CENTURY SYSTEMS PORTABLE ORGANIC VAPOR ANALYZERMODEL OVA-128

INTRODUCTIONThe Century Mode) OVA-128 Portable Organic Vapor

Analyzer (OVA) is a highly sensitive instrument design-ed to measure trace quantities of organic materials mair. It is essentially a hydrogen flame lonization detectorsuch as utilized in laboratory gas chromatographs andhas similar analytical capabilities. The flame ionizationdetector is an almost universal detector for organiccompounds with the sensitivity to analyze for them inthe parts per million range (WV) in air in the presence ofmoisture, nitrogen oxides, carbon monoxide and car-bon dioxide

The instrument has broad application, since it has acontinuous, chemically resistant air sampling systemand can be readily calibrated to measure almost allorganic vapors, it has a single linearly scaled readoutfrom Oppm to 10 ppm with a X1, X10, X100 range switch.Designed for use as a portable survey instrument, it canalso be readily adapted to fixed remote monitoring ormobile installations. It is ideal for the determination ofmany organic air pollutants and in the monitoring of airin potentially contaminated areas.

The OVA-128 is certified intrinsically safe by FactoryMutual Research Corporation (FM) for use tn Class I.Division 1, Groups A, B. C & D hazardous environments.

Simtlar foreign certifications have been obtained. In-cluding BASEEFA and Cerchar approval for Group HC,Temperature Class T4 and equivalent approval from theJapanese Ministry of Labor. This requirement isespecially significant in industries where volatile flam-mable petroleum or chemical products are manufac-tured, processed or used and for instruments which areactually used in portable surveying and m analyzingconcentrations of gases and vapors. Such instrumentsmust be incapable, under normal or abnormal condi-tions, of causing ignition of the hazardous atmosphericmixtures. In order to maintain the certified safety, it isimportant that the precautions outlined in this manualbe practiced and that no modification be made to theseInstruments.

Sections 1 through 6 herein apply to the basic instru-ment. Section 7 contains information relative to optionswhich are available and which may or may not havebeen purchased with your OVA.

It is highly recommended that the entire manual beread before operating the instrument. It Is essential thatall portions relating to safety of operation andmaintenance, including Section 5, be thoroughlyunderstood.

SIDE PACK ASSEMBLY

Recorder Connector

Igniter Button

Earphone Jack

Sample Connector

Readout Connector

PROBE/READOUTASSEMBLY

UMBILICAL CORD

Refill Connector-

FIGURE 1-1. PORTABLE ORGANIC VAPOR ANALYZERModel OVA-128

7.2.8.3 Gain Ad|u*tm«nt.. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 377.2.7 S a f a t y . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 377.2.8 Maintenance and Routine Operations ............................................................... 387.2.8.1 Changing Chart Speed* . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 387.3 Activated Charcoal Fitter AeeemOly ..... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 387.4 OVA Sampla Oltutor................................................................................ 387.4.1 Sailing Dilution Rat* ............................................................................... 397.5 OVA Septum Adapter............................................................................... 38

APPENDIX A: Sample Forma, Application/Technical Not«a, Scf.jmatlc. Drawings, Part* Usta

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Instructior 2R900AC

CENTURY SYSTEMS

Portable Organic Vapor AnalyzerModel OVA-128

XBQRD*

CENTURY SYSTEMS CORPORATIONP.O BOX 81$ / ARKANSAS CfTY, KANSAS 67005 / 316-447-3311 / TWX 910-740-6740

SECTION 1DESCRIPTION AND LEADING PARTICULARS1.1 GENERAL

The Century Portable Organic Vapor Analyzer (OVA),illustrated in Figure 1-1. is designed to detect andmeasure hazardous gases found in almost all In-dustries, it has broad application, since it has schemically resistant sampling system snd can becalibrated to almost all organic vapors. It Is extremelysensitive and can provide accurate Indication of gasconcentration In one of three ranges: 0 to 10 ppm; 0 to100 ppm; and 0 to 1,000 ppm. While designed ss slightweight portable Instrument, It can readily beadapted to remote monitoring applications.\ The instrument utilizes the principle of hydrogenyflame lonlzation for detection and measurement oforganic vapors. The instrument measures organic vaporconcentration by producing a response to sn unknownsample, which can be related to a gas of known com-position to which the instrument has previously beencalibrated. During normal survey mode operation, scontinuous sample Is drawn Into the probe andtransmitted to the detector chamber by an Internal pum-ping system. The sample flow rate is metered and pass-ed through particle filters before reaching the detectorchamber. Inside the detector chamber, the sample isexposed to a hydrogen flame which Ionizes the organicvapors. When most organic vapors burn, they leavepositively charged carbon-containing tons which arecollected by s negative collecting electrode In thechamber. An electric field exists between the con-ductors surrounding the flame and the collecting elec-trode which drives the ions to the collecting electrode.As the positive Ions era collected, s current correspon-ding to the collection rate is generated on the Inputelectrode. This current Is measured with s linear elec-trometer preamplifier which has an output signal pro-portional to the lonizstlon current. A signal conditioningamplifier is used to amplify the signal from the preampand to condition It for subsequent meter or externalrecorder display. The meter dlsplsy is an Integral part ofthe Probe/Readout Assembly and has s scale from 0 to10.

1.2 TYPICAL APPLICATIONS(1) Measurement of most toxic organic vapors pre-

sent in Industry for compliance with Occupa-tional Safety and Health Administration <OSHA)requirements.

(2) Process monitoring and evaluation.(3) Evaluation and monitoring applications In the

air pollution field.(4) Leak detection In storage, transportation and

handling equipment.(5) Survey of gas distribution and transmission

lines and equipment for compliance with Officeof Pipeline Safety (OPS) requirements.

(6) Forensic science applications.

1.3 OTHER TYPICAL USES(1) Controlling and monitoring atmospheres In

manufacturing and packaging operations.(2) Mudlogglng, gas and mineral exploration.(3) Lsak detection related to volatile fuel handling

equipment.

1.4 MAJOR FEATURESThe basic Instrument consists of two ma|or

assemblies, the Probe/Readout Assembly snd the SidePack Assembly (see Figure 1-1). The recorder Is op-tional on all models, but is normally used with all In-struments which Incorporate the GC Option. The outputmeter and alarm level adjustments are incorporated Inthe Probe/Readout Assembly which is operated withone hand. The Side Pack Assembly contains the re-maining operating controls and Indicators, the elec-tronic circuitry, detector chamber, hydrogen fuel supplysnd electrical power supply. It is a quantitative type In-strument with sensitivity to 0.1 ppm methane.

Other major features are: 250* linear scale readout.less than two second response time and minimum eighthour service life for fuel supply and battery pack. A bat-tery test feature allows charge condition to be read onthe meter. Hydrogen flame-out Is signified by an audi-ble alarm plus s visual Indication on the meter. The in-strument contains s frequency modulated detectionalarm which can be preset to sound at a desired con-centration level. The frequency of the detection alarm

varies as a (unction of detected level giving an audibleindication ot organic vapor concentration. The instru-ment is designed for one man, one hand operation andthe entire unit weighs a total of tesa than 12 pounds, in-cluding fuel supply and battery. An earphone i* provid-ed for "only operator" monitoring.

Ounng use, the Side Peck Assembly can be carded bythe operator on either his left or right side or as a backpack. The Side Pack Assembly la housed In a high Im-pact plastic case and weighs leas than 10 pounds. TheProbe/ Readout Assembly can be detached from theSide Pack Assembly and broken down tor transport andstorage. See Figure 1-2 for the breakdown capability ofthe instrument.

1.5 ADAPTABILITY FEATURES AND STANDARDACCESSORIES

1.5.1 GENERALMaximum flexibility and operablllty features are in-

cluded in the instrument design. As shown In Figure 1-2.a variety of pickup fixtures can be used. They can be in-stalled by simply turning a knurled locking nut. Smalldiameter tubing can be used for remote sampling andelectrically insulated flexible extensions can be usedfor difficult places to reach.

1.5.2 PROBEThe telescoping probe allows the length to be in-

creased or decreased over an eight inch range to suitthe individual user. A knurled locking nut la used to lockthe probe at the desired length. The probe is attachedto the Readout Assembly using a knurled locking nut.For measurements in close areas, the probe is replacedwith a Close Area Sampler, which is supplied as a stan-dard accessory.

1.5.3 PARTICLE FILTERSThe primary filter is of porous stainless and located

behind the sample inlet connector, see Side PackAssembly drawing in Appendix "A". In addition,replaceable porous metal filters are installed in the'close area" sampler, the pickup funnel and the tubularsampler.1.5.4 INSTRUMENT CARRYING CASE

An instrument carrying case is provided to transport,ship and store the disassembled Probe/ReadoutAssembly, the Side Pack Assembly and other standardequipment.

1.5.5 MOBILE INSTALLATIONThe instrument Is readily adaptable to a mobile ap-

plication by simply plugging into vehicle power andhydrogen fuel supply and making provisions for drawingsample from the vehicle primary sampling system.

l.a SPECIFICATIONSSensitivity: 0.1 ppm( methane)Response time: Less than 2 secondsReadout: 0 to 10 ppm, 0 to 100 ppm. 0 to 1.000 ppm,

250* linear scaled meter; external monitorconnector

Sample now rate: Nominally 2 unitsFuel supply: 75 cubic centimeter tank of pur.

hydrogen at maximum pressure of 2300 PSIQ.fillaOle while in case

Primary electrical power: Rechargeable andreplaceable battery pack at 12VDC

Service life: Hydrogen supply and battery power-ahours operating time minimum

SJza: Standard Unit: 8-5/6 x n-5/8 x 4-1/4 FMUnit: 8-5/8 x 11-5/8 x 4-112 Probe/ReadoutAssembly: Variable (see Figure 1-2)

Weight: Standard Unit: Side Pack Assembly. lessthan 10 Ibs. FM Unit: Side Pack Assembly.less than 11 ibs. Probe/ReadoutAssembly: less than 2 Ibs.

Operator requirements: One man, one hand opera-tion

Detection alarm: Frequency modulated audiblealarm. Can be preset to desired level. Fre-quency varies as a function of detection level

Flame-out Indication: Audible alarm plus visualmeter Indication

Battery test Battery charge condition indicated onreadout meter or battery recharger

Pickup fixtures: Variety of types for various applica-tions

Probe: Telescoping adjustment over 8 inches orprobe can be completely removed fromReadout Assembly

Umbilical cord: Cable between readout andsidepack with connectors for electrical cableand sample hose

Filtering: in-line particle filters and optional ac-tivated charcoal filter.

Side Pack case: Molded high impact plastic casewith carrying handle and shoulder strap

Electrical protection: Refer to Section 5Standard accessories:

1) Instrument carrying and storage case2) Fuel filling hose assembly3) A.C. battery charger4) Earphone5) Various pickup fixtures

Optional accessories:1) Gas chromatograph option2) Portable strip chart recorder3) Activated charcoal filter: also used

with desiccant as a moisture trap4) Dilution valve5) Septum adapter for use with gas

chromatograph option

SECTION 2DETAILED OPERATING PROCEDURES2.1 GENERAL

The procedures in this section are broken into fivepans: (1) Starting, (2) Operating. (3) Shut Down, (4) FuelRefilling, and (5) Battery Charging. After familiarization

TABLE OF CONTENTSPAGE

INTRODUCTION

SECTION 1: Description and Leading Particulars ............................................................... i1.1 General ............................................................................................11.2 Typical Applications................................................................................. 11.3 Other Typ»cat Uses. ................................................................................. 11.4 Major Features ..................................................................................... i1.5 Adaptability Features and Standard Accessories...................................................... 21.5.1 General............................................................................................21.5.2 Prop* .............................................................................................. 21.5.3 Pamela Filters ...................................................................................... 21.5.4 Instrument Carrying Case ...........................................................................21.5.5 Moblla Installation .................................................................................. 21.6 Specifications ...................................................................................... 2

SECTION 2: Detailed Operating Procedures.................................................................... 22.1 General ............................................................................................ 22.2 System Controls, indicators and Connectors..........................................................42.3 Starling Procedure.................................................................................. 42.3.1 Initial Preparation for Use............................................................................ 42.3.1.1 Initial Assembly... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .42.3.1.2 Servicing ........................................................................................... 42.3.1.3 Safety Precautions.................................................................................. 52.3.2 Turn On Procedure.................................................................................. 52.4 Operating Procedures............................................................................... 52.5 Shut Down Procedure ............................................................................... 62.6 Fuel Refilling ....................................................................................... 82.7 Battery Recharging — AC Battery Charger............................................................ 82.7.2 DC Charger......................................................................................... 72.8 Charcoal Filtering................................................................................... 72.9 Moisture Filtering................................................................................... 7

SECTION 3: Summarized Operating Procedures................................................................ 73.1 General ............................................................................................ 73.2 Start Up ............................................................................................ 73.3 Shut Down.......................................................................................... 7

SECTION 4: Calibration ....................................................................................... 74.1 General ............................................................................................ 74.2 Electronic Adjustments ...........................................................................4.2.1 Gain Adjustment..................................................................................4.2.2 Bias Adjustment..................................................................................4.3 Calibration to Other Organic Vapors. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.3.1 Setting Gas Seled Control (Span)..................................................................4.3.2 Using Empirical Data.......................'........,..............................................4.3.3 Preparation of Calibration Standard* ...............................................................4.3.3.1 Commercial Samples..............................................................................4.3.3.2 Pure Gaseous Samples............................................................................4.3.3.3 Gaseous and Liquid Samples (Alternate Method).. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .4.4 Theory...........................................................................................4.4.1 Hydrocartx>ns ....................................................................................4.4.2 Other Organic Compounds ........................................................................

SECTION 5: Safety ConskJeraliona ........................................................................... 115.1 General ........................................................................................... 115.2 Operating. Servicing and Modifying ................................................................ 115.3 Electrical Protection ............................................................................... 11

5.4 Fuel Supply and Tank . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115.5 Hj Flow Restrtctors . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 115,8 Detector Chamber ................................................................................. 115.7 Hj Filling and Emptying Operations.................................................................. n5.8 Venting ........................................................................................... n

SECTION 6: M«Jnten*nce....................................................................................136.1 General ........................................................................................... 138.2 Routine Maintenance .............................................................................. 138.2.1 Filtera............................................................................................. 136.2.1.1 Primary Filter...................................................................................... 136.2.1.2 Particle Filters.....................................................................................146.2.1.3 Miner/Burner Assembly Filter ...................................................................... 146.2.1.4 Exhaust Flame Arrester . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1 46.2.2 Pickup Fixtures.................................................................................... 148.2.3 Seal Maintenance — Cylinder Assembly . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 146.2.3.1 HJ Tank. HJ Supply and Refill Valves................................................................. 146.2.3.2 Refiller Valve Packing Adjustment................................................................... 146.2.4 Air Sampling System Maintenance .................................................................. 156.2.4.1 General........................................................................................... 156.2.4.2 Testing for Leaks .................................................................................. is8.2.4.3 Leak Isolation...................................................................................... 156.2.5 Contamination Control and Maintenance .. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . is8.2.5.1 General ........................................................................................... 156.2.5.2 Analysis snd Correction ............................................................................ 166.2.6 Fuse Replacement................................................................................. 178.3 Trouble Shooting .................................................................................. 176.4 Factory Maintenance............................................................................... 176.5 Field Maintenance ................................................................................. 186.6 Recommended Spares............................................................................. 16

SECTION 7: Optional Accessories............................................................................ 237.1 Gas Chromatograph (GC) Option.................................................................... 237.1.1 Introduction .......................................................................................237.1.2 Description and Leading Particulars.................................................................237.1.2.1 General...........................................................................................237.1.2.2 Principle of Operation . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .237.1.3 Operating Procedures... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .287.1.3.1 General ...........................................................................................287.1.3.2 GC System Controls and Components. . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 287.1.3.3 Servicing and Turn On..............................................................................297.1.3.4 Survey Mode Operation ............................................................................297.1.3.5 GC Mode Operation................................................................................ 297.1.4 Calibration ........................................................................................ 297.1.4.1 General ...........................................................................................297.1.4.2 Technical Discussion .............................................................................. 297.1.4.3 Preparation of Calibration Samples.................................................................. 327.1.4.4 Calibration Data.................................................................................... 327.1.5 Maintenance ......................................................................................327.1.5.1 General ...........................................................................................327.1.5.2 Routine Maintenance ..... . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . .327.1.5.3 Trouble Shooting .................................................................................. 357.1.5.4 Recommended Spares .............................................................................357.2 Recorder Option ................................................................................... 377.2.1 General ........................................................................................... 377.2.2 Applications....................................................................................... 377.2.3 Features .......................................................................................... 377.2.4 Controls and Connections .......................................................................... 377.2.5 Operating Procedures.............................................................................. 377.2.6 Calibration ........................................................................................ 377.2.6.1 General........................................................................................... 377.2.6.2 Mechanical Zero Adjustment ....................................................................... 37

SHOULDER CARRYINGSTRAP

SIDE PACK ASSEMBLY

PICKUP FUNNEL(NOT APPLICABLETO FM CERTIFIED

MODELS)

PROBE ASSEMBLY(ADJ. LENGTH)

"CLOSE" AREASAMPLER

EARPHONE

TUBULARSAMPLER

STANDARD 5 FT.UMBILICAL CORD

READOUT ASSEMBLY(CAN BE USED AS SHOWN WITHOUTFURTHER ATTACHMENTS INCONFINED AREAS)

FIGURE 1-2

INSTRUMENT DISASSEMBLEDTypical of All Models Except Where Noted.

with the instrument, the summarized proceduresdescribed m Section 3 may be used for simplicity.Because of the many optional applications for the in-strument, the comprehensive detailed proceduresdescribed in tnis section may seem complex. However.in normal applications the operating procedures arequite simple. A condensed operating procedure checklist is provided inside the cover of the Side PackAssembly. Refer to Section 7 for operating proceduresrelative to maior optional accessories such as the GasChromatograph Option.

2.2 SYSTEM CONTROLS, INDICATORS AND CON-NECTORS

Tables 2-1 and 2-2 describe the functions of thevarious controls, indicators and connectors illustratedm Figure 1-1. Unless otherwise noted, the listings inTables 2-1 and 2-2 are applicable to both the Model OVA-118 and OVA-128.

TABLE MSIDE PACK ASSEMBLY

Controls/indicator* — Function1) fNSTR/BATT Test Switch - This 3 position tog-

gle switch turns on all instrument electricalpower except the pump and alarm power andalso permits display of the battery charge con-dition on the readout meter.

2) PUMP (ON-OFF) Switch - This toggle switchturns on power to the internal pump and audioalarms.

3) igniter Switch - This momentary push buttonswitch connects power to the Igniter coil in thedetector chamber and simultaneously discon-nects power to pump.

4) CALIBRATE Switch (range selector) - This 3position toggle switch selects the desiredrange: X1 (0-10 ppm); X10 (0-100 ppm); X100 (0-1.000 ppm).

5) CALIBRATE ADJUST (zero) Knob - This poten-tiometer is used to "zero" the instrument.

6) GAS SELECT Knob (span control) - This ten-turn dial readout potentiometer sets the gain ofthe instrument commonly referred to aa spancontrol.

7) Recorder Connector - This 12S series 5-pin Am-phenol connector is used to connect the instru-ment to an external monitor with the followingpin connections.

Pin E-plus 12VOCPin H - GroundPin A - Signal 0-5VDC<OVA-ll8only)Pin B - Signal 0-5VDC (OVA-128 only)

8) Recharger Connector - This BNC connector isused to connect the battery pack to the batteryrecharger assembly.

9) H2 TANK VALVE - This vatve is used to supplyor close off the fuel supply from the hydrogentank.

10) H2 TANK PRESSURE Indicator - This highpressure gauge measures the pressure in thehydrogen fuel tank which is an indication of fuelsupply.

n) H2 SUPPLY VALVE-This valve is used to supp-ly or close off the hydrogen fuel to the detectorchamber.

12) H2 SUPPLY PRESSURE Indicator - This lowpressure gauge is used to monitor thehydrogen pressure at the capillary restrictor.

13) SAMPLE FLOW RATE Indicator - This indicatoris used to monitor the sample flow rate.

14) Refill Connection - This 1/4" AN fltttng is usedto connect the hydrogen refill hose to the in-strument.

15) REFILL VALVE - This valve is used to open oneend of the Instrument fuel tank for refilling withhydrogen.

16) Earphone Jack - This jack is used to connectthe earphone; it turns off speaker when used.

17) VOLUME Knob - This potentiometer adjusts thevolume of the internal speaker and earphone.

18) Readout and Sample Connectors - These con-nectors are used to connect the sample hoseand umbilical cord from the Probe/ReadoutAssembly to the Side Pack Assembly.

TABLE 2-2PROBE/READOUT ASSEMBLY

Controls/Indicators — FunctionA) Meter - This 250* linear scaled meter displays

the output signal level in ppm.B) Alarm Level Adjust Knob - This potentiometer

(located on the back of the Readout Assembly)is used to set the concentration level at whichthe audible alarm is actuated.

2.3 STARTING PROCEDURE2.3.1 INITIAL PREPARATION FOR USE2.3.1.1 INITIAL ASSEMBLY (Reference Figure 1-2)

a) Normal Survey Configuration(i} Connect the adjustable length probe to the

Readout Assembly with the captive lockingnut. Ensure that the probe is seated firmlyin the Readout Assembly.

(2) Select the desired pickup fixture and checkthat a particle filter is installed.

(3) Connect the pickup fixture to the probe us-ing the knurled locking nut.

(4) Connect the umbilical cord and samplehose to the Side Pack Assembly.

b) ' 'Close Area'' Survey Configuration(1) Check to ensure that a particle filter is in-

stalled In the close area sampler.(2) Connect the close area sampler directly to

the Readout Assembly.(3) Connect the umbilical cord and sample

hose to the Side Pack Assembly.

2.3.1.2 SERVICINGa) Fueling: Pure, dry hydrogen can normally be

, purchased locally or in a high grade from theMatheson Company of East Rutherford, NewJersey. The maximum instrument supply bottlepressure is 2300 PSIG. A high pressurehydrogen filling hose assembly is provided withthe instrument. This assembly includes theproper fittings for the instrument and supplybottle, and s three-way fill/bleed valve. Initialfueling and subsequent refilling, using the Cen-tury high pressure filling hose, should be ac-complished in accordance with the detailed in-structions described in Section 2.6 of thismanual.

b) Battery Check: Move INSTR/BATT Test Switchto the BATT position end ensure battery ischarged by reeding the indication on thereadout meter.

c) Calibration: Standard factory calibration is per-formed using methane in air. The GAS SELECT(span) Control is set and locked to the positionfor calibration to methane (factory setting is300). If the instrument is calibrated for otherorganic vapors, the reading on the GASSELECT Control must be set for that particularvapor.

2.3.1.3 SAFETY PRECAUTIONSCertain safety precautions must be followed in using

the instrument. Hydrogen gas, when mixed with air, ishighly flammable. Operating and refueling instructions•hould be strictly followed to ensure safe, reliable

aeration. Section 5 of the manual provides detailedsafety precautions.

2.3.2 TURN ON PROCEDUREThe GAS SELECT control should be preset to the

desired dial indication prior to turn on. The procedurefor determining this setting Is contained In Section 4 oftht» manual. The instrument, as received from the fac-tory, is set to measure in terms of methane in air.

a) Move the INSTR Switch to ON and allow fiveminutes for warm up.

b) To set the audible alarm to a predeterminedlevel, first turn the PUMP Switch to ON. thenadiust the meter pointer to the desired alarmlevel, using the CALIBRATE ADJUST (zero)Knob. Turn the Alarm Level Adjust Knob on theback of the Readout Assembly until the audiblealarm just comes on. Adjust speaker volumewith VOLUME Knob. If earphone is used, plugIn and readjust the volume as desired. The in-strument is then preset to activate the atarmwhen the level exceeds that of the setting.

c) Move the CALIBRATE Switch to X10 and adjustthe meter reading to zero with the CALIBRATEADJUST (zero) Knob.

d) Ensure the PUMP Switch is ON and observe theSAMPLE FLOW RATE Indicator. Indicationshould be approximately 2 units.

e) Open M2 TANK VALVE one (1) turn and observethe reading on the H2 TANK PRESSURE In-dicator. (Approximately 150 psi of pressure fs

needed for each hour of operation. >f) Open H2 SUPPLY VALVE 1/2 to 1 turn and

observe the reading on the M2 SUPPLYPRESSURE Indicator.

CAUTIONDo not leave H2 SUPPLY VALVE openwhen the pump is not running, as this willallow hydrogen to accumulate m the detec-tor chamber.

g) Confirm that meter Is still reading zero (readjustIf required).

h) Depress igniter button. There will be a slight"pop" as the hydrogen ignites and the meterpointer will move upscale of zero. Immediatelyafter ignition, release the igniter button. Do notdepress igniter button for more than 6 seconds.If burner does not ignite, let instrument run forseveral minutes and try again. After ignition,the meter pointer will indicate the backgroundconcentration. This background level is nulledout using the CALIBRATE ADJUST (zero) Knob.Reference paragraph 6.2.5.1.

NOTESince the OVA utilizes the sample air drawnby the pump into the detector chamber asthe only source of air to support thehydrogen flame, without adjustment the in-strument will read the actual backgroundconcentration (ppm) of all hydrocarbonspresent at a given location.

I) Move instrument to an area which is represen-tative of the "lowest ambient background con-centration" (cleanest air) to be surveyed. Movethe CALIBRATE Switch to XI and adjust themeter to read 1 ppm with the CALIBRATE AD-JUST <zero> Knob.

