STAR System 2â„¢ - CEM Distributor Support

STAR System 2/6600121Rev. 3

Operation Manual

STAR System 2™and

STAR System 6™

Copyright 1997 by CEM CorporationAll Rights Reserved

This manual contains proprietary information which shall not be reproducedor transferred to other documents or disclosed to otherswithout prior written permission of CEM Corporation.

CEM is a registered trademark of CEM Corporation.

US Patent No. 5,796,080titled “Microwave Apparatus for Controlling Power Levels

in Individual Multiple Cells”

CEM CorporationMatthews, North Carolina 28106

(704) 821-7015 FAX: 704-821-7894e-mail: [email protected]

MANUFACTURED IN THE UNITED STATES OF AMERICA

600121Rev. 35/2001

STAR System 2/6600121Rev. 3i

Operating Precautions

The STAR System 2/6 must be grounded. In the event of an electricalshort circuit, grounding reduces the risk of electric shock by providingan escape wire for electric current. This instrument is equipped with acord having a grounding wire with a grounding plug. The plug must beplugged into an outlet that is properly installed and grounded. Consulta qualified electrician or service technician if the grounding instruc-tions are not completely understood or if doubt exists as to whetherthe instrument is properly grounded. If it is necessary to use an exten-sion cord, use only a 3-wire extension cord that has a 3-blade ground-ing plug and a 3-slot receptacle that will accept the plug from the in-strument. The marked rating of the extension cord must be equal to orgreater than the electrical rating of the instrument.

The possibility of instrument-induced electromagnetic interference(EMI) is minimal if the instrument is operated as outlined in this man-ual. The instrument should not be placed close to any electrical devicesusceptible to EMI. It is suggested by the manufacturer that the userpost a sign warning pacemaker wearers that a microwave device is inoperation. If the instrument is suspected of inducing EMI, a micro-wave leakage measurement should be performed as outlined on page52. Leakage measured above the legal limit of 5 mW/cm2 should be re-ported to the CEM Service Department.

This instrument utilizes high voltages and microwave radiation. Instru-ment service and repair should be performed only by those trained inrepair and maintenance of high voltage and microwave power systems.

Warnings, cautions and notes are included throughout this manual andshould be read thoroughly and strictly followed.

WARNING: A warning is inserted for essential information used to empha-size dangerous or hazardous conditions to the operation, cleaning and mainte-nance of the instrument which may result in personal injury.

CAUTION: A caution is inserted for essential information used to emphasizeprocedures which, if not strictly followed, may result in damage or destruc-tion to the instrument or improper instrument operation.

NOTE: A note is inserted for emphasis of procedures or conditions whichmay otherwise be misinterpreted or overlooked and to clarify possible confus-ing situations.

This instrument complies with United States Code of Federal Regulations(CFR) Title 21, Part 1030 for microwave leakage. A verification report is onfile.

This instrument complies with United States Code of Federal Regulations(CFR) Title 47, Federal Communications Commission (FCC) Part 18 – Indus-trial, Scientific and Medical (ISM) Equipment – emissions requirements. Averification report is on file.

The name “Teflon” is used throughout this manual. Teflon is a registered trademark of the E.I.DuPont Company.

STAR System 2/6600121Rev. 3

Introduction ..............................................................................................1

System Installation ..................................................................................3Tools Required .................................................................................3Accessories Required .......................................................................3Installaltion for Non-HF Use .........................................................3Installation for HF Use ...................................................................4Unpacking System Components ....................................................5Instrument Inspection ....................................................................6Instrument Description ..................................................................7Keyboard ........................................................................................10Component Installation ................................................................11

General Safety ........................................................................................19Compounds Unsuitable for Use in The STAR System 2/6 ..........20System Cautions ...........................................................................21

Setup Menu ............................................................................................23

Instrument Setup ...................................................................................251 - Reagent Volume .......................................................................252 - Auto Print .................................................................................253 - Clear Method ............................................................................264 - Printer Setup ............................................................................275 - Change Reagent Name ............................................................276 - Wash Option .............................................................................287 - Set Clock ...................................................................................298 - Calibrate Temperature ............................................................309 - Set Overtime ............................................................................3310 - Software Version ....................................................................33

