 27

Table 4 Amounts of saturated dissolvedoxygen in water at various •temperatures • 34

301215

Section

Getting Started

This sectiomS&Sffi&es an overview of the U-10. It then shows how to set upthe your U-HSSfSaserting the DO sensor and the battery. Finally, it listsimportant picssslfas to be taken when using your U-10 Water Checker.

Son of the U-10 • • • • 2suit • •• • • 4

B>B B m p

U-10 • -•• • 8Insertmtfi&'DO'sensor •• • 8Insertintinfribattery • • 9

^'carrying strap •••: 10

301216

2 Configuration

Configuration of the U-10

Main unit

Cover for printer port

Printer port

Readout LCD

Keypad

Cable connector

Section 1

301217

Configuration 3

DO ''sensor (removable)

COND "i sensor (non-rerrcvEb'e)

Reference sensor (removable)

TEMP "3 sensor (non-remcvcble)

pH sensor (removable)

TURB ••• sensor

(non-removable)

Probe guard

' *1 DO*2COND•3 TEMP*4TURB

Dissolved oxygenConduectivityTempratureTurbidity

Section 1

301218

Configuration

The Readout

The readout is an easy-to-read LCD. The readout has two mainfunctions: (1) it displays the results of measurements, and (2) itserves as a message board to show the operating status of theU-10.

.© Data input/output

(2) MEAS or MAINT modes

Data displayed inMEAS mode

Parameters measured(Upper cursor)

(5) MAINT Sub-Modes(Lower cursor)

.OUT IN <

O Q u mV

AUTO.. ZERO. SPAN _..JN_...QUT...SiSE.TCAL — DATA —

Data input/output

OUT] Data output

Data input

MEAS or MAINT modes

The U-10 may be in one of two modes:Measurement (MEAS) mode or Maintenance mode.

the U-10 is ready to make 6-parametermeasurements

the U-10 is ready for other operations, e.g.,calibration, data input/recall, or salinity setting

Section 1

301219

Configuration

(3) Data displayed in MEAS mode

• 6-parameter results:pH, conductivity, turbidity, DO, temperature, and

• salinity• Designated value for salinity setting• Error codes

Parameters measured -

Vaiue displayed on readout is highlighted by uppercursor.

pH j pH

COND; Conductivity

TURB: Turbidity

DO i Dissolved-Oxygen

TEMPj Temperature

SAL I Salinity

MAINT Sub-Modes

One of six Sub-Modes selected is highlighted by lowercursor.

AUTO! Automatic 1-point calibration

ZERO: Manual zero calibration

SPANJ Manual span calibration

Data inputIN

OUT | Data output (recall)

S.SETJ Salinity setting correction

Section 1

301220

Configuration

The Keypad __

The U-10 is operated by the keypad on the main unit, which haseight surface-sealed keys, as illustrated.

Power Key

Parameter-Select Key

Mode Key

Expanded-Readout Key

Enter Key V-^ \^ V~^ UP/DOWN

/^\7^ r^y KeysClear Key

Section 1

Power Key (POWER)Turns the main unit ON/OFF.

When this key is pressed to turn the U-10 ON, thereadout comes in the MEAS mode, showing theparameter last displayed in the previous measurement.If the U-10 is left with the power ON for 30 minuteswithout any of the keys being activated operated, thepower will be turned OFF automatically.

Parameter-Select Key (SELECT)Use this key to move the upper cursor to the measuredparameter you want to show on the readout. It togglesthrough the six parameters in order:

-jCONDh-~[TURB!—-j DO j-^JTEMPJ—-j SAL

Mode Key (MODE)Toggles back and forth between MEAS and MAINTmodes. When in the MAINT mode, this key toggles thelower cursor through the six maintenance Sub-Modes.

AUTOr IN OUT

301221

Configuration 7

Exp.andedrReadout Key (EXP) 'Toggles between (1) standard.readout value and (2)expanded readout, for greater resolution, with decimalpoint moved one digit to the left. •

Enter Key (ENT)This acts like the RETURN Key or Enter Key on a.computer keyboard. The U-10 Enter. Key has four mainfunctions, depending on which mode the unit is in.

1. In.the AUTO Sub-Mode: Press this key to startautomatic calibration.

2. In either the ZERO or SPAN Sub-Modes: Used inmanual calibration to set the value for the standardsolution being used.

3. In the IN Sub-Mode: Inputs data being measured tomemory.

4. In the OUT Sub-Mode: Recalls values from one ofthe 20 Data-Set Nos. that is now shown on thereadout. Prints data when a printer is connected.

Clear Key (CLR)This acts like the ESCAPE Key on a computerkeyboard. It has three main functions, depending on 'which mode the unit is in.

1. In the AUTO Sub-Mode: Aborts the auto-calibrationnow in progress.

2. In the IN Sub-Mode: Deletes data in memory fromall 20 Data-Sets..

3. When the readout shows an error code: Clears theerror code from the readout.

UP/DOWN keys ' .Use these keys to select values when in one of theMAINT Sub-Modes. They have two main functions.

1. In either the ZERO or SPAN Sub-Modes: Usethese keys to select value for the standard solution.

2. In the OUT mode: Used to toggle through the 20Data-Set Nos. to select the one you wish to recall.

Section 1

301222

8 Setting up

Setting.up the U-10

Inserting the DO sensor

WARNING

The DO sensor contains a strong alkaline solution.Should any of this solution come in contact with your clothingor skin, wash it away immediately with plenty of water.Be especially careful not to allow any of the liquid in the DOsensor to get in your eyes.

The Dissolved-Oxygen (DO) sensor has a delicate membranethat can easily be ruptured. For safety's sake, the U-10 is shippedto you with the DO sensor packed separately. You should insertthe DO sensor when you unpack your U-10 unit.

1. Make sure that the DO sensor has the correct O-ring, asshown. •

2. First, fit the DO. sensor lightly into its socket, and then put onthe probe guard to align it correctly.

3. Then, tighten the DO sensor securely to the probe body.When doing this, be especially careful not to damage themembrane, which is located in the front of the DO sensor....

O-ring

DO sensor

Probe guard

Section'1

301223

Setting up 9

Inserting the battery

The U-10 is shipped from the factory with the battery packedseparately.

The battery may be inserted by loosening the set-screw on thebattery cover and pulling up the cover. Make sure that the plusand minus poles of the battery match the terminals correctly.

If the readout shows the message Er ',, it means that thebattery is defective or exhausted and should be replaced.

If you are replacing the battery-and already have data stored inthe U-10 memory that you wish to save, be sure to turn OFF thePOWER Key before you remove the old battery. This will assurethat data stored in memory will be maintained by the internalbackup battery.

Tongues

Battery cover

Battery*

Grooves

Setscrew

Use the 9V-battery.

Section 1

301224

10 Setting up

Attaching the carrying strap

Hook both ends of the strap through the metal fitting on back ofthe main unit, as illustrated.

Battery cover

Metal fitting

Rear of main unit

Section 1

301225

Section

Making MeasurementsMaking a measurement with the U-10 Water Checker is extremely simple. Justturn on the power and place the probe in the sample of water you wish tomeasure.

All six parameters are measured simultaneously.These parameters may be stored in memory, printed out, pr viewed one-by-oneon the LCD readout. For printing and data storage, see the appropriatesections following this one. To view the parameters .one-by-one on the readout,use the SELECT Key to toggle the upper cursor through them.

While the U-10 is both rugged and precise, the key to accuratemeasurements is cleanliness and frequent calibration. It is essential to cleanthe U-10 thoroughly after each measurement, and it is recommended that youre-calibrate your U-10 as frequently as possible. For best results, you shouldrecalibrate it before each measurement session. Cleaning and calibrationprocedures are described below in this section and in the following one.

How to make a measurement • 12

Initial readout • 13Select the parameter you want shown on the readout ••• 14

Expanded readout • • • • • • • • • • 15Measuring fresh water •• 16

Measuring saltwater ? '••• 17After measurement: Cleaning and storing the U-10 18

301226

12 Make a measurement

How to make a measurement

Turn the power on1

Gently place the probe into the water sample.

Basically, that's all there is to it: just turn it on andput the probe in the sample. Of course, the U-10 cando many sophisticated things with the sample data, andfor best results, you should be careful about calibratingthe unit and maintaining it in good condition. This isexplained in detail below and in the next section.

Be careful!Never drop or throw the probe into the water. Itis a precision instrument.containing five delicatesensors and five pre-amps; you can damage itbeyond repair by unnecessarily rough handling.

Section 2

301227

Initial readout 13

Initial readout

When you first turn the power on, the U-10 will be in theMEAS mode, the readout will look like this, with all the.LCD segments activated.

U U i-PmVmg/l

' pmS/cmSELECT

MODE23 BQZB ECQ1

After about two seconds, the readout will change toshow that a new measurement is being made. Thereadout will show the last parameter that the uppercursor was on when the previous measurement wasmade, i.e., pH as illustrated here.

MEAS I i 't Z****!

\ F~pH f <^—KUB COND

AUTO ZERO

..LfTURB • DO

njTEMP

SPAN INU" 1

(Expanded readout shown)

The display of the decimal point in the readoutmode will also be in the same format as was selectedwith the EXP Key in the previous measurement, i.e.,standard or expanded (as illustrated here).

Section 2

301228

14 Select the parameter

Select the parameter you want shown on thereadout "" .

All six parameters are automatically measured at once.Use the SELECT Key to toggle the upper cursor to theparameter you want. .

pH :pHCOND -.ConductivityTURB -.Turbidity .

DO : Dissolved oxygenTEMP : Temperature

SAL /Salinity .

To get a uniform reading, slowly move the probe upand down to circulate the water through it. (Move it 1 .foot (30 cm) per sec.) Then wait for the readout to.stabilize while doing this.

Section 2

301229

Expanded readout 1 i5

Expanded readout

Use the EXP readout mode v/hen you wish to see theresults with one additional decimal place of accuracy.The EXP Key toggles the readout back and forthbetween standard to expanded display. The tablebelow shows the result of using the EXP readout modefor each of the six parameters.

Table 1. Accuracy of expanded readout

Parameter

TEMP .

Range of

measurement

0-1 4 pH

0-1 mS/cm1-10 mS/cm

10-100 mS/cm

0-800 NTU

0-1 9.9 mg//

0-50°C

Accuracy

Standardreadout

0.1 pH

0.01 mS/cm0.1 mS/cm1 mS/cm

10 NTU

0.1 mg//

Expandedreadout

0.01 pH

0.001 mS/cm0.01 mS/cm0.1 mS/cm

0.01 mg//

0.1°C

Note that the salinity parameter is the only value not measured directly with itsown sensor. The U-10 obtains salinity by converting the conductivity value. Iflarge amounts of conductive ions other than salt-water components are present inthe sample, an error may occur. Be cautious when interpreting the salinityresults.

Section 2

301230

16 Fresh water/salt water

Measuring fresh water or salt water?

The U-10 can be set to the salinity for either fresh water or saltwater when measuring DO. This is done by using the S.SETSub-Mode.

Measuring fresh water

First, use the MODE Key. to put the U-10 in the MAINTmode. Keep pressing the MODE Key to toggle thelower cursor to the S.SET Sub-Mode,

Once you are in the S.SET Sub-Mode, use theUP/DOWN Keys to select the salinity value. For freshwater, set the salinity to 0.0%. '

Section 2

MAINT n nU.Lf

SELECTPH COND TURB DO TEMP SA

MODE •AUTO ZERO SPAN IN OUT

CAL — DATA —

Finally, press the ENT Key to complete the salinitysetting while in the S.SET Sub-Mode.

When the salinity setting has been made, switch backto the MEAS mode by pressing the the MODE Key.

301231

Fresh water/salt water 17

Measuring salt water

First, use the MODE Key to put the U-10 in the.MAINTmode. Keep pressing the MODE Key to toggle thelower cursor to the S.SET Sub-Mode.

For salt water, set it to R 'i.e., for auto-salinity.The f? setting should be sufficient for measurements

of normal sea water with a salinity value close to 3.3%.For sea water of an unusual salinity, however, andwhere the value is otherwise known, you may wish setthe value manually to any salinity within the range of0.0%-4.0%. (You may also possibly want to use amanual setting if, for example, the COND sensor ismalfunctioning but it is still desirable to take readings ofthe other parameters.)

Finally, press the ENT Key to complete the salinitysetting while in the S.SET Sub-Mode.

When the salinity setting has been made, switch backto the MEAS mode by pressing the the MODE Key.

Section 2

301232

18 After measurement

After measurement: Cleaning and storing theU-10

Turn OFF the'power. •Wash the probe thoroughly with tap water. Be sure

to flush off all of sample solution from the probe.

Storing the U-10 for brief periods, I.e., about 1 weekor less:

Fill the calibration beaker with tap water and fit theprobe over it. - , •

For longer storageThe pH sensor must always be kept moist. Fill the

small rubber cap with water and use it to cover the pHsensor.

The KCI internal solution in the pH reference sensormay seep out over time. Place vinyl tape around the0-ring portion to prevent this.

If you are going to store the U-10 for a prolongedperiod without using it, remove the battery from themain unit. .

Section 2

301233

Section

Calibrating the U-10The U-10 Waler Checker may be calibrated either manually or automatically.The 4-parameter auto-calibration procedure, is quite handy and should besufficient for most measurement operations.Manual calibration for each of the four parameters is more accurate but, ofcourse, also more time-consuming. This method should.be used for difficultmeasurements or where more than normal precision is required. The manualcalibration procedure is explained-below in detail, following the description oft h e auto-calibration procedure. . . .The auto-calibration procedure is extremely simple. The U-10 Water Checkeruses just a single solution to do a simultaneous calibration of four parameters:pH, COND, TURB, and DO. Your U-10 comes with a bottle of standardphthalate pH solution and a calibration beaker for this purpose.

Auto-calibration procedure • • • • 20

Manual (2-point) calibration procedures • ••• 23

pH Calibration • • • • • 241.Zero calibration ••• • 242.Span calibration • •• .25

COND Calibration •'••• ••• 26

1.Zero calibration •- • • • • • • 282.Span calibration • •••' 29

TURB Calibration •• 30

LZero calibration • • • • • • • 31

2.Span calibration ; 31

DO Calibration • •• 32LZero calibration ••• •• 332.Span calibration 33

301234

20 Auto-calibration

Auto-calibration procedure

Section 3

Fill the calibration beaker to about 2/3 with the standardsolution. Note the line on the beaker.

Fit the probe over the beaker, as illustrated. Notethat the beaker is specially shaped to prevent the DOsensor from being immersed in the standard solution.This is because the DO auto-calibration is done usingatmospheric air.

Calitra:i

With the power on, press the MODE Key to.put the unitinto the MAINT mode. The lower cursor should be onthe AUTO Sub-Mode; if it is not, use the MODE Key tomove the lower cursor to AUTO.

With, the lower cursor on AUTO, press the ENT Key.The readout will show L Hi. Wait a moment, and theupper cursor will gradually move across the four auto-calibration parameters one-by-one: pH, COND,' TURB,and DO. When the calibration is complete, the readoutwill briefly show End and then will switch to the MEASmode.

The upper cursor will blink while the auto-calibrationis being made. When the auto-calibration hasstabilized, the upper cursor will stop blinking.

301235

Auto-calibration 21

ricai' 1 1 \

fcritv:

r oL ' I

-CONO urns co

ZEnO SPAN IN

)i_TcMP SAL

CUT S.5JT

r. nL H

ZERO SPAN INCH — -

i_TEMP SAL

CUT S.ScT-.-.-

; /_/;L ML-^rt'ofCT

DC TEMP SAL

• HGC=•Ein3 ZERO SPAN IN CUT S.S5T

L n LZtaO SPAN IN CUT S.SET

t nEH ESS EEID EH

ET^ZERO SPAN IN

/ int.u

CONO TURB DO

ZERO SPAN IN

TEMP SA

CUT S.SET

First, pH is being auto-calibrated

Then, COND is being auto-calibrated

Next, TURB is being auto-calibrated

Finally, DO is being auto-calibrated

Auto-calibration now ends

And the readout switches to the MEASmode

Note: If you wish to abort the auto-calibration forany reason, press the CLR Key. Theparameters auto-caiibrated so far will be inmemory.

Section 3

301236

212 Auto-calibration

Auto-calibration' error

After the DO auto-calibration, if the unit does not switqhto the MEAS mode as it should, and the readout showseither E<-3 or 5^4 , an auto-calibration error hasoccurred. Parameters will blink where an erroroccurred.

:HVTS£' / /• i \c

c _ mL * ^

•**ci cr*TW«10l»i I'l:]:! RiiiM TEMP

ZERO SPAN IN OUT• CAL — DATA —

pH auto-calibration error

If this happens, re-do the auto-calibration. First, pressthe CLR Key to cancel the error code.

U _< _<f.L _.'

SELECT :'•ill COND TURB DO TEMP SA

MODEZERO SPAN

- CALIN OUT S.SET

— DATA —

Then press the ENT Key to re-start the auto-calibration.Restart the auto-calibration beginning again with pH.

Section 3

301237

2-point calibration 23

Manual (2-point) calibration procedures

For normal measurements, the 4-parameter auto-calibrationdescribed above is sufficiently accurate. However, you may wishto do a parameter-by-parameter, 2-point manual calibration ofone or more of the four parameters. This is recommended eitherfor high-accuracy measurements, especially v/hen using theexpanded readout mode. It is necessary if a new probe is beingused for the first time.

Parameters to'be calibrated manually.

|W . SP£n

' I— ZeroTURB

'— Span

• I— Zero• : DO

' ' . ; '— Span

Section 3

301238

24 pH calibration

pH calibration

1. Zero calibration

Wash the probe 2-3 times, using de-ionized or distilledwater. Place it in a beaker of pH 7 standard solution,i.e., a neutral phosphate standard solution.

1. With the power on, press the MODE Key to put theunit into the MAINT mode.

2. Press the MODE Key again to move the lowercursor to ZERO.

3. Use the SELECT Key to move the upper cursor topH.

4. When the readout has stabilized, use theUP/DOWN Keys to select the value of the pH 7standard solution at the temperature of the sample.Refer to Table 2 for pH values of standard solutionsat various temperatures.

MAINT c o cPH U.ULf

SELECT••3UI CONO TURB DO TEMP SA

MODEAUTO til-M SPAN IN OUT S.SET

CAL — DATA —

5. Press the ENT Key to complete the zero calibrationforpH.

Section 3

301239

pH calibration 25

2. Span calibration

Again, wash the probe 2-3 times in de-ionized ordistilled water. This time, place it in a beaker of eitherpH4 or pH9 standard solution.

1. Use the MODE Key to move the lower cursor to SPAN.

2. As in Step 4. above in zero calibration, when thereadout has stabilized, use the UP/DOWN Keys toselect the value of the standard solution (i.e., eitherpH4 or pH9) at the temperature Of the sample.Again, refer to Table 2 for pH values of standardsolutions at various temperatures.

3. Press the ENT Key to complete the spancalibration for pH.

MAINT / I / I

pH ~f.UEUI COND TURB DO

AUTO ZERO pi-JHl IN

OUTDATA-

Table 2 pH values of standard solutions at various temperatures*

Temperature

'C / F°

07 325 / 41

107 50157 5920 / 6825 / 7730 / 86357 954 0 / 1 0 4457 113

1.671.671.671.671.681.681.691.691.701.701.71

4.014.014.004.004.004.014.014.024.034.044.06

6.986.956.926.906.886.866.856.846.846.836.83

9.469.399.339.279.229.189.149.109.079.049.01

10.3210.2510.1810.1210.0610.01

9.97. 9.93

9.899.869:83

13.4313.2113.0012.8112.6312.4512.3012.1411.9911.8411.70

a: oxalate, b : phthalate, c : neutral phosphate, d : borax,e : carbonate, f: Sat.calcium hydroxide solution' These pH valves are lor Japanese standard solutions. Should you prefer to use

different standard solutions, be save to make the proper adjustments in calibration.Section 3

301240

26 . COND calibration

COND calibration

The U-10 can measure conductivity in the range of 0-100mS/cm. Depending on the sample concentration, however,the U-10 automatically selects the proper range out of itsthree possible ranges of 0-1 mS/cm, 1 -10 mS/cm, and 10-100 mS/cm.

Therefore, if you are doing a manual calibration forCOND, this must be done for each of the three ranges.However, since the zero point is common for all threeranges, only the three one-point span calibrations need bedone separately. . • . •

Section 3

301241

CON D calibration 27

Preparing the standard solution for CONDspan calibration

This procedure uses a potassium chloride standardsolution. For greater accuracy, the solution should befreshly prepared each time. If it is unavoidable to use astored solution, be sure to keep it tightly capped in apolyethylene or hard glass bottle. The shelf life of thissolution is six months. Date-stamp the bottle forreference. Never use a KCI standard solution that hasbeen stored for more than six months: the calibrationaccuracy may be adversely affected.

Use potassium chloride powder of the best qualitycommercially available. Dry the powder for two hours at1053C, and cool it down, in a desiccator. Weigh out anappropriate amount of dried and cooled potassiumchloride powder according to the table below. Make thepotassium chloride standard solution as shown.

Table 3 Making the potassium chloride standard solution

KCI standardsolution

0.005N0.05N0.5N

Conductivity'mS/cm

0.7186.67

• KCI weight9

0.3733.73

. 37.28

Range to becalibrated

0-11-10

1 0-1 00

* Temperature of solution: 25°C

To prepare the standard solution, use a 1-litervolumetric flask. First, dissolve the KCI in a smallamount of de-ionized or distilled water. Then fill theflask with de-ionized or distilled water up to the 1-literline. Finally, shake the solution to mix it thoroughly.

Section 3

301242

28 COND calibration

1. Zero calibration

Wash the probe 2-3 times, using de-ionized or distilledwater. Shake the probe to remove any water dropletstrom the COND electrode. Then allow it dry to dryexposed to fresh air.

(MODE) 1. • Use the MODE Key to move the' lower cursor toZERO. . ' . ' . . .

(SELECT) 2. ' Use the SELECT Key to move the upper cursor toCOND.

(A) 3- Use the UP/DOWN Keys to set the readout to 0.0

MAINT n n n.u u umS/cm

. .-— SELECTpH lMi\i} TURB DO TEMP SA

AUTOMODE •

SPAN IN OUT S.SET— DATA—

4. Press the ENT Key. This completes the zerocalibration for COND.

Section 3

301243

COND calibration 29

2. Span calibration

Once again, wash the probe 2-3 times using de-ionizedor distilled water. Following this, wash it a further 2-3times in the KCI standard solution you have prepared.Then place the probe in a beaker of the KCI solutionmaintained at a temperature of 25±5°C.