NOTEAdjustment to 1 ppm (rather than 0) isnecessary in the X1 range because of thesensitivity of the OVA. This permits minordownward fluctuations in the normalbackground level without dropping below0, which would actuate the flame-out alarm.It Is important, therefore, to remember dur-ing the subsequent survey that 1 ppm mustbe subtracted from all readings. Therefore,a 1.8 ppm reading would actually be only 0.6ppm.

j) If the alarm level is to be set above the normalbackground detection level, turn the AlarmLevel Adjust Knob on the back of the ReadoutAssembly until It actuates slightly abovebackground.THE INSTRUMENT IS NOW READY FOR USE

2.4 OPERATING PROCEDURESa) Set the CALIBRATE Switch to the desired

rang*. Using one hand operation, survey theareas of interest while observing the meterand/or listening for the audible alarm indica-tion. For ease of operation, carry the Side PackAssembly positioned on the side opposite thehand which hold* (he Probe/ReadoutAssembly. For broad surveys outdoors, thepickup fixture should be positioned several feetabove ground level. When making quantitativereading or pinpointing, the pickup fixtureshould be positioned at the point of Interest

0) When organic vapors are detected, the meterpointer will move upscale and the audible alarmwill sound when the preset point Is exceeded.The frequency of the audible slarm will in-crease as the detection level Increases.

c) if the flame-out alarm is actuated, ensure thatthe pump is running, then press the Igniter but-ton. Under normal conditions, flame-out resultsfrom sampling a gas mixture that is above thelower explosive level which causes the H2flame to extinguish. If this Is the case, reignt-tion is all that is required.Another possible cause for flame-out would berestriction of tne sample flow line which wouldnot allow sufficient sir Into the chamber to sup-port combustion of the H2 flame. The normalcause for such restriction would be s cloggedpanicle filter or other restriction in the line,it should be noted that the chamber exhaustport Is on the bottom of the case and blockingthis port with the hand will cause fluctuationsand/or f tame-out.

2.5 SHUT DOWN PROCEDUREThe following procedure should be followed for shut

down of the Instrument:1 > Close M2 SU PPLY VALVE.2) Close H2 TANK VALVE.3) Move INSTR Switch to OFF.4) Wait 5 seconds and move PUMP Switch to OFF.

INSTRUMENT IS NOW IN A SHUT DOWN CON-FIGURATION.

2.0 FUEL REFILLINGa) The Instrument should be completely shut

down aa described In Section 2.5 herein duringhydrogen tank refilling operations. The refillingshould be done in a ventilated area. Thereshould be no potential igniter* or flame in theare*.

b) If you are making the first filling of the instru-ment or tf the filling hose has been allowed tofill with air, the filling hose should be purgedwith N2 or H2 prior to filling the Instrument tank.This purging is not required for subsequent fill-ings.

c) The filling hose assembly should be left attach-ed to the hydrogen supply tank when possible.Ensure that the FILL/BLEED Valve on the in-strument end of the hose is in the OFF position.

Connect the hose to the refill connection on :Side Psck Assembly.

d) Open the hydrogen supply bottle valve slightly.Open the REFILL VALVE and the H2 TANKVALVE on the instrument panel and place theFILL/BLEED Valve on the filling hose assemblyin the RLL position. The pressure m the instru-ment tank will now be indicated on the H2 TANKPRESSURE Indicator.

e) After the instrument fuel tank is filled, shut offthe REFILL VALVE on the panel, theFILL/BLEED Valve on the filling hose assemblyand the hydrogen supply Dome vatve.

0 The hydrogen trapped in the hose should nowbe bled off to atmospheric pressure. CAUTIONshould be used in this operation as describedm Step (g) below, since tne hose will contain asignificant amount of hydrogen at highpressure.

g) The hose is bled by turning the FILL/BLEEDValve on the filling hose assembly to theBLEED position. After the hose is bled down toatmospheric pressure, the FILL/BLEED Valveshould be turned to the FILL position to allowthe hydrogen trapped in the connection fittingsto go into the hose assembly. Then, again, turnthe FILL/BLEED Valve to the BLEED positionand exhaust the trapped hydrogen. Then turnthe FILL/BLEED Valve to OFF to keep thehydrogen at one atmosphere in the hose sothat at the time of the next filling there will r-no air trapped In the filling line.

h) Close the H2 TANK VALVE.i> With the H2 TANK VALVE and the H2 SUPPLY

VALVE closed, a small amount of H2 at highpressure will be present in the regulators andplumbing. As a leak check, observe the H2TANK PRESSURE indicator while the re-mainder of the system is shut down and ensurethat the pressure indication does not go downrapidly, indicating a significant leak. If it doesdecrease rapidly (greater than 350 PSIG/hr),there is a significant leak in the H2 supplysystem.

2.7 BATTERY RECHARGINGa) Ptug charger BNC connector into mating con-

nector on battery cover and insert AC plug into115 VAC wall outlet. Never charge in a hazar-dous area or environment.

b) Move the battery charger switch to the ON posi-tion. Tne light above the switch button shouldilluminate.

c) Battery charge condition is indicated by themeter on the front panel of the charger; meterwill deflect to the right when charging. Whenfully charged, the pointer will be in line with"charged" marker above tne scale.

d) Approximately one hour of charging time is re-quired for each hour of operation. However, anovernight charge is recommended. Thecharger can be left on indefinitely withou'

damaging the batteries. When finished, movethe battery charger switch to OFF and discon-nect from the Side Pack Assembly.

i The following are special Instruction* relative to bat-teries which have be*n allowed to completelydischarge.

It has been established that the above batteryrecharging procedures may not be sufficient when theoperator of the instrument has Inadvertently left the IN*STR Switch ON for a period of time without rechargingand allowed the battery to completely discharge.

When this happens and the above procedures fail torecharge the battery, the following should be ac-complished:

1 > Remove the battery from the instrument case.2) Connect to any variable DC power supply.3) Apply 40 volts at 112 amp maximum.4) Observe the meter on the power supply fre-

quently and as soon as the battery begins todraw current, reduce the voltage on the powersupply at a alow rate until the meter reads ap-proximately 15 volts. NOTE: The time requiredto reach the 15 volt reading will depend ondegree of discharge.

5) Repeat steps a), b), c), and d) above to continuecharging.

2.7.2 DC CHARGERa) The optional DC charger Is designed to both

charge the battery and to provide power foroperating the instrument from a 12 volt DCsource, such as vehicle power.

b) Connect the DC charger cord to the connectoron the battery cover of the Side PackAssembly. Plug the line cord into the vehiclecigarette lighter or other power source connec-tion.

c) In mobile applications, the DC charger is usedto supply vehicle power to the instrument.Therefore, it may be left connected at all times.

2.8 CHARCOAL FILTERINGWhen it is desired to preferentially remove the

heavier hydrocarbons, such as those associated withautomobile exhaust, gasoline, etc., simply remove thepickup fixture from the end of the probe and install theoptional charcoal filter assembly.

This same charcoal filter assembly can be installeddirectly Into the Readout Assembly by using the adapterprovided.2.9 MOISTURE FILTERING

Filtering of moisture in the sample Is not normally re-quired. However, when moving in and out of buildings incold weather, excessive condensation can form in thelines and detector chamber. In this case, the charcoalfilter adapter can be filled with a desiccant such as"Driente" which will filter out the moisture contained inthe sample.

SECTION 3SUMMARIZED OPERATING PROCEDURES3.1 GENERAL

The procedures presented in this section are intend-ed for use by personnel generally familiar with theoperation of the instrument. Section 2 presents the

j comprehensive detailed operating procedures.

It is assumed that, prior to start up the positions of allswitches and valves are in shut down configuration asdescribed in paragraph 3.3.

3.2 START UPa) Move PUMP Switch to ON and check battery

condition by moving the INSTR Switch to theBATT position.

b) Move INSTR Switch to ON and allow five (5)minutes for warm-up.

c) Set Alarm Level Adfust Knob on back ofReadout Assembly to desired level.

d) Set CALIBRATE Switch to XI0 position, useCALIBRATE Knob and set meter to read 0.

e) Move PUMP Switch to ON position men placeinstrument panel in vertical position and checkSAMPLE FLOW RATE indication.

f) Open the H2 TANK VALVE and the H2 SUPPLYVALVE.

g) Depress Igniter Button until burner lights. Donot depress Igniter Button for more than six (6)seconds. (If burner does not ignite, let Instru-ment run for several minutes and again attemptignition.)

h) Use CALIBRATE Knob to "zero" out ambientbackground. For maximum sensitivity below 10ppm, set CALIBRATE Switch to XI and readjustzero on meter. To avoid false flame-out alarmindication, set meter to 1 ppm with CALIBRATEKnob and make differential readings fromthere.

3.3 SHUTDOWNa) Close the H2 SUPPLY VALVE and the H2 TANK

VALVE.b) Move the INSTR Switch and PUMP Switch to

OFF.c) Instrument Is now in shut down configuration.

SECTION 4CALIBRATION4.1 GENERAL

The OVA is capable of responding to nearly allorganic compounds. For precise analyses It will benecessary to calibrate the instrument with the specificcompound of interest. This is especially true formaterials containing elements other than carbon andhydrogen.

The Instrument is factory calibrated to a methane inair standard. However, it can be easily and rapidlycalibrated to a variety of organic compounds. A GASSELECT control is incorporated on the instrument panelwhich is used to set the electronic gain to a particularorganic compound.

Internal electronic adjustments are provided tocalibrate and align the electronic circuits. There are four(4) such adjustments all located on the electronicsboard. One adjustment potentiometer, R-38, is used toset the power supply voltage and is a one-time factoryadjustment. The remaining three adjustments, R-31, R-32 and R-33 are used for setting the electronic amplifiergain for each of the three (3) calibrate ranges. Access tothe adjustments is accomplished by removing the In-strument from its case. Figure 4-1 indicates the locationof the adjustments.

42 ELECTRONIC ADJUSTMENTSPrimary calibration of this instrument is accomplished

at the factory using methane in air sample gases.

4 2.1 GAIN ADJUSTMENTa) Place instrument in normal operation with

CALIBRATE Switch set to X10 and GAS SELECTcontrol set to 300.

b) Use the CALIBRATE ADJUST (zero) Knob andadjust the meter reading to zero.

c) introduce a methane sample of a known con-centration (near 100 ppm) and ad|uat trim pot PI-32 on circuit board {see Figure 4-1 for location)so that meter reads equivalent to the Knownsample.

d) This seta the Instrument gain for methane withthe panel mounted gain adjustment (GASSELECT) sat at a reference number of 300.

e> Turn off H2 SUPPLY VALVE to put out flame.

4.2.2 BIAS ADJUSTMENTa) Leave CALIBRATE Switch on X10 position and

use CALIBRATE ADJUST (zero) Knob to adjustmater reading to 4 ppm.

b) Place CALIBRATE Switch in X1 position and,using thmpot R-31 on circuit board, adjustmeter reading to 4 ppm. (See Figure 4-1)

c) Move CALIBRATE Switch to X10 position again.Use CALIBRATE ADJUST (zero) Knob to adjustmeter to a reading of 40 ppm.

d) Move CALIBRATE Switch to X100 position anduse trlmpot R-33 on circuit board to adjustmeter reading to 40 ppm.

e) Move CALIBRATE Switch to X10 position anduse CALIBRATE ADJUST (zero) Knob to adjustmeter reading to zero.

f) unit is now balanced from range to range,calibrated to methane, and ready to be placedin normal service.

R-33

rt-38—

FIGURE 4-1. LOCATION OF ELECTRONICADJUSTMENTS(Mode* OVA-118 shown; location typical to OVA-128)

4.3 CALIBRATION TO OTHER ORGANIC VAPORS4.3.1 SETTING GAS SELECT CONTROL (Span)

Primary calibration of the instrument is accomplishedusing a known mixture of a specific organic vapor com-pound. After the instrument is m operation and the"normal background" is "zeroed out", draw a sampleof the calibration gas into the instrument. The GASSELECT Knob on the panel is then used to shift thereadout meter Indication to correspond to the concen-tration of the calibration gas mixture.

The instrument is then calibrated for the vapor mix-ture being used. After this adjustment, the setting onthe "dlgidlal" Is read and recorded for that particularorganic vapor compound. This exercise can be perform-ed for a large variety of compounds and when desiringto read a particular compound the GAS SELECT controlis turned to the predetermined setting for the com-pound. Calibration on any one range automaticallycalibrates the other two ranges.

4.3.2 USING EMPIRICAL DATARelative response data may be obtained, which can

then be used to estimate concentrations of variousvapors. With the instrument calibrated to methane, ob-tain the concentration reading for a calibration sampleof the test vapor. The relative response, in percent, forthat test vapor would then be the concentrationread/concentration of the calibrated sample X100.

4.3.3 PREPARATION OF CALIBRATION STANDARDS4.3.3.1 COMMERCIAL SAMPLES

Commercially available standard samples offer themost convenient and reliable calibration standards andare recommended for the most precise analyses.Always remember to obtain the cylinder with thedesired sample and the "balance as air". Sampleshould be drawn from the cylinder into a collapsed sam-ple bag, then drawn from the bag by the instrument toprevent a pressure or vacuum at the sample inlet.

4.3.3.2 PURE GASEOUS SAMPLESObtain a large collapsible sample bag. preferably

polyethylene such as a 40 gallon trash can liner. Insert atube into the bag opening and tie shut around the tube.The tubing should have a shut-off valve or plug and besuitable for connecting the OVA input tube. Determinethe volume of the bag by appropriate means (I.e., wet-test meter, dimensions of the bag, etc.). Forty gallonpolyethylene bags provide a volume of approximately140-160 liters. For gas samples, flush a 10 cc hypodermicsyringe with the compound to be tested and then injecta 10 cc sample through the wail of the air-tilled bag. Im-mediately after withdrawing the needle, cover the holewith a piece of plastic tape. Allow a few minutes for thesample to completely diffuse throughout the bag. Agita-tion will ensure complete diffusion. Connect the outlettube to the OVA and take a reading. To verifyrepeatability of sampling technique, disconnect the bagand inject a second sample of the gas into the bagwithout emptying. Since only 2 or 3 liters will have beenremoved, the overall volume change will be small andthe instrument reading should now be twice that of the

original. The concentration in ppm (V/V) will be equal tothe sample size m cc divided by the volume of the bag inliters times 1000. For example, a 10 cc gas sample when"laced in a 160 liter bag will provide a sample of 63 ppm,»., 10X1000/160 equals 63 ppm.

4 3.3.3 GASEOUS AND LIQUID SAMPLES (AlternateMethod)

Obtain a five (5) gallon glass bottle and determine itsvolume by measuring the volume of water needed to fillIt (use of a 1000 ml graduated cylinder, obtainable fromscientific supply houses, is convenient). Another ap-proach is to weigh the empty bottle, fill It with water andweigh again. The difference between the two values isthe weight of water. By multiplying the weight of waterin pounds by 0.455, you obtain the volume of the botttein liters. Empty the water out and allow the bottle to dry.Place a one-foot piece of plastic tubing in the flask to aidIn mixing the vapors uniformly with the air. The volumeof such a bottle should be about 20 liters, which Is 20,000ml. If the volume were 20,000 ml, then a 2 ml sample of agas placed In the bottle would b« equivalent to 200 mlper 2 million ml or 100 ppm (V/V). Use of a gas tight syr-inge, readable In 0.01 ml. allows the preparation of mix*tures in the 1 - 2 ppm range, which are sufficient for thequantitative estimation of concentrations. A rubberstopper is loosely fined to the top of the bottle and theneedle of the syringe placed Inside the jug neck and thestopper squeezed against the needle to decreaseleakage during sample introduction. Infect the sampleInto the bottle and withdraw the needle without remov-ing the stopper. Put the stopper In tight and shake thebottle for a few minutes with sufficient vigor that theplastic tubing In the bottle moves around to ensurepod mixture of the vapors with the air.' For liquid samples, use of the following equation will

allow the calculation of the number of microiiters oforganic liquid needed to be placed into the bottle tomaKe 100 ppm (V/V) of vapor.

VI equals V2 X Mw/244D

VI - Volume of liquid in mlcrollters needed to makean air mixture of 100 ppm (V/V)

V2 - Volume of bottle in litersMw - Molecular weight of substanceD - Density of substance

This procedure has the advantage that you can seewhen all of the organic liquid has vaporized and thevolume can be determined readily.

For liquid samples, an alternate procedure involvesthe use of a diffusion dilution device such as thatdescribed by Desty, Geach and Gold up in "GasChromatography", R.P.W Scott, ed.. Academic Press,New York, 1961.

4.4 THEORYTheoretical background and empirical data related to

the Century Organic Vapor AnaJyzer is presented In4.4.1 and4.4.2.

4.4.1 HYDROCARBONSIn general, a hydrogen flame lonization detector is

more sensitive for hydrocarbons than any other class otorganic compounds. The response of the OVA vanesfrom compound to compound, but gives excellentrepeatable results with all types of hydrocarbons; i.e..saturated hydrocarbons (alkanes), unsaturatedhydrocarbons (alkenes and atkynes) and aromatichydrocarbons.

The typical relative response of various hydrocarbonsto methane is as follows:

CompoundMethanePropaneN-butaneN-pentaneEthyleneAcetyleneBenzeneTolueneEthane

Relative Response (percent)100 (reference)6461

10065

200150120

BO

-4 4.2 OTHER ORGANIC COMPOUNDSCompounds containing oxygen, such as alcohols.

ethers, aldehydes, carbolic acid and esters give asomewhat lower response than that observed forhydrocarbons. This is particularly noticeable with thosecompounds having a high ratio of oxygen to carbonsuch as found In the lower members of each serieswhich have only one, two or three carbons. With com-pounds containing higher numbers of carbons, the ef-fect of the oxygen is diminished to such an extent thatthe response la similar to that of the correspondinghydrocarbons.

Nitrogen-containing compounds (I.e., amines,amides and nitrites) respond in a manner similar to thatobserved for oxygenated materials. Halogenated com-pounds also show a lower relative response as com-pared with hydrocarbons. Materials containing nohydrogen, such as carbon tetrachlohde, give the lowestresponse; the presence of hydrogen in the compoundsresults in higher relative responses. Thus, CHCb givesa much higher response than does CCU. As in the othercases, when the carbon to halogen ratio is 5:1 orgreater, the response will be similar to that observed forsimple hydrocarbons.

The typical relative response of various compoundsto methane Is as follows:

Methane 100 (calibration sample)Ketones

Acetone 60Methyl ethyl ketone 80Methyl isobutyl ketone 100

AlcoholsMethyl alcoholEthylIsopropyl

152565

Halogen compounds

Carbon tetrachlorlde 10Chloroform 45Trlchloroethylcne 70vinyl chloride 35

The OVA has negligible response to carbon monoxideand carbon dioxide which evidently, due to thatr atruo-tura. do not product appreciably lona In th« detectorflam*. Thus, othar organic materials may be analyzed tnthe presence of CO end CO>.

10

SECTION 5SAFETY CONSIDERATIONSM GENERAL

The Models OVA-106, OVA-128 and OVA-138 have•en tested and certified by Factory Mutual Research

Corporation <FM) as intrinsically sate for use in Class I,Division 1. Groups A, B, C & D hazardous atmospheres.Similar foreign certifications have been obtained, in-cluding BASEEFA and Cerchar approval for Group IIC,Temperature Class T4 on the Models OVA-106. OVA-128and OVA-138, and equivalent approval from theJapanese Ministry of Labor for the Model OVA-126.Special restrictions must be strictly adhered to, to en-sure the certification is not invalidated by actions ofoperating or service personnel.

Atl flame lonization hydrocarbon detectors are poten-tially hazardous since they burn hydrogen (H2) or H2mixtures in the detector cell. Mixtures of H2 and air areflammable over a wide range of concentrations whetheran Inert gas such as nitrogen (N2) is present or not.Therefore, the recommended precautions and pro-cedures should be followed for maximum safety. Safetyconsiderations was a major factor in the design of theOrganic Vapor Analyzer (OVA).

All connectors are of the permanent type as opposedto quick disconnect. To protect against external ignitionof flammable gas mixtures, the flame detectionchamber has porous metal flame arresters on the sam-ple input and the exhaust ports as well as on the H2 inletconnector. The standard battery pack and other circuitsare internally current limited to an intrinsically safelevel.

v2 OPERATING, SERVICING AND MODIFYING) H Is imperative that operation and service procedures

described In this manual be carefully followed In orderto maintain the intrinsic safety which is built into theOVA. No modification to the Instrument Is permissibleTherefore, component replacement must be ac-complished with the same type pans.

5.3 ELECTRICAL PROTECTIONThe 17V battery power supply circuit is current limited

jo an intrinsically safe level. Fuses are not utilized andall current limiting resistors and other componentswhich are critical to the safety certification are en-capsulated to prevent Inadvertent replacement withcomponents of the wrong value or specification. Underno circumstances should the encapsulation be remov-ed.

5.4 FUEL SUPPLY & TANKThe OVA fuel tank has a volume of 75 to 85 cc which,

when filled to the maximum rated pressure of 2300 PSIG,holds approximately 5/8 cubic foot of gas. The fuel usedIn the OVA Is pure hydrogen which can be readily pur-chased In a highly pure form at nominal cost. The H2tanks used In the instrument are made from stainlesssteel, proof-tested to 6,000 PSIG and 100% productiontested to 4,000 PSIG.

5.5 M2 FLOW RESTRICTORSHydrogen ga* gains heat when expanding and,

therefore, should not be rapidly released from a highpressure tank to a low pressure environment. Flowrestrictors are incorporated in the H2 refill fining and H2is restricted on the output side of the tank by the lowflow rate control system. In addition, a special flowre stricter is Incorporated in the FILL/BLEED valve of thehydrogen filling hose assembly. These precautionslimit the flow rate of the H2 to prevent ignition due tosetf-heat from expansion.

5.6 DETECTOR CHAMBERThe OVA has a small flame ionization chamber cavity

with aintered metal flam* arresters on both the inputand output ports. The chamber is ruggedly constructedof teflon such that even if highly explosive mixtures ofH2 and air are inadvertently created in the chamber andignited, the chamber would NOT rupture.

5.7 H2 FILLING AND EMPTYING OPERATIONSPrecautions should be taken during H2 filling or H2

tank emptying operations to ensure that there are nosources of Ignition in the immediate area. Since the in-strument tank at 2300 PSIG holds only 5/8 cu. ft. of H2.the total quantity, if released to the atmosphere, wouldbe quickly diluted to a non-flammable level. There is.however, the possibility of generating flammable mix-tures In the immediate vicinity of the Instrument duringthe filling or emptying operations if normal care is notexercised.

5.8 VENTINGThe OVA case is vented to eliminate the possibility of

trapping an explosive mixture of H2 and air inside thecase.

11

SECTION 8MAINTENANCE8.1 GENERAL

This section describes the routine maintenanceschedule recommended and provides procedures fortrouble shooting malfunctions or failures In the instru-ment.

Appendix "A" to this manual contains the assemblydrawings snd associated parts list for the Side PackAasembly and two major subassemblles; the ElectronicComponent Assembly snd the Cylinder Assembly.These drawings and parts lists may t>e used for locatingand Identifying components. Also included in Appendix"A" is s schematic wiring diagram showing Intercon-necting wiring between major electronic assembliesand typical signal level* st selected points on the cer-tified Instruments. The enclosed drawings and partslists sre subject to change without notlc* and partreplacement on any certified instrument should beverified to comply with the "no modifications permit-ted" requirement.

CAUTIONMaintenance personnel should be thoroughlyfamiliar with instrument operation before perform-ing maintenance, it Is essential that all portions ofthis manual relating to safety of operation, servicingand maintenance, Including Section 5, bethoroughly understood. There should be no poten-

tial igniters or flame In the area when filling, empty-ing or purging the hydrogen system ana the instru-ment should be turned off.Extreme care should be exercised to ensure thatrequired parts replacement is accomplished withthe same parts specified by Century. This Isespecially necessary on thejtflodels OVA-108, OVA-128 and OVA-138 In order that their certification foruae in hazardous atmospheres be maintained. Nomodifications are permitted. Disassemble instru-ment only (n a non-hazardous atmosphere.

8.2 ROUTINE MAINTENANCENote that Figure 8-1 Is a flow diagram of the basic gas

handling system.

6.2.1 FILTERS8.2.1.1 PRIMARY FILTER

This filter is located behind the sample Inlet connec-tor (Fining Assembly) on the Side Pack Assembly and isremoved for cleaning by using a thin wall socket tounscrew the Fitting Assembly. The filter cup, "O" ringand loading spring will then come out as shown In theSide Pack Assembly drawing in Appendix "A". Theporous stainless filter cup can then be cleaned by blow-Ing out or washing In s solvent. If s solvent is used, careshould be taken to ensure that alt aolvent Is removed byblowing out or heating the filter. Reassemble In reverseorder ensuring that the "O" ring seal on the FiningAssembly Is Intact.

Cftm pit Hot*UMBILICAL CORD fc

L_ _ _»*&PS3LTj|ffXi. _ __I

I_-__ _ _ _ _ _ ]

FIGURE 6-1. Flow Diagram - Gas Handling System

13

6.2.1.2 PARTICLE FILTERSA particle filter la located in each pickup fixture. On*

of these fillers must be In the sample line whenever theinstrument Is In use. The Models OVA-38 and OVA-139use • disposable cellulose filler which should be chang-ed as often as required. The Models OVA-98, OVA-108.OVA-US and OVA-128 use a poroua metal niter whichcan be replaced or cleaned using the cleaning pro-cedure m paragraph 6.2.1.1.

fl.2.1.3 MIXER/BURNER ASSEMBLY FILTERAnother poroua metal particle filter Is incorporated in

the Mixer/Burner Assembly which screws into thePreamp Assembly. See Side Pack Assembly drawing.This filter is used as the sample mixer and inlet flame ar-reator in the chamber. This Miter should not becomecontaminated under normal conditions but can becleaned or the assembly replaced If necessary.

Access to thla filter for output surface cleaning Isgained by simply unscrewing the exhauat port from thePreamp Assembly without removing the instrumentfrom the case. The OVA-108, OVA-128 and OVA-138 in-struments require removal of the safety cover prior tounscrewing the exhaust port. The Filter Assembly cannow be seen on the side of the chamber (PreampAssembly) and can be scrapped or cleaned with a smallwire brush.

If filter replacement Is required, install a new or fac-tory rebuilt Mixer/ Burner Assembly. In several OVAmodels, this requires removal of the Preamp Assembly.

8.2.1 4 EXHAUST FLAME ARRESTORA porous metal flame arrester is located in the ex-

haust port of the detector chamber (Preamp Assembly).See Side Pack Assembly drawing. It acts as a paniclefilter on the chamber output and restricts foreign matterfrom entering the chamber. This filter may be cleaned, ifrequired, by removing the exhaust port from thePreamp Assembly. The exhaust port is removed fromthe bottom of the case without case removal. Note thatthe filter is captive to the exhaust port on the ModelsOVA-108, OVA-128 and OVA-138. Clean the filter with asolvent or detergent but ensure that it is dry and anysolvent completely baked out at 120*F before reinstall-ing.

6.2.2 PICKUP FIXTURESThe pickup fixtures should be periodically cleaned

with an air hose and/or detergent water to eliminateforeign particle matter. If a solvent is used, the fixtureshould be subsequently cleaned with detergent andbaked out at 120*F to eliminate any residual hydrocar-bons from the solvent.