Program/Edit Menu ...............................................................................34

Program/Edit Method ............................................................................35Select Vessel ..................................................................................35Change Method Name ..................................................................35Update Initial Reagent .................................................................35Reagent Volume ............................................................................36Stage ..............................................................................................37Ramp Time ....................................................................................37Temperature Target ......................................................................38Time at Temperature ....................................................................38Update Reagent .............................................................................38Reagent Volume ............................................................................38

Prime Menu ............................................................................................40

Prime Method .........................................................................................41

Run Menu ...............................................................................................42

ii

Table ofContents

Tab

le o

f Co

nte

nts

STAR System 2/6600121Rev. 3iii

Instrument Operation ............................................................................43Pause Method ................................................................................43Stop Method ..................................................................................44Insufficient Reagent ......................................................................44Manual Reagent Addition (HF) ....................................................44Method Completed ........................................................................46Print ...............................................................................................46

Routine Maintenance, Troubleshooting and Service ...........................49Routine Maintenance ....................................................................50

Routine Maintenance Schedule ..............................................50Reagent Pump Flush ...............................................................51Scrubber Solution Replacement .............................................47Microwave Leakage Measurement .........................................52Reagent Pump Syringe Replacement .....................................52Reagent Pump Syringe Seal Replacement ............................55Reagent Pump Lead Screw Lubrication ................................56Cleaning of Reagent Valve Rotor and Stator .........................58Quick Temperature Calibration .............................................60Verification of Quick Temperature Calibration ....................62

Troubleshooting Chart ..................................................................65Error Messages ..............................................................................69Service ............................................................................................72

Spill Removal ...........................................................................73Vessel Liner Replacement ......................................................76Reagent Delivery Confirmation ..............................................78Reagent Pump Valve Replacement ........................................78Diaphragm Replacement - Single Head Vacuum Pump .......80Diaphragm & Valve Replacement -Dual Head Vacuum Pump ......................................................82

System Removal .....................................................................................87

Specifications .........................................................................................93Emissions & Safety Approvals ..............................................................94

Warranty ................................................................................................95

Appendix A (Method Development)Mild DigestModerate CharRigorous Char

Appendix B (Examples of Method, Data, and Instrument SetupParameters Printouts)

Appendix C (Chemical Elements and Their Symbols)Appendix D (Conversion Tables)

Volume EquivalentsTemperature EquivalentsFractional Units of Measure Conversion Data

Appendix E (Concentrated Reagents and Their Uses)Appendix F (Examples of Aqua Regia, Reverse Aqua Regia and Multiple Char)

STAR System 2/6 Method Development Guidelines

1STAR System 2/6600121Rev. 3

Introduction STAR System 2 and STAR System 6 are designed for laboratory use indigesting, dissolving, hydrolyzing, leaching, or evaporating a widerange of materials. Their primary purpose is the rapid preparation ofsamples for analysis by atomic absorption (AA) and inductively cou-pled plasma (ICP) emission spectroscopy and gas or liquid chromatog-raphy.

The STAR systems are a breakthrough in microwave technology. Thetechnology permits multiple cavities to operate independently withindividual methods and temperature feedback control. Thus, theSTAR System 6 can digest up to six samples simultaneously or withstaggered start times. The unique design incorporates a single magne-tron, which generates microwave energy for the entire system. Micro-waves are directed through a waveguide with up to six cavitiespositioned along its length. A microwave slot is positioned between thewaveguide and each cavity. When the slot is open, microwaves enterthe cavity; when the slot is closed, microwaves cannot enter the cavity.Simultaneous temperature feedback is obtained from all cavities;therefore, microwave energy is supplied to each cavity based on theneeds of the sample.

The innovative STAR technology systems are either two or six individ-ual microwave cavities. A sample placed inside a microwave-transparent vessel with a polar liquid or ionic solution (usually anacid) is subjected to rapid heating, causing the sample to rapidlydigest or dissolve. Each cavity is independent, permitting simultane-ous performance of up to six different methods. With the temperatureautomatically controlled, the STAR systems ensure consistent andreproducible results for each digestion in each cavity. Large samplesizes can be digested, achieving lower detection limits and simplifyingpreparation for trace metals analyses. Other difficult or problem sam-ples, including highly reactive materials, can also be readily digested.