1. Use the MODE Key to move the lower cursor to SPAN.

2. After the readout stabilizes, as you did for the pHcalibration, use the UP/DOWN Keys to select setthe value of the KCI standard solution, referring tothe KCI table.

Press the ENT Key to. complete the spancalibration for this COND range.

Repeat this procedure for the three ranges, usingeach of three values of KCI standard solutions.

Section 3

301244

30 TURB calibration

TURB calibration

Wash the probe 2-3 times, using de-ionized or distilledwater. For the span calibration, use a prepared spansolution. For the turbidity zero calibration, use de-ionized ordistilled water.

Preparing the standard solution for TURBspan calibration

1. Weigh out 5.0 g of hydrazine sulfate.2. Dissolve this in 400 ml of de-ionized or distilled

i water.3. Then weigh out 50 g of hexamethylenetetramine,

and dissolve it in 400 ml of de-ionized or distilledwater.

• ' • 4. Mix these two solutions, add enough de-ionized ordistilled water-to make 1,000 ml, and stir the mixedsolution thoroughly.

5. Allow this solution to stand for 24 hours at atemperature of 25±3°G.

The turbidity of this solution is equivalent to4000 NTUs. The shelf-life of this solution is sixmonths; i.e., this 4,000-NTU value will remainaccurate for a maximum of six months.

Each time you carry out this calibration, it isnecessary to dilute the 4,000-NTU standard. .

[ solution to prepare an 800-NTU standard solutionfor calibration. To do this, measure out 50 ml ofthe 4,000-NTU solution into a 250-m/ measuring

I. flask.

It is recommended that you use a rubberpipette aspirator for this. Then add de-ionized or

. distilled water up to the 250-m/ line.I . The standard solution used here for the

turbidity calibration will precipitate easily.. Therefore, be sure to stir the solution thoroughlyI before use.

Section 3

301245

TURB calibration 31

1. Zero calibration

Wash the probe thoroughly 2-3 times using de-ionizedor distilled water. Shake off excess water droplets, andthen place it in a beaker of de-ionized or distilled water.

(MODE) 1. Use the MODE Key to move the lower cursor to^-S ZERO.

4. Press the ENT Key to complete the zero calibrationfor TURB. - .

2. Span calibration

Wash the probe thoroughly, using de-ionized or distilledwater. Shake off excess water droplets. Then place itin a beaker of the 800-NTU solution you have preparedfor this purpose. •

1. Stir this 800-NTU span standard solutionthoroughly.

2. Use the MODE Key to move the lower cursor toSPAN.

3. After readout has stabilized, i.e., about 60 to 90seconds, set the readout to "800" NTU, which isthe value for this standard solution.

4. Press the ENT Key to complete the spancalibration for TURB.

Section

301246

32 DC calibration

DO calibration

A zero standard solution is used for the DO zerocalibration. An oxygen-saturated span solution is usedfor the DO span calibration.

Preparing the standard solution

Zero solutionAdd about 50g of sodium -sulfite to 1,000 m/ of water(either de-ionized water or tap water will do). Stir thismixture thoroughly until completely dissolved.

Span solut ionPut 1 or 2 liters of water in a container (either de-ionized water or tap water will do). Use an air pump tobubble air through the solution until 'it is oxygen-saturated. .

Section 3

301247

DO calibration 3'

1. Zero calibration

Wash the probe 2-3 times in tap water, and place it inthe zero standard solution.

1. Use the MODE Key to move the lower cursor toZERO.

2. Use the SELECT Key to move the upper cursor toDO.

3. After the readout has stabilized, set it to 0.0, usingthe UP/DOWN Keys.

4. Press the ENT Key. This completes the zerocalibration for DO.

2. Span calibration

Wash the probe 2-3 times in tap water, and put it in thespan standard solution.

First, be sure the U-10 is. set for fresh waterreadings. To do this, set the S.SET Sub-Mode to0.0%.

Then, use the MODE Key to move the lower cursorto SPAN.

After the readout has stabilized, while slowlymoving the probe up and down in the solution, setthe readout value to the appropriate DO value forthe temperature of this solution. For DO values atvarious temperatures, refer to Table 4.

Press the ENT Key to complete the spancalibration for DO.

Section

301248

34 DO calibration

Table 4 Amounts of saturated dissolved oxygen in water at varioustemperatures, salinity = 0.0%

Temperature°C

012345

• 6789

1011121314151617181920

DO in mg//

14.1613.7713.4013.0412.7012.37 .12.0611.7511.4711.1910.9210.6710.4310.20" • '

9.979.769.569.37 .9.189.018.84

Temperature°c

21222324..25262728293031 .32333435

- 36373839 ,40

DOinmg//

8.688.538.398.25 -8.117.99

. 7.877.757.647.537.427.32 .7.227.137.046.946.866.766.686.59

Section 3

301249

I[IIIi

Section

Data Storage and PrintoutThe U-10 can store up to 20 sets of data, 120 data points, of the valuesmeasured for each of the six parameters: pH, COND, TURB, DO, TEMP, andSALINITY. Values stored in memory can be recalled to the readout as desired.

If a printer is connected to the U-10 printer port, whenever a Data-Set iseither stored in memory or recalled to the readout, it can also besimultaneously output to the printer.

Store •• • • 36Recall ••• 38Delete •• •• 40Printing out • • • • •• • 41

301250

36 Store

Storing data

(MODE) 1. Press the MODE Key to put the U-10 in the MAINTmode. .

2. Continue to press the MODE Key to move the lowercursor to IN, the Input Sub-Mode.

3. Use the SELECT Key to move the upper cursor to• the parameter you wish to see on the readout.

4. When the readout stabilizes on a value, press theENT Key. This will automatically input the set of sixparameters for this measurement into memory.

pHu n.1.U

•SELECTRUH COND TURB DO TEMP SAL

MODEAUTO ZERO SPAN HUB OUT S.SET

CM. ——— — OATA —

Section 4

The readout will first show the Data-Set No. forabout two seconds. At the top right-hand corner, adashed arrow points to IN, showing that data isbeing input. Then each parameter is automaticallyread into memory, one-by-one from pH to salinity.The upper cursor skips along to show this. If aprinter is connected, these six values will also beprinted out at the same time.

The upper cursor then returns to pH, with theU-10 still in the IN Sub-Mode.

You may now continue and input another set of data:simply press the ENT Key again.

The Data-Set No. will automatically advance onedigit, and the next set of six parameters will be readinto memory in the same manner. This procedurecan be repeated for up to a total of 20 Data-Sets.

301251

• Store 37

If 20 Data-Sets have been read into memory, thestorage capacity is full arid no more data may beinput. The U-10 will beep three times to indicate thememory is full.

6. To return the readout to the previous setting in theMEAS mode, press the MODE Key again.

Section 4

301252

38 Recall

Recalling data

1. Press the MODE Key to put the U-10 in the MAINTmode. .

.2. Continue to press the MODE Key to move the lowercursor to OUT, the Output Sub-Mode. The readoutwill show d.1, meaning.Data-Set No. 1.

At the top left-hand corner, a dashed arrowpoints to OUT, showing that data can be output nowto the readout. .

MAINT.

• SELECT •pH COND TURB HUB TEMP SAL

MODEAUTO ZERO SPAN IN EUJ S.SET

CAt. - CATA -

3. Use the UP/DOWN Keys to display the Data-SetNo. of the values you wish to recall.

(SELECT) 4. Use the SELECT Key to move the upper cursor tothe parameter you wish to view.

5. Press the ENT Key to display the data on thereadout.

Section 4

MAINT o c cU.U Um9"

SELECT—pH COND TURB •Ztl TEMP SAL

MODEAUTO ZERO SPAN' IN ESJ S.SET

CAl — D»TA —

If a printer is connected, all six parameters in thisData-Set will also be printed out at the same time.

301253

Recall 39

When the ENT Key is pressed again, the next Data-Set No. is displayed in order, i.e., df, if two datasets are in memory. At this point, you can eitherpress the ENT Key again to view the contents of thisData-Set, or you can use the UP/DOWN Keys to goup or down to another Data-Set No.

If a particular Data-Set is empty, three dashesappear on the readout.

mg/1•SELECT-

IdM COND TUR3 DO TcMP SAL

MODE •AUTO ZERO SPAN IN

CAl • — DATA —S.ScT

7. To return the readout to the previous setting in theMEAS mode, press the MODE Key again.

Section 4

301254

40 Delete

Deleting data

Set the U-10 as if you were going to input data:

2. Continue to press the MODE Key to move the lowercursor to IN, the Input Sub-Mode,

MAINT occ m9/l• SELECT-

pH COND TURB BEIH TEMP SAL

MODEAUTO ZERO SPAN BEB OUT S.SET

C»L — DATA —

3. Then, to erase all the data from all the Data-Sets inmemory, press the CLR Key. The readout will showthe message L~Lr for about two seconds.

MAINTI / _

| • • I I mg/l

•SELECT-pH COND TURB EDI TEMP SAL

MODEAUTO ZERO SPAN- — CAL - - -

OUT S.SET— DATA — _

Section 4

Be careful!You cannot delete individual Data-Sets. The CLRKey always erases all data from memory.

301255

Printing out 41

Printing out data

If a printer is connected to the U-10 printer port, whenever a Data-Set is either stored in memory or recalled to the readout, it is alsosimultaneously output to the printer.

The U-10 printer port is a standard Centronics parallel port. Toconnect a parallel printer to the U-10: Open the rubber printer-port cover, located directly over the readout on the main unit, andconnect the printer cable. "

Note:When a printer is not being used, disconnect thecable from the U-10 printer port, and close thecover tightly.

Sample printout NO. 1pHCONDTTO3DOTEMPSAL

NO. 2pE.CONDTCJRBDO .

. TZ-U.PSAL

NO. 3PE

DATE5.01.5

3900.5

DATE3.11.3

2700.7

DATE3.1

nS/craNTUng/1

. • • c .^/• /

nS/c3iNTOmg/1•c^/ /

Section 4

301256

Section

Daily Maintenance andTroubleshooting

For accurate measurements and prevention of malfunction, routine carefulmaintenance of the U-10 is important. In particular, failure to maintain thesensors properly can lead to "serious trouble or incorrect measurements. TheU-10 is provided with error-code functions for the ready detection of potentialproblems.

Error codes •• v 44

Normal probe maintenance 47Replacing faulty sensors 49Replacing a faulty probe •• 50

oII 301257

44 Error codes

Error Codes

The U-10 has an easy-to-understand error message function soyou can spot trouble readily. Error codes are displayed on thereadout and the unit will beep if an error occurs.(Note that if you press an incorrect sequence of keys, the unit willbeep three times to indicate you have pushed the wrong key.)

Error Code Cause Action

Bad battery

r /C ~ \

• Defective or low battery • Replace battery

Failure in main unit—I • Malfunction of memory

; ) backup 1C

Zero-calibration error.— —i (or all parameters) i~{ • Poor connection in probe-to-

main-unit cable• Water in one of the sensor-sockets

• Temperature of sampleexceeds maximum scale ofU-10

forpH• Contaminated pH sensor. .• Improper concentration of .

KCI internal solution in pHreference sensor

for COND• Contaminated COND sensor

for TURB• Contaminated or defective

LED sensor

Push POWER Key to turnthe U-10 ON again. If thiserror code is still displayed,contact your Horiba dealerfor repair or replacement.

• Connect the cable securely.

• Dry out the sensor sockets.

• Replace the probe.

Clean the pH sensor.Replace the pH referencesensor KCI internal solution.

Clean the sensor, usingtooth brush and neutraldetergent.Clean out the tubecontaining the LED turbiditysensor, using test tube brushand neutral detergent.Never use an abrasivedetergent cleanser for this.

Section 5

301258

Error codes 45

for DO• Broken DO sensor

membrane.

Span-calibration error

i f; /"7

(or all parameters• Poor connection in probe-to-

main-unit cable• Water in one of the sensor

sockets• Temperature of sample

exceeds maximum scale ofU-10

forpH• Contaminated pH sensor.• Improper concentration of

KCI internal solution in pHreference sensor

forCOND• Contaminated COND sensor

for TURB• Contaminated or defective

LED sensor.

Check the LED turbiditysensor. If it defective, theentire probe must bereplaced.Check DO sensor. Ifdefective, replace.

Connect the cable securely.

Dry out the sensor sockets.

Replace the probe.

• Clean the pH sensor.• Replace the pH reference

sensor KCI internal solution.

Clean the sensor, usingtooth brush and neutraldetergent.Clean out the tubecontaining the LED turbiditysensor, using test tube brushand neutral detergent.Never use an abrasivedetergent cleanser for this.

• Check the LED turbiditysensor. If it defective, theentire probe must bereplaced.

Section 5

301259

46 Error codes

Span-calibration errorj— j / DO Auto-calibrationI l

Memory full

Broken DO sensormembrane.

• Excessive differencebetween DO sensortemperature andatmospheric temperature.

DO aqueous solutioncalibration • •

• Broken DO sensormembrane.

• Contaminated electrode.

• Insufficient agitation ofsolution.

Data-sets for 20 samplesare already in memory.

Printer error— — • Jammed printer paper.

£7 >~ O• Poor cable connection .• Wrong printer.

• Defective printer.

• Check DO sensormembrane. If defective,replace.

• Leave DO sensor inatmosphere for 30-60 min.

Check DO sensormembrane. If defective,replace.Clean the electrode using asoft brush, taking care not toscratch membrane.Agitation solution thoroughly.

• To delete all data frommemory, put the U-10 in theIN Sub-Mode mode andpress the CLR Key.

• Eliminate jamming of printerpaper. . :

• Replace the cable.• Use proper parallel

Centronics printer.• Replace the printer as. necessary.

Section 5

301260

Probe maintenance 47

Normal probe maintenance

Washing the turbidity sensor

The sensor is a glass tube. Wash out the tube and remove stainscarefully, using tap water and a test tube brush.

Be careful not to scratch the inside of the glass tube. Neveruse abrasive detergents or cleansers.

Cleaning the conductivity sensor

Remove COND sensor guard, and carefully use a soft brush toclean off any dust from the sensor unit.

Be sure to replace the COND sensor guard before takingmeasurements.

COND sensor

COND sensor guard

Section 5

301261

48 Probe maintenance

Recharging the reference sensor with

Recharge the reference sensor with reference solution about onceevery two months, as follows.

1. Remove 'the liquid-junction rubber cap from the referencesensor, and pour out the old solution.

2. Fill the reference sensor completely with new referencesolution. Make sure there are no air bubbles.

3. Replace the liquid-junction rubber cap.

4. Carefully wash off all excess reference solution from theprobe. • • .

Reference sensor

-Liquid-junction rubber cap

Section 5

301262

Replacing faulty sensors

Three of the U-10's sensors are replaceable: the pH sensor, thereference sensor, and the DO sensor.These may be replaced as follows.

. 1. Wipe off any water droplets from the probe.

2. Remove faulty sensor.

3. Insert the new sensor carefully with your fingers.

4. Be careful not to let the sensor sockets get wet.

Sensor tool *

referencesensor

DO sensor

Sensor sockets

• pH sensor

* When replacing the DO sensor, use the sensor toolprovided as an accessary.

Section 5

301263

50 Probe maintenance

Replacing a faulty probe

Disconnect the cable from the main unit

1. Loosen the cable gasket cap, and remove cap from gasket.

Cable gasket

Cable gasket cap

2. Slide back the gasket.

3. Back off the two screws on the cable-connector cover.

-Cable-connector cover

Cable gasket

Move. •

4. Slide off the cable-connector cover to expose theconnector lock claws.

5. Press lock claws on both sides with your fingers torelease the connector. Pull out the connector from themain unit.

Lock claws

Connector

Cable-connector cover

Cable to probe

Section 5

301264

Connect the new probe

1. Insert the connector until it clicks.

2. Re-attach the cable-connector cover to the main unit.

3. Slide the cable gasket toward the cable-connector cover,and screw on the cable gasket cap.

Before you use a new probe for the first time, it isnecessary to calibrate it manually for all four parameters.Refer to Section 3, "Calibrating the U-10," for instructionson manual calibration.

Section 5

301265

Section

Reference MaterialsThe following descriptive information is provided for a better understanding ofthe U-10 Water Checker and i ts functions. ' . . - ' '

Conductivi ty (COND) ••• •• •• 54Turbidity (TURB) • • • • • • 58Salinity •• ••• • • • • • • 60Temperature ••. 60Dissolved-Oxygen (DO) • 61pH • ••• • 63Specifications 55Parts List • : :•-•- —. 68

301266

54 Conductivity

Reference .Materials.

Conductivity (COND)

Principle of measurement

Conductivity is an index of the flow of electrical current in asubstance. •

Salts dissolved in water are separated into cations and anions.Such a solution is called an electrolytic solution. An electrolyticsolution has the property of allowing the flow of current accordingto Ohm's law. This property is referred to ionic conductivity, sincecurrent flow is due to ion movement in an electrolytic solution. .Metals, on the other hand, allow the flow of current by means ofelectrons. This property is called electronic conductivity, which isdistinguished from ionic conductivity.

A cube 1 cm on each side, as each shown in Fig. 1, is used todemonstrate an electrolytic solution. Two electrode plates areplaced on opposite sides, and the cube is filled with a solution. Ifthe resistance between these two electrode plates represented byr(n), the conductivity of the solution L (S.crrr1) is i=1/r. S, standfor Siemens, a unit of measurement of conductance. .

Electrode plate

Solution

Fig. 1 Definition of conductivity'

The most general method for measuring conductivity is based onthe above principle, and is called the 2-electrode method. In thismethod, to take a measurement, it is necessary to allow flow ofalternating current between the two electrode plates.

Section 6

301267

Conductivity 55

Hdjrect eg/rent is_s_ent b_e.tw_aanJb,ern JLwJILcaus.e._causes_,_™.electroplating or decomposition, i.e., polarization; this results ininaccurate measurement of conductivity.

Even a flow of alternating current will also cause a certainamount of polarization. Measures must be taken to minimize theeffect of this polarization, such as the application of platinum blackplating to the electrode surfaces. In spite of such measures,however, the effect of polarization cannot be neglected inconductivity measurements of a high-conductivity solution. Thismakes accurate measurement difficult. Furthermore, depositionsor stains on the electrode surfaces can cause a large apparentresistance, also making accurate conductivity measurementdifficult. . - - -

The LJ-10 Water Checker has adopted the 4-electrode methodto overcome these disadvantages of the the 2-electrode method.As shown in Fig. 2, the U-10 Water Checker uses two voltage-detecting electrodes and two voltage:applying electrodes, for atotal of total four electrodes.

The voltage-detecting electrodes are for detecting AC voltage,and the voltage-applying electrodes are for applying AC voltage.

Voltage-detectingelectrodes Voltage-applying

electrodes.

Fig. 2 Principle of the 4-electro.de method

Section 6

301268

-Jtesume that the current^/f/A), flows in.a-sample of- under automatic control of the voltage-applying

that the voltage. at the voltage detecting-, remains constant at all times. Then, thesample, R (n), across the voltage-detecting

ji§P?=E//.. The resistance, R, of the sample is inversely'its conductivity, L That is, the conductivity, L, isi.the current, /. Accordingly, calibration of a

tibn of known conductivity, Ls, enables calculation of2ajpt''a sample according to the formula L=Ls(l/ls) from

4-electrode method, polarization occurs, since ACvoltage-applying electrodes. The voltage-

are,- hpwever, free from the effects ofthey, are separated from the voltage-applying

, current flow is negligible. Therefore,is an excellent method to enable

covering a very high range..., '_-iflt

301269

Conductivity 57

Temperature.com,p,e.o^.ati-on _^_ _.__.—

In general, the conductivity of a solution varies largely with itstemperature. The conductivity of a solution depends on ionicconductivity, described earlier. As the temperature rises,conductivity becomes higher, since ions begin to move moreactively.

The temperature coefficient shows the change in % ofconductivity per CC, with a certain temperature taken as thereference temperature. This is expressed in units of %/°C. Thetemperature coefficient assumes the premise that the conductivityof a sample changes linearly according to temperature. Strictlyspeaking, with actual samples, however, conductivity changesalong a curve.Furthermore, these curves form different shapes depending on thetype of sample. In the ranges of smaller temperature changes,however, samples are said to have the temperature coefficient of2%/°C; this holds for most samples, except in certain special cases.The U-TO Water Checker uses an automatic temperatureconversion function to calculate conductivity at 25°C at atemperature coefficient of 2%/°C, based on the measured value ofthe temperature. Results are displayed on the readout. TheU-10'stemperature conversion function is based on the following formula,

L2s=Lt/{l+0.02(t-25)}Where,

L25: Conductivity of solution converted to 25°C(value displayed on U-10)

t: Temperature of solution at time of measurement (°C)Lt: Conductivity of solution at t (°C)

Section 6

301270

58 Turbidity •

Turbidity (TURB)

From among several types of turbidity-measuring methodsavailable, the U-10 uses the light-absorption-scattering method,shown in Fig. 3. .Irradiation of a beam of light onto a sample brings aboutseparation of the beam into (1) the light transmitted by the solutionand (2) the light scattered by turbidity components in the sample.In the light-absorption-scattering method, the intensity of bothtransmitted light and the scattered light are measured usingseparate receptors, and the turbidity is obtained based on theratio of the two.

With the U-10, the light source is a pulse-lighting infrared-emission diode. The scattered light is measured at a point 30'offset from the light source. This light-absorption-scatteringmethod has several advantages, including the fact that (1) theactual color of the sample fluid has little effect on themeasurement of turbidity, (2) fluctuations in light quantity from thelight source are easily compensated for, and (3) it allows the U-10to be operated with relatively low power consumption.

Section G

Scattered light receptor

Light source =n f( -< }} 3=^ Transmitted light receptor

Sample fluid-

Fig. 3 Principle of the light-absorption-scattering method

301271

Turbidity 59

NTUs (Nephelometric Turbidity Units)

For the calibration of turbidity, the U-10 uses a standardformazine solution.