6.2.3 SEAL MAINTENANCE - CYLINDER ASSEMBLY6.2-3.1 H2 TANK, H2 SUPPLY AND REFILL VALVES

After some time, the teflon washers under each valvepacking nut can "cold flow" (move with pressure) andallow hydrogen to leak. Leakage can be determined byusing Leak-Tec, Snoop or a soap solution around thevatve stems. This leakage can usually be stopped bytightening the compression nut (adapter) as outlined

below. See Side Pack Assembly and Cylinder Assemblydrawings.

1) Remove instrument from the case by unlockingthe four (4) 114 turn fasteners on the panel andremoving the exhaust safety cover (if included),exhaust port and refill cap nut. Be sure refillvalve is closed before removing refill cap nut.

2) Remove the valve knob screw and knob.3) Loosen the panel nut with a 3/4" wrench.4) The valve compression nut is located fust under

the panel. Tighten the compression nut-usually not more than 1/4 turn.

Thla compression is against soft material and only asmall amount of force Is necessary to sufficientlycompres* the teflon washers, if, after tightening.leakage still occurs, it would be advisable toreplace the two teflon washers, as follows:1) Drain hydrogen system slowly and to the extent

necessary to work on the leaking velvets).Observe safety precautions (see Section 5).There should be no potential igniters m thearea.

2) Disconnect the capillary tube from the manifoldat low pressure gauge (H2 Supply Pressure).

3) Remove all three (3) knob screws and knobs.4) Remove the three (3) panel nuts and washers.5) Carefully remove the tank assembly from tne

panel. NOTE: If OVA has GC Option installed,the GC valve assembly must be loosened orremoved In order to remove the tank assemblyfrom the panel.

6) Remove the compression nut on the valve thatis not sealing properly. Remove the stem byunscrewing it from the valve body. Observe thesandwich of metal and teflon washers and notetheir order.

7) Visually check the Kel-F seat on the stem forcracks or foreign material. Wipe clean, ifnecessary, with a lint free cloth (no solvents oroils) and replace if damaged.

8) Ramove the washers and replace the teflonwashers (the factory procedure is a light wipeof hydrocarbon free siiicone grease).

9) Replace the stem assembly in the valve bodyand tighten lightly.

10) Push the washers down into the compressionarea in the same order as noted upon removal.Replace the compression nut and tighten snug-ly.

11) Close the low pressure valve and fill the tankassembly. Check valves tor leaks. Tightenagain, if necessary, and reassemble the unit.

6.2.3.2 REFILLER VALVE PACKING ADJUSTMENTAdjustment for the valve on the refiner can be made

by loosening the set screw with a 3/32" hex key, so thatthe handle turns freely on the stem. Insert two (2) 3/32"hex keys through the holes provided in the handle andturn until they engage the holes m the packing adjuster.Then tighten the packing by turning the handle.

14

TWO 3/32*

MAHOU

•losrrsorew

6.2.4 AIR SAMPLING SYSTEM MAINTENANCE6.2.4.1 GENERAL

A potential problem associated with the OVA instru-ment is that leaks can develop In the air sample pump-ing system. These leaks can result in either dilution or<oss of sample, causing low reading of vapor concentra-

in and slow response time.

6.2.4.2 TESTING FOR LEAKSThe OVA'S a re equipped with a flow gauge, which

provides a method to check for air leaks. Assemble thepickup probe selected for use to the readout assemblyand then position the sldepack vertically so the flowgauge may be observed. Cover the end of the pickupprobe with your finger and observe that the ball in the"ow gauge goes to the bottom. Indicating no air flow (if

til has slight chatter while on bottom, this Is accep-^bte). Cover the center of the chamber exhaust portwith your thumb and again observe the ball going to thebottom. Another simple check Is to expose the pickupprobe to cigarette smoke or a light vapor (butane) andobserve that the meter responds in approximately 1.5 -2.0 seconds. It should be noted that slow meterresponse may also Indicate a restriction in the air•*mpling system.

0.2.4 3 LEAK ISOLATIONFailure of the ball to go to the bottom when the inlet is

blocked indicates a leak in the system between the pro-be and the pump inlet or the inlet check valve. To isolatethe problem, remove parts, one at a time, and againblock off the air inlet. Remove the pickup probe<s) andcover the air inlet at the Readout Assembly. If the ballgoes to the bottom, check that the "readout to probe"seal washer Is In place and replace the probes, holdingthem back against this seal while tightening the nut.Recheck, and If leakage is still present. It is probably inthe probe (pickup fixture), which should be repaired orreplaced.

If leakage Is Indicated as being past the readout han-dle when the connection to the sidepack is tight,disconnect the sample line at the fitting on the sideoeckand cover this inlet with your finger. If the flow gauge

ball goes to the bottom, the problem should be a leak inthe umbilical cord/Readout Assembly, which should beinvestigated and repaired. There Is also the possibilityof a leaking check valve in the pump which would notshow up on this test. If the leakage is not found in theumbilical cord. It Is most likely In the pump check valvewhich should be repaired or replaced.

(f the ball does not go to the bottom, the leak will beeither In the flow gauge or tt's connecting tubing.Visually check mat the tubing Is connected and if so,the flow gauge should be repaired or replaced. Checkthe "O" ring installation In the sample inlet connector(Fitting Assembly).

As an alternate approach, leaks on the inlet side ofthe pump can be detected by using alcohol on a "Q" Tipand lightly swabbing the connections one at a time or bydirecting organic vapor or smoke at the potentialleakage points and observing the meter response oraudible alarm.

Leaks (beyond the pump) are easier to locate, as anyof the commercially available leak detection solutionscan be used. Cover the exhaust port, which will placethe exhaust system under pressure, and check eschconnection, one at a time. Replace the teflon tubing orretape me threaded connections with teflon joint tape.Check the Igniter and Mixer/Burner Assembly wherethey screw Into the detector, me high voltage terminalscrew on the side of the Mixer/ Burner and exhaust portitself. If attar these checks, the flow gauge ball still willnot go to the bottom with the exhaust blocked, the pro-blem is likely a leaking exhaust check valve in thepump, which should be repaired or replaced.

6.2.5 C O N T A M I N A T I O N C O N T R O L ANDMAINTENANCE

6.2.5.1 GENERALOn occasion, the background reading of the OVA may

be relatively high under normal ambient conditions. Am-bient background readings will vary somewhat depen-ding on the geographical location where the instrumentIs being used. However, the background reading nor*mafly should be In the range of 3 to 5 ppm as methane.The acceptable background reading consists of 1 to i-1/2 ppm of methane which Is present In the normal airenvironment. In addition to the measurement of a nor-mal methane background, there will normally be 2 to 4ppm of equivalent methane background caused by ac-ceptable levels of contamination in the hydrogen fueland/or hydrogen fuel handling system resulting in atotal equivalent methane reading of 3 to 5 ppm In cleanair.

If the background reading goes above 5 ppm to 6 or 7ppm, this is normally still acceptable since anymeasurement is additive to that background reading.I.e., 2 ppm on top of 5 or 2 ppm on top of 7 provides thesame differential reading, however, the towerbackground Is obviously desirable.

The background reading on the linear OVA's iszeroed out or nulled out—even though in reality thebackground still exists. The background reading on the

15

linear OVA's la measured by zeroing the meter with ttwflame out and noting the meter indication after the Mam*la on. However, on the logarithmic scaled OVA'a mebackground reading la observed on the meter at alltlmea. This ia considered desirable since it assures m*operator that the instrument la. in fact, operating pro-perly. The background reading on the OVA'3 serves aaa low level calibration point since it doea represent themeasurement of ambient levels of methane In the air,which are extremely stable and predictable any place inthe world.

The cause for a high background reading la uauallyassociated with contamination In the hydrogen fuelsystem. Thla will, of course, cauae a backgroundreeding since thla la the function of the basic detector"to measure contamination entering the detectorchamber". In addition, contamination present in thehydrogen will many times Leave a small unobservabledeposit on the burner face which can continue togenerate a background reading when the detector Is Inoperation and the burner aaaembly la heated.

Another possible cause of contamination ia the mlx-•r/burner aaaembly when the contamination ia trappedin the porous bronze sample filter. Thla la not a commonproblem and uaually only happens when an unusuallyhigh level of contaminant la drawn Into the assembly.Another possible cauae of high background reading iscontamination someplace In the air sample line to thedetector. Thla la aiao uncommon but can be the sourceof the problem. .

NOTEOVA's that include the Chromatograph Option in-stalled can also have an indication of highbackground related to saturation or contaminationof the activated charcoal filter, which la in the lineduring chromatograph analysis, or of the columnwhich la in the hydrogen line at all times.

6.2.5.2 ANALYSIS AND CORRECTIONPrior to analyzing the problem, the OVA should be

checked for proper electronic operation. Checklogarithmic instruments for proper high and low calibra-tion points and for proper gaa selector operation (seeSection 4). On logarithmic OVA's, check Gaa Selectorby turning to 500 and observing the flame-out alarmcomes on as the needle goes below 1 ppm. It should beensured that the instrument Is calibrated to methane asreferenced.

if. after checking that the OVA ta properly calibrated,the background Is still higher than normal for ambientconditions, the following procedure should be followedto isolate the cause of the problem.

1} Let the OVA run for a period of time (IS to 30minutes) and see If the background leveldecreaaea aa a function of time. Thebackground could go down and stay down as aresult of clearing line contamination which Isremovable simply by the normal flow of airthrough the sample line.

2) Take a reading in a known, relatively clean airenvironment. Normally, outside air environ-

ment is ctean enough to assess by comparisonwhether the background reading la internal tothe instrument or la present in the laboratory,office or location where the instrument Is beingused.

3) if the OVA Includes the Gas Chromatograph Op-tion, depress the sample inject valve so that theactivated charcoal la In the line and observewhether the background reading goes downand stays steady after the elutlon of the airpeak. The reading should always go down orstay the same but never be a higherbackground reading with the sample valvedepressed, since the charcoal filter will takeout any trace elements of organic vapors in theair heavier than a Ca. If another activated char-coal filter ia available, this may be attached tothe end of the probe to scrub the air so that aclean air sample would be going to the detec-tor. The external activated charcoal can be us-ed on any Instrument, with or withoutchromatograph, for providing a clean air sam-ple to aasess background level.

4) if background still staya up and cannot bereduced by any of the previous steps, the safe-ty cover (If included) and the exhaust port onthe detector chamber (Preamp Assembly) onthe bottom of the case should be removed andthe Mixer/Burner Assembly scraped or brush-ed with s small wire brush. (Referenceparagraph 6.2.1.3.) This will remove any smallquantities of contamination that are on the Mix-er/Burner Aaaembly which could be the sourceof the background vapor. After cleaning theface of the burner and tube, replace the ex*hauat port and safety cover (if included) andreignite the OVA. If contamination on theburner face was the cause, the problem shouldbe immediately resolved and the ambientbackground will drop to an acceptable level.

5) if the background Is still present, place yourfinger over the inlet of the probe so as toreduce the flow of air to the detector chamber.Reduced flow rate may be observed either onthe sample flow gauge or can normally beobserved by the sound of the pump motor.

6) if the background drops immediately Inresponse to the reduced flow of air to thechamber, this Is an indication that the con-tamination Is in the air sample line. Therefore,the various parts of the sample flow line suchas pickup probes, umbilical cord to the Instru-ment, etc., should be Investigated by the pro-cess of elimination to see if the contaminationcan be Isolated.

7) Serious contamination In the air sample line isvery uncommon. However, if very large dosesof very heavy compounds are sampled, there Isa possibility of a residual contamination whichwould eventually clear itself out but may take aconsiderable period of time. A typical cause forthe high background from the sample line Is a

16

contaminated Mixer /Burner Assembly. Seeparagraph (4) above for cleaning procedure. Ifheavy contamination of the Mixer/Burner is stillindicated by a high background, replace theMixer/ Burner Assembly. In several OVAmodels, this will require removal of the PreampAssembly. The old Mixer/Burner Assemblyshould be either discarded or returned to thefactory for cleaning and rebuilding.

8) in the event there is contamination in the pumpor other internal parts of the sample flow lineswhich cannot be removed, the sample flowcomponents would have to be disassembledand cleaned. This is normally a factory typeoperation. However, the components such asthe pump can be replaced in the field along withany contaminated tubing tn the sample lines.

9) High background readings on OVA's which in-clude the Gas Chromatograph Option can becaused by other sources of contamination. Ifthe charcoal in the charcoal filter mounted onthe panel of the instrument is contaminated orsaturated, contaminated air would be suppliedto the detector and raise the ambient levelbackground. To check for this, the charcoalfilter cartridge can be removed from the paneland either a bypass tube put between the twoconnectors or the charcoal can be removedfrom the charcoal cartridge and the cartridgerefilled with clean activated charcoal. Thiswould determine If the charcoal was the sourceof the background reading. It Is possible that anapparent high background reading could bedue to contamination In the column that Is onthe instrument. This background could becaused by compounds that are slowly elutingfrom a column which has become con-taminated. The easiest way to check for columncontamination is to replace the column with aknown clean column or a short empty piece ofcolumn tubing and see If the high backgroundreading drops.

10} If all the above steps do not correct the highbackground problem, the cause will normallybe contamination in the hydrogen fuel system.

Contamination in the hydrogen fuel system is usuallythe direct result of contamination m the hydrogen gasused or contamination introduced during the fillingoperation. Filling hose contamination can be caused bystoring the hose in a contaminated area.

To remove contamination from the hydrogen fuelsystem, II should be purged with hydrogen. Effectivepurging of the hydrogen system is accomplished bydisconnecting the capillary tube fitting which attacheson to the manifold block which has the low pressuregauge (H2 Supply Pressure Gauge and H2 SupplyValve). This disconnects the capillary tubing from thehydrogen line so that hydrogen may be purged at areasonable rate from the tank assembly through theregulators, gauges and valves. After disconnecting thecapillary, the hydrogen tank can be filled in the normal

manner. The tank valve and H2 supply valve can then beopened which will bleed the hydrogen from the tankthrough the H2 fuel system purging out the contamina-tion which Is In vapor form. There Is the possibility thatcontamination has been Introduced into the hydrogenfuel system which Is not readily purged out by thehydrogen gas but this la unlikely. After purging withclean hydrogen, approximately two or three times, thecapillary tub* should be reconnected and thebackground again checked. Five or ten minutes shouldbe allowed before assessing the background reading,since contaminated hydrogen may still have been trap-ped in the capillary tube.

If another tank assembly in a clean instrument isavailable, the fuel system from the clean instrument canbe connected to the contaminated instrument to ab-solutely verify that tt Is or Is not In the hydrogen fuelsupply system. The Interconnection should be made tothe capillary tube of the contaminated instrument.

6.2.6 FUSE REPLACEMENTThis paragraph applies only to the standard (non-

certified) OVA's. There are two (2) overload fuses in-corporated in the Battery Pack Assembly, one is a 3AG-1 AMP Slo-Blo In the power line to the pump and igniterand the other a 3AG-1/4 AMP in the power line to theelectronics. Both fuses follow the current limitingresistors which provide primary short circuit protection.However, in the event of an excessive overload, thefuses will open and prevent overheating of the currentlimiting resistors. It should b* pointed out that the iAMP Slo-Blo fuse will blow in approximately 8 to 12seconds If the Igniter switch Is kept depressed. NormalIgnition should take place In not more than 6 seconds.Therefore, do not depress Igniter button for more than 6seconds. If Ignition does not occur, wait i to 2 minutesand try again. If the required 1 AMP Slo-Blo fuse cannotbe readily obtained, replace temporarily with a 3 AMP-3AG standard fuse.

6.3 TROUBLESHOOTINGTable 6-1 presents a summary of recommended field

trouble shooting procedures. If necessary, the instru-ment can be easily removed from the case by unlockingthe four <4) 1/4 turn fasteners on the panel face andremoving the refit) cap and exhaust port. The batterypack is removed by taking out the four (4) screws on thepanel and disconnecting the power connector at thebattery pack.

6.4 FACTORY MAINTENANCETo ensure continuous trouble-free operation. Century

recommends a periodic factory maintenance, overhauland recaltbration. The recommended schedule is everysix (6) to nine (9) months. This maintenance program in-cludes replacement of plastic seals and pans as re-quired, pump overhaul, motor check, new batteries.sample line cleaning, H2 leak check, recaiibration,replacement of plastic hose as required, and detailedexamination of the unit for any other requiredmaintenance and repair.

17

The recommended procedure for maintenance endrepair beyond the scope of this manual Is to send thecomplete Instrument or subassembly to the Centuryfactory for repairs. The assemblies will be handled ex-pedltlously for rapid turn-around.

fl.5 FIELD MAINTENANCEAlthough not recommended, where field

maintenance beyond that described herein Is con-sidered essential, the assembly drawings, parts listsand schematics in Appendix "A" will be of assistance.

6.6 RECOMMENDED SPARESCentury does not recommend that spares be main-

tained for its Instruments. However, If the Instrument tato be used in a remote area or spares are desired forother reasons, the following list should be used a* aguide.

RECOMMENDED SPARES

Item

1234567891011121314151617IB

Description

IgniterIgniterPump ValvePump Diaphragm (Buna-N)Pump Diaphragm (Teflon)Cup, Filter (3/8 OD, 55}Mixer/Burner AssyMixer/Burner AssyMixer/Burner Assywafer. Teflon, H2 ValveWasher, Brass, Hj ValveExhaust Port AssyExhaust Port AssyBattery Pack AssyBattery Pack AssySample Line AssyParticle FiltersParticle Filters

Recommended Quantity

Part No.

510027-1510461-1510067-3 (10/pkg.)51"5J10091-1L0063-1

510318-1 (5/pkg.)510557-2510557-1510513-1510160-1 (10/pkg.)510160-2 (10/pkg.)510425-1510530-1510070-1510542-1510316-1510114-1510116-1

Standard98

2

11

11

111

1

1

98

2

1

11

1

111

1

1

1

118

2

1

11

1

111

1

Approved108

21

11

11I

1

i1 ! L!X 1

128

21

11

111

1

11

I

138

211

1

111

1

1L1

NOTE: Unit quantity is each unless otherwise noted.

18

3UBLE1) Low sample flow rate on How Indicator.

Nominally 2 units on flow gauge (See also 6below and refer to paragraph 6.2 4)

TROUBLE SHOOTING PROCEDURE•) Check primary filter In aldepack and particle

inters In the pickup assembly.b) Determine assembly containing restriction by

process ol elimination. I.e., remove probe,remove Readout Assembly, remove primaryfilter, etc.

c) II the restriction la In the Side Pack Assembly,further Isolate by disconnecting the sampleMow tubing at various points. I.e., pump output,chamber Input, etc.Note: The Inherent restrictions due to length ofsample line, flame arresters, etc., must betaken Into account when trouble shooting.

REMEDYReplace or clean filter If clogged. (See paragraph 02.1)

Investigate the assembly containing this restriction lodetermine cause of blockage. Clean or replace as re-quired.

If In the detector chamber, remove and clean or replaceporous metal flame arresters If pump Is found to be theproblem, remove and clean or replace.

2) H2 flame will not light. (See also 6 below) a) Check sample flow rate (see 1 above).

b) Check Igniter by removing the chamber ex-haust port and observing the glow when the IG-NITE Button Is depressed.

c) Check for rated H2 Supply Pressure. (Listed oncalibration plate on pump bracket.)

d) Check H2 flow rate by observing the PSIdecrease In pressure on the H2 Tank Pressuregauge. The flow rate should be about 130 PSIdecrease In pressure per hour. (Approximately12 cc/mln. at detector )On Instruments with GC Option, disconnect col-umn and measure H2 flow rate with a bubblemeter.

e) Check all H2 plumbing Joints for leaks usingsoap bubble solution. Also, shut off all valvesand note pressure decay on H2 lank gauge. Itshould be less than 350 PSIG per hour.

() Check lo see If H2 supply system Is frozen upby taking unit Into a warm area.

If sample flow rate Is low, follow procedure 1 above.

It Igniter does not light up, replace the plug. If Igniterallll does not light, check the battery and wiring.

If tow. remove battery pack and adjust lo proper level byturning the alien wrench adjustment on the lowpressure regulator cap.

The normal cause for H2 flow restriction would be ablocked or partially blocked capillary tuba. If flow rate Ismarginally low, attempt lo compensate by Increasingthe H2 Supply Pressure by one-hall or one PSI. If flowrate cannot be compensated for, replace capillary tub-Ing.

Repair leaking Joint

If there la moisture In the H2 supply ayslem and the unitmust be operated In subfreezlng temperatures, purgethe H2 system with dry N2 and ensure the H2 gas usedIs dry.

g) Remove exhaust pod and check lor contamina-tion. (See Figure 6-2 )

h) Chuck spacing between collecting electrodeand burner tip. Spacing should be 0.1 to 015 In-ches.

II the chamber Is dirty, clean with ethyl alcohol and dryby running pump lor approximately 15 minutes II H2fuel jet Is misaligned, ensure the porous metal Dame ar-reslor Is properly sealed.

Adjust by screwing Mixer/Burner Assembly In or ouiThis spacing problem should only occur alterreassembling a Mixer/Burner Assembly to a PreampAsaembly.

3) H2 (lame lights but will nol slay lighted a) Follow procedures 2 (a), (c), (d), (a), (g) and (h)above. Also refer to 5 below.

4) Flame-out alarm will nol go on when H2 flame Isout

a) Check instrument calibration selling and GASSELECT control selling Refer to paragraphs23.1.2and2.3.2.

b> Remove exhaust port and check for leakagecurrent path In chamber (probably moJalure ordirt In chamber).

c) If above procedures do nol reaolve the pro-blem, the probable cause la a malfunction Inthe preamp or power board assemblies.

d) Check volume control knob Is turned up.

Readjust as required lo proper setting Note thai onlinear OVA'a the flame-out alarm Is actuated when themeter reading goes below zero. On logarithmic OVA'S,the alarm la actuated when the signal level goes below 1ppm methane or equivalent.

Clean contamination and/or moisture from the chamberusing a swab and alcohol, dry chamber by runningpump for approximately 15 minutes.

Return preamp chamber or power board assembly tothe factory for repair.

Adjust for desired volume.

5) False (lame-out alarm. (Applies to linear OVA's) a) Flame-out alarm Is actuated on linear In-struments when signal goes below electroniczero (evenlhough flame la al|H on). This can bedue lo inaccurate Initial setting, drill or adecrease In ambient concentration. Verily Ifthis Is the problem by zeroing meter with flameout and retgnlllng. (See paragraph 2.3.2)

When using the XI range, adjust meter to 1 ppm ratherthan zero. See paragraph 2.3.2. Be sure Instrument hasbaan zeroed lo "lowest expected ambient backgroundlevel".

6) Slow response lime, la. lime lo obtainresponse alter sample is applied lo input(Refer to paragraph 6-2.4)

a) Check lo ensure that probe Is (Irmly sealed onthe rubber seal In the readout assembly.

b) Check sample flow rale per procedure 1 above

Reseat by holding the probe (Irmly against the rubberseal and then lock In position with the knurled lockingnut.

See 1 above.

7) Slow recovery lime. I.e.. too long a time tor thereading to get bach to ambient after exposureto a high concentration of organic vapor

a) This problem Is nor ma.., caused by contamina-tion In the sample Input line, requiring pumpinglor a long period to get the system clean ofvapors again. Charcoal In the lines would be theworst type of contamination. Isolate throughthe process of elimination. (See 1 (b)).

b) Check flame chamber for contamination

Clean or replace contaminated sampleas required.

or assembly

Clean as required.

B) Ambient background reading In clean environ-ment la too high. (Refer to paragraph 6.2.5)

a) An ambient background reading can be causedby hydrocarbons In the M2 fuel supply system.Place finger over sample probe lube restrictingsample flow and If meter Indication does no) godown significantly the contamination Is pro-bably In the H2 fuel.

b) An ambient background reading can be causedby a residue of sample, building up on the faceof the sample Inlet filter. If the leal In 0 (a) aboveproduces a large drop In reading, this Is usuallythe cause.

c) An ambient background reading can also becaused by hydrocarbon contamination In thesample Input system. The moat likely causewould be a contaminant absorbed or condens-ed In the sample line.Nole: It should be emphasized that running theInstrument lends to keep down the buildup ofbackground vapors. Therefore, run the unitwhenever possible and store It with the carry-Ing case open In clean air.

Use a higher grade of hydrocarbon free hydrogenCheck for contaminated fitting a on filling hoseassembly.

Remove the exhaust port (II Is not necessary to removeInstrument from case), use amall wire brush from thelool kll or a knife blade and lightly scrub surface of sam-ple Inlet filter.

Clean and/or replace the sample Input lines. Normallythe lines will clew up with sufficient running.

9) Pump will not run a) Check 1 AMP Slo-Blo fuse on the battery packcover. NOTE: Certified OVA'8 do not havefuses.

Replace fuae. IMPORTANT: Nole that fuse Is a SloBlotype. If fuse continues to blow when Igniter twitch Isclosed, check Igniter for short circuit. If Igniter Is not theproblem, there Is a short In the wiring or pump motor.Return OVA to factory or authorized repair facility.

10) No power to electronics but pump runs a) Check 114 AMP fuse on the battery pack coverNOTE: Certified OVA'a do not have fuses.

Replace fuse. If fuse continues to blow, (here Is a shortIn the electronics assembly. Return OVA lo factory orauthorized repair facility.

II) No power lo pump or electronics a) Place bailery on charger and see If power Isthen available Recharge In a non-hazardousarea only.

If power la available, battery pack Is dead or openRecharge battery pack If still defective, replace batterypack Reference paragraph 2 7.

Vi'1

ACTIVATED CHARCOALFILTER ASSEMBLY

STRIP CHART RECORDER(See paragraph 7.2)

:u~ h^^;-m>• • .• il"'1.

OCBAtiKFLUSHVALVE

FIOIIPC 7-1-1 AnniTinMAl nOMTBOl R A rOMPONFNTS - OC OPTION

SECTION 7OPTIONAL ACCESSORIES

GAS CHROMATOGRAPH (GO OPTION.1 INTRODUCTION

The Century Portable Organic Vapor Analyzers(OVA's), when used as described In the previous sec-tions of this manual, are very efficient and accurate in-dicators of total organic compound concentrations on acontinuous sampling basts for a period of eight (8) hoursminimum and with a response time of one to twoseconds. However, In areas where mixtures of organicvapors are present. It often becomes necessary todetermine the relative concentration of the componentsand/or to make quantitative analysis of specific com*pounds.

To provide this additional capability, a built-in gaschromalograph (GC> system has been added as an op-tion to the OVA aerie* of Instruments, See Figure 7-1-1for the location of the major components and controlsassociated with the GC Option. When the GC Option isuaed as described In this section, the capability of theOVA will include both qualitative and on-the-spot quan-Mtatlve analysis of specific components present in thembient environment. The Strip Chart Recorder option,

which is used with the GC Option, is describedseparately in paragraph 7.2.

This section is applicable only to OVA's wtth the op-tional gas chromatograph system, it Is recommendedthat this entire section be reed, along with the cor-responding sections of the baste Operating and ServiceManual, prior to operating the Instrument.

- 1.2 DESCRIPTION AND LEADING PARTICULARS12.1 GENERALMien the GC Option Is Installed on a Century OVA,

the OVA will have two modes of operation. The firstmode is the measurement of total organic vapors in thesame manner as described In the basic operatingmanual for the OVA instrument. This mode Is referred toas the "Survey Mode". The OVA will be In the "SurveyMode" of operation .whenever the Sample Inject Valve' In the "out" position.

The second mode of operation Is called the "GC~Mode ' The OVA is In this mode of operation any time asample has been injected Into the GC system and thesample is being transported through the GC column.This section provides a brief description of how a gaschromatograph (GO operates and specifically how theCentury Instruments perform the required operations. Acomplete, comprehensive discussion of gaschromatography theory, column selection and dataanalysis is beyond the scope of this manual.

It should be pointed out that the GC Option wasdesigned to extend the capabilities of the Century OVAas a field type instrument. A "field type" Instrument ssused herein is defined as a fully portable, self'contained Instrument capable of making direct on-slteanalysis of organic vapors In aJr. The OVA with GC Op-tion can be utilized for many types of analysis in the out-door or Indoor ambient environment or for specific

laboratory type analysis. The OVA was not designed tocompete with the research or process type gaschromatograph but to compliment these instruments oreliminate their need In field type applications.

This manual la Intended to provide an operator withsufficient information to operate and maintain the Cen-tury Instrument. Century further publishes Applica-tion/Technical Notes to aasist the operators in applyingthe Instrument to actual field monitoring situations. Thecriteria for the design of the GC Option was the same asthe basic OVA, that Is. simplicity, ease of operation,high reliability, field ruggednesa and minimized poten-tial for operator error.

7.1.2.2 PRINCIPLE OF OPERATIONa) GENERAL

For those not specifically trained or familiarwith gas chromatography, the techniqueemployed In the OVA during GC Mode opera-tion Is basically a separation of components ma sample gas contacted with the material in acolumn. When non-Interference can be achiev-ed, each component of the sample mixtureelutes from the column singly into the flamelonizatlon detector chamber to provide Its ownmeasurable response on the meter andrecorder. When used as directed in thismanual, the GC Option can drastically reduceand in moat cases eliminate the need forelaborate grab sample and laboratory analysistechniques and the analysis can be made on-the-spot at the point of interest.All flame lonlzatlon detector (FID) gaschromatographs require certain elements fortheir operation. These elements include threeflow regulated gas supplies as follows: 1) A car-rier gas (normally nitrogen or helium) totransport the sample through the columns; 2)Hydrogen gas for operation of the FID; 3) Aclean air or oxygen supply to support combus-tion of the FID. In addition, a method for infec-ting a known volume of sample air (aJiquot) tobe analyzed Is required.In standard gas chromatographs these three (3)flow regulated gases are Individually suppliedfrom pressurized cylinders equipped withregulators and 'low control apparatus. The Cen-tury GC system differs In that the hydrogen <H2)fuel for the FID Is also used as the carrier gas.The clean air supply Is simply the normal airsample pumped to the FID. But, during GCanalysis, the air Is scrubbed In a charcoal filterto provide a clean air supply. The end result Isthat no additional gas supplies are required toadapt the GC Option to the basic OVA instru-ment.A valvlng arrangement is Incorporated to pro-vide a method for transferring a fixed volume ofthe air normally being pumped to the FID in theSurvey Mode Into the GC system for analysis.The sample air Infected Into the GC system is

23

the s*me sample being analyzed by the OVA fortotal organic vapor concentration. Therefore,the instrument provides the unique capabilityto observe the total organic vapor concentra-tion of the sample prior to injecting it Into the)GC system. This operating feature is invaluablem field work where the environment Is con-tinually changing and where valuable GCanalysis time must be expended only on thesamples of concern.

D) SAMPLE FLOWFigure 7-1*2 is a Mow diagram illustrating theflow paths of the hydrogen <H2) fuel, sample airsupply and QC Injected sample aliquot. Thereare two push-pull valves used in the GCsystem, the Sample Inject Valve and theBackflush Valve.Slock 0 of Figure 7-1-2 illustrates the flow pathswith the Sample Infect Valve in the "out" posi-tion which leaves the OVA in the Survey Mode.With this valve in the "out" position, the OVAwill function in its normal manner aa a totalorganic vapor analyzer.Block C of Figure 7-1-2 illustrates the flow pathsafter the Sample Inject Valve is moved to the"in" position to initiate the GC Mode, it can beobserved that the hydrogen flow path Is nowthrough the sample loop which enables thehydrogen to sweep the air sample from the loopand carry it through the GC column. It can alsobe observed that the sample air going to the FIOchamber la now routed through the activatedcharcoal filter where essentially all organicvapor contamination Is removed from the air.The activated charcoal filter will effectively ad-sorb most organic vapors with the exception ofmethane and ethane. The functions of the Sam-pie Inject Vslve sre. therefore, to transfer a fix-ad volume sample of the air being monitored In-to the hydrogen stream and to reroute the sam-ple air supply through a filter (scrubber).The Backflush Valve has no preposition ing re-quirement to function. It can be tn either the"in" or "out" position at the time a sample isinjected into the GC system for analysis. TheBackflush Valve simply reverses the directionof the hydrogen flow through the GC column. Ifthe Backflush Valve is in the "out" positionduring sample injection and analysis, it is simp-ly moved to the "In" position whenbackflushtng is desired or vice versa. Seeblocks A and B of Figure 7-1-2.it should be noted in Figure 7-1-2 that hydrogenis always flowing through the column and ontothe FID detector and that the sample air supplyis always flowing to the FID detector to provideoxygen for the hydrogen (tame regardless ofthe operating mode.The recommended H2 flow rate is 12 cc/min. forproper FIO operation and as a standard flowrate for generating GC reference /calibration

data. This H2 flow rate is adjusted by varyingthe H2 Supply Pressure, which <s the hydrogenpressure at the input of the flow controlcapillary tube of the OVA. The pressure ischanged by adjusting the set screw in the bon-net of the low pressure regulator, accessible byremoving the battery pack from me instrumentpanel. To monitor the H2 flow rate, connect abubble meter to an end of the GC column whichhas been disconnected from the panel fittingand move the Backflush Valve so that hydrogenis flowing out of the column. Primary H2 flowcontrol la accomplished by the capillary tube ofthe OVA. However, the flow restriction of a GCcolumn will also affect the H2 flow rate and theaffect will vary with column length, type ofpacking and packing methods. The nominal H2Supply Pressure is around 10 PSIQ and thepressure drop across a typical 24 inch long col-umn packed with 60/80 mesh material is ap-proximately i to 1.5 PSIQ. Normally, whentheH2 flow rate is set at 12 cc/min. with a Centurystandard 24 Inch long column, no ad|uatmentneeds to be made when using columns fromthree (3) inches to four (4) feet long. Longer col-umns may require H2 flow adjustment for pro-per operation. Adjustment would be required ifand when precisely controlled analysis was be-ing conducted or when the hydrogen flow wa*too low to keep the flame burning.The sample air flow in the OVA Is not adjustableand la nominally 1.0 liter/ minute. Thla flowrate should remain relatively constant. A Sam*pie Flow Gauge is provided on the OVA panel tmonitor the sample flow rate. (NOTE: Panegauge is not calibrated in LPM.) When the Sam-ple inject Valve is in the "in" position, theremay be a slight increase or decrease in sampleairflow rate (0 to 15%). This change will normal-ly not affect operation of the instrument as longas the flow rate is consistent from analysis toanalysis. Basically, if the sample air flow rate isconsistent between calibration and end usage,there will be suitable precision in themeasurements.

c) GC ANALYSIS1) Sample injection

When the Sample Inject Valve is depress-ed, the small volume of the input air samplewhich is in the sample loop is injected intothe hydrogen stream which transports thesample through the column for separationof its components and on to the flamechamber for analysts. This small volume ofinjected sample is, therefore, qualitativelyanalyzed based on the retention time of theindividual components of that sample whilepassing through the column. Quantitativeanalysis can then be accomplished by peakheight or peak area analysis methods.

24

PL€ At* TO f/D CJUMBf

_ _ _ _ _ J

FIGURE 7-1-2. FLOW.OIAQRAM -QC OPTION

2) The ColumnThe column conaists of tubing packed witha material which phyaically interacts withthe organic vapors In the air sample in amanner which stows down the passage ofthe vapors through the column. Since thepacking material has a different attractionfor each individual organic substance, eachcomponent In a mixture of gases will beslowed down to a different extent whenpassed through the column. The net effectIs a separation of the gases in such a waythat each component elutea from the col-umn at a different time. The individualgases are then automatically fed to thedetector which gives a response to themeter or to an external strip chart recorder.For example: Suppose that a sample con-taining benzene and toluene is Infected on-to the column containing appropriate peck-ing material. As Illustrated In Figure 7-1-3, aportion of the benzene and toluene ere ad-sorbed on the packing material. Theamounts involved depends on the relativeaffinities of the two components for thepacking material. The earner gas movesthe gaseous phase forward a shortdistance, and since benzene will have leasaffinity than does toluene. It will be movedthrough the column more readily and thus aseparation of these two components takesplace and benzene reaches the detector atthe exit of the column first.

3) Qualitative AnalysisAs each organic substance has a umaue in-teraction with the column packing material,the time that the substance is retained onthe column fs also unique and thuscharacteristic of that particular substance.The "retention-time" (RT) is primarilydependent on the type of packing material.the length of the column, the flow rate ofthe gaa carrying the mixture through thecolumn and the temperature range of thesystem.When these variables are controlled, theretention times can be used to identifyeach of the components in a mixture.Because of these variables, it is usuallynecessary to establish retention times toreach instrument by making a test with thepure substances of Interest or to refer toestablished time data charts prepared inadvance for that specific Instrument, inthose cases where retention times of thecomponents are too close together for sgood analysis, an adjustment in one ormore of the operating variables will effect asufficient difference in retention times toenable meaningful analysis.

4) Quantitative AnalysisThe response of the detector to any com-ponent after It has been separated by thecolumn Is proportional to the quantity oforganic material passing through thedetector at any given time. However, since

TO DETECTORRECORDER

TOLUENE BENZENE

•TOLUENEDETECTOR RECORDER

CAAK1ERGAS IN

PICTORIAL SEPARATION OF BENZENE AND TOLUENE - "A" AT BEGINNING OFSEPARATION; "»" DURING SEPARATION; "C" BENZENE HAS A L R E A D Y PASSEDTHE DETECTOR AND IS RECORDED. TOLUENE (DOTTED LINES) WILL APPEARON RECORDER AS IT PASSES THE DETECTOR.

FIGURE 7-1-3. TYPICAL COLUMN SEPARATION SEQUENCE

27

not all of the separated components elutefrom the column at the same Instant, butvartes from low to a maximum and then fallsto ambient again, it Is necessary to have ameans to measure the total amount of theindividual component vapors. When usinga strip chart recorder, the curve drawn onthe paper la triangularly shaped and thearea under the peek is related to theamount of substance being analyzed. Forthe OVA systems which have logarithmicoutputs, direct measurement of area*under the peek Is extremely difficult. Themethods of peak height analysis describedherein provide a convenient means forquantitatively Interpreting peaks whenoperating either the logarithmic or linearreadout OVA's.

5) BackflushThe column Backftush Valve Is provided toreverse the flow of the carrier gas(hydrogen) through the column. It isnecessary that the column be back Hushedafter each Individual analysis except undercertain special conditions. The primarypurpose of the backflush function is toclear the column of heavy compounds (withlong retention times) which would con-taminate the column and cause in-terference to the total organic reading andfuture GC analysis. The BacKflush Valvehaa no "sense" (preposittoning require-ment). It is simply reversed from eitherposition it was in during QC analysis. TheBackflush Valve should be actuated im-mediately after the peak of the last com-pound of interest elutes. Figure 7-1-2 il-lustrates the functions of the Backflushvalve.In the Century GC system, the backflush is'to the detector". This is possible due to

the fact that the carrier gas and detectorfuel are one in the same, i.e.. hydrogen.The backflush function, therefore, provideaa convenient means of quantifying the totalcompounds in the backflush by simplyrecording the peak that elutea during thebackflush operation. For field type in-struments, this quantitative backflush in-formation is very valuable. The backflush todetector also provides a direct means ofobserving the condition of the column andseeing when the column is clean and thedetector response has returned tobaseline. The time required for thebackflush is usually 1.2 to 1.5 times the GCanalysis time.

6) Survey to GC Mode InterfaceThere is an inherent advantage to in-tegrating the GC system to the basic totalOrganic Vapor Analyzer (OVA). The OVAprovides a direct reading of total organicvapors present in the air being sampled.

which provides the operator with in-telligence of what he is injecting into theQC system. He can then use this informa-tion to predict and verify the peaks thatresult during the GC analysis, including thebackflush peak.This feature completely eliminates expen-ding valuable GC analysis time where thereis no contamination concentrations of con-cern (comparable to taking noisemeasurements In quiet corners). This"front end" intelligence also enables theoperator to select the most appropriatelocation to conduct an analysis, which Isnormally the area of highest concentration.

7.1.3 OPERATING PROCEDURES7.1.3.1 GENERAL

The Gas Chromatograph (GC) Option Is a supplemen-tary system which Is built Into the OVA instrument dur-ing manufacture. This system provides sn additionalgaa chromatographlc analysis (GC Mode) of operationwhich can be Initiated at any time during a survey bysimply depressing the Sample Inject Valve. After com-pletion of the analysis and backflush operations, theSample Inject Valve Is pulled out and the survey con-tinued or another sample iniected. Note that when theSample inject Valve is in the out (Survey Mode) positionthe OVA operates in . the same manner as a standardOVA which does not incorporate the GC Option.

7.1.3.2 GC SYSTEM CONTROLS AND COMPONENTSRefer to Figure 7-1-1 for a view of the four (4) basic

controls and system components provided in the GCOption. Table 7-1-1 below describes their functions.

TABLE 7-1-1GC OPT1OH-COMPONENTS

Controls/Indicators — Function1} Sample Inject Valve - This 2 position valve

(shown schematically in Figure 7-1-2) is used toselect either Survey Mode (valve out) or GCMode (valve in).

2) Backflush Valve - This 2 position valve (shownschematically in Figure 7-1-2) is used to reversethe flow of H2 through the column to:

a) Backflush the column for clearingb) Quantitatively measure total com-pounds after a selected point. Example:Separation of methane from non-methanehydrocarbons to read total non-methanehydrocarbon level.

3) Column - Separates components of a gas mix-ture so that each component of the mixture•lutes from the column at a different time.

4) Activated Charcoal Filter Assembly - Thisassembly functions only in the GC Mode (Sam-ple Inject Valve "In") as shown schematically inFigure 7-1-2. it removes organic compounds(except simple Ciand C: hydrocarbons) by ad-sorption from the sample air supply.

7.1.3.3 SERVICING AND TURN ONPiece the Sample Inject Valve in the "out" position

and put the OVA instrument in operation per Section 2of this manual. NOTE: Leave the hydrogen fuel andlump "on" lor three (3) to four <4) minutes before at-.empting ignition to enable hydrogen purging of the col-umn.

7.1.3.4 SURVEY MODE OPERATIONWhen using the OVA In the Survey Mode, ensure that

the Sample Inject Valve remains in the full "out" posi-tion and that the Backflush Valve Is either full "in" orfull "out". Note that when changing from the GC Modeto the Survey Mode the OVA output readings will con-tinue to change as long aa any compounds are stillelutlng from the GC column. Therefore, under normalfield conditions, the GC column should be backflushedfor clearing, which takes approximately 1.2 to 1.5 timesthe already elapsed forward analysis time. Thebackflush peak may be observed returning to baseline,after which the Sample inject Valve may be moved to theSurvey Mode (out) position.

When the compound(s) being analyzed are known tobe the only compound(s) present In the air sample,backflushing may be omitted.

7.1.3.5 GC MODE OPERATIONIn normal GC analysis, a strip chart recorder Is used

to record the output concentration from the OVA as afunction of time. This record, called a chromatogram. Isutilized for Interpretation of the GC data. The Centuryportable strip chart recorder Is further described inparagraph 7.2.

a) OPERATION1) Turn on recorder and push Sample Inject

Valve "In" with a fast, positive motion. Thisstans the GC analysis which is automaticup to the point of backflushing. NOTE:Rapid and positive motion should be usedwhen moving either the Sample Inject orBackflush Valves. On occasion, the flameIn the FID detector may go out, whichwould be Indicated by a sharp and con-tinued drop of the concentration level. Ifthis occurs, simply relgnite the flame in thenormal manner and continue the analysis.NOTE: A negative "sir" peak typically oc-curs shortly after sample Infection andshould not be confused as flame-out.

2) The negative air peak and various positivecompound peaks will be Indicated on theOVA readout meter and the atrip chartrecorder and represent the chromatogramof the analysis.

3) After the predetermined time for theanalysis has elapaed (normally Immediate-ly after the peak of the last compound ofconcern), rapidly move the Backflush Valveto It's alternate position (In or out). Leavethe Instrument In this condition until thebackflush peak printed on the recorderreturns to baseline, then pull the Sample

inject Valve to the "out" position If nooackfluah peak appears, pull the Sampleinject Valve out after being m the backflusncondition for a period at least as long as theanalysis time. The OVA Is now back in theSurvey Mode and ready tor survey use orinjection of another,sample into the GCsystem.

b) INTERPRETATION OF RESULTSInterpretation of the recorded chromatogram isalways baaed on predetermined calibrationdata. A discussion of calibration methods andchromatogram Interpretation is presented mparagraph 7.1.4.

7.1.4 CALIBRATION7.1.4.1 GENERAL

The Century OVA with GC Option Is a field instrumentIntended for applications where there are a limitednumber of compounds of Interest and the compoundsare normally known. Under these field conditions, theoperator must simply know the retention time and peakheight characteristics of the compounds of Interest ssnormally presented on his OVA instrument under hisspecific operating conditions. Therefore, to calibratethe OVA In the GC Mode, simply determine by test theretention time and peak area (using peak heightanalysis) characteristics for the compounds of concern.These tests should be conducted on the column to beutilized and over the concentration and temperaturerange of concern. When representative characteristicdata is available, such as In the Century Applica-tion/Technical Notes, a spot calibration check Is nor-mally all that Is required.

H should be noted that under normal field conditions,the vapor concentrations vary continually as a functionof time, location and conditions. Field measurementsfor Industrial hygiene work are normally associated witha threshold l»vel around a preestabllshed concentra-tion. Surveys for locating fugatlve emission sourcespresent s continually varying situation. Under thesetypical field conditions. It is desirable to have a fast andsimple method of Interpreting the GC data for on-the-spot analysis and decision making. High precision isnormally not a requirement for these type analysissince the environment Is continually changing. Themethods presented In this section are designed to pro-vide a means for typical field analysis. When the OVA isused under laboratory conditions, standard laboratorymethodology may be used for greater precision.

7.1.4.2 TECHNICAL DISCUSSIONThe chromatogram Is a strip chart recorder printout ol

the Instantaneous organic vapor concentration from theCentury Organic Vapor Analyzer (OVA) as a function oltime. A typical chromatogram is Illustrated m Figure 7-i-4 and Is seen to be a series of triangular shape peaksoriginating and returning to a fixed baseline. QualitativeInterpretation of a chromatogram involves Identifyingthe compound causing a peak by analyzing the time ntook for the peak to appear after initial injection (refer-red to as retention time (RT)) and comparing this RT to

reference data. Quantitative interpretation of a peak in-volves analyzing the area under the peak and relatingthis area to calibration data of peak area versus concen-tration for that specific compound under the conditionspresent during the GC analysts.

it can therefore be seen that Interpretation of acnromatogram requires the use of calibration referencedata. GC reference data is always generated empirical-ly, i.e.. through tests. Century publishes Applica-tion/Technical Notes which may be used as a referencefor selecting columns and interpreting chromatograms.However. In most cases, certain relatively simple testamust be conducted to obtain the required referencedata. A method for obtaining this type data and applyingit to a calibration chart is presented along with a typicalexample of the exercise.

a) QUALITATIVE ANALYSISUnder s given set of operating conditions, theretention time Is characteristic of that particularsubstance, and can be used to identify specificcompounds. It will be necessary to calibrateretention times by making tests with the purecompounds of Interest.The retention time <RT) is defined as that periodof time from injection of the sample into the GCsystem until the point of maximum detectorresponse for each substance. Retention time Ismeasured from the point of sample injection tothe apex of the triangle shaped curve obtainedon the strip chart recorder. (See Rgure 7-1-4.)The strip chart recorder operates on a clockmechanism such that the distance along thebsseline is proportional to time. While retentiontimes are characteristic for each compound, itis possible that two materials could have thesame retention tlmea. Thus. If there is anyquestion as to the identity of the vapor, it maybe necessary to verify identification by reten-tion times on two different columns.Use of a longer column will increase the reten-tion times of those components it is capable ofseparating. The time between peaks willtherefore also be increased. This is especiallyuseful to know if a component to be studiedcomes through too fast after injecting a sampleor if certain desired peaks are so close thatthey overlap on the strip chart.

b) COLUMN SELECTIONTwo columns are normally supplied with the in-strument. These are general purpose columnsand are useful in a wide variety of applications.If they do not perform the separations for yourparticular application. It may be necessary toselect other packing materials or lengths of col-umns to meet your needs. Century Systemswill guide you in this selection or prepare acustom column to meet your needs.If columns are made by the customer or pur-chased from other sources, care must be exer-cised to ensure that their packing density doesnot create too large a pressure drop as com-

pared to columns furnished by Century. Cen-tury's method of coding it's GC columns ispresented on most Century published Applica-tion/Technical Notes. Several applicationnotes have been inserted aa an appendix to thismanual to illustrate typical GC separations.

c) TEMPERATURE EFFECT ON RETENTION TIMEAn increase in temperature will decrease col-umn retention time (RT) and vice versa. Normal-ly, retention time (RT) as a function oftemperature changes linearly over the range of0 to <0*C. For complex qualitative analysis, acalibration plot of RT versus temperature willbe required. In typical ambient field usage suchas inside a factory, the effect of temperaturecan be compensated for by the operator duringcnromatogram interpretation. A single compo-nent tracer compound can be sampled at anytime to provide a "Key" for other compoundidentification.

d) CARRIER GAS FLOW RATE EFFECT ONRETENTION TIMEAn Increase In carrier gas flow rate willdecrease retention time. For reproducible data,the carrier gas (hydrogen) flow rste must berecorded In association with a cnromatogram.Primary control of the H2 Mow rate Is ac-complished In the OVA by regulating thehydrogen pressure across a capillary tube. Thehydrogen flow rate is also affected by therestriction of the GC column but most columnshave a limited effect. The hydrogen flow rate isfactory set st 12 cc/minute with a typical 24 inchcolumn.

e> QUANTITATIVE ANALYSISThe area under s specific peak Is a function ofthe concentration of the compound whichcreated the peak. This area can be calibratedby Injecting known concentrations of the com-pound. When the base of a symmetrical GCpeak remains constant, the height of the peakmay be used to measure the area. Typically, asthe retention time of a peak increases on thesame column, the base broadens and the peakheight decreases for a given sample concentra-tion. If the hydrogen flow rate is considered tobe constant, the retention time of the peak willchange as a function of temperature.tn general, the more triangularly symmetricalthe peak, the better the peak height analysiscapability. However, many GC peaks have "tail-ing" as illustrated In Figure 7-1-4. Peak heightcalibration is still an acceptable method forquantitative analysis as long as the area underthe tail Is small compared with the total peakarea. If severe tailing occurs, empirical calibra-tion data generated through tests may be re-quired to plot the peak height versus the con-centration curve. If the GC Option is used on aCentury "logarithmic" OVA, there will be a ma-jor apparent increase in peak tailing. This ap-parent tailing is the result of the logarithmic

30

TOTAL ANALYSIS TIME i TOTAL BACKFLUSH TIME

RETENTION TIME OfSECOND COMPONENT H

!h!Nr444

, .BACKFLUSM

•ACKFLU8H SWTTCHINOTRANSIENT PEAK

ftQ 7-1-4

TYPICAL CHROMATOQRAM (ILLUSTRATIONI

scaling, which amplifies me low level signals.This apparent tailing does not appear on tne"linear" OVA's, even though the same actualtailing Is present.Only peak height analysis will be discussed inthis manual. The method presented Is simply toinject a known concentration of the compoundbeing tested and record me height of the peckunder the test conditions. The peak heightcharacteristics can be established for variouscolumns and at various temperatures. Normal-ly, botn retention time and peak heightcharacteristics will be measured simultaneous-ly during the same test.When peak are* measurements are desired.the areas may be measured using an Integratoron the OVA output signal. Other manualmethods may also b* used, such as countingsquares, weighing curves or simple trtangula-tion. When the QC peaks have good symmetry,triangulatlon (area equals 112 base x height) Is aconvenient method.

7.1.4.3 PREPARATION OF CALIBRATION SAMPLESSamples for calibration of the GC system may be

prepared with tne procedures discussed in paragraph4.3.3 of this manual. Sample mixtures are mad* byrepeating the procedures presented for the compound*desired in the sample.