Kaolin has been the conventional standard solution for manyyears. However, the composition of kaolin solutions often varydepending on the country of origin, and turbidity varies with thedegree of purify. Furthermore, there is often individual error inpreparing the solution. Kaolin is thus known for bringing about verylarge disparity in measurement results. As a turbidity standardsolution, formazine standard solution is now increasingly being usedinternationally. In view of these facts, the U-10 uses the formazinestandard solution for its calibration of turbidity.In addition, the U-10 uses NTUs as the unit of turbidity. Otherunits conventionally used are formazine degrees and FTUs.When the measurement of turbidity is based on the phenomenonof scattering, the use of NTUs is preferable, and in fact, these arebeing used increasingly. It should be noted that NTUs used asturbidity units of the formazine standard solution are equivalent to

. formazine degrees and to FTUs.

Section 6

301272

60 Salinity

Salinity (SAL).,.™.

The U-10 is designed to measure salinity as well as the otherparameters.

Note that the "salinity" referred to here is the salinity of seawater. There is a constant relation between conductivity andsalinity at certain temperatures.

Therefore, if data on the conductivity and temperature areavailable, the corresponding salinity is known. In other words, thesalinity measurement of the U-10 is based on the.principle ofcalculating the salt content, making .use of the measured values ofconductivity and temperature.Note carefully, therefore, that measured results of all substanceswhose conductivity is detected are displayed as salinity. Forexample, the measured result is displayed as NaCI concentration,even if in fact the sample component is, for example, hydrochloricacid (HCI).

Temperature measurement in the U-10

Temperature changes in water have extreme biological effectson the life cycles of fish and seaweed, as well as on that of theminute organisms that cleanse the water of organic pollutants. Ingeneral, as the temperature of water increases, the amount ofoxygen dissolved in the water decreases and there is a tendencyfor the amount of pollutants to increase.

The U-10 uses a thermistor to measure temperature. Athermistor also measures the change in electrical resistanceaccompany changes in temperature; these changes in resistanceare measured by the thermistor and are used to calculate thetemperature.

This temperature data is used by the U-10 in four differentways: (1) in pH temperature compensation, (2) in conductivitytemperature conversion, (3) in the calculation of salinity, and (4) indissolved-oxygen temperature compensation.

Section 6

301273

Dissolved-Oxygen 61

Dissolved-Oxygen (DO)

The "DO" referred to here means the concentration of oxygendissolved in water.

. Dissolved oxygen is essential to self-purification of rivers andseas, as well as to living of aquatic organisms and fish.Therefore, measurement of DO is vital in both waste-watertreatment and water quality control.

Fig. 4 shows the principle of measurement using a DO sensor.

*• Current

Anode (lead)

Alkaline electrolyte

Cathode (silver) ^ '• ^ Oxygen-permeablediaphragm

Fig. 4 Principle-of DO sensor

A noble metal (silver) is fitted closely to an oxygen-permeablediaphragm to make the cathode; a base metal (lead) is used asthe anode. Both are immersed in an alkaline electrolyte with theanode-to-cathode external circuit complete. Oxygen diffusing,through the oxygen-permeable diaphragm causes a reductionreaction at the cathode; this allows flow of current in the externalcircuit:

O2 + 2H2Q + 4e~ = 4OHTAt the anode, oxidation reaction occurs as follows:

2Pb = 2Pb^ + 4e~The current is proportional to the quantity of oxygen diffusing

through the oxygen-permeable diaphragm. Accordingly,measurement of the current makes the DO in a sample known.

The DO measuring method based on this principle is calledthe diaphragm-electrode method. This method allows convenientmeasurement of DO, especially when compared with chemical-analysis methods, which need complicated pre-treatment toeliminate the effects oi oxidizing or reducing substances.

Section 6

301274

62 Dissolved-Oxygen

DO correction for salinity

When a solution and air are in contact and in completeequilibrium (saturated), DO:C[mg// ] in the solution, and theoxygen partial-pressure.:Ps[MPa] in air are in the followingrelation: ' .

C-Ps/H

H(MPa/(mg/l)] is referred to as Henry's constant, whichdepends on .the composition of the solution. In general, Cbecomes smaller as the salinity in the solution increases, since Hbecomes larger.

A DO sensor is intended to detect Ps in theabove expression.Therefore, the DO measurement of an aqueous solutioncontaining salt would be in error if the DO electrode werestandardized either on air-saturated pure water or on air. To settlethis problem, it is necessary to correct the DO reading based onthe salinity of the sample.

Conventional DO meters make this salinity correction byinputting a known salinity value. This poses no problems if thesalinity of the sample is known. In practice, however, the salinityof the sample usually not known, unless measured by a devicesuch as the U-10. Therefore, until now, DO meters have not beenpractical, even if they were provided with a salinity-correctingfunction. .. '

The U-10 is capable of measuring the salinity of a sample andautomatically correcting the DO reading for the amount salinitymeasured in the sample.

Section 6

301275

Dissolved-Oxygen 63

pH ..___

The following is the basic equation for obtaining pH:

pH = -log aH-Where, ' '

aH-: the activity of hydrogen ions

If a thin glass membrane is used to separate two liquids ofdiffering pH values, an electric current will be generated inproportion to the difference between these two pH values. Thevalue of this electrical current, E(V} , is shown by the folowingNernst equation:

E = 0.0001983T (pHi - pHo) + e .Where,

T: the temperature of the liquidspHi: the pH of the internal liquid

• (i.e., inside the glass membrane)

pHo: the pH of the sample liquid(i.e., the iliquid outside the glass membrane)

e : the irregular electrical potential difference

A conventional glass electrode for measuring pH contains afluid inside the electrode with a pH of 7. If this is used to measurea sample that also has a pH value of 7, the irregular electricalpotential difference-will be close to 0V. Consequently, when a ;glass pH electrode is immersed in an acid solution, a positiveelectric current is generated; when it is immersed in an alkalinesolution, a negative electric current is generated.

For actual use in a pH meter, a pair of referance electrodeswith extremely stable characteristics is used. These areconfigured as shown in Fig. 5. As shown in Fig. 5, it can be seenthat the electrical potentials generated in the internal electrodes,E' and E", are canceled out by each other, so that the onlyelectrical potential difference obtained is the current generated bythe glass membrane, E, through the resistance of the membrane,r, and transmitted to terminals G and R.

Section 6

301276

64 Dissolved-Oxygen

In ph[_meteis^areadout of this voltage.between the twoterminals is'obtained" b~y~incre~asing it wittran-anrvplifierHn actual--practice, the pH meter is first calibrated using a standardreference solution of known pH, then the pH of the sample liquiedis measured.

Fig. 5 Principle for Measuring pH

Section 6

301277

Specifications 65

Specifications

RepeatabilityTemperature compensation

ReadoutCalibration

Principle Glass electrode. Range pHO-14

Resolution Standard : O.lpHExpanded : O.OIpH±0.05pH0°-50°CLCD1-point auto (Zero)Manual 2-ppint

Temperature of the sample

PrincipleRange

Resolution

ReadoutCalibration

ThermistorP°-50°CStandard : 1°CExpanded :0.1°C±0.3°C

PrincipleRange

Resolution

ReadoutCalibration

Membrane galvanic cell0-19.9mg//Standard : 0.1 mg//Expanded : 0.01 mg//±0.1 mg//0°-40°CLCD1-point auto (Span)Manual 2-point

Section 6

301278

66 Specifications

Conductivity

Principle 4-electrodeRange

Resolution

' Repeatability

Temperature compensationReadout

Calibration

0-100ms/cmStandard:' 0-1 mS/cm :0.01 mS/cm

0-10mS/cm: 0.1mS/cm10-1 OOmS/cm : 1 mS/cm

Expanded: 0-1 mS/cm : 0.01 mS/cm0-10mS/cm : 0.1mS/cm10-1 OOmS/cm : 1 mS/cm

±1%/F.S, within each measurementrange0°-50°CLCD1-point auto (Span)Manual 2-point

Turbidity

PrincipleRange

' Resolution

ReadoutCalibration

Scattered/Transmitted light0-800 NT.UStandard :'10NTUExpanded:1 NTU±3%/F.S.

LCD1-point auto (Zero)Manual 2-point

Salinity

PrincipleRange

Resolution

ReadoutCalibration

Conversion based on conductivity0-4%Standard : 0.1%Expanded : 0,01%±0.1%0°-30°CLCD

Section 6

301279

Specifications 67

Common specification

Data storagePrinter output

Operating temperatureWeight

Max. 20 samplesCentronics specs.Battery 9V,with auto power-off function0°-45°CMain unit: Approx. 400gProbe, with 2-m cable: Approx. 800g

Output connector pin layout

8 -\ . r 14

Pin No.1234567

NameSTBDBoDB>DBzDB3DB*DBs

Pin No.891011121314

NameDBe

Not usedBUSY

Not usedNot used

• GND

Section 6

301280

68 Parts List

Parts ListThe following expendable parts are available from Horiba for theU-10 Water Checker. "

Part name

pH sensor

DO sensor

pH reference sensor

Liquid junction(1 pair)

KCI internal solutionfor ph referencesensor

pH standard solution- pH2

pH standard solutionPH4

pH standard solutionpH7

pH standard solutionpH9

Calibration beaker

Model No.

Details

Special design forthe U-1 0

3.3 mol/ /gel type, 250 ml

Special design forU-10 automaticcalibration

Order P/No.

9037-0047-00

9037-0048-00

9037-0049-00

9037-0050-00

9037-0051-00

9037-0052-00

9003-0015-00

9003-0016-00

9003-0017-00

9003-0018-00

9037-0053-00

Section 6

301281

Unpacking 69

Unpacking the U-10

The following items are included with your U-10 Water QualityChecker.When you unpack the probe and main unit, confirm that all the otheraccessories are included as well.• Main unit • Calibration breaker ".

Dissolved-Oxygen (DO)sensor:-1 unit (boxed)

Standard solution (PhthalatepH standard solution): 1 500m/ bottle

• KCI internal solution forreference sensor: 1 250m/bottle

9.V battery

Carrying strap for main unitstrap

DO sensor tool

This Instruction Manual

301282

70 Precautions

Precautions when using the U-10

The U-10 Water Quality Checker is carefully designed for trouble-freeoperation. However, it is a sophisticated electronic instrument, and itcan be damaged if used carelessly. Please read the followingprecautions and observe them when using your U-10 Water Checker.

Do not swing or jerk the probe by itscable.Do not subject the cable connector tostress by pulling or stretching it.

Do not drop the either the U-10 probeor main unit. Never subject eithercomponent to sudden impact.

Do not store the U-10 where may beexposed to prolonged direct sunlight.Never leave the U-10 inside a vehiclewith the windows closed.

301283

Precautions 71

Never immerse the main unit directlyin water. . • . .

The main unit is water-resistantand may be safely used in the rain;however, it is not of waterproofconstruction. Immersing the main unitin water or any other liquid candamage the internal electronic circuits

Never allow any organic solvent tocome in contact with either the probeor the main unit. This includes suchliquids as methylethyl ketone (MEK)and acetone.

(The probe is made ofpolyphenylene ether (PPE); the mainunit case is acrylic resin.)

II 301284

PARTS LIST U-;

"No. HIT P/N

362177

..: 362283 .362193 ;

362194 -

362174

362175

362195

362196

362197

360249

362176 :

380169'.

362198 :

10 SENSOR Drawing No. S410157-03

Description . ' :

Sensor.assembly with 2 meter cable

Sensor assembly with 10 meter cableScrew, panhead - G1SB111TM3X 6(S-ZN3)

0-ring - NOK S 11.2(SI) .

DO Tip - U-10 sensor

Reference Tip - U-.10 sensor

0-Ring, S18 - NOK S18 FPM

Screw, panhead - M3-6L SUS304

Cond guard - U-10 sensor

0-Ring, P9 - B2401 P9 FPM

PH Tip - U-10 sensor

0-Ring , P5 - B2401 P5 FPM

Protecting tube - U10 Sensor

301285 48

IPARTS LIST U-10 METER for Drawing No. S410156-03

2.3.4.

>n.12.

HII P/N

362181

3612182-

362183362184,

362185

362186

362187

362T88

362189

362190

362191

362192

362193

Description

Sheet Switch - .Hater checker U-10

Case assembly, top - U-10

PRT Cover.- U~10Meter

Window, LCD - U-10 H357887-01

Tapping screws, M3X 6(S-ZN3)

PCB Assembly

Case packing - U-10 meter.

Case assembly, bottom

Cover assembly, BAT - U-10

Seal washer - U-10 Meter

Meter strap -' U-10 20X13001=1.8

Battery packing - U-10 meter

Screw, panhead 01581111 M3X 6(S-2N3)

301286

b Index

accessories, included with the U-1069

acid solution, effect on glasselectrode 63

alkaline solution (in DO sensor) 8;effect on glass electrode 63

atmospheric air, used for DOauto-calibration 20

atmospheric temperature(excessive difference from thatof DO sensor) 46

auto-calibration procedure 20-22;aborting of 21; error in 22

auto-salinity function 17battery, defective or low 44; .

inserting and replacing 9borax 25calcium hydroxide 25calibrating the U-10 19-34calibration beaker, special shape of

20;calibration, automatic 20-22; error in

auto-calibration 22; manual (2-point) 23-34

carbonate 25carrying strap, attachment of 10cleaning the U-10 18clearing data, from memory 40CLR (Clear Key) 7color of sample fluid, effects of in

measuring turbidity 56COND calibration (manual 2-point)

' 26-29COND sensor (non-removable) 2;

contamination of 44-45;malfunction of 17; washing of 47

conductivity 57; principle ofmeasurement used in the U-1054-56; relation to salinitymeasurement 60

conductivity specifications 66cursors, upper and lower 4dashed arrows (on upper part of

readout to show datainput/output 36, 38

dashes, on readout (3 dashes meanData-Set is empty) 39

data, saving in memory whenreplacing battery 9; storage,retrieval, deleting, and printout of35-41

Data-Sets, total number in memory36-37

deleting data 40diaphragm-electrode method (used

' in measuring DO) 61dissolved oxygen sensor: See "DO

sensor"dissolved oxygen: See "DO"DO calibration (manual 2-point) 32-

34Do correction for salinity 62DO sensor (removable) 2, 49;

(excessive difference fromatmospheric temperature) 46;breakage of membrane 44,46;inserting into U-10 probe 8

DO specifications 65DO values at various temperatures

- 33-34DO, principle of measurement used

in the U-10 61-62

301287

electrical potential difference (usedin obtaining-pH-)-63

electrical resistance, changes inused to measure temperature 60

electrolytic solution 54 •electronic conductivity 54ENT (Enter Key) 7error codes 44-46error, in auto-calibration 22; in span-

calibration 45; in zero-calibration 44; printer 46

EXP (Expanded Readout Key) 7,13,15

expanded readout mode, 7,13,15faulty probe, replacement of 50-51faulty sensors, replacement of 49formazine degrees (used in

measuring turbidity) 59formazine standard solution (used

in measuring turbidity) 59four-electrode method 55-56fresh water, measuring of 16-17FTUs (used in measuring turbidity)

59glass membrane (used in obtaining

pH) 63Henry's constant (used in

measuring DO) 62hexamethylenetetramine (used in

solution for turbidity calibration)30

Horiba, worldwide marketinglocations ??

hydrazine sulfate (used in standardsolution for turbidity calibration)30

hydrochloric acid, as a salinitycomponent 60

initial readout 13Input Sub-Mode (used in data

storage) 36; (used in deleting

data) 40inputting data 35-37 _ _ . _ . .ionic conductivity 54Kaolin (used in measuring turbidity)

59KCI internal solution, filling the

reference sensor 48; improperconcentration in referencesensor, 44-45; (standard solutionused for COND calibration) 27

keypad, explanation of 6LED sensor, contaminated or

defective, 44-45; washing of 47;light-absorption-scattering method

(used in measuring turbidity) 58lower cursor 4main unit, failure in 44•MAINT mode 4MAINT Sub-Modes 5maintenance and troubleshooting

43-51manual (2-point) calibration

procedures 23-34MEAS mode 4 . 'measurements, how to make 12-17memory backup 1C, malfunction of

44; capacity 37; full 46; savingdata in memory when replacingbattery 9

MODE (Mode Key) 6modes, MEAS and MAINT 4NaCI concentration, in salinity •

measurements 60Nephelomtric Turbidity Units (used

in measuring turbidity) 59Nernst equation (used in obtaining

pH)63non-removable sensors 2NTUs (used in measuring turbidity)

59organic solvents, avoiding use of on

II 301288

theU-1071~?Gkj.tpui_Sub- Mode (used in data

retrieval) 38oxalate 25Parameter-Select Key (SELECT) 6,

14parameters measured by U-10 5;

shown on readout 14parts list 68pH calibration (manual 2-point) 24-

25pH sensor (removable) 2, 49;

contamination of 44-45; keepingmoist when storing the U-10 18

pH specifications 65pH values of standard solutions 25pH, basic measurement principles

o f63phosphate, neutral 25phthalate 25 'polarization 55-56potassium chloride, KCI (solution

used for COND calibration) 27,44-45, 48

POWER (Power Key) 6precautions, when using the U-10

70printer error 46printer port 2, 40printing data 40-probe, faulty, replacement of 50-51;

maintenance of 47; using a newprobe for the first time 23

readout, expanded mode 7,13,15;explanation of 4; initial 13;showing parameters on 14

recalling data 38reference sensor (removable) 2, 49;

filling with KCI internal solution48; improper concentration ofinternal KCI solution 44-45;

washing of 48removable sensors 2,49S.SET Sub-Mode 16salinity parameter 15salinity, DO correction for 62;

principle of measurement usedin the U-10 60; unusual values ofin sea water 17; specifications66

salt water, measuring of 16SELECT (Parameter-Select Key) 6,

14sensor sockets, water in 44-45sensors, faulty, replacement of 49;

non-removable 2; removable 2,49

shelf life (of KCI, potassium chloridestandard solution) 27; (ofstandard solution used inturbidity calibration) 30

sodium sulfate (used in zerostandard solution for DOcalibration) 32

span-caiibration error 45specifications 65-67stable readings, to obtain 14standard solution for COND

calibration 27; for turbiditycalibration 30; for DO calibration32; for pH calibration 25

storing data 36-37storing the U-10 18, 70strap (carrying), attachment of 10Sub-Modes (in MAINT MODE) 5;

(used in data storage andretrieval) 36-40

temperature (sample temperatureexceeds maximum scale of U-10)44-45

temperature compensation,principle, used in the U-10 57

301289

temperature measurement in the U-

temperature sensor (non-removable) 2 .

temperature specifications (for 'sample) 65

temperature, affect on amount ofpollutants in water 60; affect ondissolved oxygen in water 60;atmospheric (excessivedifference from that of DOsensor) 46

thermistor (i.e. /temperature sensor)2,60

troubleshooting and maintenance43-51

turbidity calibration (manual 2-point)30-31

turbidity readings, affected bycontamination of LED sensor,44-45

turbidity sensor (non-removable) 2; •washing of 47

turbidity specifications 66turbidity, principle of measurement

• used in the U-10 58-59' two-electrode method 54 .two-point calibration: See "manual

(2-point) calibration procedures"uniform readings, to obtain 14UP/DOWN Keys (used in MAINT

Sub-Modes) 7upper cursor 4washing the COND sensor 47washing the turbidity sensor 47water-resistance of the U-10 71zero-calibration error 44

301290

HO RIB A Worldwide Marketing Locations

f»IIIIII

HORIBA INSTRUMENTS-INCORPORATED

Irvine Facility17671 Armstrong Ave., Irvine,Calif. 92714, U.S.A.Phone: (1)714-250-4811Telex: (23) 425494Fax: (1)714-250-0924

Ann Arbor Facility3901 Varsity Drive, Ann Arbor,Mich. 48104, U.S.A.Phone: (1)313-973-2171Telex: (23) 0230176Fax: (1)313-973-7868

Silicone Valley Office1080E Duane Ave., Suite J,Sunnyvale, Calif. 94086, U.S.A.Phone: (1)408-730-4772Fa*: (1)408-730-8975

HORIBA ASIA/PACIFICREPRESENTATIVE OFFICE

Parkway Parade £07-0380, Marine Parade Road, Singapore, 1544Phone: (65) 3453030 Telex: (87) 37257Fax (65)3452930

HORIBA KOREA SALES Co.,Ltd.112-6 Sogong-Dong, Choong-kuSeoul, KoreaPhone: (82) 2-753-7911-7912Fax: (82) 2-756-4972

HORIBA EUROPE GmbHIndustriestrasse 8, D-6374 Steinbach.GermanyPhone: (49) 6171-7755-7758Telex: (41) 410829Fax: (49) 6171-8044

HORIBA FRANCERue L. et A. Lumiere Technoparc01630 ST-GENIS-POUILLY, France

, Phone: (33) 50-42-27-63. Telex: (42) 385-054

Fax: (33) 50-42-07*74 ; '

HORIBA AUSTRIAKaplanstraRe 5, A-3430 Tulln,Phone: (43) 2272-5225Telex: (47) 136482'Fax: (43) 2272-5230

HORIBA SWITZERLANDAv. des Baumettes 11-13CH-1020 Renens, SwitzerlandPhone: (41) 21-635-77-41Telex: (45) 455-354.Fax: (41) 21-635-40-82

HORIBA INSTRUMENT LIMITED"1 Harrowden Road BrackmillsNorthampton, NN4 OEB EnglandPhone: (44) 604-765171Telex: (51) 311869Fax: (44) 604-765175

HORIBA Ltd.Head officeMiyanohigashi, Kisshoin, Minami-ku,Kyoto. JapanPhone: (81) 75-313-8123Telex: (54) 22130Fax: (81) 75-321-5725

Tokyo Sales Office2-12-5 Iwamoto-cho, Chiyoda-ku,Tokyo, Japan

-Phone: (81) 3-3861-8231Fax: (81) 3-3861-8259

I 301291

I "• HNU PID (101)

PROCEDURE F-15

301292

I OBJECTIVE

I 1 The objective of these guidelines is to provide general reference informationon the use of the HNu Systems PI 101 Photoionization Detector.

I LIMITATIONS

These guidelines are for information only and are not to take precedence over• the requirements of project-specific plans for the HNu photoionization detector.

15.2 HNU PI-101

15.2.1 Purpose

Subsection 15.2 discusses the use, maintenance, and calibration of the HNU PI-101.

15.2.2 Definitions

15.2.3 Theory and Limitations

15.2.3.1 Theory

The HNU is a portable, nonspecific, vapor/ gas detector employing the principle of photoionization todetect a variety of chemical compounds, both organic and inorganic.

The HNU contains an ultraviolet (UV) light source within its sensor chamber. Ambient air is drawn intothe chamber with the aid of a small fan. If the ionization potential (IP) of any molecule present in the am-bieni air is equal to or lower than the energy of the UV light source, ionization will take place, causing adeflection in the meter. Response time is approximately 90 percent at 3 seconds. The meter reading is ex-pressed in parts per million (ppm). All readings must be stated as equivalent readings that depend on thecalibration gas being used. For example, the standard gas used to calibrate the HNU is benzene, which al-lows the instrument to provide results in benzene equivalence. Exhibit 15-4, modified from the "Instruction

301293

Exhibit 15-3TROUBLESHOOTING PROCEDURES

FIELD EQUIPMENT: PHOTOVAC 10A10

Problem Probable Cause

1. No chromatographic

response

There is no carrier gas flow,

Batteries are flat (if on battery

operation).

Remedy

Check at OUT port with flow

gauge.

Plug into AC and check

again.

Electrometer is saturated. Turn ATTENUATION to 10,

set meter toO. If OFFSET

reads 10 or more, the

instrument is saturated.

Syringe is plugged.

UV source Is not on.

Allow to self-purge until

clear.

Try a new syringe.

Check SOURCE ON light; if

it is on, see item 9 in this

exhibit

2. Unacceptable baseline drift Unit has been subjected to

large temperature change.

Allow to stabilize.

A very concentrated sample

has recently been introduced,

resulting in excessive tailing.

Allow to self-purge until

clear.

Unacceptable baseline drift Unacceptable contamination

levels are in carrier gas supply.

The unit is charging, and the

resulting heat is affecting the

column.

Change carrier gas supply,

and allow instrument to

stabilize.

Turn CHARGE switch to

301294

Exhibit 15-3(continued)

Problem

3. Deterioration of sensitivity

Probable Cause

Syringe has leaky plunger.

Column needs conditioning.

Septum is leaking.

Column fittings leak.

Remedy

4. Unacceptable low frequency Column needs conditioning.

. Peaks elute very slowly

6. Peaks eluting too fast

7. Peak has flat top

8. Peak is misshapen, withconsiderable tailing

Peak is misshapen, with

considerable tailing

Carrier flowrate is too slow.

Carrier fiowrate is too high.

Electrometer has saturated.

Flow is too slow.

There is an improper injection

technique.

Compound is wronglymatched to column; perhaps

too polar.

Peak is developing from an

earlier injection (overlap of

peaks).

Try a new syringe.

Condition column.

Change septum.

Disassemble and check for

leaks around fittings, whileunder pressure, with soap

solution.

Condition column.

Adjust flowrate.

Dilute sample and repeat.

Adjust flow.

Repeat.

Select appropriate column.

Allow greater time between

injections, or install shorter

column.

301295

Exhibit. 15-3(continued)

Problem^ Probable Cause Remedy

i . - • • • ' • - ' • .Source OFF light stays on Batteries are low (if battery Plug in AC connector.

afterSmin. operation).

'Tube driver Is mismatched. Contact Photovac for

advice (416/881-8225).

.9. Electrometer does not Electrometer is saturated. Allow to self-purge,

return to zero after startup

If problems persist after trying all suggested remedies, contact Photovac Incorporated for advice.

' Photovac Inc.

Unit 2 .

134 Doncaster Avenue

Thornhill. Ontario, Canada L3T 1L3

416/881-8225 Telex: 066-964534

301296

Manual for Model PI-101 Photoionization Analyzer* HNU Systems Inc., 1975, lists the relative sensitivities forvarious gases.

15.2.3.2 Limitations

1. If the IP of a chemical contaminant is greater than the UV light source, this chemical will notbe recorded. Some contaminants cannot be determined by any sensor / probes.

2. It should be noted, specifically, that the HNU will not detect methane.i i

3. During cold weather, condensation may form on the UV light source window, resulting in er-roneous results.

I 4. Instrument readings can be affected by humidity and poweriines, making it difficult to inter-pret readings.

5. Total concentrations are relative to the calibration gas (usually benzene) used.Therefore,true contaminants and their quantities cannot be Identified. Also/while the instrument scalereads 0 to 2,000 ppm, response is linear (to benzene) from 0 to about 600 ppm. Greater con-centrations may be "read" at a higher or lower level than the true value.

6. Wind speeds of greater than 3 miles an hour may affect fan speed and readings, dependingon the position of the probe relative to wind direction.

15.2.4 Applicability

This procedure is applicable to HNU Pl-101 instruments used for air monitoring.

15.2.5 Responsibilities

The SM is responsible for monitoring the implementation of these procedures.

15.2.6 Records

Training records, maintenance records, and calibration records will be generated and maintained bythe responsible organization. The maintenance, calibration, and results obtained in the field will berecorded in the site logbook.

15.2.7 Procedure

15.2.7.1 Maintenance and Calibration Responsibilities

The instrument user Is responsible for properly calibrating and operating the instrument. When the in-strument is scheduled for or requires maintenance, these functions should be conducted only by qualifiedindividuals. If possible, maintenance responsibilities should be restricted to one or two individuals who willalso bear responsibilities lor logging the equipment in and out. Documentation of instrument user, dates of

301297

Exhibit 15-4RELATIVE SENSITIVITIES FOR VARIOUS GASES

(10.2 eV Lamp)

P-xylene

M-xylene

Benzene

TolueneDiethyl sulfide

. Diethyl amineSerene . • . . .

Trichloroethylene

Carbon disulfide

Isobutylene

AcetoneTetrahydrofuran

Methyl ethyl ketoneMethyl isobutyl ketone

CyclohexanoneMaptha (86% aromatics)

Vinyl chlorideMethyl isocyanate

IodineMethyl mercaptanDimethyl sulfide

Ally! alcohol

Propylene

Mineral spirits2,3-Dichloropropene

Cyclohexene

Crotonaldehyde

Acrdein

PyridlneHydrogen sullide

Ethylene dibrornide

N-octaneAcetaldehy.de Oxime

Photoionization

Sensltb

11.411.210.0 (reference standard)

8.97.1

5.15.0

301298

Exhibit 15-4(continued)

Species

Photoioniztion

Sensitivity*

Hexane

Phosphine

Heptane

Ally! chloride(3-chloropropene)

Ethyiene

Ethytene oxide

Acetic anhydride

Alpha pinene

Dibromochloropropane

Epichlorohydrin

Nitric oxider

Beta pinene

CitraJ

Ammonia

Acetic AcidNitrogen dioxide

Methane

Acetylene

Ethyiene

•Expressed in ppm (v/v).

Source: Instruction Manual for Model Pl-101

Photoionization Analyzer, HNU Systems, Inc., 1975.

301299

iiiiii

use, instrument Identification number, maintenance and calibration functions, and project identificationshould be maintained.

15.2.7.2 Operator Qualifications

The HNU,-although a relatively simple instrument to use, can be incorrectly operated H the user is notthoroughly familiar with Its operation. An appropriate training and certification procedure must bedeveloped and.Incorporated into the responsible organization's training procedures. The users must com-plete the training and be certified for HNU operation before using the instrument in the field. Refreshercourses should be obligatory every 6 months. Courses are given by the manufacturer, by commercial en-tities, and by EPA at their Cincinnati, Ohio, and Edison. New Jersey, facilities. .

15.2.7.3 Startup / Shutdown Procedures

Startup

1. Check the FUNCTION switch on the control panel to make sure it is in the OFF position. At-tach the probe to the readout unit. Match the alignment key, and twist the connector clock-

' wise until a distinct locking is felt.

2. Turn the FUNCTION switch to the BATTERY CHECK position. Check that the indicatorreads within or beyond the green battery arc on the scale plate. If the indicator Is below thegreen arc, or if the red LED comes on, the battery must be charged before using.

/ • .

3. To zero the instrument, turn the FUNCTION switch to the STANDBY position and rotate theZERO POTENTIOMETER until the meter reads zero. Wait 15 to 20 seconds to confirm that thezero adjustment is stable. If It Is not, then readjust.

4. Check to see that the SPAN POTENTIOMETER is set at the appropriate setting for theprobe being used (5.0 for 9.5 eV probe, 9.8 for 10.2 eV, and 5.0 for 11.7 eV).

5. Set the FUNCTION switch to the desired-ppm range. A violet glow from the UV lampsource should be observable at the sample Inlely at the glow, since eye damage could result.)

6. Listen for the fan operation to verify fan function.

I . source should be observable at the sample Inlet of the probe / sensor unit. (Do not look direct-

I7. Check instrument wtth an organic point source, such as a "magic marker," before survey toverify instrument function.

Shutdown

1. Turn FUNCTION switch to OFF.

2. Disconnect the probe connector.

3. Place the instrument on the charger.

I 301300

15.2.7.4 Maintenance and Calibration Schedule

function

• Perform routine calibration

Frequency

Prior to each use*

_-• _ Inrtiate factory checkout and-calibration _ Yearly or when malfunctioning-ofr-after changingUV light source

• Wipe down readout unit

• Clean UV light source window

• Clean the ipnization chamber

• Recharge battery

After each use

Every month or as use and site conditions dictate

Monthly

After each use.

During extended field us«, the HNU PM01 must be calibrated at least once every three days.

15.2.7.5 Calibration Procedure No. 1

For, HNU calibration canisters without regulators:. «

1. Run through startup procedures as in Subsection 15.2.7.3.

2. Fill a sampling bag with HNU calibration gas of known contents.

3. Connect HNU probe to sampling bag by using flexible tubing. .

4. Allow sample bag contents to be drawn into the probe, and check response in ppm.

5. Adjust the span potentiometer to produce the concentration listed on the span gascylinder.This procedure shall be followed only until the span potentiometer reaches the follow-ing limits:

9.5 eV10.2eV11.7 eV

Initial SpanPot. Setting

5.09.85.0

MaximumAcceptance Span

Pot Setting

1.08.52.0

6. If these limits are exceeded, the instruments must be returned for maintenance andrecalibration. This maintenance will be done only by qualified individuals.

7. Each responsible organization must develop a mechanism for the documentation of calibra-tion results. This documentation includes the following:

301301

. a. Date Inspected

b. Person who calibrated the instrument

c. The Instrument number (Serial number or other ID number)

d. The results of the calibration (ppm, probe eV, span potentiometer setting)' • ' . - .-r-vg-- ytatsfc;- • L _• '

e. Identification of the calibration gas (source, type, concentration)

15.2.7.6 Calibration Procedure No. 2

For HNU calibration canisters equipped with a regulator

1. Run through startup procedures as described in Subsection 15.2.6.3.

2. Connect a sampling hose to the regulator outlet and the other end to the sampling probe ofthe HNU. ' •

3. Crack the regulator valve.

4. Take a reading after 5 to 10 seconds.

5. Adjust span potentiometer using the steps outlined in step No. 5 of Subsection 15.2.7.5.

6. ^ Calibration documentation should be as in step No. 7 in Subsection 15.2.7.5.

15.2.7.7 Cleaning the UV Light-Source Window

1. Turn the FUNCTION switch to the OFF position, and disconnect the sensor / probe from theReadout / Contrd unit.

2. Remove the exhaust screw located near the base of the probe. Grasp the end cap in onehand and the probe shell in the other. Separate the end cap and lamp housing from the shell.

3. Loosen the screws on the top of the end cap, and separate the end cap and ion chamberfrom the lamp and lamp housing, taking care that the lamp does not fall out of the lamp hous-ing.

4. Tilt the lamp housing with one hand over the opening so that the lamp slides out of thehousing into your hand.

5. The lamp window may now be cleaned using lens paper with any of the following com-pounds:

a. Use HNU Cleaning Compound on all lamps except the 11.7 eV.

301302

b. Clean the 11.7 eV lamp with a freon or chlorinated organic solvent Do not useHMD cleaner, water, or water miscible solvents (i.e., acetone and methano!).

6. Following cleaning, reassemble by first sliding the lamp back into the lamp housing. Placethe ion chamber on top of the housing, making sure the contacts are property aligned.

7. "Place the end cap on top of the ion chamber, and replace the two screws. Tighten thescrews only enough to seaJ the 0-ring. Do not overtighten.

8. Line up the pins on the base of the lamp housing with pins inside the probe shell, and slidethe housing assembly into the shell.lt will fit only one way.

9. Replace the exhaust screw.

15.2.7.8 Cleaning the lonizatlon Chamber•

1. Turn the FUNCTION switch to the OFF position, and disconnect the sensor/probe from theReadout/Control unit.

2. Remove the exhaust screws located near the base of the probes. Grasp the end cap in onehand and the probe shell in the other. Separate the end cap and lamp housing from the shell.

3. Loosen the screws on the top of the end cap, and separate the end cap and ion chamber.'. from the lamp and lamp housing, taking care that the lamp does not fall out of the lamp hous-

ing. ' " ••

4. The ion chamber may now be cleaned according to the following sequence:

a. Clean with methanol using a Q-tip.

b. Dry gently at 50°C to 60°C for 1/2 hour.

5. Place the ion chamber on top of the housing, making sure the contacts are properlyaligned.

6. Place the end cap on top of the ion chamber and replace the two screws. Tighten thescrews only enough to sea) the 0-ring. Do not overtighten.

7. Line up the pins on the base of the lamp housing with pins inside the probe shell, and slidethe housing assembly into the shell. It will fit only one way.

15.2.7.9 Troubleshooting

The following steps should be performed only by a qualified technician:

1. The meter does not respond in any switch position (including BATT CHK).

a. Meter movement is broken.

301303

(1) Tip Instrument rapidly from side to side. Meter needle should move freelyand return to zero.

b. Electrical connection to meter is broken

•= (1) -Check.all wires leading,to meter.

(2) Clean the contacts of quick-disconnects.

c. Battery Is completely dead.

(1) Disconnect battery.

(2) Check voltage with a volt-ohm meter.

d. Check 2 mp fuse.

e. If none of the above solves the problem, consult the factory.

2. Meter responds in BATT CHK position, but reads zero or near zero for all others.

a. Power supply Is defective. .

(1)Check power supply voltages as" shown in Figure 11 of the HNU InstructionManual. If any voltage is out of specification, consult the factory.

b. Input transistor or amplffier has failed.

(1) Rotate zero control; meter should deflect up'or down as control is turned.

(2) Open probe. Both transistors should be fully seated in sockets.

c. Input signal connection is broken In probe or readout.

(1) Check input connector on printed circuit board. The input -connectorshould be firmly pressed down.

(2) Check components on back of printed circuit board. All connectionsshould be solid, and no wires should touch any other object

(3) Check all wires in readout lor solid connections.

3. Instrument responds correctly in BATT CHK and STBY but not in measuring mode.

a. Check to see that the light source is on. Do not look directly at UV light source,since eye damage could result.

0) Check high-voltage power supply.

f301304 I*

(2) Open end of probe, remove lamp, and check high voltage on lamp ring.

(3) If high voftage Is present at all above points, light source has probablyfailed. Consult the factory.

4. Instrument responds correctly In all positions, but signal is lower than expected.

a. Check span setting for correct value. :

b. Clean window of light source.

c. Double check preparation of standards.

d. Check power supply 180 V output

e. Check for proper fan operation. Check fan voltage.

f. Rotate span setting. Response should change if span potentiometer is workingproperly.

5. Instrument responds in all switch positions, but is noisy (erratic meter movement).

a. Open circuit in feedback circuiLConsult the factory.I • ' . .

b. Open circuit in cable shield or probe shield. Consult the factory.

6. Instrument response is slow and/or irreproducible.

a. Fan is operating improperly. Check fan voltage.

b. Check calibration and operation.

7. The battery indicator is low.

a. Indicator comes on if battery charge is low.

b. Indicator also comes on if ionlzation voltage is too high.

15.2.8 Region-Specific Variances

No region-specific variances have been identified; however, all future variances will be incorporated insubsequent revisions to this compendium. Information on variances may become dated rapidly. Thus,users should contact the regional EPA RPM for full details on current regional practices and requirements.

301305

PROCEDURE F-16

DISSOLVED OXYGEN METER

301306

tYSi MODEL 57

Dissolved Oxygen Meterinstructions

YSI IncorporatedYellow Springs Ohio 45387 USA

w- "'TABLE OF CONTENTS

DESCRIPTION i

SPECIFICATIONS .1

ACCESSORIES AND REPLACEMENT PARTS 3

PREPARING THE INSTRUMENT 4

CALIBRATION

Air Calibration .....5

The YSI 5075A Calibration Chamber 5

Air-Saturated Water Calibration 7

Winkler Titration 7

Calibration Tables 10

Table I: Solubility of Oxygen In Fresh Water ...10

Table II: Altitude Correction Factors 11

DISSOLVED OXYGEN MEASUREMENT 12

High Sensitivity Membrane 12

Recorder Output .,.12

Recorder Output Plug 13

MAINTENANCE 14

DISCUSSION OF MEASUREMENT ERRORS 15

WAJIRANTY AND REPAIR .' 17

SCHEMATIC.... : 8

DESCRIPTIONThe YSI Model 57 Dissolved Oxygen Meter is intended fordissolved oxygen and temperature measurement in waterand wastewater, but is also suitable for use in certain otherliquids. Dissolved Oxygen is indicated In mg/L (milligramsper liter) on 0-5, 0-10 and 0-20 mg/L scales. Temperature isindicated in 'C on a -5'to -M5'C scale. The dissolved oxygenranges are automatically temperature compensated forsolubility of oxygen in water and permeability of the probemembrane, and manually salinity compensated.

The probes use membrane covered Clark-type polarographicsensors with built-in thermistors for temperature measurementand compensation. A thin, permeable membrane stretchedover the sensor isolates the sensor elements from theenvironment, but allows oxygen and certain other gases toenter. When a polarizing voltage is applied across the sensor,oxygen that has passed through the membrane reacts at thecathode, causing a current to flow.

The membrane passes oxygen at a rate proportional to thepressure difference across it. Since oxygen is rapidly consumedat the cathode, it can be assumed that the oxygen pressureinside the membrane is zero. Hence, the force causing theoxygen to diffuse through the membrane is proportional tothe absolute pressure of oxygen ouiside the membrane. Ifthe oxygen pressure increases, more oxygeh diffuses throughthe membrane and more current flows through the sensor.A lower pressure results in less current.

SPECIFICATIONS

Oxygen MeasurementI*IV14*JWI VI > l ^ > i»

Ranges: 0-5, 0-10 and 0-20 mg/L (0-2.5, 0-5 and 0-10 mg/Lwith YSI 5776 High Sensitivity Membrane)

Accuracy: ±1% of full scale at calibration temperature (±0.1mg/L on 0-10 scale), or 0.1 mg/L (whichever is larger).

Readability: .025 mg/L on 0-5 scale; .05 mg/L on 0-10 scale;0.1 mg/L on 0-20 scale.

rTemperature Measurement

Range: -5° to *45°C-

Accuracy: ±0.5°C plus probe which is -KXTC

Readability: 0.25°C

Temperature Compensation±1% of DO reading for measurements made within ±5°C ofcalibration temperature.

±3% of DO reading over entire range of-5° to -M5°C probetemperature.

System Response TimeTypical response for temperature and DO readings is 90% in10 seconds at a constant temperature of 30°Cwiih YSI 5775Membranes. DO response at low temperature and low DOis typica l ly 90% in 30 seconds. YSI 5776 High SensitivityMembranes can be used to improve response at lowtemperature and low DO concentrations. If response limeunder any operating conditions exceeds two minutes, probeservice is indicated.

Operating Temperature RangeInstrument and probe operating range is -5° to +45°C. Largeambient temperature changes will result in 2% loss ofaccuracy unless Red Line and Zero are reset.

Recorder Output0 to 114-136 mV. Recorder should have 50,000 ohms:minimum input impedance.

Power Supply .Two C size batteries provide approximately 1000 hours x>foperation. ' .

ACCESSORIES AND REPLACEMENT PARTS•i' ' !

Oxygen Probes ii5720A: Self-stirring BOD bottle probe.

5750: Non-stirring BOD botUe probe.5730: Self-stirring Dissolved Oxygen probe for lab use.

5739; Dissolved Oxygen probe for field use. Use with theYSI 5740 detachable cable, listed below.

for the 5720A, 5739 and 5750YSI 5680: Probe Reconditioning Kit. Includes a sanding tooland ten adhesive disks.YSI 5775: Membrane and KCI Kii:, Standard. Includes two 15-membrane packets (.001" thick standard FEP Teflonmembranes) and a 30 ml bottle of KCI with Kodak Photo Flo.

YSI 5793: Membranes, Standard. Ten 15-membrane packets.YSI 5776: Membrane and KCI Kit, High Sensitivity. Includestwo 15-membrane packets (.0005" thick FEP Teflonmembranes) and a 30 ml bottle of KCI with Kodak Photo Flo.Used for measurements below 15°C,orforlow oxygen levels.

YSI 5794: High Sensitivity Membranes. Ten 15-membranepackets.YSI 5945: Six replacement sensor body O-rings.

YSI- 5486: Stirrer Boot Assembly, for the 5720A ONLY.

for the 5739 OnlyYSI 5075A Calibration Chamber.

YSI 5986 Diaphragm KitYSI 5740-10: 10'cable YSI 5740-100: 100'cableYSI 5740-25: 25' cable YSI 5740-150: 150' cableYSI 5740-50: 50' cable YSI 5740-200: 200' cable

YSI 5795A: Submersible Stirrer with 50' combined probe andstirrer cable.YSI 5492A: Battery Pack. Powers the submersible stirrer.

for the 5730 OnlyYSI 5732: Battery Adapter Cable.YSI 5731: Six Membrane Assemblies, and KCI with KodakPhoto Flo, plus a replacement sensor body O-ring.

woHU)HO

SPARING THE INSTRUMENTIt is Important that before the meter is prepared for use andcalibrated, it should be placed in the intended operatingposiiion: vertical, lilted, or on its back. Readjustment may benecessary when the Inst/ument operating position is changed.Prepare the probe as described In ihe probe instructions,then proceed as follows:

1. With the switch set to OFF, adjust the meter pointer to Zerowith the screw in the center of the meter panel. Readjustmentmay be necessary if the instrument position is changed. Donot force this adjustment, or you may damage the meter.