7.1.4.4 CALIBRATION DATAWhen conducting tests to obtain QC calibration data,

the following information should be recorded to qualifythe data:

a) Column - description and serial number as ap-plicable

b> Temperature - column temperature, normallyroom ambient

c) Chart speed - distance/unit timed) Carrier flow rate * hydrogen flow rate through

the column (cc/mln.). (Reference paragraph7.1.2.2 b)

a) Sample concentration - ppm for each com-pound

f) Sample volume - OVA by serial number ortyptcaity 0.2S cc for standard valve

fl) Recorder scaling - ppm per unit deflectionn) Range - range of OVA being used, i.e., XI, X10,

X100i) OVA type and serial number

To obtain a calibration point, inject a known concen-tration sample into the GC system and record theresulting chroma tog ram peak. The retention time forthe peak may be scaled from the record or timed with astop watch. The peak height may b* scaled from therecord or the OVA readout meter may be observed dur-ing the elution of the peak. Figure 7-1-5 presents the for-mat of a chart which may be used to record calibrationdata. Experience has Indicated that the peak heightresponse of a compound Is linear up to concentrationa

of greater than 1.000 ppm. Therefore, a single calibra-tion point, preferably around the concentration of mostconcern, is normally all that is required to plot a peakheight response in ppm as a function of compound con-centration. Data for other compounds on the same col*umn may also be plotted along with their associatedretention times, percent relative response in the totalorganic Survey Mode. TLV, etc. Note that to keep thecalibration curves readable on the chart a multiplier (X)column is included. It is recommended that copies ofthe actual chroma tog rams be kept with the charts forobserving the peak shapes, peak interferences, etc. Itshould be noted that a cnromatogram can be utilizedIlk* a fingerprint for compound identification or peakheight and shape comparison. Transparent overlays aresometimes an aid In chromatogram analysis.

When temperature variations are anticipated, datashould be taken at several points and recorded on thechart as a new curve or as a relative change as a func-tion of temperature as illustrated in Figure 7*1-5.

Preparing and using the calibration chart is verystraightforward. As an example, once the elution se-quence of a group of compounds is determined, a mix-ture of 100 ppm of each can be prepared and run on theGC for chart data. The retention time of each compoundand the peak height of each can be read directly fromthe chromatogram and the data put on the chart, ittemperature data is to be taken, additionalchromatograma may be run with the same sample andthe RT and peak height plotted as a function oftemperature.

When complex mixtures such as gasoline are analyz-ed, it may b* desirable to keep the record of thebackflush peak for future reference and peak area corn-comparison. It Is also recommended that the totalorganic vapor concentration reading on the OVA berecorded for each calibration sample used. This readingshould be put on the chromatogram and is used for ar-riving at relative response numbers and as a check onsample preparation precision.

Samples of forms for uae in recording individualchromatogram data and also a sample form for thecalibration chart are included in Appendix "A" and maybe used as a guide or copied and used as is.

7.1.5 MAINTENANCE7.1.5.1 GENERAL

This section describes the routine maintenance, trou-ble shooting and spare pans peculiar only to the GasChromatograph (GC) Option.

7.1.5.2 ROUTINE MAINTENANCEa) COLUMN

Any column can be contaminated with com-pounds having long retention times. This willresult in high background readings. This condi-tion can be checked by installing a new columnor a blank column (tubing only), tf this reducesthe background reading, the contaminated col-umn should be baked at 100*C (212»F) for tnree(3) to four (4) hours in a drying oven while pass-ing nitrogen through the column. Higher

32

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Compound

Heptane

PentaneHexane

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r-rikiMiTMTQ.10 20 30 40 50 60 70

C O N C E N T R A T I O N ( P P M )

80 90 100

FIGURE 7-1-5. CALIBRATION CHART

Date 1/31/78 Type Injectioa 2. 5 ml valve5104S4-C-48

°C Chart Speed . S'Vmin.GC OVA-118 S/N 1646 Range X1QRecorder Scaling 4. 125 ppm/iach

1 ' Carrier flow_ Other Condition!: Total; 850 ppm: 11 100 onm Bcntana 5) 200 onm fcoltien*

2) 100 DDin hexane3) 100 ppm benzene4) 100 ppm heptane

Ex*m»let '6,35 XI60/.5

.._.... ..,:_., 4 1 3 9 in.

125 = 18.11

34

temperatures may permanently damage thecolumn packing. Columns may be cleanedwhile Installed on the OVA by heating the col-umn with hot. wei toweia.When installing any column, avoid touching theends, aa this may causa contamination. Alao.ensure that the fittings are tight to avoid H2leakage.IMPORTANT: The following simple teat may berun to determine whether the QC column Iscontaminated. While In a clean ambient airbackground, place the Sample inject Valve mthe "in" (QC Mode) position. Observe thebackground reading on the meter or recorder.Aftar one (i) to two (2) mlnutea, change theposition of the Backflush Valve and againobsarve the background reading. If thebackground reading went down when theBackflush Valve was actuated and then stanedto Incraasa in one (1) to two (2) mlnutea, the col-umn la probably contaminated and needs to becleaned. Note that If hydrogen Is flowing Intoone end of the column for a period of time, thecontamination Is being pushed into the columnand Is therefore cleaning the front endportlonof tha column. Then when the hydrogen flow iareversed, the exhauat end of the column will bewhat was the Input end previously. Therefore,for a period of time the now exhaust end of thecolumn will be claan until the contamination taagain pushed through. Remember that to cleana column the hydrogen or other purge gaa mustbe run through the column In one direction untilall of the contamination Is removed. NOTE:Contaminated columns can be avoided by•imply backflushing tha column after everyanalysis,

b) CHARCOAL FILTER ASSEMBLYAfter repealed use, the Charcoal FilterAssembly will become saturated. Periodically,the operator should check the effectiveness ofthe activated charcoal to perform Its screeningfunction. This can easily be done by operatingthe unit with the Sample Inject Valve "In" andpassing the probe near s concentrated sampleof the compounds being analyzed. The readoutshould remain nearly steady (should not risemore than 0-2 parts per million (ppm)). If rise Ismore than 2 ppm, remove assembly from thepanel and pull tha knurled cap from the end ofthe filter tube (pull—not twist), and replace theold charcoal with activated charcoal (BarnebeyCheney. Columbus. Ohio, Type Gt orequivalent). Care should be taken to complete-ly fill the tube so there will not be a path for thesample to bypass the charcoal. The life of thecharcoal depends on the time (length) of ex-posure and the concentration level during thatexposure. When changing charcoal, be surethat any fine particle charcoal dust Is removedfrom the sssembly.

Another simple test of the charcoal filter is tonote the background reading with the SampleIntact Valve "out" and then note the baselinereading with the valve "In". The level shouldnever be higher when the valve is In the "in"position and the charcoal filter Is m the air line.If the reeding wrth the valve In me "In" positionis higher, the charcoal filter is probably con-taminated and acting like a contamination emit-ter.

Characteristics of the recommended activated charcoalare provided below:

Raw Materiel: Coconut ShellNominal Mean Size: a x 14 (Tyler Standard Screens)Size Distribution: On 8 mesh. 5% maximum;

through 8 on 10.80% maximum; through 10 on14,60% maximum; through 14 mesh, 5% max-imum

Ash: 0% maximumMoisture Content: 3% maximum, as packedStandard Packages: SO Ibs, net weight fiber con-

tainer; 58 Ibs. gross weight (typical). 1 ib. con-tainer, shipping weight approximately 1-1/2Ibs. Canon containing 12 each 1 ID. units,shipping weight approximately 16 Ibs.

Aopitaattona: Removal of medium and high concen-trations of organic vapors from air. Purifica-tion of gaaea. Safety respirators. Gas separa-tion.

7.1.5.3 TROUBLESHOOTINGTable 7-1-2 presents recommended field trouble

snooting procedures which are peculiar to the GCsystem. These procedures are in addition to thosefound In Table 6-1 of the basic manual.

7.1.5.4 RECOMMENDED SPARESSpare parta and supplies which are recommended to

support only the GC system (and recorder) are asfollows:Mem Description Part Number Quantity1) Quad Rings 510496-1 (10/pkg.) 1 pkg.2) Tubing. Teflon .148" 10 x .020 wall 12"3) Tubing. Teflon .120" ID x .030 wall 12"4) Activated Charcoal Type Gl or equivalent lib.5) "O"Rlng 2-15 26) Chart Paper (log) Type "J"(6rls./pKg.) 2 pkg.7) Chart Paper (linear) Type "WA" (6 rts./pkg.) 2 pkg.

Activated charcoal may ba purchased direct from:Barnebey Cheney825 North CassadyColumbus, Ohio 43219(614)256-9501

Chart paper may be purchased direct from:Gulton Recorder Systems Div.Gulton Industrial ParkEast Greenwich, Rhode Island 02816(401)884-6800

35

TROUBLE1) Low sample flow rate on How Indicator

TABLE 7-1-2

TROUBLE SHOOTING PROCEDUREa) Check lotion tubing on valve assembly for

kinks, etc.t» Check flow rate with valve In down position

REMEDYStraighten or replace teflon tubing

Check lor over restriction of charcoal filter

2) H2 flame will not light a) Check column connections on lop of unit tomake sure they are tight.

b) Check column for sharp bends or kinks,(Hydrogen flows through this column at alltimes and a sharp bend will compact packingtoo tightly for proper hydrogen flow.)

c) Check charcoal filler fittings to make aure theyare light.

d) Check H2 flow rate from the column.el Check that the Inject and Backflush Valves are

both completely In or out. A partially activatedvalve will block the H2 and air flow palha.

I) If a new column was Installed prior to problemIdentification, check for proper hydrogen Howrale through the column (should be approx-imately 12 cc/mlnule). Reference paragraph7.1.4.2 d.

Tighten fittings

Replace column

Tighten linings

Adjust hydrogen pressure to obtain 12cc/mln. How rale.Ensure both valves are either completely In or out.

Increase hydrogen pressure to obtain proper hydrogenflow rale or If column la excessively res trie live, replaceor repack the column.

3) Ambient background reading In clean environ-ment la loo high

a) Check for contamination In charcoal fillerassembly. This can be detected If ambientreading Increases when going In to thechromalographlc mode. Reference paragraph7.1 52b.

b) Check lor contamination In column. Referenceparagraph 7.1.5 2a

c) Check for contamination In column valveassembly.

Replace activated charcoal In charcoal filler assembly.

Replace or clean column.

Remove valve stems and wipe wllh clean llnl-lrea clothHeal valve assembly during operation to vaporize andremove contaminants

4) Flame-out when operating either valve a) Ensure valves are being operated with a quick.positive motion.

b) Either H2 or air may be leaking around one ormore of the valve quad rings. Assess by testsand "O" ring Inspection.

c) Damaged or worn quad rings causing leak.

Operate valve with a positive motion.

Remove stems and lightly coat with allicone grease, only on contact surface of Ihe "O" ring.Wipe off excess(do not remove quad rings).Replace quad rings and grease as above.

5) Excessive peak tailing a) Change or clean GC column and see If problemdisappears.

b) Inspect GC valves for excessive slllcone greaseor contamination.

Ensure columns are clean prior to use Relar loparagraph 7.1.5.2 a tor cleaning Instructions. If one ol asame type of column tails worse than others, repack thecolumn or discard.Excessive lubricant or foreign matter In Ihe valveassembly can cause excessive tailing. Clean valveassemblies and lightly relubrlcale as required Lubri-cant should be put only on the oulsi - contact surfaceof thft "O" ring. DO not gnt on In in "O" ring

/.2 RECORDER OPTION1 GENERALPortable Strip Chart Recorder Is available from Cen-

ury for use with the OVA Instruments (reference Figure/-2-1). The recorder Is powered from the OVA batterypeck and the output can be scaled to match the OVA•eedout meter, thereby providing a permanent recordor subsequent analysis or reference. The recorder Isavailable In two models. P/N 510445-1 la used with stan-dard Models OVA-66, OVA-96 and OVA-118. P/N 510445-2s certified Intrinsically safe and la used with the cer-ifled Models OVA-106, OVA-126 and OVA-136.

7.2.2 APPLICATIONSThe recorder can be used with the OVA to provide a

ecord of the long term monitoring profile of an area Intotal organic vapor concentrations, or can be used withthe Gas Chromatograpn Option to provide arhromatogram of the GC analysis.

7.2.3 FEATURESThe recorder prints dry (no Ink) on pressure sensitive

hart paper. Housed In rugged die-cast aluminum, it-weighs approximately four (4) pounds and Is 5-5/8"nigh, 3-5/6" wide and 4-1 /8" deep.

The recorder Is available for use with either the Cen-tury logarithmic or linear scaled OVA's by simply chang-ing the scale and paper style. The recorder Is equippedwith two gain ranges and an electronic zero adjustmentcontrol. The HIGH gain position Is normally used onlywith the logarithmic OVA to provide a means of scale ex-aanslon.

.4 CONTROLS AND CONNECTIONSDescribed below are the functions of the various con-

trols and connectors. Reference Figure 7-2-1.Controls and Connections—Function

1) HIGH-LOW Switch - This switch, located on theright hand side of the recorder, provides 2ranges. The LOW range is set for the same fullscale reading as the OVA readout meter. TheHIGH range can be set to give an increasedsensitivity to the recorder without effecting theOVA calibration.

2) ZERO ADJUST Knob - This potentiometer, alsolocated on the right hand aide of the recorder,permits "nulling" of the background readingon the recorder only (without affecting thecalibration of the OVA as displayed on the OVAreadout meter). In the full clockwise position ofthe knob, the recorder will display the samereading as the OVA meter. Counterclockwiserotation will reduce the reading on the recorderonly.

3) Power Connector - This 126 series. 5 pin Anvphenol connector provides power and signal tothe recorder, as follows:

Standard510445-1

AEH

FM510445-2

BEH

FunctionInput signalpos. 12VDC InputGround

7.2.5 OPERATING PROCEDURESConnect cable between recorder and OVA. Turn

recorder on by selecting either the HIGH or LOW posi-tion of the switch. (Normel (s "LOW".)

When using the HIGH geln position (typically only onlogarithmic OVA's), It may be desirable to 'nut!" out thebackground on the recorder. To accomplish this, pro-vide clean air to the OVA or place a charcoal filter In linewith the OVA Input to establish a "zero" reference anduse the ZERO ADJUST Knob to set the recorder needleto the zero line. Remove the filter and the Instrumentand recorder are ready for use. NOTE: During normalsurvey use, tt Is best to turn the recorder off to conservepaper and battery power.

7.2.6 CALIBRATION7.2.6.1 GENERAL

Electronic and mechanical adtustments, other thanthe operational adjustments on the side panel, are pro-vided to calibrate and align the recorder.

7.2.6.2 MECHANICAL ZERO ADJUSTMENTa) Snap out the front panel nameplate (using a

small blade screwdriver in the left hand slot) foraccess to mechanical zero adjust screw, placeHIGH-LOW Switch In OFF position.

b) Unscrew knurled fastener at top left of frontpanel, open recorder. Pull down plastic chassislatch on right side to release sticker bar tensionon paper and adjust mechanical zero as re-quired. Replace nameplate, chassis latch andresecure front panel.

7.2.6.3 GAIN ADJUSTMENTSeparate adjustments are provided for the HIGH and

LOW ranges on the recorder. (Refer to Figure 7-2-1 forlocation.)

a) Connect recorder to OVA and adjust OVA forfull scale reading on readout (about 5 VDC).

b) Loosen knurled fastener on upper left of thefront panel and pull front panel down.

c) Place HIGH-LOW Switch in LOW and adjust R1until recorder orints full scale.

d) Place HIGH-LOW Switch In HIGH and adjustOVA to read the desired full scale with frontpanel CALIBRATE ADJUST Knob, typically halfscale on the readout. Adjust R2 until recorderreads full scale. NOTE: Full scale adjustment ofthe recorder for 112 scale on the OVA gives again Increase of two (2) in the height of the peakon the chromatograms. This is the factory setpoint for the HIGH gain range; however, otherpoints can be set as desired with 30 ppm fullscale on the logarithmic units and a gam ofthree (3) on the linear units being the maximumobtainable without amplifier loading.

7.2.7 SAFETYDue to the low power requirements of the recorder,

one model has been approved for use with Century'sline of certified intrinsically safe instruments. The onlydifference between the two models Is a heavy blue

37

epoxy powder coat on the certified model and differentpower connector pin arrangement to prevent accidentalinterchange of the recorders.

7.2.8 MAINTENANCE AND ROUTINE OPERATIONSRefer to the manufacturer's (Gulton) manual on the

recorder which Is enclosed with each recorder whenshipped.

7.2.8.1 CHANGING CHART SPEEDSThe recorder is equipped with a 16 RPM motor which

gives a writing speed of four (4) strikes per second. Thechart advance speed is determined by the gear trainassembly number used. The inches per hour for eachgear train Is given in the table on page 9 of the Gultonrecorder manual. Refer to the bottom line of the chartadjacent to drive motor 16 and note lor example that anumber 1 gear train has a chart speed of 8"/hour.

a) To change the paper speed, open the recorder,remove gear box spring (on left side), movegear box In direction of arrow on its case and liftout from top. Do not force out from bottom. In-sert new gear, bottom first, slide into positionagainst arrow direction. Replace gear box spr-ing.

7.3 ACTIVATED CHARCOAL FILTER ASSEMBLYThe Activated Charcoal Fitter Assembly. P/N 510095*1,

Is an optional accessory that can be used with any of theCentury portable OVA'S. The filter can be Installedthe OVA Readout Assembly or attached at the endthe telescoping probe. The filter assembly is typicallyfilled with activated charcoal which acts as an adsorbentand effectively filters out most non-methane or non-ethane organic vapors. A screw cap on the probe end laremoved for refilling the filter with activated charcoal orany other filtering media desired.

Applications of the filter include:1) Obtaining a clean air sample for zero baseline

check and adjustment on linear OVA's or for abackground check on logarithmic OVA's.

2) Running "blank" chromatograms to assess In-strument contamination.

3) Rapid screening of methane and non-methaneorganic vapors.

4) Selective screening for natural gas surveys.5) As a moisture filter when filled with a deslccant

such as silica gel.A press fit. large adapter on the back of the titter

assembly is removed when Installing the unit on thetelescoping probe. When replacing the cap end afterrefilling, one wrap of 1 /4 Inch teflon tape should be usedto seal the threads. The recommended activated char-coal for use In the filter la Bamebey-Cheney, Type Gl-8879.

The life of the filter will depend on the time In use andthe concentrations of the compounds being filtered.Under typical Industrial air monitoring conditions, thefHter will last for many days of continuous sampling.

7.4 OVA SAMPLE OILUTORAn adjustable Sample Dllutor Assembly, P/N 51061.

1, Is available as an optional accessory for use on allCentury portable Organic Vapor Analyzers. The dllutormay be adjusted over the range of 5:1 to 50:1 In OVAresponse. In operation, the dllutor Is attached to theand of the telescoping probe or may be connected byexternal tubing to the input fining of the OVA side packcase. Dilution of the air being monitored Is accomplish-<M Dy stream splitting through the use of a needle valveon th« sample Input. An activated charcoal scrubber lainserted In the main air supply line to the OVA andscrubs the air clean of organic vapors and si so creates sslight vacuum at Its output side of the scrubber and thevacuum at this point draws the sample air through theneedle valve where It mixes with the main air supply go-ing to the OVA detector.

This dilution valve provides a means of samplingvapor levels above the lower explosive level (LEU) andIn oxygen deficient atmospheres. These conditions canoccur in normal leak or source survey as the operatorgets close to the leak or vapor source or In monitoringvarious manufacturing or material handling processes.Approximately 14% oxygen Is required to sustain opera-tion of the FID in the OVA.

FIGURE 7-2-1. RECORDER CONTROLS ANDADJUSTMENTS

38

7.4.1 SETTING DILUTION RATEPrepare a sample In a bag at a high level, typically

1,000 to 5,000 ppm. Any suitable gas can be uaed. suchas butane from a cigarette lighter; however, a com-pound similar to those to be measured provides greateraccuracy. The actual concentration of the gas does nothave to be known, since the dilution rate Is simply arelative level.

Obtain an OVA reading on the vapor sample with thedilution valve removed. Then install the valve, loosenthe tarn nut and turn the needle valve until the meterreading corresponds to the original reading divided bythe dilution factor desired. Relight en the (am nut.

It should be noted that when the dilution valve is usedfor natural gas leak survey and pinpointing that the char-coal filter will not remove the methane from the dilutionair supply. Care should be taken so that natural gas isnot allowed to enter the main air Inlet.

7.5 OVA SEPTUM ADAPTERA Septum Adapter. P/N 510645-1. is available for direct

on-line sample Infection to the GC column inlet. TheSeptum Adapter mounts directly on the OVA front paneland sample injections from .025 to 2.5 cc may be made

Readout Adap te r

7

using a gas tight syringe. This provides a range of sen-sitivity of approximately 10% to 1000% of the OVA stan-dard valve, which has a sample loop volume of approx-imately 0.25 cc. Syringe injection can cause a flame-out;however, the OVA may be retgnited after the injection ismade. The air in the sample must 0lute from the columnbefore reignltion can be made. The time tor the air peakto elute will be a function of the column length and thevolume of the sample injected. For example, a 1 cc sam-ple into a 12" column will require waiting approximately5 seconds; and, a 2.S cc sample into a 48" column willrequire approximately 20 seconds.

The Septum Adapter also provides a means wherebysamples can be taken from oxygen deficient at-mospheres or process streams and injected directly in-to the chromatograph. Headspace analysis may also beaccomplished using the Septum Adapter and a syringe.

When the Septum Adapter is Installed on the OVA, thenormal GC sample valve may still be used alternatelywith the syringe infection. In addition to vanable samplesize and sensitivity, syringe injections will normally pro-vide greater symmetry and reduced tailing ofchromatogram peaks as compared with the standardvalve injection.

Unscrew to replace charcoal

V S

Slip Fit ——^ ^- Teflon Tape on threads

FIGU RE 7-3-1. ACTIVATED CHARCOAL FILTER ASSEMBLY

•Tygon Tubing Main Air Inlet(approx. 1 1pm

Dilution Valve

1——OVA Telescoping Probe

Jam Nut

Needle Valve with Wrench Flats

FK3URE 7-4-1. OVA SAMPLE DILUTOR

39

APPENDIX "A"OVA-128

This Appendix Includes the following:

Sample forms and typical Application /Tech Notes

Side Pack Assy Dwg. No. 510605Side Pack Assy Parts List No. LM510605

Electronic Component Assy Dwg. No. 510570Electronic Component Assy Pans List No. LM510570

Cylinder Assy Dwg. No. 510055Cylinder Assy Parts List No. LM510055

Schematic Wiring Diagram Dwg. No. 510555

The assembly drawings and parts lists provide loca-tion/identification Information necessary formaintenance, trouble shooting and parts ordering. Thedrawings sre furnished only for reference and are sub-led to change without notice. The schematic wiringdiagram Is for use In trouble shooting for possible elec-tronic or wiring problems. Note that components thatare not accessible for safely reasons on the certified In-struments are not shown on the schematic. However,typical signal levels at selected points are shown.

In using the drawings and parts list to locate Itemsdescribed In the Maintenance Section of this manual. Itmay first be necessary to Identify the Item In the partslist (by nomenclature), then refer to the correspondingItem number on the drawing for location.

OPERATING AND SERVICE MANUAL

for

CENTURY SYSTEMS'

Portable Organic Vapor Analyz«r (OVA)Mod«l OVA-128

and Optional Acc«aaorl«a

REVISION C

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CENTURY SYSTEMS CORP. TITLE SIDEPACK ASSY/COLUMNARKANSAS CITY. KANSAS OVA- 128

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Screw, 4-40X3/8 Ft. Hd. Phillips

Screw, 4-40X1 /4, Pan Hd. Phillios

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CENTURY

CYLINDER ASSY

510055

CENTURY SYSTEMS CORP.ARKANSAS CITY. KANSAS

1RUCYLINDER ASSY

.1 Conf. OVA-88. 98, 118, 108, 128, 138 LM 510055

510056-1

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510100-2 Regulator Assy.. Low Pressure

510008-1 Gauge H. P.

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10 640-FB-1/4 Nut. Cap. 1/4" x 45*. Brass

11 SI 0108-1 Manifold

12 Nut. 5/8" - 24. Brass

13 510283-1 Connector, Filter Assy

14 112-B-1/8 Nipple. Close. 1/8" Brass

15; 1 510109-1 Connector (MOD)

A69007 Tape. Pipe Thread. 1/4" Teflon

17 Filter. Porous Bronze. 1/4 dla.

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18 510152-1 Ident. Plate VnnH

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ATTACHMENT VI

SOPS FOR DATA VALIDATION

NON-CLP ANALYSES

INTRODUCTION

Sample results will receive QA reviews in batches according totheir time of receipt from the laboratory. The review for eachbatch will be a summary narrative report that includes threecheck sheets (several of each may be required). The contentsof the narrative are summarized in the following section.

NARRATIVE REPORT OUTLINE

The narrative report that will be prepared by Golder Associatesto discuss the results of QA review on each batch of sampleswill include the following items:

1. Sample Integrity

Golder Associates will check that holding times and properchain-of-custody procedures were followed. Forms H(Holding Time) and COG (Chain-of-Custody) will becompleted (examples of these forms are attached).

2. Methodology

Golder Associates will check that the correct extractionand analytical procedures were used and discuss anydeviations. Procedures used will be indicated on form H.

3. Trip Blanks and Rinsate Blanks

Golder Associates will check that the proper number ofblanks were analyzed. An ID (Sample Identification) formwill be completed (an example of this form is attached) .This form, when completed, will indicate the relationshipbetween a batch of samples and the corresponding QAsamples and the QA sheets used. The information on thisform will permit identification of samples affected by anyfailed QA parameters.

4. Field Sample Duplicates

Golder Associates will check whether the correct numberof sample duplicates were collected and analyzed and notesignificant differences (expressed as RPD) between thesamples and the duplicates. The ID checklist forms willbe used in conjunction with the sample analysis sheets tocomplete this assessment.

5. Matrix Spike/Matrix Spike Duplicate

Colder Associates will check whether the correct numberof matrix samples were taken by reference to the IDchecklist forms.

6. Accuracy and Precision

Colder Associates will check whether the accuracy andprecision results for spikes and surrogates were receivedfrom the laboratory and note any outliers. ColderAssociates will also check that the correct surrogateswere used for each sample analysis.

7. Summary

Colder Associates will summarize any deviations fromproject requirements and discuss corrective actions thatresult. Examples of corrective action may includeresampling and reanalysis due to overrun holding times orbroken bottle receipt.