2. Switch 10 RED LINE and adjust the RED LINE knob untilthe meter needle aligns with the red mark at the 31'Cposition.

3. Switch to ZERO and adjust to zero with zero control knob.

4. A t t a c h the prepared probe to the PROBE connector of theinstrument and adjust the retaining ring finger tight.

5. Before ca l ibra t ing , allow 15 minutes for optimum probestabilization. Repolarize whenever the instrument has beenOF? or the probe has been disconnected.

CALIBRATION

Calibration is accomplished by exposing the probe to aknown oxygen concentration, such as water-saturated air(%), or water.of a known oxygen content (mg/L), and thenadjusting the calibration controls so the display shows areading matching the oxygen concentration of the knownsample.

The operator has a choice of three calibration methods:Winkler Titration, Saturated Water, and Air. Experience hasshown that air calibration is quite reliable, yet far simplerthan the other two methods.

Daily calibration is generally appropriate. Calibration can bedisturbed by physical shock, touching the membrane, foulingof the membrane or drying out of the electrolyte. Check calib-ration after each series of measurements. In time you willdevelop a realistic schedule for recalibration. When probesare not in use, store them as described In the probeinstructions.

Air Calibration -1. Place the probe in moist air. BOD probes can be placedin partially filled (50 rrvL) BOD bottles. Other probes can beplaced in the YS! 5075A Calibration Chamber (refer to thefollowing section describing calibration chamber) or thesmall storage bottle (the one with the hole In the bottom)along with a few drops of water. The probe can also bewrapped loosely in a damp cloth' taking care the cloth doesnot touch the membrane. Wait approximately 10 minutes fortemperature stabilization.

2. Switch to TEMPERATURE arid read. Refer to Table I:Solubility of Oxygen in Fresh Water, and determine calibrationvalue. i3. Determine altitude or atmospheric correction factor fromTable II. |I4. Multiply the calibration value from Table I by thecorrection factor from Table II. I

EXAMPLE: Assume a temperature of 21'C and an altitude of1100 ft From Table I, the calibration value for 21'C is 8.92mg/L. From Table H, the correction factor for 1100 ft. is about0.96. Therefore, the corrected calibration value Is 8.92mg/L x 0.96 - 8.56 mg/L j

5. Switch to the appropriate mg/L range, set the SALINITYknob to zero and adjust the CALIBRATE knob until the melerreads the correct calibration value from Step 4. Wait twominutes to verify calibration stability. Readjust if necessary.

t' - .

The YSI5075A Calibration ChamberThe Calibration Chamber is an accessory that helps obtainoptimum air calibration in the field. H is also a useful tool formeasuring at shallow depths (less than 4 feet) and in rapidlyflowing streams. It is used only with the YSI 5739 probe, andis illustrated in Figure 1. |

rH consists of a 4-1/2 foot stainless steel tube (1) attached tothe calibration chamber (2), the measuring ring (3), and twostoppers (4) and (5). !For calibration, insert the solid stopper (4) in the bottom ofthe calibration chamber (2). p|ush the oxygen probe (6)through the hollow stopper (5)iuntil the small end of the

• IE

stopper is situated at about the top of the notch where thepressure compensation unit is located. It is Important thatthis stopper be positioned so that 2 water-light seal is formedwhen the stopper and probe are inserted into the calibrationchamber.

Place the probe in the measuring ring (view C, below), andimmerse it in the sample for five minutes; this permits theprobe to come to the same temperature as the sample. Wetthe inside of the calibration chamber with fresh water tocreate a 100% relative humidity environment for calibration.Drain excess water from the chamber, shake any dropletsfrom the probe membrane, and promptly insert the probeinto the calibration chamber. Place the chamber in thesample for an addi t ional five minutes for final thermalequilibration. Calibrate the probe as described in the aircalibraiion procedure. Keep the handle above water at alltimes.

After calibration, return the probe to the measurement ringfor shal low measurements. Move the probe up and down, orhor izon ta l ly , approximately one foot a second whilemeasuring. In rap id ly flowing streams (greater than 5 feet persecond) install the probe in the measuring ring with thepressure compensating diaphragm towards the chamber.

Figure 1. The YSI5075A Calibration Chamber

Air-Saturated Water Calibraticm1. Air saturate a volume of water (300 to 500 mL) by aeratingor stirring for at least 15 minutes at a relatively constanttemperature.

2. Place the probe in ihe sample and stir. Switch toTEMPERATURE. Refer to Calibration Table I for the mg/Lvalue corresponding to the temperature.

3. Determine local altitude or thej'irue" atmospheric pressure(note that "true" atmospheric1! pressure is as read on amercury barometer. Weather Bureau reporting of atmosphericpressure Is corrected to sea level). Using Table II determinethe correct factor for your pressure or altitude.

4. Multiply the mg/L value from Table I by the correctionfactor from Table II to determine the corrected calibrationvalue for your conditions.EXAMPLE:Assume temperature - 21'C and altitude « 1100 ft.From Table I the calibration value for 21 'C is 8.92 mg/L.'FromTable II the correction factor for 1100 ft. is about 0.96. Thecorrected calibration value Is 8.92 mg/L x 0.96 - 8.56 mg/L.

5. Switch to an appropriate mg/L range, set the SALINITYknob to zero, and adjust the CALIBRATE knob while stirringuntil the meter reads the corrected calibration value fromStep 4. Leave the probe in the .sample for two minutes toverify calibration stability. Readjust if necessary.

Winkler Tilration1. Divide a volume of water into four samples. Determine theoxygen in three using of them Using the Winkler Titrau'ontechnique and average these values. If one of the valuesdiffers from ihe other 2 by more than 0.5 mg/L, discard thatvalue and average the remaining two.

2. Place the probe in the fourth sample and stir.

3. Set the SALINITY control to zero or the appropriate salinityvalue of the sample.

4. Switch to desired mg/L range and adjust the CALIBRATIONcontrol to the average value determined in Step 1. Allow theprobe to remain In the sample for at least two minutes beforesetting the calibration value, then leave it in the sample foran additional 2 minutes to verify stability. Readjust if

necessary. .' '

-r •SCHEMATIC

I ??« OK-r. JlI o . j j ' c ST?, W 4.SljC \\

NOTES: 1. Switch decks S-l-C through S-l-E contact the 0-5 position when theswitch b off.

2. A1J resistor values are in ohms. K • 1,000. M • 1,000,000.Unless otherwise specified, resistors are 1/4VC, 194, meul film.

3. Stirrer batteries ire optlonaj.

4. If my Instrument component vaJue differs from the vaJue on iheschematic, either value may be used

THS SCHFIUTC IS BEPBESE HTAHYE AND U»Y K SUGHRY Wff EflEWT FHOU THE CinCUT IH YWR KSTflUMEKTI I

Calibration TablesTable I shows the amount of oxygen in mg/L that is dissolvedin air saturated fresh water at sea level (760 mmHg atmospheric

U)oHU)HU)

Table II • Altitude Correction Factors

pressure) as temperature varies from 0' to 45'C. •

Table 1 • Solubility of Oxygen In Fresh Waler

Temp Solubilily Temp Solubility Temp Solubility'C mg/L 'C mg/L 'C mg/L

0 14.62 17 9.67 .34 7.071 14.22 18 9.47 35 7.952 18.83 19 9.28 36 7.843 13.46 20 9.09 37 6.734 13.11 21 8.92 38 6.62

' 5 12.77 22 8.74 39 6.526 12.45 23 8.58 40 6.417 12.14 24 8.42 41 8.318 11.84 25 8.26 42 6.219 11.56 26 8.11 43 6.12

10 11.29 27 7.97 44 6.0211 11.03 28 7.83 45 5.9512 10.78 29 7.69 46 5.8413 10.54 30 7.56 47 5.7414 10.31 31 7.43 48 5.6515 10.08 32 7.31 49 5.5616 9.87 33 7.18 50 5.47

Derived from 17th Edition, Standard Methods/or the Examination

of Water and Was tcrwa ter.

Table II shows the correction factor that should be used tocompensate for the effects of variation in atmosphericpressure or altitude. Find true atmospheric pressure in the .left hand column and read across to the right hand columnto determine the correction factor. (Note that "true"atmospheric pressure is as read on a barometer. Weather . t

Bureau reporting of atmospheric pressure is corrected to sea •level.) If atmospheric pressure Is unknown, the local altitude •may be substituted. Select the altitude in the center column jand read across to the right hand column for the correction

1 • •

factor.

Pressure Ininches Hg mm Hg kPa

30.23 768 102.329.92 760 101.329.61 752 100.329.33 745 99.329.02 737 98.328.74 730 97.328.43 722 96.328.11 714 95.227.83 707 94.227.52 699 93.227.24 692 92.226.93 684 91.226.61 676 90.226.34 669 89.226.02 661 88.225.75 654 87.125.43 646 86.1.25.12 638 85.124.84 631 84.124.53 623 83.124.25 616 82.123.94 608 81.123.62 600 80.023.35 593 79.023.03 585 78.022.76 578 77.022.44 570 76.022.13 562 75.021.85 555 74.021.54 547 73.021.26 540 71.920.94 532 70.920.63 524 69.9

ii' Altitude In Correclior

i Feet Meiers Factor (%

-276 -84 1010 0 100*J V 1 VV

970 oc onf 'lo oj yy

558 170 98841 256 97

1126 343- 961413 431 951703 519 94

' 1995 608 932290 698 922587 789 912887 880 903190 972 893496 1066 883804 1160 87

,4115 1254 86S4430 1350 854747 1447 845067 1544 835391 1643 825717 1743 816047 1843 806381 1945 796717 2047 787058 2151 777401 2256 767749 2362 758100 2469 748455 2577 738815 2687 729178 2797 719545 2909 709917 3023 69

20.35 517 68.9 10293 3137 6820.04 509 67.9 10673 3253 6719.76 502 66.9 11058 3371 66

Derived from !7th Edition, Star^t]Q of Water and Wcatewattr.

tfMetksdsfcr !bs Examination

^ \ \ / \ / / * \ r~ i i i tf— »^s i i r-» ft I r"K IT" ^^i^

DISSOLVED OXYGEN MEASUREMENT

1. With ihe instrument prepared for use and the probecalibrated, place Ihe probe in the sample and stir.

a. Stirring for the 5739 Probe can best be accomplished witha YSI submersible sUrrer. Turn the STIRRER knob ON. If thesubmersible stirrer is not used, provide manual stirring byraising and lowering the probe about 1 ft per second. If the5075A Calibration Chamber is used, the entire chamber maybe moved up and down in the water at about! ft. per second.

b.The YSI5720A and 5730 have built-in power driven stJrrers.

c. With the YSI 5750, sample stirring must be accomplishedbyother means, such as with the use of a magnetic stirring bar.

2. Adjust the SALINITY knob to the salinity of the sample.

3. Allow sufficient time for the probe to equilibrate to thesample temperature and dissolved oxygen. Read dissolvedoxygen.

High Sensitivity MembraneAn extremely thin membrane increases oxygen permeabilityand probe signal current, and hastens a probe's response;but it achieves this at the expense of ruggedness. For specialcircumstances, an 0.5 mil (.0005") membrane is available.(Order YSI 5776 Membrane and KC1 Kit, High Sensitivity.)This half-thickness membrane hastens response at lowtemperatures and helps suppress background current at verylow dissolved oxygen levels. (When data is routinely collectedwith sample temperatures below 15'C and at dissolvedoxygen levels below 20% air saturation, the low signalcurrent resulting from the use of the standard membranestends to magnify the probe's inherent constant backgroundsignal. Using the high sensitivity membranes in this situationwiJ! decrease the percentage of error due to the probe'sbackground current.) ,

Recorder Output . •Output at full scale is 114 to .136 mV.

Use a 50K or higher Input impedance recorder and operateIt with the terminals ungrounded.

'CVCv,an adj'USUble

s t h V * t y p e - u s e J h sst the full scale (span, range control, sensitivity, etc)

control to gjve full scale chart deflection with full sea eoxygen meter deflection. Refer to the recorder instrucJonFor recorders without this feature, the simple driver networkshown ,n Figure 2 can be constructed. This is adequate to

vT?' fU" SC3le Chart and ™'er ^flection onmv fixed range recorders.

Figure 2. Driver network for recordersfeature Mlhoutfull scale sensitivity

Recorder Oulpul Plug :

The parts necessary to construct a waterproof recorder plugfor the Model 57 are supplied with the instrument. The cableand potting materials are noi Included. (See Figure 3).General purpose epoxy potting materials of medium viscosityand moderate cure rate are recommended. The kits availablein hardware stores are satisfactory.

.1. Prepare the cable end by stripping back 3/16" (5mm) ofinsulation. Tin the ends with rosin core solder. If polarity isimportant, pin A Is the positive:00 terminal.

2. Disassemble the connector pieces and slide the mold, ring,extension, and coupling nut over the cable. Solder the leadsto the appropriate connector pins with rosin core solder.

3. Check all connections. The two leads should showelectrical continuity to the pins and should not contact thebody or each other. 1

4. Reassemble the pieces and hold the connector upright.Pour the epoxy mix Into the plastic mold until full . Refill asthe epoxy settles.

5. After the epoxy cures, the plastic mold may be removedwiih pliers or knife .

"(HO »I"G (XHNS10M NUT

Figure. 3. Recorder Output Plug assembly

MAINTENANCE

The case Is water resistant when properly closed. As aprecaution aga ins t damaged gaskets or loose f i t t ings , theinstrument case should be opened and inspected for moisturewhenever the instrument has been subjected to immersionor heavy spray. The instrument case is opened by removingthe screws on the rear cover and l i f t ing the cover off.

The batteries that operate the instrument are the two C sizecells located inside the case at the meter end. These shouldbe replaced when the RED LINE knob is at its extremeadjustment or at least annually. The amount of remainingadjustment is an indication of the battery condition. Observepolarity when Installing new batteries; the positive (+) endfits into the red washer on the battery holder. (See Figure 4.)

LJoHU)HU1

l NI-C*0 M C M A U G f A t l tSU8M(«s»l l S l l f tMA SAt lCmls

otsroUeuCA«ION.{INCINSIItUMCM'B»mmts

Figure 4. Battery placement in the Model 57

(57$ mad* in«r$irt i l no. U772 hm jtlrrerbattiry polarity ravirstd from Illustration above.)14

DISCUSSION OF MEASUREMENT ERRORS

This discussion can be used to attach a confidence to anyparticular reading of dissolved oxygen.

There are three basic types of errors. Type 1 errors are relatedto limitations of the instrument design and tolerances of theinstrument components. These are chiefly the meterlinearityand the resistor tolerances. Type 2 errors are due to basicprobe accuracy tolerances, chiefly background signal, probelinearity, and variations in membrane temperature coefficient.Type 3 errors are related to the operator's ability to determinethe conditions at the time of calibration. If calibration isperformed against more accurately known conditions, type3 errors are appropriately reduced.

Type 1 Errorsa. Meter linearity error: ±1% of ful l scalereading

b. Mode-to-mode error due to taking a reading on a differentrange of the instrument than the calibration range:

one range away: ±1% of readingtwo ranges away: ±2%jbf reading

c. Salinity compensation circuit error:±2.5% of meter reading x'l T""1??""0 ,] 40 pjx »Ulnlijr

Type 2 Errors ;a. Probe background current error: ±.005 x (l-a/b)c

a - calibration value i;b • solubility of oxygen in fresh water at 760 mm Hg and

at measurement temperaturec » measured DO value

b. Probe nonlinearity error: ±0.3% of reading' t .

c. Error due to probe membrane temperature coefficientvariability:

readings taken at calibration temperature: none

readings taken within 5°C of calibration temperature:±1% of reading ;, • .

readings taken u nder a!! other conditions: ±3% of reading

U)oHWV-1

3 Errorsa. Errors due to Instrument thermometer accuracy when

used to measure the exact probe temperature duringcalibration: ±1.5% of reading

h. Error due to barometric pressure uncertainty of ±13mmHg: ±1.7% of reading

c. Error due to altitude estimation uncertainty of ±500 ft:±1.8% of reading

d. Errors due to variation in humidity. If the actual RH at theLime of calibration is 50% instead of 100%, the error willbe as follows:

calibrationtemp. In °C

0102030-10

error in %of reading

±0.3±0.6±1.15±2.11±3.60

Error Calculation ExampleThis example presumes that air calibration is used. Ifcalibration is done with air-saturated water, the relativehumidity consideration (3d) fs eliminated. If the Winklercalibration method is used, type 3 errors are replaced by theuncertainty attributable to the overall Winkler determination.

Calibration conditions:

air calibration25°C2000 ±500 feetnormal assumed7.8 mg/L10 mg/L mode

method:temperature:altitude:bar. pressurecalibrated to:calibrated in:

Measurement conditions:

temperature: 20°Creading: 4.5 mg/Lmode: 5 mg/Lsalinity: 20 ppt

rTYPE DESCRIPTION

la linearity

mode change

salinity

, CALCULATION

ERROR (mg/LJ0^1 rn xr / f-t-v.ui />. to ±0.0/15

±0-01 X 4.5 ±0.045

±0.025 X 4.5 X (20/40) i0.056-. r W»W»V^V

probe background ±0.005 X(l-7.8/9.07) X4.5 ±0.003

probe linearity ±0.003 X 4.5 ±0.014

temp, compensation ±0.01 X 4.5 ±0.045

temp, measurement ±0.015 X 4.5 ±0.068

pressure ±0.017 X 4.5 ±0.076

altitude ±0.018X4.5 ±0.081

RH ±0.016X4.5 ±0.072

maximum possible error «• ±0.505 mg/L

It Is unlikely that the actual error In any measurement will bethe maximum possible error. A better error indication isobtained by an r.m.s. calculat/on:

r.m.s, error - (.0451 + .045' + 056' + .003*' + .OH1 + .045'+.058' +.076* + .081' + .072' ]1/J - ±.178 mg/L

WARRANTY AND REPAIR

All YSI products carry a one-year warranty on workmanshipand parts, exclusive of batteries. Damage through accident,misuse, or tampering will be repaired at a nominal charge,if possible, when the item is returned to the factory or to anauthorized YSI dealer.

If you are experiencing difficulty with any YSI product, itmay be returned for repair, even If the warranty has expiredYSI maintains complete facilities for prompt servicing for allYSI products. I

Product Service Department .Yellow Springs Instrument Co., Inc.1725 Brannum LaneYellow Springs, Ohio 45387, U.S.A.

Phone: (513) 767-7241, (800) M3-HELP, Telex: 20-5437Fax (513)767-9353

YSI MODEL 57 OPERATING INSTRUCTIONST: Srftxr uw>c ma ins/umcm. oftrjwcs. UVHik! bt UmUjr

c UoOd 57 nuniuf tnu »itti It* 5700 Sfrin aifjen (WXn insvuaions.YSI Incorporated

Ydlirw Sf>"nR> livarunvrm Co.. Inc. Yellow Springs. Ohio 45 JB7 USA

SCTUP1 . Pi epa/ « and connect a YSJ 57OO Series dissolvedoryoen probe. (S*e probe- irtsznjciion sstrtmert manuaJ kx mons details,)

2. Wan iastPv*T*ert C/J. w^ust rnrtcrl**n i nooessiry.

3. Sw** to RED UN£ fcxl »djosi tf nccesiary.4. S~vKh 10 2£flO * d ndjusi ID 0 on m^ scale.

CALB3RATK>«lOCTX A« SATURATION

r cakxarion procwJkX^s »re 6escnbe<3 in theCAUaflATlON vftdxxi o* your instrumer* manual.)

r . (P\*ce 5739 pojbc In caJtoratioo botOe wrthmoifl Spon9eor wrap in moisl ckXIl to prwieJ*naMo rvrrxiiry.) Wa>

2. S«i SAJJN/TY contro* to FRESH.3. Swttft toTEMP and r«ad on *C scale.4. L>» poab* le<r<x» Iijro reading and IAM localdmoe^xnc pressure (or tort abow sea tewl) loOcienwe ca)>txaton values Irom T*JS« I and 11.

EXAMPLE:

ltxai'on value to/ 2l"C is

F rc-n Tatx H (Tx afutuo> tacux kx 1 000 ft. isiitxjut5€.

T>»s ccxrea caTtxarton value is: 8.92 mgl. x .96

5,&»iich»otT>e 0- 5,O- 10 or 0- 2O range and adjusl• with (^AllBRATE control lo if>e caJ<xation vakx

MEASUREMEKT1 . Adjust SALINITY control 10 saWvty ot lArr&t.2. Piaca calibrated probe in sample and si'tf.3. Wart unti you can Jtscwuin probe eQjiftxalionby observing temperature and d»ssotv«d oxyoenreadings thai an* siabie kx • lufl minute.4. Read drsso*ved o*yoen on appropriate scale(0-S,0-10ofO-20m$'L).5. The instrumert stxxAJ normal be left on duringme working day lo avoid the CeUy of waning kxprobe repolanution.

1 . Replace instnxncrt bat levies whenever you can-no( mak* the RED LINE adjustmenL

2. ki the BATT CHECK position on the ST1RRERjwflch. the voftaoe & ihe nirtef baitencs »s tfs-pUy«don the redO-10scaic. Do not pe«nvt them lodisctiaroe beto** 6 vofts. B baneries are recharoe-at^e.use YSt 5728 cha/ye* kx 14-1 6 hours.3. RepUce membrane every 2 lo 4 weeks Depend-ing on application. Probes mxrtd be suved in a

d envi<Onrr»erU lo pfevrru Crying ovrt.

»« TJJ

MU«1J«Utrj

•M n.t

b.«« »n

£«•*8

301317

PROCEDURE P-18

KECK INSTRUMENTS, INC.KIR-89 INTERFACE PROBE

Powell Environmental Services/ Inc.REVISED: MARCH 18, 1993

301318

INSTRUCTIONMANUAL

KIR-89Interface Probe

and Reel

301319

TABLE OF CONTENTS

x'rt •:•'!

I N T ; R O C N

: i N $ C E PROBE & REEL

PROCEDURE

^DECONTAMINATION & CLEANING

:5!T BATTERY REPLACEMENT

6. WARRANTY & REPAIRS

Vr!\V"S5S

JL_J..

Df*!™4 '\^:\-

*X^V "\ •> v^ ^ "•'?lS£S^ s\-X N\,J£5$35 ^^-N-* v.N>5

301320

1 INTRODUCTION

KIR-89INTERFACE PROBE & REEL

The Keck Instruments, Inc. KIR-89 InterfaceProbe is a portable reel-mounted instrumentcapable of providing accurate product leveland thickness with water level measurements.The KIR-89 features aTefzelcoated engineer'stape marked in feet and 10Oths of afoot perma-ne'ntly affixed to a polypropylene downholeprobe. The. probe uses a phenolic float todetect product level and a pair of stainless steelcontacts for conductive fluids (water). Thepresence of product and water is indicated bythe following devices:

1. Visual indicator (red light)2. Audible indicator (buzzer)

The instrument is powered by a replaceable 9volt DC battery mounted behind the KIRfaceplate.

THEORY OF OPERATION

When the KIR-89 Probe is lowered down thewell, the float switch will activate the light andaudible signal at the first fluid level. The floatwill detect any .fluid with a specific gravity of .75or greater. As the probe is lowered deeper intothe well the stainless steel contacts touch water(a conductive fluid), the steady light and theaudible signals will begin to oscillate. If the firstfluid is not water, and therefore non-conduc-tive, the emitted light and audible signals will becontinuous.

301321

2 INTERFACE PROBE&REEL

Retaining Clip

Carry Handle

Reel Handle

Storage Reel

Face Plate

Engineer's Tape

Downhole Probe

301322

FACEPLATE

KECK INSTRUMENTSKJR-89

0 Power On/Off Switch

Light Signal

Battery Test Button

KIR-89 PROBE

Engineer's Tape

Polypropylene Probe

Float Shaft

Adjustable Contact

Phenolic Float

"E"Clip

301323

3 OPERATION PROCEDURE

Testing Battery, Signals IMPORTANT

SteplTurn the instrument power switch to on andpress the battery test button. A loud audiblesignal and bright light indicates adequate bat-tery voltage tor proper operation.

Step 2Remove the probe from the retaining clip andengage the phenolic float. A continuous au-dible signal and light should be present. With .the float engaged, moisten fingertips and makecontact with the float shaft and the adjustablecontact. The steady tone and light should beginto oscillate thus indicating proper operation ofthe device.

Measuring Fluid Levels

Step 1Lower the KIR-89 probe down the well until acontinuous audible signal and light is indicated.Take the footage measurement from the tape atthe top of casing or other reference point andrecord this figure as the first fluid level.

Step 2Continue to lower the probe until the audiblesignal and light begin to oscillate. Record thefootage measurement from the reference pointas the perond fluid level.

To maintain an accuracy of plus or minus0.01 ft., the specific gravity of the product tobe measured must be accounted for. Tocalculate the required correction factor,identify the specific gravity of the product,then refer to the "Measurement Correction"chart on page 7. The correction factor willbe used in the following equations.

Calculating Product Thickness

Subtract the first fluid level from the second fluidlevel, then add the specific gravity correctionfactor taken from the chart on page 7. This isthe thickness of the product layer.

Example:Specific gravity of product = 0.81st fluid level = 10.0'2nd fluid level = 12.5'Correction factor from chart = -0.015'12.5' -10.0' + (-0.015') = 2.485' productthickness

Calculating Product Level

Add the specific gravity correction factor takenfrom the chart on page 7 from the first fluid level.This is the product level.

ExampleSpecific gravity of product = 0.9first fluid level = 15.25'Correction factor from chart = -0.007'15.25' + (-0.007') = 15.242' product level

301324

Measuring Water Levels in_Pr_c.d ucLFre_e_WeJ Is

The lack of a continuous tone and light with anoscillating audible signal and light will indicateabsence of any nonconductive fluid .on thesurface of the water.

QUESTIONS? Call 1-800-542-5681ii

301325

OmQ.co

KIR-89MEASUREMENT

CORRECTION CHART

-0.030 -0.022 -0.015 -0.007 0.000 0.007

CORRECTION FACTOR

Factor = 0.075 (specific gravity) - 0.075

301326

f4 II HUH DECONTAMINATION &

CLEANINGCleaning Procedure

the KlR-89 can bexleaned with ahy^etergent-such as Trisodium Phosphate (TSP), Alkenox'or Liquenox. If other detergents are used, careshould be taken to select detergents that arecompatible with polypropylene, stainless steeland phenolic materials. The reel should not besubmerged in any liquid, but can be cleaned bywiping with a damp cloth.

If the float becomes covered with silt or mud,remove the bottom "E" clip, slide the float off theshaft and clean both the float and stainless steelshaft. Replace the float with the word "CLOSED"pointing toward the top of the probe and replacethe "E" clip.

8301327

BATTERY REPLACEMENT

Battery Replacement Procedure Step 5

Replace the battery when the audible signaland light become reduced in their intensity, asfollows:

SteplRemove the three screws from the faceplate.

Step 2Gently pull the faceplate out of the reel. Ob-serve the orientation of the faceplate and thebattery.

Step 3Replace with a new 9 volt DC transistor battery(grasp black connector, not the wires).

Step 4Position the battery in the notch of the printedcircuit board and align the battery with therecessed slot in the bottom of the cavity of thereel.

to^scwnnfre'reelrb

The faceplate may have to be rotated back andforth slightly so the battery will drop into therecessed slot in the bottom of the reel.

Step 6Replace the three screws through the faceplateand into the reel. Again the faceplate may haveto be rotated back and forth so the screws willline up with their respective holes.

Step?Check for operation as outlined in section 3 olthis manual, "Operation Procedure".

Step 8If the KIR-89 is to be stored for long periods oftime while not in use, it is recommended thatthe battery be removed.

QUESTIONS? Call 1-800-542-5681.

301328

KECK INSTRUMENTS, INC.

The Keck "Tape Guard" was developed toprotect instrumentation, tapes and sample tub-ing from the wearing edges of well casing.Made of smooth flexible polystyrene, the "TapeGuard" easily adapts to any 2" or 4" well.

Instructions _Simply compress the Tape Guard" and insert

FIGURE 1TAPE GUARD

FIGURE 2TAPE GUARD USAGE

into the opening of any 2" to 4" well pipe. Allowinstrumentation, tubing or tape to ride on thesmooth surface of the "Tape Guard" to preventwear.

301329

PROCEDURE F-19

GEOPROBE MACRO-CORE ANDLARGE-BORE SAMPLING DEVICES

PowelKHarpstead, Inc.

301330

GEOPROBE MACRO-CORE® SOIL SAMPLER

STANDARD OPERATING PROCEDURE

Technical Bulletin No. 95-8500

PREPARED: November, 1995

REVISED: September, 1996

+ V^ v P-S

A. Previously cored or pre-probed hole with sloughed soil.B. Closed-piston sampler driven to next sampling interval.

C. Releasing piston assembly.D. Closed-positon sampler filled with soil.

SAMPLING WITHTHE MACRO-CORE® CLOSED-PISTON SOIL SAMPLER

301331

nGeoprobe SystemsA DIVISION OF KJEJR ENGINEERING

Geoprobe® is a RegisteredTrademark ofKejr Engineering, Inc., Salina, Kansas

Macro-Core®is a RegisteredTrademark ofKejr Engineering, Inc., Salina, Kansas

or by any means, electronic or mechanical, including photocopy,recording, or any information storage and retrieval system, without

permission in writing from Kejr Engineering, Inc.

IStandard Operating Procedure

301332Page 2 Macro-Core* Soil Sampler

1.0 OBJECTIVE

The objective of this procedure is to collect a soil sample at depth and recover it for visual inspection and/orchemical analysis.

2.0 BACKGROUND

2.1 Definitions

Geoprobe* Soil Probing Machine: A vehicle-mounted, hydraulically-powered machine that utilizesstatic force and percussion to advance small diameter sampling tools into the subsurface for collecting soilcore, soil gas, or groundwater samples.* Geoprobe is a registered trademark ofKejr Engineering, Inc., Salina, Kansas

Macro-Core® Soil Sampler*: A 48-inch long x 2.0-inch diameter (1219 mm x 51 mm) soil samplercapable of recovering a sample that measures up to 1300 ml in volume in the form of a 45-inch x 1.5-inch(1143 mm x 38 mm) core. The Macro-Core® Sampler may be used for open-tube as well as closed-pistonsampling.* Macro-Core® is a registered trademark of Kejr Engineering, Inc., Salina, Kansas

Liner: A 46-inch longx 1.75-inch diameter (1168 mmx44 mm) removable/replaceable, thin-walled tubeinserted inside the Macro-Core® sample tube for the purpose of containing and storing soil samples. Linermaterials include stainless steel, Teflon®, PVC, and PETG.

2.2 Discussion

In this procedure, the assembled Macro-Core Soil Sampler is attached to the leading end of a Geoprobeprobe rod and driven into the subsurface using a Geoprobe soil probing machine. Additional probe rodsare connected in succession to advance the sampler to depth. The Macro-Core Sampler may be used as anopen-tube or closed-piston sampler.

The simplest and most common use of the Macro-Core Sampler is as an open-tube sampler (Fig. 2.1 A). Inthis method, coring starts at the ground surface with an open-ended sampler. From the ground surface, theMacro-Core Sampler is advanced 48 inches (1219 mm) and retrieved from the hole with the first soil core.In stable soils, the open-tube sampler is inserted back down the same hole to obtain the next core. Geoprobeoperators have reported coring to depths exceeding 30 feet (9 m) with this method.

In unstable soils which tend to collapse into the core hole, the Macro-Core Sampler can be equipped witha closed piston assembly (Fig. 2. IB). This assembly actually locks into the cutting shoe and prevents soilfrom entering the sampler as it is advanced in the existing hole.

The Macro-Core Closed-Piston Sampler is not designed to be driven through undisturbed soil. Soil is firstremoved to sampling depth with an open-tube sampler, or a pilot hole may be made with a Macro-CorePre-Probe. A closed-piston tip is then installed and the sampler is inserted or driven back down the samehole. When the lead ing end of the sampler reaches the top of the next sampling interval, the piston isunlocked using extension rods inserted down the inside of the probe rods.

Standard Operating Procedure Page 3 Macro-Core® Soil Sampler301333

Once the piston is relieved, the sampler is simply driven another 48 inches (1219 mm). Soil entering thesampler pushes the piston assembly to the top of the sample liner where it is retrieved upon removal of thesoil liner and core.

Loose soils will sometimes fall out of the Macro-Core Sampler as it is retrieved from depth. The Macro-Cere Core Catcher(Fig. 2.-l-)-v/3s*designed to alleviate this problem. "Excellent results are obtainecl when:

the core catcher (sometimes called a basket retainer) is used with saturated sands and other non-cohesivesoils. A core catcher is not necessary when sampling tight soils and may actually inhibit sample recovery.Constructed of PVC, the core catcher may be used with PVC, PETG, Teflon®, and stainless steel liners..

Standard Operating Procedure301334

Macro-Core* Soil Sampler

A. Open-Tube System

MC Drive Head

MC SampleTube

MC Liner (Inside)

MC Core Catcher

MC Cutting Shoe

MC ReleaseRod

MC LockingRing

MC PistonTip

B. Closed-Piston System

FIGURE2.1

Macro-Core® Soil Sampler Assemblies

PageS Macro-Core® Soil Sampler

3.0 REQUIRED EQUIPMENT

le following equipment is required to recover soil core samples using the Geoprobe Macro-Core Soil Samplerand probing system. Note that sample liners are available in three different materials. Liner material should beselected based upon sampling purpose, analytical parameters, and data quality objectives. Figure 3.1 identifiesthe major components of-the-Macro-Coresamplerr •— ~ ~~ - — - — - -

MACRO-CORE SAMPLER PARTS*

MC Drive Head, 1-inch probe rod (optional)MC Drive Head, 1.25-inch probe rodMC Sample Tube, Ni-platedMC Sample Tube, unplated (optional)MC Cutting Shoe.MC Cutting Shoe, heavy-duty (optional)MC Cutting Shoe, 0.125 inch undersized (optional)MC Piston BoltMC Piston WasherMC Locking Ring AssemblyMC Piston Tip AssemblyMC Piston Release RodMC Combination WrenchNylon Brush For MC Tubes

MACRO-CORE SAMPLER ACCESSORIES*

MC Stainless Steel LinerMC Teflon® Liner AssemblyMC PETG LinerMC Vinyl End Cap (black)MC Vinyl End Cap (red)MC Core Catcher (optional)MC Spacer RingMC Locking Ring SpringMC PVC Heavy-Duty Liner Assembly

CEOPROBE TOOLS**

Drive Cap, fits 1.25-inch probe rodPull Cap, fits 1.25-inch probe rodProbe Rod, 1.25 inch x 36 inchesProbe Rod, 1.25 inch x 48 inchesMC Pre-Probc, 2 inchMC Pre-Probe, 2.5 inch (optional)MC Pre-Probe, 3 inch (optional)Extension Rod, 36 inch (optional)Extension Rod, 48 inchExtension Rod CouplerExtension Rod HandleExtension Rod Quick Links (Optional)

ADDITIONAL TOOLS

Locking PliersAllen Wrench, 1/8 inchPipe WrenchHook Blade U t i l i t y Knife

QUANTITY

-2--2-

QUAMrry

VariableVariableVariableVariableVariableVariableVariableVariableVariable

QUANTITY

-1--1-

VariableVariable

-1--1--1-

VariableVariableVariable

-1-Variable

QUANTITY

-1--1--2-

PART NUMBER

AT-8510

AT-8512AT-8520AT-8522AT-8530AT-8535AT-8537AT-8540AT-8550AT-8560AT-8570AT-8580AT-8590BU-700

PART NUMBER

AT-7235AT-724AT-725SAT-726BAT-726RAT-8531AT-8532AT-8561AT-925S

PART NUMBER

AT-1200AT-12 04AT-1236AT-124 8AT-147BAT-151BAT-152B.AT-67AT-671AT-68AT-69AT-694K

* K i t s provide parts in various combina t ions . Parts l is ted are not sold separately. Refer to page 34 fo ra list ing of availablek i t s and specific components.

** Probe rods and accessories are also avai lable in 1-inch O.D. (outside diameter).

Standard Operat ing Procedure301336

Macro-Core® Soil Sampler

MC Drive Head -(AT-8510.AT-8512)

MC Combination Wrench(AT-8590)

MC Core Catcher(AT-8531)

MC Spacer Ring(AT-8532)

MC Piston Bolt(AT-8540)

MC Piston Washer(AT-8550)

MC Locking Ring(AT-8560)

MC PistonTip Assembly(AT-8570)

MC Cutting Shoe(AT-8530, AT-8535, AT-8537)

MC SampleTube(AT-8520, AT-8522)

MC Release Rod(AT-8580)

FIGURES.!Macro-Core® Soil Sampler Paris

Standard Operating Procedure 301337 Page? Macro-Core® Soil Sampler

4.0 OPERATION

Size and material options have resulted in an extensive list of Macro-Core part numbers. To simplify theinstructions presented in this document, part numbers are listed in the illustrations only. Refer to page 6 for acomplete parts listing. Section 5 contains a complete listing of Macro-Core kits available.

4.1 Decontamination

! Before and after each use, thoroughly clean all parts of the soil sampling system according to projectrequirements. A new, clean liner is recommended for each use if using PETG, PVC, or Teflon® liners.

Stainless Steel Liners from Geoprobe Systems are cleaned at the factory with an agitated detergent bath ata temperature of approximately 180 degrees F. After rinsing with 180-degree tap water, the liner is airdried, wrapped in PVC outer cladding, and capped with vinyl end caps.

Thoroughly clean the sampler before assembly, not only to remove contaminants but also to ensure correctoperation. Dirty threads complicate assembly and may lead to sampler failure. Sand is particularlytroublesome as it can bind liners in the sample tube resulting in wasted time and lost samples.

4.2 Field Blank

It is suggested that a field blank be taken on a representative sample liner prior to starting a project and atregular intervals during extended projects. Liners can become contaminated in storage. A field blank willindicate that the liners do not carry contaminates which can be transferred to soil samples. The followinginformation is offered as an example method which may be used to take a field blank. Make the appropriatemodifications for the specific analytes of interest to the investigation.

Example Procedure:REQUIRED EQUIPMENT

MCLiner (1)MC Vinyl End Caps (2)Decontaminated Aluminum Foil Squares, 3 in. x 3 in... (2)Distilled Water (100ml)VOA Vial (or other appropriate sample container) (1)

1. Place a foil square and a vinyl end cap on one end of the liner.

2. Pour 100 mill i l i ters of dist i l led water (or other suitable extracting fluid) into the liner.

3. Place a foil square and a vinyl end cap on the open end of the liner.

4. From the vertical position, repeatedly invert the liner so that the distilled water contacts the entireinner surface. Repeat this step for one minute.

5. Remove one end cap from the liner, empty contents into an appropriate sample container, and cap thecontainer.

6. Perform analysis on the extract water for the analytes of interest to the investigation.

Standard Operating Procedure Page 8 Macro-Core® Soil Sampler301338

4.3 Open-Tube Sampler Assembly

la. With MC Core Catcher. Place the open end of an MC Core Catcher over the threaded end of an MCCutting Shoe as shown in Figure 4.1. Apply pressure to the core catcher until it snaps into the machinedgroove on the cutting shoe.

1 - - -'--'——-"Hs=:3^=^- . _ . . . • • _ _ _ _ - . _ , _ „ , : • . . . .

NOTE: AT-725S (PETG) liners have a swedged end which is generally slipped directly over thegroove in the cutting shoe (Fig. 4.2). To use a core catcher with these liners, simply cut approximately0.45 inches (10 mm) of material from the swedged end of the liner and proceed to Step 2

Ib. Without MC Core Catcher. Push the base of an MC Spacer Ring onto the threaded end of a cuttingshoe until it snaps into place (Fig. 4.3).

NOTE: With the exception of AT-725S (PETG) liners, all liners must utilize either a spacer ring orcore catcher. PETG liners have a swedged end which slides directly over the end of the cutting shoe.Attach the liner to the cutting shoe (Fig. 4.2) before proceeding to Step 2.

2. Thread the cutting shoe into one end of an MC Sample Tube (Fig. 4.4). Tighten until the end of thesample rube contacts the machined shoulder of the cutting shoe.

3. Insert the appropriate liner into the sample tube (Figure 4.4). (The liner is all ready installed if usingPETG liners without a core catcher).

4. Connect an MC Drive Head to the lop of the sample rube (Fig. 4.4) and securely tighten with the MC. Combination Wrench (Fig. 4.5). The end of the sample tube must contact the machined shoulder of the

drive head.

MC Core Catcher MC Cutting Shoe(AT-8531) (AT-8535 or AT-8537, above)

(AT-8530, below)

Correct Attachment ofMC Core Catcher to MC Cutting Shoe

FIGURE 4.1Macro-Core® Core Catcher Attachment

rtTt \

MCPETG Liner(AT-725S)

MC Cutting Shoe(AT-8535 or AT-8537, above)

(AT-8530, below)

Correct Attachment ofSwedged PETG Liner

to Cutting Shoe •

FIGURE 4.2Macro-Core® PETG Liner Attachment

MC Cutting Shoe(AT-8535 or AT-8537, above)

(AT-8530, below)

Correct Attachment ofMC Spacer Ring toMC Cutting Shoe

FIGURE 4.3Macro-Core® Spacer Ring Attachment

MC Drive Head(AT-8510orAT-8512)

MC SampleTube(AT-8520orAT-8522)

MC Liner(AT-7235, AT-724,AT-725S, AT-925S)

MC Core Catcher (AT-8531, shown) or MC Spacer Ring (AT-8532)

MC Cutting Shoe(AT-8530, AT-8535, AT-8537)

FIGURE 4.4Macro-Core® Open-Tube Sampler Assembly

Tighten/LoosenMC Piston Bolt

Tighten/LoosenMC Drive Head

Tighten/LoosenMC Cutting Shoe

FIGURE4.5Macro-Core® Combination Wrench Applications

ClosedrPiston Sampler Assembly (Fig. 4.6)

1. Install an O-ring in the machined groove on the piston bolt head (A) and piston tip (B).

2. Place a piston washer on a piston bolt with the radius side away from bolt head.

3. Position a locking ring on the piston bolt and thread the bolt into the piston tip.

NOTE: Piston bolt and tip are left-hand threaded.

4. Screw the piston bolt down tight and install a 1/4-inch-20 x 1/4-inch half dog set screw in the hole on. the side of the piston tip. With a 1/8-inch alien wrench, tighten the set screw until it contacts the stem

of the piston bolt, then back it out one-quarter turn.

5. Back the piston bolt out until set screw hits the bottom shoulder on the bolt (approximately four fullturns). The bolt must be tight against the set screw to prohibit the set screw from turning while completingStep 6.

6. Lock the half-dog set screw into place by installing a 1 /4-inch - 20 x 3/16-inch cup point set screw in thesame hole. The cup point set screw should be tight but the bolt should remain free to turn approximatelyfour full turns.

O-Ring MC Piston Bolt(AT-8540)

MC Locking Ring(AT-8560)

O-Ring Groove" ' (A)

MC Piston Washer(AT-8550)

Assembled Macro-Core Piston

1/4-in. -20x3/16 in.Cup Point Set Screw

1/4 in. - 20x1/4 in.Half Dog Set Screw

O-Ring Groove(B)

IO-Ring MC Piston Tip

FIGURE 4.6Macro-Core® Piston Assembly

NOTE: The top of the cup point set screw must not protrude from the piston tip. File or grind the setscrew flush with the side of the tip if necessary. The piston assembly is ready to install in the cuttingshoe.. . .. . •

7. Slide an assembled piston into a cutting shoe. The piston should be placed so that one half of the seti^

8. Tighten the piston bolt (left-hand threads) using the combinationwrench (Fig 4.8).

9a. With MC Core Catcher. Place the open end of a core catcherover the threaded end of a cutting shoe (Fig. 4.9). Apply pressureto the core catcher until it snaps into the machined groove on thecutting shoe.

NOTE: AT-725S (PETG) liners have a swedged end which isgenerally slipped directly over the groove in the cutting shoe (Fig.4.10). To use a core catcher with these liners, simply cut

. approximately 0.4 inches (10 mm) of material from the swedgedend of the liner and continue to Step 10.

Figure 4.8. UsingMC Combination Wrench to

tighten MC Piston Boltinside MC Cutting Shoe.