50LOH ASSOCIATES INC. LABORATORY ANALYSIS CHICK SKEfT

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COLDER ASSOCIATES IMC. LAIOftATORY ANALYSIS CHECK SHlCT

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QA Sht<ts Attached:

CLP ORGANIC ANALYSES

STANDARD OPERATING PROCEDURE

Title: Evaluation of Organics DataAttachment X.I: Data Assessment

(Total Review - Organics)

PROJECT

REPORT #

REVIEWER _________________

X£S HQ N/A

X.I.I Sample Traffic ReportPresent or on file? j;_i __ __

Legible? f ] __ __

ACTION: If no, request from colderProject Manager.

X.l.2 Cover PagePresent? f ] __ __

Do sample numbers on cover pageagree with sample numbers on:

(a) Traffic Report sheets? r ] __ __

(b) Colder Associates SampleIdentification Summary? I_]_ __ __

ACTION: If no for any of the above,contact Colder Project Mana-ger.

X.I.3 Chain of Custody FormPresent?

Sample I.D.s - Present?

Sampler's Name - Present? j;_]_

Date of Sampling - Present? [ ]

Date of Shipment - Present? j;_]_

Date of Receipt at Laboratory -Present? _[_]_

Shuttle Seal Intact at Laboratory? r ] __ __

ACTION: If no for any of the above,contact Colder Project Mana-ger.

X.I.4 Analytical ResultsPresent?

Detection Limits- Present?Within Required DetectionLimits?

Units - Present?

Sample Results - Present forall required compounds?

Matrix - Description?

Proper units for matrix?

Units - Present for allrequired compounds?

Are all "less than11 valuesproperly coded?

ACTION: If no for any of the above,prepare Telephone Memorandumand contact the laboratoryfor corrected data.

Were any samples dilutedbeyond requirements ofcontract?

If so, were dilutions doc-umented?

ACTION: If any sample was dilutedbeyond contract requirements,note under non-compliance ofData Assessment Narrative.

XES

-L-l

L-L

L-LLJ.

-LJ.

-LJ.

X.I.5 Holding Times - (Examine Chain of CustodyForm and Traffic Reports)

Aromatic Volatiles (Unpreserved) -Exceeded (7 Days)? __

Aromatic Volatiles (Preserved) -Exceeded (14 Days)? __

L-L

-L-l

XE5 NQAll other Volatiles - Exceeded(14 Days)? __

Extractables - Were any holdingtimes for extraction exceeded(7 Days)? __

Extractables - Were any holdingtimes for analysis exceeded(40 Days)? __ _[_]_

Pesticides - Were any holdingtimes for extraction exceeded(7 days)? __ r ]

Pesticides - Were any holdingtimes for analysis exceeded(40 days)? __ f ]

ACTION: Prepare a list of all samplesand analytes for which holdingtimes have been exceeded.Specify the number of days fromdate of collection to the dateof analysis (from raw data).Attach to checklist. Reject(red-line) values less thanInstrument Detection Limit(IDL),flag as estimated (J) thosevalues above IDL.

X.I.6 GC/MS Tuning

X.I.6.1 Ion Abundance Criteria

X.1.6.1.1 Decafluorotriphenylphosphine (DFTPP)

m/z Ion Abundance

51 30.0 - 60.0% Of m/z 19868 less than 2.0% of m/z 6970 less than 2.0% of m/z 69127 40.0 - 60.0% Of m/z 198197 less than 1.0% of m/z 198198 base peak, 100% relative abundance199 5.0 - 9.0% of m/z 198275 10.0 - 30.0% Of m/z 198365 greater than 1.00% of m/z 198441 present, but less than m/z 443442 greater than 40.0% of m/z 198443 17.0 - 23.0% of m/z 442

N/AX.I.6.1.2 Bromofluorobenzene (BFB)

m/z Ion Abundance

50 15.0-40.0% of the base peak75 30.0-60.0% of the base peak95 base peak, 100% relative

abundance96 5.0 - 9.0% of the base peak173 less than 2.0% of m/z 174174 greater than 50.0% of the base

peak175 5.0 - 9.0% of m/z 174176 greater than 95.0%, but less

than 101.0% of m/z 174177 5.0 - 9.0% Of m/z 176

X.I.6.2 Tuning Results (For instrument tuned using DFTPP)

Calibration Data - Present? I_L __ __

ACTION: If no, prepare TelephoneMemorandum and request submit-tal by laboratory.

Do all Ion Abundance Criteria fallwithin the values listed in Sectionx.i.6.1.1? r i _ _

ACTION: If no, complete checklistitems below marked with "*"

* Is m/z 51 between 22.0 - 75.0%of m/z 198? r 1

* Is m/z 127 between 30.0 - 75.0%of m/z 198? f ]

* Is m/z 275 between 7.0 - 37.0%of m/z 198? r ]

* Is m/z 365 greater than 0.75%of m/z 198? r ]

* Is m/z 442 greater than 30.0%of m/z 198? r 1

ACTION: If more than one of theexpanded criteria above (*)are out of bounds, or if anyof the other criteria listedin Section X.I.6.1.1 are outof bounds, flag all data

HQ N/Aassociated with that run asunusable (red-line).Otherwise,the data reviewer has theoption of accepting the data,depending on project priori-ties.

Is calibration data present foreach 12-hour period samples areanalyzed? r ] __ __

Are there any transcriptionerrors? __ _[_l __

Are there any calculation errors? __ _[_1 __

Is the appropriate number of sig-nificant figures used to reporttuning results (same asX.I.6.l.l)? r l __ __

ACTION: Prepare a Telephone Memorandumand contact the laboratory forclarification or resubmittal.

X.I.6.2 Tuning Results (For instrument tuned using BFB)

Calibration Data - Present? j;_1 _

ACTION: If no, prepare TelephoneMemorandum and request submit-tal by laboratory.

Do all Ion Abundance Criteria fallwithin the values listed in SectionX.I.6.1.2? r ] _

ACTION: If no, complete checklistitems below marked with "*"

* Is m/z 50 between ll.o - 50.0%of the base peak? i_1 _

* Is m/z 75 between 22.0 - 75.0%of the base peak? r 1 _

ACTION: If more than one of theexpanded criteria above (*)are out of bounds, or if anyof the other criteria listedin Section X.I.6.1.2 are outof bounds, flag all data

NQ N/Aassociated with that run asunusable (red-line).otherwise,the data reviewer has theoption of accepting the data,depending on project priori-ties.

Is tuning data present foreach 12-hour period samples areanalyzed? _[_1 __ __

Are there any transcriptionerrors? __ .[_]_ __

Are there any calculation errors? __ l_\ __

Is the appropriate number of sig-nificant figures used to reporttuning results (same asX.I.6.1.2)?

ACTION: Prepare a Telephone Memorandumand contact the laboratory forclarification or resubmittal.

X.I.7 Calibration - VOA & SNA

Calibration Data - Present?

Legible?

ACTION: If no, prepare TelephoneMemorandum and contactlaboratory for clarificationor resubmittal.

X.I.7.1 Initial Calibration

Are all average Relative ResponseFactors (Reported) for TCL com-pounds > 0.05? r 1

Are all Percent Relative standardDeviations (%RSD) < 30%? [ 1

NOTE: Perform a spot-check ofone or more of the reportedcalibration values, com-puting the RRF and %RSD.If errors are detected inthe calculations of eitherthe RRF or the %RSD, perform

XES NQ N/Aa more comprehensive recalcu-lation.

ACTION: If any volatile or semivolatileTCL compound result has anaverage RRF of less than 0.05:

a. Flag positive results forthat compound as estimated(J).

b. Flag non-detects for thatcompound as unusable (R) .

If any volatile or semivolatileTCL compound has a %RSD ofgreater than 30%:

a. Flag positive results forthat compound as estimated(J).

b. Non-detects may be qualifiedusing professional judgement.

X.I. 7. 2 Continuing Calibration

Are all average Relative ResponseFactors (Reported) for TCL com-pounds > 0.05? 1 _ 1 __ __

Are all Percent Relative StandardDeviations (%RSD) < 25%? r 1

NOTE: Perform a spot-check ofone or more of the reportedcalibration values, com-puting the RRF and %RSD.If errors are detected inthe calculations of eitherthe RRF or the %RSD, per forma more comprehensive recalcu-lation.

ACTION: If any volatile or semivolatileTCL compound result has anaverage RRF of less than 0.05:

a. Flag positive results forthat compound as estimated(J).

b. Flag non-detects for that

XES. NQcompound as unusable (R).

If any volatile or semivolatileTCL compound has a %RSD ofgreater than 25%:

a. Flag positive results forthat compound as estimated(J).

b. Non-detects may be qualifiedusing professional judgement.

X.l.8 Blanks - VOA &BNA

ACTION:

ACTION:

Has a Method Blank been reportedfor :

each matrix? r 1

concentration level?

each GC/MS system (VGA)? [ ]

.L-1each extraction batch(semivolatiles)?

Prepare a Telephone Memorandumand contact the laboratory forclarification or resubmittal.

Was a detection reported in ablank for:

Methylene chloride?

Acetone?

Toluene?

2-Butanone (MEK)?

Phthalate esters?

No positive sample resultsshould be reported unlessthe concentration of thecompound in the sample exceeds10 times the amount in anyblank for the compounds listedabove. The results should bequalified by elevating thedetection limit for that com-pound. For compounds not listed

above, results should be qual-ified if the reported concen-tration is not at least 5times the blank value.

If gross contamination exists(saturated peaks by GC/HS),all compounds affected shouldbe flagged as unusable (R), inall samples affected.

If low levels of compounds areconsistently found in blanks,make a note in the Data Accept-ability Narrative, prepare aTelephone Memorandum, and con-tact the laboratory.

X.I.9 Surrogate Recovery fVOA & BNA1

X.I.9.1 Volatile surrogate Recoveries (Water)

QC LIMITS

Toluene-d8 88 - 110%Bromofluorobenzene 86 - 115%l,2-Dichloroethane-d4 76 - 114%

X.l.9.2 Volatile Surrogate Recoveries (Soil)

QC LIMITS

Toluene-d8 81 - 117%Bromofluorobenzene 74 - 121%l,2-Dichloroethane-d4 70 - 121%

X.l.9.3 Semivolatile Surrogate Recoveries (Water)

QC LIMITS

Nitrobenzene-d5 35 - 114%2-Fluorobiphenyl 43 - 116%Terphenyl-dl4 33 - 141%Phenol-d6 10 - 94%2-Fluorophenol 21 - 100%2,4,6-Tribromophenol 10 - 123%

X.l.9.4 Semivolatile Surrogate Recoveries (Soil)

QC LIMITS

Nitrobenzene-dS2-Fluorobipheny1

23 - 120%30 - 115%

Terphenyl-dl4 18 - 137%Phenol-d6 24 - 113%2-Fluorophenol 25 - 121%2,4,6-Tribromophenol 19 - 122%

X.I.9.5 Surrogate Analysis

Is any surrogate in a VGA oracid fraction out of specification,or does any VOA surrogate have arecovery of less than 10%? __ I_1

Are any two surrogates in a base/neutral or acid fraction out ofspecification, or have recoveriesless than 10%? __ r 1

Do any blanks have surrogates outof specification? __ I_1

ACTION: If at least two surrogates ina base/neutral or acid frac-tion, or one surrogate in aVOA fraction are out of spec-ification, but have recoveriesgreater than 10%:

a. Positive results for thatfraction are flagged asestimated (J).

b. Negative results for thatfraction are flagged withthe sample guantitationlimit as estimated (UJ).

If any surrogate in a fractionshows less than 10% recovery:

a. Positive results for thatfraction are flagged asestimated (J).

b. Negative results for thatfraction are flagged asunusable (R).

If surrogate recoveries areout of specification for ablank, prepare a TelephoneMemorandum and contact thelaboratory.

XES. N/A

X.I.10

X.I.10.1

X.I.10.2

X.I.10.3

X.I.10.4

Matrix Soike/Matrix Spike Duplicate(VOA & SNA)

Volatile Matrix Spike/Matrix SpikeDuplicate Recovery (Water)

QC LIMITS

1,1-DichloroetheneTrichloroetheneBenzeneTolueneChlorobenzene

Recovery RPD61 - 145%71 - 120%76 - 127%76 - 125%75 - 130%

1414111313

Recovery59 -62 -66 -59 -60 -

172%137%142%139%133%

RPD2224212121

Volatile Matrix Spike/Matrix SpikeDuplicate Recovery (Soil)

QC LIMITS

1,1-DichloroetheneTrichloroetheneBenzeneTolueneChlorobenzene

Semivolatile Matrix Spike/Matrix spikeDuplicate Recovery (Water)

QC LIMITSRecovery RPD

Phenol 12 - 89% 422-Chlorophenol 27 - 123% 401,4-Dichlorobenzene 36 - 97% 28N-Nitroso-di-n-prop.(1) 41 - 116% 381,2,4-Trichlorobenzene 39 - 98% 284-Chloro-3-methylphenol 23 - 97% 42Acenaphthene 46 - 118% 314-Nitrophenol 10 - 80% 502,4-Dinitrotoluene 24 - 96% 38Pentachlorophenol 9 - 103% 50Pyrene 26 - 127% 31

Semivolatile Matrix Spike/Matrix SpikeDuplicate Recovery (Soil)

QC LIMITS

Phenol2-Chlorophenol1,4-DichlorobenzeneN-Nitroso-di-n-prop.(1)1,2,4-Trichlorobenzene

Recovery26 - 90%25 - 102%28 - 104%41 - 126%38 - 107%

RPD3550273823

XES.2-Chloro-3-raethylphenol 26 - 103% 33Acenaphthene 31 - 137% 194-Nitrophenol 11 - 114% 502,4-Dinitrotoluene 28 - 89% 47Pentachlorophenol 17 - 109% 47Pyrene 35 - 142% 36

X.l.10.5 Matrix Spike/Matrix Spike DuplicateAnalysis (VGA & BNA)

Are there any transcriptionerrors? __

Are any recoveries outside oflimits (X.I.10.1 - X.l.10.2)? __ r 1

Are any RPDs exceeded? __ j;_]_

ACTION: Make a note in the DataAcceptability Narrative,prepare a Telephone Memo-randum, and contact thelaboratory.

X.l.11 Field Duplicates

Are field duplicates identified? j;_1 __

ACTION: If there are field duplicates,calculate the Relative PercentDifference. Make a note in theData Acceptability Narrative.

X.l.12 Internal Standards Performance

Are Internal Standards Dataavailable? _[_]_ __

ACTION: If no, prepare a TelephoneMemorandum and contact thelaboratory.

Are all internal standard areacounts within 50 - 200% of theassociated calibration standards? .[_i

ACTION: If an IS area count is outsidelimits:

a. Positive results for com-pounds quantitated usingthat IS are flagged asestimated for that sample

fraction.

b. Non-detects for compoundsquantitated using that ISare flagged with the samplequantitation limit classi-fied as estimated (UJ) forthat sample fraction.

c. If extremely low area countsare reported, or if perform-ance exhibits a major abruptdecline, non-detects shouldbe flagged as unusable (R).

Are all retention times within + 30seconds of the associated calibra-tion standard? _[_1

ACTION: If any IS retention time variesby more than 30 seconds, exam-ine the chromatographic profileto determine if any false pos-itives or negatives exist. Hakea note in the Data AcceptabilityNarrative, prepare a TelephoneMemorandum, and contact the lab-oratory.

x.l.13 TCL Compound Identification

Are all compounds within 0.06 rela-tive retention time (RRT) units ofthe standard RRT?

Are all ions present in the standardmass spectrum at a relative intens-ity > 10% present in the sample massspectrum? r 1

Do the relative intensities of ionsagree within ± 20% between the stan-dard and sample spectra? [ ]

Are ions having relative intensitiesgreater than 10% in the sample spec-trum but not present in the standardspectrum accounted for? _[_i

ACTION: If no for any of the above,note in the Data AcceptabilityNarrative, prepare a TelephoneMemorandum, and contact the

NQ N/Alaboratory.

X.I.14 Compound Quantitation and ReportedDetection Limits

Was the correct internal standardused to quantitate each compound? ,[_j. __ __

Was the correct quantitation ionused for each compound (SeeAttachment X.8)? r ] __ __

Was the correct Relative ResponseFactor (RRF) used for eachcompound? .[_1 __ __

Have the Quantitation Limits beenadjusted to reflect all sampledilutions, concentrations, splits,clean-up activities, and dry weightfactors? r 1 __ __

ACTION: If no for any of the above,note in the Data AcceptabilityNarrative, prepare a TelephoneMemorandum, and contact thelaboratory.

X.I.15 Tentatively Identified Compounds (TIC1

Are all major ions (greater than 10%relative intensity) in the referencespectrum present in the sample spec-trum? r i _ _

Do the relative intensities of themajor ions agree within ± 20%between the reference and samplespectra? ,[_]_ __ __

ACTION: If it is determined that atentative identification of anon-TCL is not acceptable, thetentative identificationshould be changed to "unknown"or an appropriate identifica-tion.

Are any TIC peaks present in a sam-ple also found in any blanks? __

ACTION: TIC results which are not suf-ficiently above the level in

NO N/Athe blank should not be re-ported. When a compound isnot found in any blanks, butis a suspected laboratorycontaminant, the result maybe flagged as unusable (R).

X.l.16 System Performance

Are there any abrupt shifts in re-constructed ion chromatogram (RIC)baselines? __ _[_j __

Are there high RIC backgroundlevels? __ r 1 __

Is there excessive baseline riseat elevated temperatures? __ _[_]_ __

Are there significant extraneouspeaks? __ r 1 __

Is any peak tailing or peak split-ting identified? __ r ] __

ACTION: Positive responses for any ofthe above may indicate generalsystem deterioration. Note inthe Data Acceptability Narra-tive, prepare a Telephone Mem-orandum, and contact the lab-oratory.

X.I.17 Instrument Performance (Pesticides)

X.I.17.1 DOT Retention Time

Is the retention time for DOTgreater than 12 minutes?

Is there adequate resolutionbetween DOT peaks?

ACTION: If the retention time is lessthan 12 minutes (except onOV-l and OV-101), a close ex-amination of the chromatogra-phy is necessary to ensure thatadequate separation of indiv-dual components is achieved. Ifadequate separation is notachieved, flag all affected com-pound data as unusable (R).

XES NO N/AX.I.17.2 Retention Time Windows

Are retention time windowsreported? I_1 __ __

ACTION: Prepare a Telephone Memorandumand contact the laboratory.

Are all pesticide standards withinestablished retention time windows?!_i __ __

ACTION: If the standards do not fallwithin the retention time win-dows, the associated sampleresults should be carefullyevaluated. All samples inject-ed after the last in-controlstandard may be affected.

Check to see if chromatogramscontain peaks near the com-pound of interest. If no peaksare present either within orclose to the retention timewindow of the deviant compound,there is usually no effect onthe data.

If the affected sample chromat-ograms contain peaks close toor within the retention timewindow of the pesticide of in-terest, the affected positiveresults and quantitation limitsmay be flagged as unusable (R),or more thorough reanalysis ofthe affected retention timewindows may be performed, atthe discretion of the reviewer.

X.1.17.3 DDT/Endrin Degradation Check

Does the percent breakdown for4,4'-DOT exceed 20% (see AttachmentX.9 for formula)? __ r 1 __

Does the percent breakdown forendrin exceed 20% (see AttachmentX.9 for formula)? __ j_i __

Does the combined percent breakdownexceed 20% (see Attachment X.9 forformula)? __ _L_L __

NO N/AACTION: If DOT breakdown is greater

than 20%, beginning with thesamples following the lastin-control standard:

a. Flag all quantitative re-sults for DOT as estimated(J). If DOT was not detected,but ODD and DDE are positive,then flag the quantitationlimit for DOT as unusable(R).

b. Flag results for ODD and/orDDE as presumptively presentat an estimated quantity (NJ).

If endrin breakdown is greaterthan 20%:

a. Flag all quantitative resultsfor endrin as estimated (J).If endrin was not detected,but endrin aldehyde and endrinketone are positive, then flagthe quantitation limit forendrin as unusable (R).

b. Flag results for endrin ketoneas presumptively present at anestimated quantity (NJ).

X.I.17.4 Retention Time Check

Is the percent difference in re-tention time for dibutylchlorendatein all standards and samples < 2.0%for packed columns, < 0.3% for cap-illary columns, or < 1.5% for wide-bore capillary columns? _[_1 __ __

ACTION: If no, the analysis may beflagged as unusable (R), atthe discretion of the reviewer.

X.I.18 Calibration (Pesticides)

X.I.18.1 Initial Calibration Linearity Check

Does the Percent Relative standardDeviation (%RSD) of calibrationfactors for aldrin, endrin, DOT, anddibutylchlorendate exceed 10% (seeAttachment X.9 for formula)? __ r J __

XES HQ N/AACTION: If yes, flag all associated

quantitative results asestimated (J).

Were all standards analyzed within72 hours of any sample? I_I __ __

If DOT or toxaphene was identifiedand quantitated, was a three-pointcalibration used? I_1

ACTION: If no, flag all associatedquantitative results as est-imated (J) .

X.I.18.2 Analytical Sequence

X.I.18.2.1 Primary Analysis

Were all standards analyzed at thebeginning of each 72 hour sequence(see list below)? [ 1

Required Standards:Evaluation Standard Mix AEvaluation Standard Mix BEvaluation Standard Mix CIndividual Standard Mix A*Individual Standard Mix B*ToxapheneAroclors 1016/1260Aroclor 1221**Aroclor 1232**Aroclor 1242Aroclor 1248Aroclor 1254

* These may be combined into onemixture.

** Aroclors 1221 and 1232 must beanalyzed on each instrument andeach column at a minimum of onceper month.

ACTION: If no, flag all associated dataas unusable (R).

N/Ax.l. 18. 2. 2 Confirmation Analysis

Were Evaluation Standard Mix A, B,and C analyzed within 72 hours ofanalysis of all samples? _[ _ ]_ __ __

Was the Individual Standard Mixcontaining the compounds to beconfirmed analyzed after every5 samples? _[ _ l __ __

Was Evaluation Standard Mix Banalyzed after every 10 samples? j; _ ]_ __ __

ACTION: If no for any of the above,all associated data may beflagged as estimated (J) .

x.l. 18. 3 Continuing Calibration

Was the percent difference (%D)between the calibration factorsgreater than 15% for compound (s)being quant itated, or 20% forcompound(s) being confirmed (seeAttachment X.9 for formula)? __ r ] __

ACTION: If yes, flag all associatedquantitative results as est-imated (J) .

X.l. 19 Blanks (Pesticides)

Was a method blank analysis reportedfor each matrix, concentration level,extraction batch, and different GCsystem used to analyze samples? .[ _ ]_ __ __

ACTION: Make a note in the Data Ac-ceptability Narrative, pre-pare a Telephone Memorandum,and contact the laboratory.

Do any method blanks have reportedconcentrations of any Pesticide/PCBabove Required Quantitation Limits? __ _[ _ ]_

ACTION: If yes:a. If a Pesticide/PCB is found

in the blank but not in thesample(s), no action is taken.

XES. HQ N/Ab. If a Pesticide/PCB is found

in a sample and in the as-sociated blank, and thesample concentration isless than 5 times the blankconcentration, the sampleresult should be qualifiedas not-detected with anelevated detection limit (U).

X.I.20 Surrogate Recovery (Pesticides)

Is the recovery of Dibutylchloren-date within 24 - 254% for watersamples or 20 - 150% for soil sam-ples? r i _ _

ACTION: If no, the associated datamay be qualified. If low re-coveries are obtained, flagassociated positive resultsand quantitation limits asestimated (J). If high reco-veries are obtained, profes-sional judgement should beused to determine appropriateaction. A high bias may be dueto co-eluting interferences.If zero recovery is reported,the reviewer should examine thesample chromatogram to determineif the surrogate is present, butslightly outside its retentiontime window. If the surrogateis not present, flag all negat-tive results as unusable (R).

X.I.21 Matrix Spike/Matrix Spike Duplicate(Pesticides!

X.I.21.2 Water Matrix Spike/Matrix Spike DuplicateRecovery (Pesticides)

QC LIMITS

Recovery RPDgamma-BHC (Lindane) 56 - 123% 15Heptachlor 40 - 131% 20Aldrin 40 - 120% 22Dieldrin 52 - 126% 18Endrin 56 - 121% 214,4'-DDT 38 - 127% 27

YES NO N/A

X.I.21.2 Soil Matrix Spike/Matrix Spike DuplicateRecovery (Pesticides)

QC LIMITS

Recovery RPDgamma-BBC (Lindane) 46 - 127% 50Heptachlor 35 - 130% 31Aldrin 34 - 132% 43Dieldrin 31 - 134% 38Endrin 42 - 139% 454,4'-DDT 23 - 134% 50

X.I.21.3 Matrix Spike/Matrix Spike DuplicateAnalysis (Pesticides)

Are there any transcriptionerrors? __

Are any recoveries outside oflimits (X.I.21.1 - X.I.21.2)? __ r 1

Are any RPDs exceeded? __ _[_1

ACTION: Make a note in the DataAcceptability Narrative,prepare a Telephone Memo-randum, and contact thelaboratory.

X.I.22 Field Duplicates (Pesticides)

Are field duplicates identified? 1__]_ __

ACTION: If there are field duplicates,calculate the Relative PercentDifference. Make a note in theData Acceptability Narrative.

X.I.23 Compound Identification fPesticides!

Were all reported positive detec-tions within appropriate retentiontime windows? I_1

ACTION: If no, examine the chromato-grara to see if there are otherpeaks near the compound ofinterest that may be interfer-ing with the signal. If no,qualify the compound as notdetected.

mWas a 3% OV-1 column used for con-firmation if both dieldrin andDDE were reported? __ _[_]_

ACTION: If yes, flag all affected dataas unusable (R).

Did all positive identificationshave dissimilar column analysis? j;_]_ __

ACTION: If no, flag all affected dataas unusable (R).

For chlordane, toxaphene or PCBs(multicomponent analytes), do theretention times and relative peakratios of major component peaksmatch the expected patterns? j;_1

ACTION: If PCBs or multipeak pesti-cides exhibit marginal patternmatching quality, professionaljudgement should be used to es-tablish whether the differencesare attributable to environmen-tal "weathering". If the pres-ence of a PCB/multipeak pest-icide is strongly suggested,results should be reported aspresumptively present (N). Ifan observed pattern closelymatches more than one Aroclor,professional judgement shouldbe used to decide whether theneighboring Aroclor is a bettermatch, or if multiple Aroclorsare present.

Was GC/MS confirmation performed forpesticide/PCB concentrations in thefinal sample extract which exceeded10 ng/uL? r 1

ACTION: If no, note in the Data Accept-ability Narrative, prepare aTelephone Memorandum, and con-tact the laboratory.