MC Piston Assembly MC Cutting Shoe(AT-8530, shown or AT-8535, AT-8537)

Correct Position ofPiston Assemblyin Cutting Shoe

MC Curling Shoe (AT-8535) MC Cutting Shoe (AT-8530)

FIGURE 4.7Installation of Macro-Core® Piston Assembly into Cutting Shoe

MC Core Catcher(AT-8531)

MC Cutting Shoe(AT-8530, above or

AT-8535, below)with Piston Assembly

Correct Attachment olMC Core Catcher, Piston Assembly,

and MC Cutting Shoe

FIGURE4.9Macro-Core® Core Catcher Attachment with Piston Assembly

MCPETG Liner(AT-725S)

MC Cutting Shoe(AT-8530, above)(AT-8535, below)

with Piston Assembly

Correct Attachment ofMC Core Catcher, Piston Assembly,

and MC Cutting Shoe

FIGURE 4.10Macro-Core® PETG Liner Attachment with Piston Assembly

9b. Without Core Catcher. Push the base of an MC Spacer Ring onto the threaded end of a cutting shoeuntil it snaps into place (Fig. 4.11).

NOTE: With the exception of AT-725S (PETG) liners, all liners must utilize either a spacer ring orcore catcher. PETG liners have a swedged end which slides directly over the end of the cutting shoe.

10. Thread the cutting shoe into one end of an MC Sample Tube (Fig. 4.12). Tighten until the end of thesample tube contacts the machined shoulder of the cutting shoe.

11. Insert the appropriate liner into the sample tube (Fig. 4.12). (The liner is all ready installed if usingPETG liners without a core catcher.)

12. Connect a drive head to the top of the sample tube (Fig. 4.12 and securely tighten with the combinationwrench (Fig. 4.5). The end of the sample tube must contact the machined shoulder of the drive head.

4.5 Pilot Hole

A pilot hole prevents excessive sampler wear in tough soils and saves time when a discrete soil core isdesired. The pilot hole is created by driving a 2.0-, 2.5-, or 3.0-inch MC Pre-Probe (see page 6) forpart numbers) to the top of the sampling interval. Soil surfaces containing gravel, asphalt, hard sands,or rubble should be pre-probed to reduce wear on the cutting shoe and to avoid damage to the sampler.To save time when collecting a discrete soil core, pre-probe to the sampling interval rather than coringto depth with the sampler.

4.6 Open-Tube Sampling

The Macro-Core Open-Tube Sampler is used to gather continuous soil cores from the surface todepths exceeding 30 feet. A representative soil sample is obtained by driving the sampler 48 inches(1219 mm) into undisturbed soil. Upon retrieving the sampler, the liner and soil core are removed.The sampler is then reassembled with a new liner and inserted back down the same hole to take thenext soil core.

The Macro-Core Cutting Shoe is tapered to minimize the amount of soil scraped from the core wallswhen inserting the sampler back down an existing hole. In spite of this, non-cohesive soils will oftencollapse to the bottom of the hole. This slough material then enters the sampler as the next soil core iscollected, resulting in a non-representative sample. A Closed-Piston Macro-Core Sampler is requiredunder such conditions. Instructions for sampling with the Open-Tube Macro-Core Sampler follow.

1. Attach a drive cap to the drive head of an assembled Open-Tube Macro-Core Sampler (Section 4.3).

2. Install a hammer anvi! and anvil retainer cap assembly. Raise the hammer latch while driving theMacro-Core Sampler to avoid contact with the drive head.

3. Raise the hammer assembly to its highest position by ful ly extending the probe cylinder. If workingwith a Model 4200, 4220, or 420U, raise the machine foot to allow sufficient room to position thesampler below the hammer.

Standard Operating Procedure 301345 Page 15 Macro-Core* Soil Sampler

MC Cutting Shoe withPiston Assembly(AT-8530, above)

(AT-8535 or AT-8537, below)

Correct Attachment ofMC Spacer Ring, Piston Assembly

MC Cutting Shoe

FICURE4.11

Macro-Core® Spacer Ring Attachment With Piston Assembly

MC SampleTube(AT-8520orAT-8522)

MC Drive Head(AT-8510orAT-8512)

MC Liner(AT-7235, AT-724,AT-725S, AT-925S)

MC Core Catcher (AT-8531, shown) or MC Spacer Ring (AT-8532)

MC Cutting Shoe (AT-8530 or AT-8535)with Closed-Piston Assembly

FIGURE 4.12

Macro-Core® Closed-Piston Sampler Assembly

FIGURE4.13Macro-Core® Soil Sampler in Driving Position

ExtendedProbeCylinder

ProbeHammer

AssembledMacro-CoreSampler

4. Place the sampler in the driving position (Fig. 4.13). The sampler should always be positioned parallelto the derrick axis.

5. If using the Model 4200, 4220, or 420U, begin applying downward force on the sampler by loweringthe machine foot. When the foot contacts the ground surface, apply downward force with the probecylinder control only. Model 54GO-ai3d^540U operators may start initially with the probe"cylindercontrol.

GEOPROBETIP: Activate the hammer whenever collecting soil. Hammering forces soilinto the sample tube and increases recovery.

6. Drive the sampler until the drive head reaches the ground surface (Fig. 4.14A).

£ A :UJT! ONSome soil conditions may warrant using an MC Pre-Probe before attemptingto collect a soil core. Damage may occur if the sampler is driven into rock

or any other impenetrable layer.

.7. To sample at consecutive intervals, push a sampler down the previously opened hole (Fig. 4. J 4B) untilthe top of the next sampling interval is reached (Fig. 4.14C). Drive the probe string another 48 inches.to fill the.sampler with soil (Fig. 4.14D). An open-rube sampler may be used for consecutive samplingor, if soil slough is expected, a closed-piston sampler is available.

^CAUTIONAll parts must be completely threaded together before being driven.

Driving an incompletely assembled sampler will result in component damage.

8. Retrieve the sampler as described in Section 4.8: Sampler Retrieval.

4.7 Closed-Piston Sampling

It is often d i f f icul t to collect representative soil cores from significant depths with an open-tube samplerdue to soil slough. Because of this , the Macro-Core sampler can be equipped with a piston which locksin to the cu t t i ng shoe. This allows the sealed sampler to pass through the slough material and be opened atthe appropriate sampl ing in te rva l .

NOTE: The closed pis ton system is meant to be inserted th rough previously opened holes. It is notdesigned to be dr iven from the su r f ace th rough u n d i s t u r b e d m a t e r i a l s .

The MC Closed-Piston System can be used only with AT-8500 series Macro-Core tools. The AT-8500series replaces the AT-720 series Macro-Core tools.

A. Sampler driven to proper depth.

B. Open hole from previous sample.

C. Open-tube sampler driven back down previous hole.

D. Sampler driven to proper depth for sampling second interval.

FIGURE4.14Phases of Macro-Core® Open-Tube Soil Sampling

1. Attach a drive cap to the drive head of an assembled Closed-Piston Macro-Core Sampler (Section 4.4).

2. Install a hammer anvil and anvil retainer cap assembly. Raise the hammer latch while driving thesampler to avoid contact with the drive head.

3. Raise, the hammer- assembly to its highest position by fully extending "tiTrptobe cylinder. If-working""with a Model 4200, 4220, or 420U, raise the machine foot to allow sufficient room to place thesampler below the hammer.

4. Place the sampler tip in the previously opened hole (Fig. 4.15A). Lower the probe until the hammer. anvil contacts the sampler drive head.

5. If using the Model 4200,4220, or 420U, begin applying downward force on the sampler by loweringthe machine foot. When the foot contacts the ground surface, apply downward force with the probecylinder control only. Model 5400 and 540U operators may start initially with the probe cylindercontrol.

6. Drive the sampler until it reaches the desired sampling interval (Fig. 4.15B). Add probe rods asneeded.

Care should be taken when driving the Macro-Core Sampler down a previouslyopened hole. Low side friction may allow the sampler and probe rods

to drop down the hole. To prevent equipment loss, attach a pair of locking pliersor a pipe wrench to the rod string when advancing or retrieving the sampler.

7. Move the probe unit away from the top of the probe rods to allow room for work.

8. Remove the drive cap and insert an MC Piston Release Rod (Fig. 3.1) down the inside of the proberods (Fig. 4.16). (Refer to Fig. 4.19 for identification of extension rod accessories.) Hold onto therelease rod and attach an Extension Rod Coupler or Extension Rod Quick Links. Attach an ExtensionRod to the release rod (Fig. 4.17) and lower the jointed rods down hole. Continue adding extensionsunt i l the release rod contacts the bottom of the sampler. The operator may opt to use the ExtensionRod Jig to hold the down-hole extension rods while adding additional rods.

9. Attach an Extension Rod Handle to the top extension rod and slowly rotate the handle clockwise (Fig.4.15C and 4.18). The release rod wil l drop into the groove in the piston bolt (Fig. 4.20). The operatorshould feel the extension rods move s l ight ly as the release rod falls into the groove. Rotate the handleclockwise approximately four complete revolutions. Resistance to rotation is generally noted at thispoint. If the rods continue to rotate, however, do not continue for more than four complete revolutions.The pis ton assembly is now released and wi l l be pushed to the top of the sampler as the l iner is filledwith soil (Fig. 4.15D).

* •"

A. Previously cored or pre-probed hole with sloughed soil.B. Closed-Piston Sampler driven to next sampling interval.C. Releasing piston assembly.D. Closed-piston sampler filled with soil.

FICURE4.15

Phases of Macro-Core® Closed-Piston Soil Sampling

Figure 4.16. MC Release Rodis inserted down inside of the

probe rods.

Figure 4.17. Extension Rodsare attached to the MC PistonRelease Rod using Extension

Rod Quick Links.

Figure 4.20. MC Release Rodfits into groove in

MC Piston Bolt Head.

Figure 4.18. Extension Rodsarc rotated clockwise to

release the MC Pistonassembly.

Standard Operating Procedure 301352 Page 22 Macro-Core® Soil Sampler

Extension Rod, 36 inch (AT-67) or 48 inch (AT-671)

Extension Rod Coupler(AT-68)

Female Quick LinkExtension Rod Coupler

(AT-696)

Extension Rod Quick Links(AT-694K)

includes (1) AT-696 and (1) AT-695

Male Quick LinkExtension Rod Coupler(AT-695)

oExtension Rod Jig —Top View

(AT-690)

Extension Rod Jig — Side View(AT-690) Extension Rod Handle

(AT-69)

FIGURE4.19

Ceoprobe Extension Rods and Accessories

10. Remove the release rod and extension rods. The piston assembly will not be attached to the end of theextension rod but will remain inside the sampler tube.

11. Add a probe rod, attach the drive cap to the tool string, and reposition the probe unit. Drive thesampler another 48 inches (1219 mm) to fill the liner with soil. It will be necessary to add another

if-ulnl!|p3^ """ n"MK^--:r- •—

GEOPROBETIP: Activate the hammer whenever collecting soil. Hammering forces soilinto the sampler tube and increases recovery.

4.8 Sampler Retrieval

1. Attach a pull cap to the top probe rod. Close the hammer latch over the pull cap and pull the tool stringup one rod length by actuating the PROBE control lever.

2. Remove the rod and repeat Step 1 unti l the sampler drive head is just above the ground surface. Proberods are sometimes diff icul t to loosen by hand. Use pipe wrenches to free tight threads.

CAUTIONCare should be taken when retrieving the Macro-Core sampler.

Low side friction may allow the sampler and probe rods to drop down the hole.Attach a pair of locking pliers or pipe wrench to the rod string to prevent equipment loss.

3. Attach the pull cap to the sampler drive head (Fig. 4.21). Pull the sampler out of the ground (Fig. 4.22)by raising the PROBE control lever. If using a Model 4200, 420U, or 4220 Geoprobe unit, the probecylinder wi l l - ful ly extend before the sampler is completely free. Attempt to raise the sampler byactuating the FOOT control.

'CAUTION

The rear of the carrier vehicle may be pulled downward as the foot cylinderis activated if the sampler is lodged tightly in the ground.

Damage to the unit base frame may occur under such circumstances.

If the sampler cannot be retrieved without excessive resistance, follow these steps:

1. Lower the FOOT control and disengage the hammer latch from the pul l cap.

2. Raise the probe foot al least 12 inches (305 mm) above the ground.surface. Stack severalboards or place timber blocks under the foot to act as a foot extension.

3. Lower the hammer assembly and close the hammer latch over the sampler pull cap.

4. Use the PROBE control to l i f t the sampler completely out of the ground.

4.9 Soil Core Recovery

The soil sample is easily removed from the Macro-Core Sampler by unscrewing the cutting shoe andpulling out the liner. A few sharp taps on the cutting shoe will often loosen the threads sufficiently toallow removal by hand: If needed, the exterior of the cutting shoe features a notch for attaching the

~^^~cblrlblnatTori~wrencfr^simply pull the liner and soil core from the sample tube (Fig. 4.25).

If the closed-piston sampler is used, the piston assembly is now retrieved from the end of the liner(Fig. 4.26). Secure the soil sample by placing a vinyl end cap on each end of the liner.

Undisturbed soil samples can be obtained from Teflon®, PVC, and PETG liners by splitting the liner.Clamp one end of the liner to a board with locking pliers. Expose the soil core by making a longitudinalcut completly through the liner with a hook blade utility knife. A hook.blade is recommended becauseit is not only easier to use, but it is also safer.

4.10 Macro-Core Closed-Piston Operating Tips

The Macro-Core piston assembly requires proper maintenance to ensure reliable operation. Thefollowing tips will increase the effectiveness of closed-piston sampling:

1. Cleanliness is the most important factor affecting piston operation. Ensure piston bolt threadsand locking ring are free of soil particles and corrosion before each use. Completely thread andunthread the piston bolt to verify operation. Disassemble the piston tip and wash the individualparts using clean water and a nylon Macro-Core tube brush (BU-700) if necessary. Allow partsto dry before assembling if piston is to be stored. Disassemble used pistons before storing toprevent piston bolt corrosion.

2. Never store a cutting shoe with the piston installed. Install the piston assembly immediatelybefore sampling.

3. Lubricate piston assembly with distilled water before installing in the cutting shoe.

4. Once the assembly is fully seated in the cutting shoe, tighten the piston bolt with an oscillatingmovement; thread the bolt in 90 degrees then back 45 degrees. When the end of thread travel isreached, work the last 30 degrees of travel back and forth several times. Tightening the pistonbolt in this manner allows the metal pins of the locking ring to correctly align in the cutting shoe.

5. Do not lock the piston bolt 100 percent counterclockwise. Fully tighten the bolt and then loosenapproximately 10 degrees.

6. When releasing the piston downhole, only turn the piston bolt 4 clockwise revolutions.

7. Clean the piston assembly with dist i l led water and a nylon Macro-Core tube brush between samples.It is not necessary to completely disassemble the piston at this time. Pay particular attention to thelocking ring and ensure that all sand and grit is removed from between the metal lock pins.

Figure 4.21. Pull Capattached to MC Drive Head.

Figure 4.22. MC Soil Sampleris pulled with Geoprobe unit.

Figure 4.23. Loosening theMC C u t t i n g Shoe with theMC Combinat ion Wrench.

Figure 4.24. RemovingMC Cut t ing Shoe and liner from

MC Sampler Tube.

Figure 4.25. Macro-Core liner filled

with soil core.

Figure 4.26. MC Piston assemblyis retrieved from l iner at the top

of the soil core.

8. Locking rings are expensive but can be restrxmg on new springs. If a locking ring breaks, save thepieces for reuse. To restring a locking ring, follow these simple steps:

a. There is a small loop at each end of a new locking ring spring. Make sure one loop is bentperpendicular to the other. One loop should also be completely closed while the other is

b. Attach a clamp as close to the open end as possible (without contacting the loop) to hold thespring. Fisherman fly-tying pliers work well for this procedure. Take care when attaching theclamp as the spring may be damaged if too much pressure is applied.

c. String 12 locking ring pins (macaroni-shaped metal pieces) on the closed end, stretching the. spring as necessary. Be careful not to overstretch and damage the spring.

d. Hook the open end of the spring through the closed end and bend the loop closed.

e. Remove the clamp and gently stretch the locking ring several times to ensure that the loopswill not open. Assembly is complete.

9. A locking ring groove is machined into the cutting shoe. Over time, the edges of this groove maybegin to mushroom from use (Fig. 4.27). The raised metal lip formed by the mushroomed groovemay cause the locking ring (and subsequently the piston) to bind in the.cutting shoe. Remove theraised metal with a file or die grinder

See Detail A-A

Detail A-ARaised metal lip.

MC Cutting Shoe(AT-8530, shown, or AT-8535)

FIGURE4.27Macro-Core® Cutting Shoe with Mushroomed Locking Ring Groove

Standard Operating Procedure 301357Page 27 Macro-Core* Soil Sampler

4.11 Tips to Maximize Sampling Productivity

The following suggestions are based on the collective experiences of Geoprobe operators:

1. Organize your truck or van to maximize efficiency. Assign storage areas to all tools and equipment_ for easyJocatipn. Store sampleis,-exjensionTO^^

of items lying loose in the back of the vehicle.

2. Take three or four samplers to the field. This allows the collection of several samples before stoppingto clean and decontaminate the equipment. A system is sometimes used where one individual operatesthe probe while another marks the soil cores and decontaminates the used samplers.

3. A machine vise is a real plus. With the sampler held in a vise, the operator has both hands free toremove the cutting shoe (Fig. 4.28), drive head, and sample liner (Fig. 4.29). Cleanup is also easierwith both hands free. Geoprobe offers an optional Machine Vise (FA-300) which mounts directly onthe probe derrick (Fig. 4.30).

4. Extension Rod Quick Links (Fig. 4.31) are the best choice among connectors. These are real timesavers. The quickest and easiest method for deploying extension rods is to assemble sections of up tothree rods with threaded connnectors. Each section is then connected with Quick Links. Up to threerods can be inserted or removed from the probe string at once, greatly reducing deployment time.

. 5. When releasing the piston assembly, insert extension rods in the probe string until the piston bolt isreached. Once the release rod falls into the groove in the bolt head, use a pair of locking pliers to turnthe extension rods and release the piston. The locking pliers are quicker and easier than installing anextension rod handle.

6. It is most practical to use 48-inch probe rods when using the Macro-Core sampler . If .using 36-inchprobe rods, some rods must be partially driven in order to add up to the 48-inch sampler length. Tomaximize sampling efficiency, take 36-inch (9 1 4 mm) sample cores when 36-inch probe rods must beused.

7. Organize your worksite. The best way to maximize sampling efficiency is to practice with the samplerand identify a comfortable setup. Lay out all tools and equipment before probing. An example layoutis shown in Figure 4.32.

A collapsible table or stand is handy to hold decontaminated sampler tubes and liners. Equipmentmay also be protected from contamination by placing it on a sheet of plastic on the ground.

Keep probe rods separate by identifying a location for "new" rods as well as a "put down pile."Init ial ly drive the sampler with a new rod. As the rod is removed during sampler retrieval, place it inthe put down pile for reuse. Drive the sampler to the top of the next sampling interval by using all ofthe rods in the put down pile. A new rod (located in a separate pile) is added and the string is drivento collect the next soil core. Once again, each probe rod is removed and placed in the put down pile asthe sampler is retrieved. The cycle is repeated until all of the soil cores are recovered. This methodeliminates the need to count rods while driving the sampler.

Cleanup is very important from the standpoint of operation as well as decontamination. Remove alldirt and grit from the threads of the drive head, cutting shoe, and sample tube with a nylon brush (BU-700). Without sufficient cleaning, the cutting shoe and drive head will not thread completely onto thesample tube. The threads may be damaged if the sampler is driven in this condition.

Ensure that all soilTs femovedTrom"rinifi"ae the sample tube. Sand'p~afticfes are especially troublesome"as they can bind liners in the sampler. Full liners are difficult to remove under such conditions. Inextreme cases the soil sample must be removed from the liner before it can be freed from the sampletube.

9. The piston assembly may remain lodged in the cutting shoe when disassembling by hand, even thoughthe piston bolt is completely loosened. This is because the locking ring and piston washer do notrelease from the groove in the cutting shoe as the piston bolt unthreads out of the tip. Hammering on thepiston tip will have no effect because you are, in essence, forcing the tip tighter against the locking ring.To dislodge the piston, turn the assembly over and tap the top of the cutting shoe on a solid object. If theassembly still does not release, tap on the piston bolt with a hammer (taking care not to damage .therelease rod slot). This will jar the piston tip and bolt enough to release the locking ring from the groovein the cutting shoe.

Do not push the piston assembly out of the cutting shoe by placing your handson the piston tip. The cutting shoe is sharp and may cause injury

when the assembly suddenly comes free. It is best to place the tipagainst a solid object, grasp the cutting shoe, and push the shoe over the assembly.

10. Although available for use with two sizes of probe rod, 1.25-inch O.D. rods are recommended for theMacro-Core Sampler. The larger rod diameter limits downhole deflection of the tool string and ultimatelyprovides a more durable system. A new thread design also makes the 1.25-inch rods quicker and easierto thread together than previous 1-inch probe rods.

11. The Heavy-Duty Macro-Core Cutting Shoe (AT-S535) is machined with more material at the criticalwear areas. It can be used in place of the standard cutting shoe (AT-8530) and is designed to lengthenservice life under tough probing conditions.

Expansive clays and coarse sands can "grab" and collapse liners as the sample rube is filled with soil. A1/8-inch undersized cut t ing shoe (AT-8537) will help alleviate this problem. The smaller diameter core(1.375 inches) allows expanding clays and coarse sands to travel up the sample liner without binding.The piston assembly can not be used with this cutting shoe.

12. Maximize the thread life of the sample rube by varying the ends in which the drive head and cutting shoeare ins ta l led . The dynamic forces developed while driving the sampler are such that the threads at thedrive head wear more quickly than at the cutting shoe. Regularly switching ends will maintain relativelyeven wear on the sample tube.

Figure 4.28. RemovingMC Cutt ing Shoe with filled sampler

tube held in Machine Vise.

Figure 4.29. Removing filled linerwith sampler tube held

in Machine Vise.

Figure 4.30. Machine Visemoun ted directly on

Gcoprobc uni t .

Figure 4.33. Using ExtensionRod Quick Links to connect

Extension Rods.

Macro:Core® Soil Sampler

"New" (Undriven)Probe Rods

Previously DrivenProbe Rods in

"Put Down Pile"For Reuse

Filled and Capped Liners(Placed on Plastic)

Machine Vise on Stand

Cleaning Water

DECONAREA

Clean SampleTubesBox of New Liners

Extension Rod Sections(Placed on Plastic)

FIGURE 4.32Equipment Layout Example to Maximize Sampling Productivity.