X.I.24 Compound Ouantitation and ReportedDetection Limits (Pesticides)

Do reported sample results match

STANDARD OPERATING PROCEDURE

Title: Evaluation of Organics Analyses

1.0 Scope

1.1 This procedure is applicable to organic data obtainedfrom laboratories contracted to provide analyticalservices.

1.2 The data validation protocols have been developed byGolder Associates Inc. using "Laboratory DataValidation - Functional Guidelines for EvaluatingOrganics Analyses", Hazardous Site Evaluation Division,USEPA, February, 1988.

2.0 ResponsibilitiesData reviewers will complete the following tasks asassigned:

2.1 For a Total Review:

2.1.1 Data Assessment - "Total Review - Organics"Attachment X.I.

2.1.2 Data Assessment - Data Acceptability NarrativeAttachment X.2.

2.1.3 Non-ComPliance Report Attachment X.3This report is to be completed only when a seriousdiscrepancy is encountered, or upon the request ofthe Golder Data Review Manager. Forward __copies, one each for the addressees on the MailingList for Data Review (Attachment X.4). In othercases involving more routine discrepancies,notations should be made in the Data AcceptabilityNarrative (Sec. X.2.2).

2.1.4 Data summary Sheet - Summary of Organic QualityControl Data Attachment X.5.Enter on Data Summary Sheet all values for QualityControl Parameters found in the AnalyticalReports.

2.1.5 Data Acceptability Summary Form Attachment X.6Fill out as necessary for each category. Place an"X" in boxes where analyses were not performed, orcriteria do not apply.

IES NO N/Acalculations performed using theraw data? f 1 __ __

Have Required Detection Limitsbeen adjusted to reflect allsample dilutions, concentrations,splits, clean-up activities, anddry weight factors? I_1 __ __

ACTION: If no, note in the Data Ac-ceptability Narrative, preparea Telephone Memorandum, andcontact the laboratory.

Are quantitation limits affected bylarge, off-scale peaks? __ j;_]_ __

ACTION: If yes, flag affected resultsas unusable (R). If the inter-ference is on-scale, the re-viewer can provide an estimatedquantitation limit (UJ) foreach affected compound.

Note: Single-peak pesticide re-sults should be checked forrough agreement between quant-itative results obtained on thetwo GC columns. The reviewershould use professional judge-ment to decide whether a muchlarger concentration obtainedon one column versus the otherindicates the presence of an in-terfering compound. If an inter-fering compound is indicated, thelower of the two values should bereported and qualified as an est-imated quantity (NJ). This neces-sitates a determination of an es-timated concentration on the con-firmation column. The narrativeshould indicate that the presenceof interferences has obscured theattempt at a second column confir-mation.

2.1.6 Data Review Log;The data reviewer will maintain a log of reviewscompleted to include:a. Date of start of case reviewb. Date of completion of case reviewc. Site named. Laboratorye. Number of samplesf. Matrixg. Reviewer's initials

2.1.7 Telephone MemorandumThe data reviewer should enter the bare facts ofthe inquiry before initiating any phoneconversation with the laboratory. File the yellowcopy in the Project Telephone Memorandum folderand attach a photocopy of the Telephone Memorandumto the completed Data Acceptability Narrative(Attachment X.2).

2.1.8 Forwarded Paperwork

2.1.8.1 Upon completion of the review, the following areto be forwarded to IEPA and USEPA Region VRemedial Project Managers:a. Completed data assessment checklistb. Data Summary Sheet (Attachment X.5) along with

completed Data Acceptability Narrative(Attachment X.2)

2.1.8.2 Forward 1 copy of completed Data AcceptabilityNarrative (Attachment X.2) along with TelephoneMemoranda, if any, to each of the four addressees(4 copies total) on the Mailing List for DataReview Recipients (Attachment X.4).

2.1.9 Filed PaperworkUpon completion of review, the following are to befiled within Colder files:a. Completed Data Acceptability

Narrative (Attachment X.2)b. Telephone Memorandac. Data Summary Sheet - summary of

Organics Quality Control Data (Attachment X.5)d. Non-Compliance Report (Attachment X.3)e. Data Acceptability Summary Form

(Attachment X.6)f. Checklist of Total Review (Attachment X.I)g. Sample Identification Summary (Attachment X.7)

3.0 Timeliness

3.1 Data CompletenessIncomplete data packages must be brought to the

attention of the IEPA and USEPA Remedial ProjectManagers whenever the lack of any information wouldcause the rejection of data.

3.2 Colder will contact the laboratory within one workingday of discovery of any incomplete data package.Designee will again contact the laboratory two weeksafter first contact if data has not been received.

3.3 If incomplete data packages are held longer than sixweeksfrom the date of receipt of the initial datapackage, the IEPA and USEPA Region V Remedial ProjectManagers will be contacted with an explanationspecifying which reported values could be consideredvalidated and which required further clarification.

4.0 Rejection of DataAll values determined to be unacceptable on the OrganicAnalysis Data Sheet must be lined through with a red pencil.As soon as any review criteria causes data rejection, thosedata can be eliminated from any further review orconsideration.

5.0 Acceptance CriteriaAcceptance criteria as stated in Attachment X.l will beused.

6.0 Request for ReanalysisData reviewers must note all items of non-compliance withinthe Data Assessment Narrative. If holding times and samplestorage times have not been exceeded, Colder may requestreanalysis if items of non-compliance are critical to dataassessment. Requests are to be made by telephone.

7.0 A sample Identification Summary will be completed by theColder Remedial Project Manager identifying all samples byCRL-type and site number.

CLP METALS/CYANIDE ANALYSES

STANDARD OPERATING PROCEDURE Section:Revision:

Title: Evaluation of Metals Data Date:Page:

1.0 Scope

1.1 This procedure is applicable to inorganic data obtainedfrom York Laboratories. This Standard operatingProcedure is substantially derived from a documententitled "Evaluation of Metals Data for the ContractLaboratory Program, Revision VII, o.s. EPA Region II,February 1988".

1.2 All modifications have been made by Solder AssociatesInc. (Golder) with no discussions or other input fromU.S. EPA Region II.

2.0 Responsibilities - Data reviewers will complete the followingtasks:

2.1. For a total review;

2.1.1 Data Assessment - "Total Review-Inorganics" Checklist

Attachment - Al

2.1.2 Data Assessment * Data Acceptability Narrative (Attachment -A21

2.1.3 Non-Compliance Report (Attachment - A3)This report is to be completed only when a serious violationis encountered, or upon the request of the Golder DataReview Manager. Forward 5 copies: one each for theaddressees of Mailing List for Data Review Recipients(Attachment - A4). In other cases, all violations shouldbe appended to end of Data Acceptability Narrative (Sec. A-2) .

2.1.4 Data 8"f" ry Sheet - Summary of inorganic Quality ControlData (Attachment * AS).Enter on Data Summary Sheet all values from the RASdeliverable package. Circle all values out of controllimits in red.

2.1.5 CLP Type Data Acceptability f'lmarv Form (Attachment - A€)Fill out as necessary for each category. Place an "X" inboxes where analyses were not performed, or criteria do notapply.

Colder Associates

STANDARD OPERATING PROCEDURE Section:Revision:

Title: Evaluation of Metals Data Date:Page:

2.1.6 Data Review Log; The data revievar will maintain a log ofreviews completed to include:a. date of start of case reviewb. date of completion of case reviewc. site named. laboratorye. number of samplesf. matrixg. reviewers initials

2.1.7 Sample Identification fiUBfflflrv (Attachment - A71

2.1.8 Telephone Memorandum - the data reviewer should enter thebare facts of inquiry, before initiating any phoneconversation with the York laboratory. File yellow copy inthe Project Telephone Memorandum folder, and attach aphotocopy of the Telephone Memorandum to the completed DataAcceptability Narrative (Attachment).

2.1.9 Forwarded Paperwork

2.1.9.1 Upon completion of review, the following copies are tobe forwarded to the IZPA and U.S. EPA, Region V RemedialProject Managers:a. completed data assessment checklistb. Data summary Sheet (Attachment) along with completed

Data Acceptability Narrative (Attachment).

2.1.9.2 Forward 4 copies of completed Data AcceptabilityNarrative (Attachment) along with Telephone Memorandum,if any,: one each for the addressees of Mailing List forData Review Recipients (Attachment) .

2.1.10 Filed Paperwork - Upon completion of review, the followingare to be filed within Solder files:a. completed Data Acceptability Narrative (Attachment - A2)b. Telephone Memorandum (copy)c. Data Summary Sheet - Summary of Inorganics Quality

Control Data (copy) (Attachment - AS)d. Non-compliance report (Attachment - A3)e* CLP Type Data Acceptability Summary Form (Attachment -

AC)f. Checklist of Total Review (Attachment - ADg. Sample Identification Summary (Attachment - A7) .

3.0 Timeliness

Golder Associates

STANDARD OPERATING PROCEDURE Section:Revision:

Title: Evaluation of Metals Data Date:Page:

3.1 Data Completeness - Incomplete data packages must be broughtto the attention of the IE PA and U.S. EPA Remedial ProjectManagers whenever the lack of any information would cause therejection of data.

3.2 colder will contact York Laboratories within one working dayof discovery of an incomplete data package. Designee willagain contact laboratory two weeks after first contact if datahas not been received.

3.3 If incomplete data packages are held longer than six weeksfrom date of receipt of initial data packages the IEPA andU.S. EPA Region V Remedial Project Managers will be contactedwith an explanation specifying which reported values could beconsidered validated and which were avaiting further data.

4.0 Rejection of Data - All values determined to be unacceptableon the inorganic Analysis Data Sheet (Attachment - AS) mustbe lined over with a red pencil. As soon as any reviewcriteria causes data to be rejected, that data can beeliminated from any further review or consideration.

S.o Acceptance Criteria - Acceptance criteria as stated in theAttachment, will be used.

6.0 Request for Reanalysis - Data reviewers must note all itemsof non-compliance within Data Assessment Narrative (Attachment- A2). If holding times and sample storage times have notbeen exceeded, Qolder may request reanalysis if items of non-compliance are critical to data assessment. Requests are tobe made by telephone.

7.0 A Sample Identification Summary sheet will be completed by theGolder Remedial Project Manager identifying all samples by CRLtype and site number (Attachment - A7) .

Golder Associates

STANDARD OPERATING PROCEDURE Section:Titla: Evaluation of Metals Data Revision:

: Data Assessment Data:(Total Review - Inorganics) Page:

Xfifi NQ N/A

A.1.1 Sanole Traffic Report - Present or on file? [__]Legible? [__j

ACTION: If no, readiest from ColderProject Manager

A. 1.2 Cover Page - Present? [__]

ACTION: If no, prepare Telephone Memorandumand contact laboratory

Do sample numbers on cover page agree withsample numbers on:

(a) Traffic Report Sheets? [__]

(b) Form I»s? [__]

(c) Golder Associates1 sampleIdentification Summary? [__]

ACTION: If no for any of the above,contact Golder Project Manager

A. 1.3 Form I (Final Data) - Are all Form I'spresent and complete? [__]

ACTION: If no, prepare Telephone Memorandumand contact laboratory for submittal

Are correct units (ug/1 for waters and mg/kgfor soils) indicated in Form I's? [__3

Are sample results for each parametercorrected for percent solids on soils? [__]

Do any computation/transcription errorsexceed 10% of reported values? [__]

Are all "less than" values properly codedwith "0"? [__]

ACTION: If no for any of above, prepareTelephone Memorandum, and contactlaboratory for corrected data.

Golder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Date:(Total Review - inorganics) Page:

S I i s IZ5

Was a brief physical description of samplesgiven in comments section? [__] __ __

Here footnotes indicated on cover page usedcorrectly vith final data? [__] __ __

Were any samples diluted beyond requirementsof contract? __ [__] __

if yes, were dilution* noted on Form Is? [__3 __ __

ACTION: If no for any of above, note undernon-compliance of data assessmentnarrative.

A.1.4 Holding Times -

Mercury (28 days) . . . . . . . . . . . . .exceeded? __ [__] __

Cyanide (14 days) . . . . . . . . . . . . . exceeded? __ [__] __

Other Metals (6 months) .......exceeded? __ [__] __

Which parameters?_________________

ACTION; Prepare a list of all samples andanalytes for which holding timeshave been exceeded, specify thenumber of days from date ofcollection to the date of analysis(from raw data). Attach a checklist.

If yes, reject (red-line) values less thanInstrument Detection Limit ( IDL) flag asestimated (J) those values above IDL.

A.1.5 Rav Data

A. 1.5.1 Digestion Log* for flame AA/ICP present? [__] __ __

Digestion Log for furnace AA present? [__] __ __

Digestion Log for mercury present? [__] __ __Digestion Log for cyanides present? [__] __ __

* Weights, dilutions and volumes used to

Gofder Associates

Title: Evaluation of Metals Data Revision:Data Assessment Data:

(Total Review - Inorganics) Page:

obtain values.

Nfi

Percent solids calculation present forsoil (sediments)? [ __ ]

Are preparation dates present onDigestion Log? [ __ ]

A. 1.5. 2 Measurement read out record present?[ __ ]

Flame AA [ __ j

Furnace AA [ __ ]

Mercury [ __ ]

Cyanides [ __ ]

A. 1.5. 3 Are all rav data to support all sampleanalyses and QC operations present? [ __ ]

Legible? [ __ ]

Properly Labeled? [ __ ]

ACTION: If no for any of above, writeTelephone Memorandum and contactlaboratory.

A. 1.5. 4 Is record of at least 2 point calibrationpresent for ICP? [ __ ]

Is record of 4 point calibrationpresent for: Flame AA? [ __ ]

Furnace AA? [ __ ]

NOTE i If less than 4, other standards mustbe run immediately aftar calibration and be± 5% of true value.

ACTION: Flag associated data if standardsare not within ±5% of true values.

Golder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Motals Data Revision:

Data Ass«s*Mnt Data:(Total Review - Inorganics) Page:

i l l N O

Is record of 4 point calibration present for:Mercury? [__]

Cyanide? [__]

ACTION; If no for any of the above, prepareTelephone Memorandum and contactlaboratory.

A. 1.6 Data Validation and Verification

A.1.6.1 Form II (Initial and ContinuingCalibration Verification! -

A.1.6.l.l Present and complete for every aetaland cyanide? [__]

Present and complete for AA and ICP whenboth are used for same analyte? [__]

ACTION; If no for any of the above/ prepareTelephone Mamoraadum and contactlaboratory*

A.1.6.1.2 Circle all values on data summary sheetthat are outside of windows. Are allcalibration standards (initial andcontinuing) within control limits?

Metals 90-110% [__]

Hg and sn ao-120% [__]Cyanides 85-115% [__]

Are all calibration standards (initial andcontinuing) within 50-150%? [__]

ACTIONi Flag as estimated (J) all positivedata (not flagged with a "U")analysed between a calibrationstandard of 50-«f% (50-79% for Hg)or 111-150% (121-150% for Rg)recovery and nearest adjacentcalibration standards, flag asestimated (J) all positive cyanidedata if calibration standards are

Golder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Data:(Total Review - Inorganics) Page:

X f i S N Q H Z S

between 50-64% or 116-150%. Reject(red-line) as unacceptable data ifrecovery of calibration standard isbelow 50% or above 150% for nearestadjacent standards.

was continuing calibration performed every10 samples or every 2 hours? [__3 __ __ACTION: If no, flag the excess samples

(eleventh and up) data asestimated (J).

A.1.6.2 Form III (Initial and ContinuingCalibration Blanks)

A.1.6.2.1 Present and complete? [__] __ __

For both AA and ICP when both areused for same analyte? [__] __ __

ACTION; If no, prepare TelephoneMemorandum and contact laboratory

A.1.6.2.2 circle all calibration blank values onData Summary Sheet that are above IDL.Are all calibration blanks less thancontract Required Detection Limits(RDL)? [__] __ __

Are all calibration blanks less thanInstrument Detection Limit (if IDL>RDL)when sample concentrations are greaterthan 2XIDL? [__] __ __

ACTION; If no for any of above flag asestimated (J) on form I'S all databetween calibration blank with valueover RDL or IDL and nearest adjacentcalibration blank.

A. 1.6-2.3 Was an initial calibration blankanalysed? [__] __ __

Was a continuing calibration blankanalyzed after every 10 samples or every2 hours (whichever is more frequent)? [__] __ __

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

. Data Assessment Date:(Total Review - inorganics) Page:

HP.

ACTION; If no, flag as estimated (J) allvalues not analyzed within 5 samplesof calibration blank.

A.1.6.3 FORM III (Preparation Blank)

A.1.6.3.1 Was one prep, blank analyzed for:•ach 20 samples? [__] __

each batch? [__] __

aach matrix type? [__] __

For both AA and ICP when both are usedfor same analyte? [__] __

ACTION; If no for any of above, flag asestimated (J) all associated datafor which prep, blank was notanalyzed.NOTE: If only one blank was analyzedfor more than 20 samples, then first20 samples analyzed do not have to beflagged as estimated (J).

A.1.6.3.2 Do concentrations of prep, blank fallbelow two times ZDL when IDL is greaterthan RDL? [__] __

ACTION; If no, reject (red-line) all datathat has a concentration less than10 times the prep, blank value, butnot flagged with a "U" (less than).

(Note: The preparation blank for mercury isthe same as the calibration blank.)

A.1.6.3.3 Is concentration of prep, blank greaterthan RDL when ZDL is less than RDL? __ [__]

If yes, is the concentration of thesample with the least concentratedanalyte less than 10 times the prep.blank value? __ [__]

ACTION; If yes, reject (red-line) allassociated data that has a con-

Colder Associates

STANDARD OPERATING P ROC ED ORB Section:Title: Evaluation of Metals Data Revision:

Data Assessment Date:(Total Review - Inorganics) Page:

xEl KQ N/A

centration less than ten tines theprep, blank value, but not flaggedwith a "U" (less than).

A. 1.6. 4 Form IV ftCP Interference checfc

A. 1.6. 4.1 Present and complete? [ __ ]

(Note: Not required for furnace AA,flame AA, mercury/ and cyanide.)

A. 1.6. 4. 2 circle all values on Data summary Sheetthat are more than ± 20% of true orestablished mean-value* Are allinterference Check Sample results insideof control limits (± 20%)? [ __ ]

ACTION: if no, flag as estimated (J) thosesample results for which ICS recoveryis between 50~7f% or 121-150% of meanvalue; and reject (red-line) thosesample results for which ICS recoveryis less than 50%. If ICS recovery isabove 150%, reject positive resultsonly (not flagged with a "U") .

A. 1.6. 5 Form IX fICP Serial Dilution)

A. 1.6. 5.1 Was Serial Dilution analysis performed for:each 20 samples? [ __ ] __

each matrix type? [ __ 3 __

•ach concentration range (i.«. low, [ __ ] __med. , high)?

If no for any of above, is any sample (s)concentration (undiluted) greater than10 x IDL? __ [ __ ]

ACTION; If yes, flag ell associated dataas estimated (J) for which SerialDilution Analysis was not performed.

A. 1.6. 5. 2 Was field blanfc(s) used for SerialDilution Analysis?

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Date:(Total Review - inorganics) Page:

X f i l N O

If yes, was fiald blank described assuch on Traffic Raport? __ [__]

ACTION; If yes, flag all associatad data> 10 x IDL as estimated (J).

A.1.6.5.3 circla all valuas on Data Sunaary Sbaatwith a parcant diffaranca graatar tban10%. Ara all ICP Serial Dilution rasultswithin control limit of 10%. [__] __

If no, ara all assooiatad data on Form I'sflaggad with an "B«? [__] __

ACTION; If not flaggad with an "E", flagas astimatad (J) all associatadsampla rasults for which parcantdiffaranca is graatar than 10% butlass than 100%; rajact (rad-Una) allassociatad sampla rasults for whichPD is abova 100%.

A.1.6.6 Porn V (Spike ffasjpja Recovery) - (Nota:Not raquirad for Ca, Kg, X, and Na(both matrices), Al, and Fa (soil only)).

A. 1.6. 6.1 Present and complata for: each 20 samples? [__] __

aach matrix type? [__] __

aach cone, ranga (i.a. low, mad., high)? [__] __

For both AA and ICP whan both are usad forsame analyte? [__] __

ACTION; If no for any of abova, flag asastimatad (J) all data for whichspiked sampla vas not analyzed.VOTE: If ona spiked sample wasanalyzed for more than 20 samples,tban first 20 samples analyzed donot have to ba flaggad as astimatad (J).

Qoldar Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Date:(Total Review - Inorganics) Page:

SSs is N/A

A.1.6.6.2 Was field blank used for spiked sample? [__] __ __

If yes, was field blank described assuch on Traffic Report? [__] __ __

ACTION: If yes, flag all positive data asestimated (J) for which field blankwas used as spiked sample.

A. 1 .6 .6 .3 Circle all values on Data Summary Sheetthat are outside of control limits(75% to 125%). Are all recoverieswithin control limits? [__] __ __

If no, is sample concentration greaterthan four times spike concentration? [__] __ __

ACTION; If yes, disregard spike recoveriesfor analytas whose concentrations aregreater than four times spike added.If no, circle those analytes onForm V for which sample concentrationwas not greater than four times thespike concentration.

A . 1 . 6 . 6 . 4 Aqueous

Are any spike recoveries:(a) less than 30%? __ [__] __

(b) between 30-74%? __ [__] __

(c) between 126-150%? __ [__] __

(d) graater than 150% __ [__] __

ACTION: If less than 30%, reject allassociated aqueous data. Ifbetween 12«-150%, flag as estimated(J). If between 126-150%, flag asestimated (J) all associated aqueousdata not flagged with a "U". Ifgreater than 150%, reject (red-line)all associated aqueous data notflagged with a "U",

A.1.6.6.5 Soil/Sediment

Goldtr Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metal a Data Revision:

Data Assessment Date:(Total Review - Inorganics) Page:

HIHo

Are any recoveries (a) less than 75%? __ [ __ j

(b) greater than 125%? __ [ __ j

ACTIOH; If less than 75%, flag all associateddata as estimated (J) . If greaterthan 125%, flag as estimated (J) allassociated data not flagged with a "U".

A. 1.6. 7 Fora VI (Lab Duplicates i

A. 1.6. 7.1 Present and complete for:

each 20 samples? [ __ j __

each matrix type? [ __ j __

each concen. range (i.e. low, [ __ j __ned. , high)?

For both AA and ICP when both areused for same analyte? [ __ ] __

ACTION; If no for any above, flag asestimated (J) all data >RDL forwhich duplicate sample was notanalyzed. Mote; If one duplicatesample was analysed for more than20 samples, then first 20 samplesanalyzed do not have to be flaggedas estimated (J) .

A. 1.6. 7. 2 Circle all values on Data Summary Sheetthat are outside control limits:

Aqueous Samples (a) 20% RPD or

(b) RDL

Are all values within control limits? [ __ ] __

If no, are all results outside thecontrol limits flagged with an * onForm I's and VI? [ __ ] __

ACTION; If no, write in the contract

Qoider Associates

STANDARD OPERATING FROC2DUM Saction:Titla: Evaluation of Metala Data Revision:

Data Assessment Data:(Total Review - Inorganic*) Page:

SH NO K/A

problems/non-compliance sactionof narrativa.

A.1.6.7.3 Was field blank used for duplicataanalysis? __ [__] __

If yes, vas fiald blank idantifiadas such on Traffic Raport? __ [__] __

ACTION; If yas, flag all data >RDL as•stimatad (J) for which fialdblank vas usad a* duplicata.

A. 1.6.7.4 Is »NC" reported in RFD column for anysanpla duplicata pair where aitharvalue is lass than RDL? [__] __ __

ACTION; If no, vrita in "NC" with rad pancilon fora vi and iaitial. Nota undarData Acceptability Narrativa(non-compliance).

A. 1.6.7.5 is any valua for sample duplicata pairlass than RDL and othar valua greaterthan 10 x RDL. __ [__] __

ACTION; If yas, rajact associated data.

A.1.6.7.6 Aqueous

Is any RFD graatar than 50% where sampleand duplicata ara both graatar thanfiva tines RDL? __ [__] __

is any difference between sample andduplicate graatar than RDL wheresaapla and/or duplicate) is less than5 times RDL but graatar than RDL? __ [__] __

ACTIONI if yes, rajaet (rad-line) allassociated data*

A.1.6.7.7 Soil/Sediment

Is any RPD greater than 100% wheresample and duplicata ara both greaterthan'5 times RDL? [__J

Golder Associates

STANDARD OPERATING PROCEOOU Saction:Title: Evaluation of Metala Data Revision:

Data Assesaaaat Data:(Total Review - Inorganics) Page:

2H UQ N/A

Is any differenca between saapla andduplicata graatar than 2 tiaas RDLvbara saapla and/or duplicata is lassthan 5 tiaas RDL but graatar than RDL? __ [__

ACTION; If yes, rajaet (red-line) allassoeiatad data,

A.1.6.a Piald Duplicate*

A. 1.6.8.1 Wara fiald duplicatas analyzad? [__]

ACTION; If yes, prapara a Fora VI foreach saapla duplicate pair,calculate RPD where both valuesare greater than RDL.

NOTE: Reject (red-line) all associateddata for fiald duplicates only.

A.1.6.8.2 Circle all values en Form vi for 7. oup,that are outside control limits;

Aqueous samples (a) 20% RPD or(b) RDL

Are all values vitbia control limits? [__]

A. 1.6.8.3 Report "NC" in RPD column for a sampleduplicate pair where either value isless than RDL.

A.1.6.8.4 Is any value for sample duplicate pairless than RDL and other value greaterthan 10 x RDL? __ [__j

ACTION; If yes, reject associated data.

A.1.6.8.5 Aqueous

Is any RPD greatar than 50% where sampleand duplicate are both greater than 5times RDL? __ [__j

Is any difference batvaen sample andduplicate greater than RDL where sample

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Data:(Total Review - Inorganics) Pages

NO

and/or duplicate is lass than 5 timesRDL but greater than RDL? __ [ __ ]

ACTION; If yes, raj act (red-line) allassociated data.

A. 1.6. 8. 6 Soil/Sediment

Is any RPD graatar than 100% where sampleand duplicate are both greater than 5tines RDL? __ [ __ ]

Is any difference between sample andduplicate greater than 2 times RDL wheresample and/or duplicate is less than 5times RDL but greater than RDL? __ [ __ ]

ACTION; If yes, reject (red-line) allassociated data.