5.0 Macro-Core" Kits Listing

MACRO-CORE ACCESSORY KITS

w.vJ^.V5MGiFETG7Einers^(BwFof:5'"6)'Tr ~r:~"

AT-726K MC Vinyl End Caps (66 Pairs)

AT-8513K MC Core Catchers (Box of 25)

AT-8532K MC Spacer Rings (Box of 25)

AT-8570R.. MC Piston O-Rings (Pkt. of 25)

AT-8561K MC Locking Ring Springs (Pkt. of 10)

AT-925K MC PVC Heavy-Duty Liners (Box of 66)

MACRO-CORE SAMPLER KITS

AT-8500K MC Starter Kit, Ni-Plated (fits 1-inch probe rods)(1).... AT-8501K... MC Closed Piston Kit(1)... AT-8510...(1) AT-8520...(1) AT-8530...(1) .....AT-8580...(2) AT-8790 ...(2) BU-700

MC Drive Head... MC Sample Tube, Ni-Plated... MC Cutting Shoe

MC Release Rod... MC Combination Wrench... Nylon Brush for MC Tubes

AT-8514K MC Starter Kit, Ni-Plated (fits 1.25-inch probe rods)(1) AT-8501K ... MC Closed Piston Kit(1) AT-8512 MC Drive Head(1) AT-8520 MC Sample Tube, Ni-Plated(1) AT-8530 MC Cutting Shoe(1) AT-8580 MC Release Rod(2) AT-8590 MC Combination Wrench(2) BU-700 Nylon Brush for MC Tubes

AT-8501K MC Closed-Piston Kit(10) AT-8561K ... MC Locking Ring Springs(1) AT-8530...(1) AT-8540...(1) AT-8550...(2) AT-8560...(1) . : AT-8570

MC Cutting ShoeMC Piston BoltMC Piston Washer

... MC Locking Ring Assembly

... MC Piston Tip Assembly

AT-8502K MC Standard Sampler Kit, Ni-Plated (fits 1-inch probe rods)(1) AT-8510 MC Drive Head(1) AT-8520 ...... MC Sample Tube, Ni-Plated(2) AT-8530 MC Cutting Shoe

i;Sampje^Kjt,,NigEiated^(fu^.2S^;nch probe rodi) ~-(1) AT-8512 MCDriveHead(1) AT-8520 MC Sample Tube, Ni-Plated(2) AT-8530 MC Cutting Shoe

AT-8503K MC Standard Sampler Kit, Unplated (fits 1-inch probe rods)(1) AT-8510 MCDriveHead .(1)........... AT-8522 MC Sample Tube, Unplated(2) AT-8530 MC Cutting Shoe

AT-8511K MC Standard Sampler Kit, Unplated (fits 1.25-inch probe rods)(1) AT-8512 MCDriveHead(1) AT-8522 ...... MC Sample Tube, Unplated ;(2) AT-8530 MC Cutting Shoe

AT-8506K ..... MC Starter Kit, Unplated (fits 1-inch probe rods)(1) AT-8501K ... MC Closed Piston Kit(1) AT-8510 .MCDriveHead(1) AT-8522 MC Sample Tube, Unplated(1) AT-8530 MC Cutting Shoe(1) AT-8580 MC Release Rod(2) AT-8590 MC Combination Wrench(2) BU-700 Nylon Brush for MC Tubes

AT-8513K MC Starter Kit, Unplated (fits 1.25-inch probe rods)(1) AT-8501K ... MC Closed Piston Kit(1) AT-8512 MC Drive Head(1) AT-8522 MC Sample Tube, Unplated(1) AT-8530 MC Cutting Shoe(1)........... AT-8580 MC Release Rod(2) AT-8590 MC Combination Wrench(2) BU-700 Nylon Brush for MC Tubes

Standard Operating Procedure -,„,-,<--, Pa8e 33 Macro-Core" Soil Sampler301363

6.0 REFERENCES

Geoprobe Systems, May, 1995, "1995-96Tools and Equipment Catalog".

Standard Operating Procedure Page 34301364

Equipment and tool specifications, including weights, dimensions,materials, and operating specifications included in this brochure aresubject to change without notice. Where specifications are critical to

your application, please consult Geoprobe Systems.

No part ot this publication may be reproduced or transmitted in anyform or by any means, electronic or mechanical, including photocopy,

recording, or any inlormation storage and retrieval system, withoutpermission in writing from Kejr Engineering, Inc.

Geoprobe SystemsA DIVISION OF KEJR ENGINEERING, INC.

Corporate Headquarter i601 N.Broadway Salina, Kansas 67401 • l-800-GEOPROBE (1-800-436-7762) • Fax (913) 825-2097

Eastern Regional OfficeP.O. Box 264 • Lewes, Delaware 19958 • (302) 645-0550 • Fax (302) 645-6054

Southeastern Regional Office3465 E. SW Palm City School Ave. • Palm City, Florida 34990 • (407) 286-1566 • Fax (407) 286-2035

Western Regional Office1448 Kramct R i d f t • Rccdky, California 93654 • (209) 637-1696 • Fax (209) 637-1796

Hydraul ic Probing Machines • Mobile Laboratories • Small Diameter SamplingTools

301366

GEOPROBE LARGE BORE SOIL SAMPLERDISCRETE INTERVAL SOIL SAMPLER

STANDARD OPERATING PROCEDURE

Technical Bulletin No. 93-660

September, 1996

A. Driving the Sealed Sampler .

B. Removing the Stop-PinC. Collecting a SampleD. Recovering Sample in Liner

DRIVING AND SAMPLING WITH THE LARGE BORE SOIL SAMPLER

301367

nGeoprobe® Systems ™

Geoprobe0 is a Registered Trademark ofKejr Engineering, Inc., Salina, Kansas

Macro-Core8 is a Registered Trademark ofKejr Engineering, Inc., Salina, Kansas

Large Bore Soil Sampler: U.S. Patent No. 5,186,263

No part of this publication may be reproduced or transmitted in anylorm or by any means, electronic or mechanical, including photocopy,

recording, or any inlormation storage and retrieval system, withoutpermission in writing from Kejr Engineering, Inc.

Standard Operating Procedure 301368 Page 2 Large Bore Soil Sampler

1.0 OBJECTIVE

The objective of this procedure is to collect a discrete soil sample at depth and recover it for visual inspectionand/or chemical analysis.

2.0 BACKGROUND

2.1 Definitions .

Geoprobe® Soil Probing Machine: A vehicle-mounted, hydraulically-powered machine that utilizesstatic force and percussion to advance small diameter sampling tools into the subsurface for collecting soilcore, soil gas, or groundwater samples.* Geoprobe® is a registered trademark ofKejr Engineering, Inc., Salina, Kansas

Large Bore Soil Sampler: A 24-inch longx 1-1/2-inch (610 mm x 38 mm) diameter soil sampler capableof recovering a discrete sample that measures up to 320 ml in volume in the form of a 22-inch x 1-1/16-inch (559 mm x 27 mm) core contained inside a removable liner.

Liner: A 24-inch long x 1-1/8-inch diameter (610 mm x 29 mm) removable/replaceable, thin-walled tubeinserted inside the Large Bore Sample Tube for the purpose of containing and storing soil samples. Linermaterials include brass, stainless steel, Teflon®, and clear plastic (cellulose acetate butyrate).

2.2 Discussion ,

The Large Bore (LB) Soil Sampler is used primarily as a discrete interval sampler; that is, for the recoveryof a sample at a prescribed depth. In certain circumstances, it is also used for continuous coring.

The assembled Large Bore Sampler is connected to the leading end of a Geoprobe brand probe rod anddriven into the subsurface using a Geoprobe Soil Probing Machine. Additional probe rods are connectedin succession to advance the sampler to depth. The sampler remains sealed (closed) by a piston tip as it is

I being driven. The piston is held in place by a reverse-threaded stop-pin at the trailing end of the sampler.When the sampler tip has reached the top of the desired sampling interval, a series of extension rods,sufficient to reach depth, are coupled together and lowered down the inside diameter of the probe rods.

I The extension rods are then rotated clockwise (using a handle). The male threads on the leading end of theextension rods engage the female threads on the top end of the stop-pin, and the pin is removed. After theextension rods and stop-pin have been removed, the tool string is advanced an additional 24 inches. Thepiston is displaced inside the sampler body by the soil as the sample is cut. To recover the sample, thesampler is retrieved from the hole and the liner containing the soil sample is removed. The operation isillustrated in Figure 1.

tStandard Operat ing Procedure 301369 Page 3 Large Bore Soil Sampler

A. VB. V

A. Driving the Sealed Sampler

B. Removing the Stop-Pin

C. Collecting a Sample

D. Recovering Sample in Liner

FIGURE 1Driving and Sampling with the Large Bore Soil Sampler

Standard Operating Procedure 301370 Page A Large Bore Soil Sampler

3.0 REQUIRED EQUIPMENT

The following equipment is required to recover soil cores using the Geoprobe Large Bore Soil Sampler (Fig. 2)and driving systems. Note that the sample liners forjhe, Larae Bore Sampler.ars available in four differentmaterials. Liner materials should be selected based Ojij^plingpj]rrx)sj5,_analytica]-pararneters,-and data quality-

""orJjectives^

LARGE BORE SAMPLER PARTS QUANTITY

LB Heavy-Duty Cutting Shoe -1-LB Heavy-Duty Drive Head, fits 1.25-inch probe rods -1-LB Heavy-Duty Sample Tube -1-LB Piston Tip -1-LB Piston Rod -1-LB Clear CAB Liner variableLB Brass Liner variableLB Stainless Steel Liner variableLB Teflon® Liner variableLB Cutting Shoe Wrench -1-Vinyl End Caps variableLB Piston Stop-Pin -1-LB Piston Stop-Pin O-Ring variableTeflon® Tape (optional) variableNylon Brush for LB Tubes -1-

GEOPROBE TOOLS* . QUANTITY

Drive Cap, fits 1.25-inch probe rod -1-Pull Cap, fits 1.25-inch probe rod -1-Probe Rod, 1.25 inch x 12 inches -1-Probe Rod, 1.25 inch x 24 inches -1-Probe Rod, 1.25 inch x 36 inches (optional) VariableProbe Rod, 1.25 inch x 48 inches VariableExtension Rod, 36 inch (optional) VariableExtension Rod, 48 inch VariableExtension Rod Centering Plug -2-Extension Rod Coupler VariableExtension Rod Handle -1-Extension Rod Jig -1-Extension Rod Quick Links (Optional) VariableLB Sampler Manual Extruder Kit -1-

ADDITIONAL TOOLS QUANTITY

Locking Pliers -1-Adjustable Open-End Wrench, 1-1/4 inch or -1-MC Combination Wrench -1-Open-End Wrench, 3/8 inch -1-Pipe Wrench -2-

* Probe rods and accessories are also available in 1-inch O.D. (outside diameier).

PART NUMBER

AT-6601

AT-6612AT-6621AT-663AT-664AT-665KAT-666AT-667AT-668AT-669AT-641KAT-63AT-63RAT-640TBU-600

PART NUMBER

AT-1200

AT-1204AT-1212AT-1224AT-1236AT-1248AT-67AT-671AT-6712AT-68AT-69AT-690AT-694KAT-659K

AT-8590

Standard Operating Procedure 301371 PageS Large Bore Soil Snmr.

LB Stop-Pin(AT-63)

LB Drive Head(AT-6612)

LB Sample Liners(AT-665K, AT-666, AT-667, AT-668)

LB Cutting Shoe(AT-6601)

FIGURE 2Large Bore Soil Sampler Parts

1.0 OPERATION

4.1 Decontamination

"Before and after each use, thoroughly clean ail parts of the soii sampling system according to specificproject requirerneritsrAl:leanrnew"linef is recommenaed'foTeacKusev'Parts should also be inspected for-wear or damage at this time,

i - . . .4.2 Assembly

1. Install a new AT-63R O-Ring into the O-Ring groove on the stop-pin.

2. Seat the pre-flared end of the LB liner over the interior end of the cutting shoe as shown in Fig. 3. Itshould fit snugly.

3. Insert the liner into either end of the sample tube and screw the cutting shoe and liner into place. Ifexcessive resistance is encountered during this task, it may be necessary to use the LB shoe wrench.Place the wrench on the ground and position the sampler assembly with the shoe end down so that therecessed notch on the cutting shoe aligns with the pin in the socket of the wrench (Fig. 4). Push downon the sample tube while turning it until the cutting shoe is threaded tightly into place.

4. Screw the piston rod into the piston tip. Insert the piston tip and rod into the sample tube from the endopposite the cutting shoe. Push and rotate the rod until the tip is seated completely into the cuttingshoe.

5. Screw the drive head onto the top end of the sample tube, aligning the piston rod through the centerbore.

6. Screw the reverse-threaded stop-pin into the top of the drive head and turn it counterclockwise witha 3/8-inch wrench until securely tightened (Fig. 5). Hold the drive head in place with a 1-1/4-inch oradjustable wrench while completing this task to assure that the drive head stays completely seated.The Macro-Core® Combination Wrench will also fit the drive head for 1.25-inch probe rods. Theassembly is now complete. .

4.3 Pilot Hole

A pilot hole is appropriate when the surface to be penetrated contains gravel, asphalt, hard sands, orrubble. Pre-probing will prevent unnecessary wear on the sampling tools. A Large Bore Pre-Probe maybe used for this purpose. The pilot hole should be made only to a depth above the sampling interval.Where surface pavements are present, a hole may be drilled with the Geoprobe Soil Probing Machineusing a drill steel (AT-3524, AT-3536, or AT-3548 depending upon the thickness of the pavement),tipped with a 1.5-inch diameter carbide drill bit (AT-36) prior to probing.

NOTE: Some soil conditions may warrant using a solid drive point (AT-142B) to pre-probe the hole tothe desired sampling depth. Information about the subsurface and depth to bedrock should be knownbefore driving the sampler. Damage may occur if the sampler is driven into rock or other impenetrablematerial.

Figure 3. Liner fits snugly over interior end of cutting shoe.

Figure 4. Using the AT-669 Cutting Shoe Wrench to attachcutting shoe.

Figure 5. Tightening the Stop-pin.

Figure 7. Coupling Extension Rods together.

Standard Operating Procedure 301374

Figure 8. Rotating the Extension Rod Handle.

Large Bore Soil Sampler

.4 Driving

1. Attach a drive cap to a one-foot probe rod and thread the rod onto the assembled sampler. Position theassembly for driving into the subsurface.

2. Drive the assembly into the subsurface unt i l the drive head on the sample tube is just above theground surface.

i .3. Remove the drive cap and one-foot probe rod. Secure the drive head with a 1-1/4-inch open-end,

adjustable wrench or a Macro-Core® combination wrench, and re-tighten the stop-pin with a 3/8-inchopen-end wrench (Fig. 5).

4. Attach the drive cap to a two-foot probe rod and continue driving the sampler into the ground. Attachthree- or four-foot probe rods in succession until the leading end of the sampler reaches the top of thedesired sampling interval.

4.5 Preparing to Sample

1. When sampling depth has been reached, position the Geoprobe machine away from the top of theprobe rod to allow room to work.

2. Insert an extension rod down the inside diameter of the probe rods. Hold onto it and place an extensionrod coupler or Quick Link extension rod connectors (Fig. 6) on the top threads of the extension rod(the downhole end of the leading extension rod should remain uncovered). Attach another extensionrod to the coupler and lower the jointed rods down hole (Fig. 7). An extension rod jig (Fig. 6) may beused to help hold the rods during Steps 2 and 3.

3. Couple additional extension rods together in the same fashion as in Step 2. The-leading extension rodmust reach the stop-pin at the top of the sampler assembly. When coupling extension rods together,you may opt to use the extension rod jig to hold the downhole extension rods while adding additionalrods. . • .

4. When the leading extension rod has reached the stop-pin down hole, attach the extension rod handle,to the top extension rod.

5. Turn the handle clockwise unt i l the stop-pin detaches from the threads on the drive head (Fig. 8). Pullup lightly on the extension rods during this procedure to check thread engagement.

NOTE: The larger inside diamter (I.D.) of the 1-1/4-inch probe rods can make it difficult to engagethe stop-pin. To remedy this problem, attach an Extension Rod Center Plug to the bottom of the firstextension rod. Another centering plug may be necessary between the first and second extension rodsif the extension rods are slightly bent.

6. Remove the extension rods and uncouple the sections as each joint is pulled from the hole. Theextension rod jig may be used to hold the rod couplers in place as the top extension rods are removed.

1. The stop-pin should be attached to the bottom of the last extension rod upon removal. Inspect it fordamage. Once the stop-pin has been removed, the sampler is ready to be driven to collect a sample.

I Standard Operating Procedure 301375 Page 9 Large Bore Soil Sampler

Extension Rod, 36 inch (AT-67) or 48 inch (AT-671)

-— Extension Rod Coupler(AT-68)

JUr— I

Female Quick LinkExtension Rod Coupler

' (AT-696)

Extension Rod Quick Links(AT-694K)

includes (1) AT-696 and (1) AT-695

oExtension Rod Jig — Top View

(AT-690)

Extension Rod Jig — Side View(AT-690)

Male Quick LinkExtension Rod Coupler(AT-695)

Extension Rod Handle(AT-69)

FIGURESGeoprobe Extension Rods and Accessories

Sample Collection

1. Reposition the Geoprobe machine over the probe rods, adding an additional probe rod to the toolstring if necessary. Make a mark on the probe rod 24 inches above the ground surface (this is the

__„_.-„ . : djstance rhe-tppl string -will be advanced).-^ _^.:..;r_=.,._=.t^,_..,,--.,.-J-._ .'."1T."": !±"' ,;„„,

2. Attach a drive cap to the probe rod and drive the tool string and sampler another 24 inches. Acutatethe hammer function during sample collection to increase sample recovery. Do not over-drive thesampler.

4.7 Retrieval

1. Remove the drive cap from the top probe rod and attach a pull cap. Lower the hammer assembly andclose the hammer latch over the pull cap.

2. With the machine foot firmly on the ground, pull the tool string out of the hole. Stop when the top(drive head) of the sampler is about 12 inches above .the ground surface.

3. Because the piston tip and rod have been displaced inside the sample tube, the piston rod now extendsinto the two-foot probe rod section. In loose soils, the two-foot probe rod and sampler may be recoveredas one piece by using the Foot Control on the probe machine to lift the sampler the remaining distanceout of the hole.

4. If excessive resistance is encountered while attempting to lift the sampler and probe rod out of thehole using the Foot Control, unscrew the drive head from the sampler and remove it with the proberod, the piston rod, and the piston tip. Replace the drive head onto the sampler and attach a pull capto it. Lower the hammer assembly and close the hammer latch over the pull cap and pull the samplerthe remaining distance out of the hole with the probe machine foot firmly on the ground.

4.8 Sample Recovery

1. Detach the two-foot probe rod if it has not been done previously.

2. Unscrew the cutt ing shoe using the LB Cutt ing Shoe Wrench, if necessary. Pull the cutting shoe outwith the liner attached (Fig. 9). If the liner doesn't slide out readily with the cutting shoe, take off thedrive head and push down on the side wall of the liner. The liner and sample should slide out easily.

4.9 Core Liner Capping

1. The ends of the liners can be capped off using the vinyl end caps for further storage or transportation.A black end cap should be used at the bottom (down end) of the sample core and a red end cap at thetop (up end) of the core.

2. On brass, stainless steel, and Teflon® liners, cover the end of the sample tube with AT-640T Teflon®tape before placing the end caps on the liner (Fig. 10). The tape should be smoothed out and pressedover the end of the soil core so as 10 minimize headspace. However, care should be taken not tostretch and therefore t h i n the Teflon® tape.

Figure 9. Removing the liner to recover the Sample.

Figure 10. Covering the liner end with Teflon tape for capping.

Figure 11. Extruding a sample in a metal liner using the AT-659Kmanual extruder.

Standard Operating Procedure 301378 Page 1 2 Large Bore Soil Sampler

0 Sample Removal

1. Large Bore clear plastic liners and Teflon® liners can be slit open easily with a hooled-blade utilityknife for the samples to be analyzed or placed in appropriate containers.

~27~Large~Bore'-"brass andrstainless-steel liners come with-plastic cladding on the.outside of the linerlp_keep four 6-inch sections aligned. Remove the cladding and cut the sections apart with a knife. TheLarge Bore Manual Extruder may be used to push the soil cores out of the liner sections for analysisor for transfer to other containers (Fig. 11).

CAUTION: Use extreme care when using the Large Bore Manual Extruder.. Gradually apply downpressure on slow speed. Use of excessive force could result in injury to the operator or damage of thetools:

1^^ 6.0 REFERENCES

f^Geoprobe Systems, August, 1993, "1993-94 Tools and Equipment Catalog". .

I Geoprobe Systems, May, 1995, "1995-96 Tools and Equipment Catalog". -.

_ !_ „_ . __________ .___.r."77T... --- _______ _._._._ ____________ _. ___ __ '_ . ._ . ________ .__ _____

i • ' • . • • - ; / . . ' ' ' - • • • - • . 'I'- " . '

Standard Operating Procedure PappidPage 14 Large Bore Soil Sampler

301380

Equipment and tool specifications, including weights, dimensions,materials, and operating specifications included in this brochure aresubject to change without notice. Where specifications are critical to

your application, please consult Geoprobe Systems.

No part of this publication may be reproduced or transmitted in anyform or by any means, electronic or mechanical, including photocopy,

recording, or any information storage and retrieval system, withoutpermission in writing from Kejr Engineering, Inc.

SystemsA DIVISION OF KEJB ENGINEERING, INC.

Corporate Headquarters601 N. Bioadwa; • Saliiu. Kansas 61401 • I-800-OEOPROBE (1-800-436-7762) • Fax (913)825-2097

F-aslcrn Regional OfficeP.O. Box 264 • Uu-cs. Delaware 19958 • (302) 645-0550 • Fax (302) 645-6054

Southeastern Regional Office3465 E. SW Palm City Schcwl Avt. • Palm Cily. Florida 34990 • (407) 286-1566 • Fax (407) 286-2035

Western Rcpional Office1448 Kiamci Ridge • Recdley. Calilomia 93654 •(209)637-1696' Fax (209)637-1796

Hydraul ic Probing Machines • Mobile Laboratories • Small Diameter Sampling Tools

301382

Powell -Harpstead, Inc. - Records Collections

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