A. 1.6. 9 rorm VII (Instrument Detection Limits) -(Note; IDL - not required for cyanide.)

A. 1.6. 9.1 Are IDLS present for all analytes? [ __ ] __

For both AA and ICP when both are usedfor same analyte? [ __ ] __

ACTION; If no for any of above, prepareTelephone Memorandum and contactlaboratory.

A. 1.6. 9. 2 Is IDL greater than RDL for any analyte? __ [ __ ]

If yes, is the concentration of the sampleanalyaed on the instrument whose IDL exceedsRDL, greater than two times IDL. [ __ ] __

ACTION: If no, reject (redline) all values lessthan two times IDL of the instrument whoseIDL exceeds RDL.

A. 1.6. 10 Fora VJI (laboratory Control(Note; LCS - not required for aqueous Rg.)

A. 1.6. 10.1 Was one LCS prepared and analyzed for:every 20 water samples? [ __ ]

Golder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Data:(Total Review - Inorganics) Page:

__ — __

•very month for solid saaples? [__] __ __

for both AA and ICP whan both ara uaad forsana analyta? [__] __ __

ACTION; If no for any of above, praparaTelephone Memorandum and contactcontact laboratory for subaittal ofaonthly results of solid LCS. Flagas estimated (J) all aqueous datafor which LCS vaa not analysed.

NOTE: If only one LCS was analysed for morethan 20 samples, than first 20 saaplesclose to LCS do not have to be flaggedas estimated.

A.1.6.10.2 circle all LCS values outside of controllimits (80% to 120%) on Data Summary Sheet.

Is any LCS value: less than 50%? __ [__] __

between 50% and 79%? __ [__j __

between 121% and 150%? __ [__] __

greater than 150%? __ [__j __

ACTION; Less than 50%, reject (red-line)all data; between 50% to 79%, flagall associated data as estimated (J) ;between 121% to 150%, flag all positive(not flagged with a "U") results asestimated; greater than 150%, rejectall positive results.

A. 1.6.10.3 is "NC" reported for an analyte in % Rcolumn of Form VXl? __ [__] __

If yes, does concentration of the analytefall within acceptable range of LCS? [__] __ __

ACTION; If no, flag associated data asestimated (J).

A.1.6.11 Furnace Atomic Absorption (AA) PC Analysis

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data. Assessment Date:(Total Review - Inorganics) Page:

3 1 N O N / A

A. 1.6-ll.l Ars duplicate injections present infurnace raw data (except during fullMethod of Standard Addition) for eachsample analysed by QFAA? [__] __

ACTION; If no, reject the data on Form I'sfor which duplicate injectionsvere not performed.

A. 1.6* 11.2 Is post digestion spike recovery lessthan 10% for any result? __ [__3

ACTION; If yes, reject (red-line) theaffected data.

A. 1.6.11.3 Do the duplicate injection readings agreewithin 20% Relative Standard Deviation(RSD) or coefficient of variation (CV)for concentration greater than RDL? [__] __

Was a dilution analysed for sample withpost digestion spike recovery lessthan 40%? [__] __

ACTION; If no for any of the above, flagall the associated data as estimated( J ) .

A.1.6.12 Form VIII (Method of StandardAddition Results)

A.1.6.12.1 Present? [__] __

If no, is any Form I result codedwith »S« or a »+»? __ [__]

ACTION; If yes, write request on TelephoneMemorandum and contact laboratoryfor submittal of rent vill.

A. 1.6.12.2 was MSA required for any sample butnot performed? __ [__]

Is coefficient of correlation for MSAless than 0.995? [ ]

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data, Revision: .

Data Assessment Data:(Total Review - laorganica) Page:

__ _ __

ACTION: If y«s for any of above, flag allassociated data as estimated (J) .

A. 1.6.12.3 Is coafficiant of correlation for MSAlass than 0.990 for any sample? __ [__] __

ACTION; If yes, reject (red-line) affecteddata.

A.1.6.12.4 Was proper quantitation procedurefollowed correctly? [__] __ __

ACTION: If no, note exception under contractproblem/non-compliance of dataassessment narrative, or prepare aseparate list.

A.1.6.12.5 Are MSA calculations within the linearrange of the calibration curve generatedat the beginning of the analytical run? [__] __ __

ACTION! If no, flag all affected data asestimated (J).

A.1.6.13 Dissolved Inorganics

A. 1.6.13.1 Were any analyse* performed fordissolved as well as total analyteson the same sample? __ [__] __

If yes, apply the following questionsonly if both dissolved and total con-stituents are above RDL (For SASparameters: above 5 * IDL) .

A. 1.6.13.2 Is the concentration of any dissolvedanalyte greater than its total con-centration by more than 10%? __ [__] __

A. 1.6.13*3 Is the concentration of any dissolvedanalyte greater than its total con-centration by more than 50%? __ [__] __

ACTION; Prepare a list comparing differencesbetween all dissolved and totalanalytes. Compute the differencesas a percent of the total analyte

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Data:(Total Review - Inorganics) Page:

5 H N O N / A

only whan both above RDL (5 * IDLfor SAS parameters). If more than10%, flag both dissolved and totalvalues as estimated (J); if more than50%, reject (red-line) the data forboth values.

A.1.6.14 Form I to IX

A. 1.6.14.1 Are all the Form I through Torn IXlabeled with: CRL Type sample number? [__] __ __

Site sample number? [__J __ __

Lab ID sample number? [__] __ __

QC report number? [__] __ __

date? [__] __ __

correct units? [__] __ __

matrix? [__] __ __

ACTION; If no for any of above, note undercontract problem/non-complianceof data assessment, narrative.

A.1.6.14.2 Do any computation/transcription errorsexceed 10% of reported values on FormsI-IX for:

(NOTE; Check all forma against rav data.)

(a) all analytes analyzed by ICP? __ [__] __

(b) all analytes analyzed by GFAA? __ [__J __

(c) all analytes analyzed by AA Flame? __ [__] __

(d) Mercury? __ [__] __(e) cyanide? __ [__] __

ACTION; If yes, prepare Telephone Memorandum,contact laboratory for corrected dataand correct errors with red pencil

Colder Associates

STANDARD OPERATING PROCEDURE Section:Title: Evaluation of Metals Data Revision:

Data Assessment Date:(Total Review - Inorganics) Page:

__ __ __

and initial.

A. 1.6. 15 Form I (Field Blank) - Do concentration offield blanks fall below two tines IDL forall aqueous and soil parameters? [ __ ] __ __

If no, was field blank value alreadyrejected due to other QC criteria? [ __ ] __ __

ACTION; If no, reject (red-line) all aqueousand soil/sediment data (except fieldblank) that has a concentration lessthan five times the field blank valuenot flagged with a "U" (less than).

A. 1.6. IS Form XI. XII, XIII (Quarterly Verificationof instrument

A. 1.6. 16.1 Is quarterly verification report presentin MMB file for:

Instrument Detection Limits? [ __ ] __

ICP Interelement Correction Factors? [ __ 3 __

ICP Linear Ranges? [ __ ] __

ACTION; If no, contact York Laboratories.

A. 1.6. 16. 2 Was any sample result higher thanlinear range of ICP by more than lo%? __ [ __ ]

Was any sample result higher thanhighest calibration standard fornon-ICP parameters? __ [ __ ]

ACTION: If yes for any of the above, flagresult reported on Fora I asestimated (J) *

Golder Associates

STANDARD OPERATING PROCEDURE

Evaluation of Metals DataData Acceptability

Section:Revision:Date:Page:

Site

Lab

Matrix: Soil

water,

other

A.2.1 Are all data of acceptable quality? Yes, No

If no, list exceptions with reason(s) for rejection orqualification as estimated value (J) .

Colder Associates

STANDARD OPERATING PROCEDURE Section:Revision;

Evaluation of Mettals Data Data:Data Acceptability

A.2.1 (continuation)

A. 2.2 Problems/Non-complianca

Solder R«vi*w«r:__________________________ Date

Colder Associates

STANDARD OPERATING PROCEDORES Section:Revision:

Evaluation of Metal* Data DatexNon-compliance Report Page:

NON-COMPLIANCE REPORT

CASE NO.

The hardcopied (laboratory name) ________________________^inorganic data package received at Golder Associates Inc. has beenreviewed and the quality assurance and performance data summarized.The data review included:

Site Sample No.:__________________________________._______

CRL Type Sample No.:

Cone. £ Matrix:___

The general criteria used to determine the performance were basedon an examination of:

o Data Completeness o Duplicate Analysis Resultso Matrix Spike Results o Blank Analysis Resultso Calibration Standards Results o MSA Results

Items of non-compliance with the above contract are describedbelow.

Comments:

Reviewer's Initial Date

Golder Associates

STANDARD OPERATING PROCEDURE Saction:Ravision:

Evaluation of Matals Data Data*Mailing List Pagas

MAILING LIST FOR DATA REVIEW RECIPIENTS

1. Jaffray J. Larson, L.A.radaral Sita Projact ManagarDivision of Land Pollution Control2200 Churchill Roadp. o. Box 1927*Springfiald, Illinois 62794-9276

2. U.S. EPA Ragioa V - Tinka Hyda

3. U.S. EPA V QAPP MANAGER ______________

4. IEPA QAPP MANAGER ____________________

QoMar Associates

STANDARD OPERATING PROCEDURE Section:Raviaion:

Evaluation of Matala Data Data*Suaaary of QC Data Paga:

VPPENDIX A.5 SUMMARY OF INORGANICS QUALITY CONTROL DATA

LABORATORY: CASE NO. SOW NO. .SAMPLE TYPE:

3ITE STUDY DESCRIPTION: SAMPLE NOS:

FIELD BLANK SAMPLE NO. FIELD DUP. #'S: .LAB DUP. f«8:

MATRIX SPIKE f*S: .COMPLETION DATE: REVIEWERS IHITIALSz_

VII III VI III II IV V VII IX

P B Lab.Para- UG L r 1 Pup.latar a *

calibration Calib. Var. ICP IT? M s_ Blanfca________\ R chacfc t p LCS Sar Fialdc Cont»d coat*d r i % R oil Blank

CRDL ID o n PD Lim Init 123 IMIT 123 INIT TIN x te

"M.Sb

200

60

10

200

5000

10

GO 50

25

Fa 100

QoMar Associates

STANDARD OPERATING PROCEDURE tf«CCiOn:Revision:

Evaluation of M«tals Data Data:suaaary of QC Data Pages

— )1

5000

ta____is.

5000

Ma 5000

ifiL

ifl.

Ifl.

Qoldtr Associates

STANDARD OPERATING PROCEDURE Section:Revision:

. CLP Type Data Acceptability Date:Summary form (Inorganics) Page:

CLP TYPE DATA ACCEPTABILITY SUMMARY FORM (INORGANICS)

rype of Review:________________________Data:_____________Case I:

Site:_______________________________Lab Name:__________________

•leviewer's Initials:_______________________ Number of Samples:

Analvtes Rejected Due to Exceeding Review Criteria:*

Holding Calibra- Prep Field Inter- spike Duplicate DetectionTimes tion Blank Blank ferences Recovery Lab Field Limits I

CCP ______/lame AA _Furnace AA.

TotalOther

Analytes Flagged as Estimated (J) Due to Exceeding criteria For:*

ICP____.'lane AA.furnace AA.Mercuryotal____

Mther____

_ Mote: Asterisk (*) indicates additional exceedances of review criteria.

Colder Associates

STANDARD OPERATING PROCEDURE

: Saapla identification

Section:Revision;DatotPag*:

SAMPLE IDENTIFICATION SUMMARY SHEET5it« Nam«:

Laboratory:

Conntnts:

Colder Associates

ATTACHMENT VII

SOP FOR GLASSWARE PREPARATION

Section NO. 1.3Revision No. 1Date: June 12, 1986Page 1 of 7

Glassware Preparation SOP 1.3: Preparing SampleSaver Glassware

The SampleSaver contains 5 different kinds of glassware. The proceduresfor preparing this glassware follow. Even though they all go Into one con-

tainer, they are all prepared differently. They are not prepared with otherlaboratory glassware because their preparation procedures are different.

Organic* - 1-liter glass bottles

NOTE: New liter bottles are washed 1n the dishwasher, rinsed, drainedand dried, Recyled liter bottles are washed 1n hot, soapy water,

-" rinsed, drained, and dried,1. Wash Mn dishwasher or

a. Wash 1n hot, soapy water andb. Rinse well with tap water.

2. Rinse twice with delonlzed water.3. Invert and drain,4. Sake at 450-500'F for one hour.5. Wash Teflon caps In the same manner (as 1n SOP 1.4).

\_ Metals and Mercury - 500 ml Plastic Bottles (Metals)1. Wash in dishwasher or hand wash with hot, soapy water.2. Rinse three times with tap water.3. Rinse three times with delonlzed water.4. Invert on counter-top for drying.5. Wash caps per SOP 1.4.

Volatile*.- 40 ml glass bottles (Cyanide and Phenols)1. Wash in dishwasher.

2. Rinse twice with delonlzed water.

Section No. 1.3Revision No. 1Date: June 12, 1986Page 2 of 7

3. Place 1n oven at 500'F for 1 hour. Remove to volatile* area tocool. Cap Immediately after they are cool enough to touch.

4. Caps and septa should be washed and dried per SOP 1.4.

Glassware Quality Control CheckQuality Assurance monitors the SampleSaver glassware to ensure that the

glassware 1s not contaminated. This monitoring process Is conducted In thefollowing ways for each type of glassware.

Quality Control of VOA Bottles (40 mj_ glass bottles); Checked for VolatileCompounds ConunTfaaTTon

After the bottles are taken out of the oven, they are allowed to cool 1nthe "Unapproved" storage cabinet 1n the volatile prep area. After they arecool, they are capped and put Into boxes (72 per box), which are called batches.The boxes are stored in the cabinet marked "Unapproved."

The SampleSaver Custodian completes the "VOA Glasswre Prep Batch Check"

(See Example 1 at the end of these SOPs), assigns a number to the bottle(numbers are consecutive and ascending), and removes one bottle from the batch.

The Custodian then moves the box to the storage cabinet marked "UnderEvaluation1* and attaches a copy of the Batch Check sheet to the box. He/Shealso notes on the Batch Check sheet that the results of the analysis areto be sent to Quality Assurance.

He/She then delivers the bottle to be tested to the Manager of theVolatlles Laboratory. In this way, there 1s a record of the testing, the bottlehas a unique number, this number 1s associated with the batch of bottles with

Section No. 1.3Revision No, 1Date: June 12. 1986Page 3 of 7

which u 1s processed, and the results are forwarded directly to Quality

Assurance. Quality Assurance maintains a file containing copies of all BatchChecksheets, Including which batches have passed and which have not. This fileserves as the ongoing documentation of this process.

The Manager of the Volatile* Laboratory tests the bottle for volatile com-pounds and forwards the results to Quality Assurance.

The Quality Assurance Specialist determines 1f the bottle's analysis Indi-cates any contamination. If the analysis detects any volatile compound at one-half the detection limit for that compound, another VGA bottle from the same

*batch 1s tested. If the second bottle 1s also found to be contaminated, the QASpecialist notifies the Supervisor of Sample Preparation, and the entire batch1s reprocessed. If the analysis Indicates no contamination Is present, theSupervisor of Sample Preparation moves the batch to a storage cabinet label ltd"Approved," which indicates that the bottles are free of contamination and canbe Included 1n the S&mpeSavers shipped to clients. The QA Specialist advisesthe Vice President of Quality Assurance 1f there are persistent or frequentproblems with the glassware preparation process. When VOAs are needed, they aretaken from the storage cabinet marked 'Approved."

Quality Control of liter Bottles; Checked for Organic Compounds ContaminationFifty, liter bottles are furnaced together and are called a batch. After

the bottles are taken out of the oven, they are allowed to cool 1n the"Unapprov«d" storage cabinet located 1n the Glass Prep area. One bottle out ofeach batch 1s tested for organic compounds contamination.

Section No. 1.3Revision NO, 1Date: June 12. 1986Page 4 of 7

The Supervisor of tht Sample Preparation Laboratory completes a "SVGlassware Prep Batch Check" (See Example I at the end of this SOP), which Indi-cates that the test results are forwarded to Quality Assurance, (numbers areconsecutive and mending), and removes one bottle from the batch. TheSupervisor then moves the batch to the storage cabinet In the Sample Prep areamarked 'Under Evaluation" and attaches a copy of the Batch Check to the batch.

«•

He/She also notes in writing on the Worksheet that the results of the analysis

are to be sent to Quality Assurance.- In this way, there 1s a record of the testing, the bottle has a unique

testing number, this number Is associated with the batch of bottles with which

U was processed, and the results are forwarded directly to Quality Assurance.^

f The Supervisor of the Sample Preparation Laboratory keeps a notebook containing

copies of -ill Batch Check sheets, Including which batches have passed and whichhave not. This notebook 1s called the Quality Control For SampleSaver and ser-ves as the ongoing documentation of this process.

The Supervisor of the Sample Preparation Laboratory fills the bottle with'~ distilled, deionized water, assigns It a CompuChem number,

and indicates 1n the comments section that this bottle is used as a QC samplefor a SampleSaver check. The water It then extracted as an acid and base

neutral blank and analyzed by GC/MS. A portion of the B/N fraction Is exchangedto Hcxani and analyzed by GC. The results are quantfteted and forwarded to QA.

The Quality Assurance Specialist determines 1f the bottle's analysis Indi-cates any contamination. If the analysis detects any extraneous peaks (peaksother than the surrogates), another liter bottle from the same batch 1s tested.

Section No. 1.3Revision No. 1Date: June 12. 1986Page 5 of 7

If the second bottle 1s also found to be contaminated, the QA specialist noti-fies the Supervisor of Sample Preparation, and the entire batch Is reprocessed.

If the analysis Indicates no contamination 1s present, the Supervisor of Sample

Preparation 1s notified and the batch 1s moved to a storage cabinet labeled•+

•Approved", located 1n the Sample Receiving area, which Indicates the bottles arefree of contamination and can be Included 1n the SampleSavers shipped toclients. The QA Specialist advises the Director of Quality Assurance If thereare persistent or frequent problems with the glassware preparation process.

When liter bottles are needed, they are taken from the storage cabineti

marked "Approved."^

( Quality Control of Plastic Bottles (500 ml); Checked for Inorganicsv contamination (HetaTsT

Fifty, plastic bottles are dried together and are called a batch. After<

the bottles are taken out of the oven, they are put in the "Unapproved" storage^

area located in the Glassware Prep area. One out of each batch Is tested formetals contamination.

When bottles are needed, the Supervisor of the Sample PreparationLaboratory completes an "Order Form For Test Samples" (see Example 3 at the endof these SOPs), checks "glassware check" as the reason for initiating the test(which also Indicates that the test results are forwarded to Quality Assurance),

— assigns a number to the bottle (numbers are consecutive and ascending), and

removes one bottle from the batch. The Supervisor then moves the batch to the~~ storage cabinet marked "Under Evaluation" 1n Sample Receiving and attaches a

Section NO. 1.3Revision No. 1Date: June 12, 1986Page 6 of 7

copy of the Worksheet to the batch. He/She also notes In writing on the

Worksheet that the results of the analysis are to be sent to Quality Assurance.In this way, there 1s a record of the testing, the bottle has a unique

testing number, this number 1s associated with the batch of bottles with which1t was processed, and the results are forwarded directly to Quality Assurance.The Supervisor of the Sample Preparation Laboratory keeps a notebook containingcopies of all Forms, Including which batches have passed and which have not.This notebook is called the Quality Control for SampleSaver and serves as theongoing documentation of this process.

The Supervisor of the Simple Preparation Laboratory fills the bottle with

d1tt1lled/de1oni2ed water, assigns 1t a CompuChem number, and Indicates In thecomments section that this r>ottle1s used as a QC sample for a SampleSaver check. He/She tikes the bottle to the

Inorganics Laboratory, where it 1s analyzed for all metals, the results arequantltated, and forwarded to QA.

The Quality Assurance Specialist determines 1f the bottle's analysis 1n<cates any contamination. If the analysis Indicates contamination another frfrom the same batch 1s tested. If the second bottle 1s also found to be 'tamln*ted, the QA Specialist notifies the Supervisor of Sample Preparat*the entire batch 1$ reprocessed. If the analysis Indicates no contamlpresent, tht Supervisor of Sample Preparation 1s notified and the btto a storage cabinet labeled "Approved", which Indicates that the

free of contamination and can be Included In the SampleSavers it

Section No. 1.3Revision No. 1Date: June 12, 1986Page 7 of 7

clients. The QA Specialist advises the Vice President of Quality Assurance ifthere are persistent or frequent problems with the glassware preparation pro-

cess.

When bottles are needed for cyanide and phenols, they are taken from the

storage cabinet marked "Approved."

ATTACHMENT VIII

COLDER ASSOCIATES1 SOILS LABORATORYCHAIN-OF-CUSTODY PROCEDURES

Yeoman CreekSection No.: Atchmnt VIIIRevision No.: 1Date: 4/2/91Page: 1 of 4

COLDER ASSOCIATES' SOILS LABORATORYCHAIN-OF-CUSTODY PROCEDURES

Scope and Application: This chain-of-custody procedure appliesto the handling and tracking of soilsamples within a geotechnical laboratoryof Colder Associates, Inc.

Sample Receipt: Field personnel will notify the laboratorymanager prior to shipping samples to thelaboratory for geotechnical analysis.

Samples from a hazardous site shall belabelled with a red tag in addition to thestandard sample label. This tag will alertthe laboratory technician responsible forlogging in the samples to open the sampleshuttle under a hood and subsequently routethe samples to the hazardous waste area ofthe laboratory. Samples identified with a redtag will be handled as described in the ColderAssociates' Laboratory Safety Manual andChemical Hygiene Plan.

Samples arriving at the laboratory forgeotechnical analyses shall also be identifiedby the standard sample tags (as described inSection 6.0 of the QAPP, Volume III) andaccompanied by Chain-of-Custody forms. Chain-of-Custody forms shall be signed and routed tothe project file as appropriate.

Labelling of sample tags and containers willbe checked and completed, if necessary, suchthat:

1. All samples are to be identified with theproject number, short name, samplenumber(s), and project location.

2. Jar samples will have the standard jarlabels (with the details filled in)attached to the side of the j ar. Thesample jars will be arranged in sequencein a compartmented cardboard box. The

Goldtr Associates

Yeoman CreekSection No.: Atchmnt VIIIRevision No.: 1Date: 4/2/91Page: 2 of 4

box will be clearly marked on the outsideas to the project name, project number,borehole number, and enclosed samplenumbers.

3. Each Shelby tube sample or individualrocK sample will have the requiredidentification either written on thesample or on a label that is securelyattached to the sample.

4. Bag or bulk samples will be placed inbuckets which will have the requiredidentification on the outside of thecontainer and on a label that is placedon the inside of the container with thesample.

5. Rock core boxes will be marked on the topof the box with the requiredidentification plus the box number, totalnumber of boxes, and the core run lengthin the box. Both ends will have theproj ect j ob number, boring number, boxnumber, and total number of boxes.

Sample Log-In: Incoming samples shall be logged in on a SampleTracking Record Form (Figure 1) and on theLaboratory Schedule Board. Upon completion of theSample Tracking Record Form, samples shall berouted to separate controlled storage areas withinthe hazardous waste section of the laboratorypending performance of the required analyses.

Sample Analysis: The laboratory technician assigned to performthe required analyses will retrieve thenecessary samples from the controlled storagearea immediately prior to performance of thelaboratory testing. The laboratory technicianperforming the analytical work will beresponsible for maintaining sampleidentification, following sample custodyprocedures throughout analysis, anddocumenting results.

Copies of the Sample Tracking Record Form andthe Chain-of-Custody Form shall accompany eachsample through analysis.

Colder Associates

Yeoman creekSection No.: Atchmnt VIIIRevision No.: iDate: 4/2/91Page: 3 of 4

Sample Storage after Testing: All residual sample materials shallbe collected and returned to propersample storage areas pendingimmediate return to the site orclient for disposal after alltesting is complete.

All discarding of samples will berecorded on the Sample TrackingRecord. The original will be sentto the pro j ect file with a copyretained in the laboratory proj ectfile.

Laboratory Records: All original laboratory records shall berouted to individual project files whencompleted, and consequently are subject to therecords management controls required by theData Management Plan.

(26010847.upl/cap)

Goldcr Associates

r rr

iM

RAF

TIN

Q A

IDE

S

aoa

;

i

SAMPLE TRACKING RECORD *.JOB NAUF- JOB NUMBER: 1 ORATION:

RAUPIFnHV: DATE! SHIPPED HY DATE:

SHIP FROM: SHIP TO: PRO.I MGR:

FIELD

SAMPLELOCATION

SAMPLENUMBER

SAMPLETYPE(1)

HAZARD(Z)

LABORATORY

DATESAMPLE

RECEIVEDRECEIVED

BYSAMPLE

CONDITION(3)

STORAGE

STORAGELOCATION

STORAGEDATE

PROJ.MGR.INT.

SHEET OF

DISPOSAL

DISPOSALDATE

PROJ. MGR.INT.

DISPOSALMETHOD

(4)

SPECIAL INSTRUCTION AND NOTES (5)

* THIS FORM IS FOR TRACKING SAMPLES THROUGH THE COLDER ASSOCIATES LABORATORY.ADDITIONAL DOCUMENTATION SHALL BE USED FOR SAMPLES SENT TO OTHER LABORATORIES.

(1) SAMPLES TYPES: J-JAH. T-TU9E. B-BAG. Cfl-CORE. W-WATEH. P-PAIL. GX-GEOTEXTILE. GM-GEOMEMBRANE. GN-GEONET (4) T.TRASH. C-OJENT PICKUP R-RETURN TO CLIENT O-OTHEH(2) CODE: C-CHECMICAL, R-RADtOACTIVE. E-EXTREME HAZARD (5) Sp£C(AL Rocy. . yog LABORATORY TEST(3) G-GOC». D-OAMAGED. W-UISSING ASSIGNMENTS, PACKING. STORAGE. OR DISPOSAL.

CLIENT/PROJECT

PRP/YEOMAN/ILLINOIS

DRAWN CHECKED 't£ft* REVIEWED(^>fr

0Golder AssociatesChicago, Illinois

DATE :4-2-91

ICALE JOB NO.N.T.S. 893-8O26.OI

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TITLE

SAMPLE TRACKING RECORD FORM

FILE NO.893-6026.01

DWG. NO.fREV. NO. FIGURE119 1