An automated reagent addition, with up to four reagents, is availableas an option. The reagent addition module eliminates operator han-dling of the reagents and constant monitoring of the system operation.

WARNING

Do not use the automated reagent addition for pumpinghydrofluoric acid (HF). The syringe barrel of the reagentaddition pump is constructed of glass which dissolveswhen it comes in contact with HF. This could cause apossible HF spill or operator contact. HF must be addedmanually.

Each system is equipped with a vapor containment module to treatthe vapors produced during the digestion process.

Intro

du

ction

2STAR System 2/6

600121Rev. 3


For use with all reagents other than hydrofluoric acid, the STAR Sys-tem 2/6 should be installed on a laboratory work bench with access toa fume hood or other means of fume disposal. For use with hydrofluo-ric acid, the STAR System must be installed in a fume hood.

Flat Blade Screwdriver#2 Phillips ScrewdriverPliersLab CoatGlovesEye Protection

Two (2) Waste Containers (bottle and beaker (flask))Reagents (i.e. HNO3, H2SO4, H2O2, and HCl)Containers for Reagents (up to 4)

To install the STAR System 2/6 for use with reagents other than HF,follow the procedures outlined below. Choose a location for instrumentinstallation that:

1. provides at least 8 in. (20 cm) open space on each side and 6 in.(15 cm) open space in the rear of the instrument for ventilation.

2. is free from vibration of large equipment and/or excessive walk-through traffic.

3. provides adequate bench space for sample handling and optionalaccessories (printer), if applicable.

4. permits the instrument to be connected to a dedicated, groundedoutlet. The STAR System 2/6 should be operated on a stabilized,constant voltage AC power supply, and the voltage must bewithin ±10% of the specified level. (See “Specifications,” page 89.)

Note: Measure line voltage to ensure that it meets system specifica-tions.

CAUTION

Line voltage fluctuations greater than 10% will affectinstrument performance.

5. provides a temperature range of 60 °F (15 °C) to 104 °F (40 °C)and a humidity range of 10-85 percent relative humidity.

6. provides access to a fume hood or other means of fume disposal.

CAUTION

If hydroflluoric acid is not to be used for digestions, donot place the STAR System inside a fume hood. Vent theinstrument fumes into a fume hood by means of the out-put tubing attached to the vacuum pump. Contact CEMCorporation for information on the proper external airintake.

SystemInstallation

ToolsRequired

AccessoriesRequired

System

Installatio

n

Installation fornon/HF Use

4STAR System 2/6

600121Rev. 3

For use of hydrofluoric acid in addition to other reagents for diges-tions, the entire STAR System 2/6 must be installed inside a fumehood as illustrated on page 18. Installation requirements include:

1. At least 6 in. (20 cm) open space on each side and in the rear ofthe instrument for ventilation.

2. Adequate bench space for sample handling and optional accesso-ries (printer), if applicable.

3. A dedicated, grounded outlet. The STAR System 2/6 should beoperated on a stabilized, constant voltage AC power supply, andthe voltage must be within ±10% of the specified level. (See “Spec-ifications,” page 85.)

Note: Measure line voltage to ensure that it meets system specifica-tions.

CAUTION

Line voltage fluctuations greater than 10% will affectinstrument performance.

4. A temperature range of 60°F (15°C) to 104°F (40°C) and a humid-ity range of 10-85 percent relative humidity is required.

Installation forHF Use


UnpackingSystemComponents

1. Unpack the system components – main instrument, vapor con-tainment system (including vacuum pump and reagent additionmodule, if applicable) and accessories.

2. Remove all protective materials. Retain all packing and protectivematerials.

3. Verify that all accessories listed below and illustrated in figure 1are included.

System 2 System 6Vessel (Pyrex glass) 2 6Condenser 2 6Vessel Clamp 2 6Shield 2 6Vessel Rack 1 1Power Cord 1 1Fuse 2 2Communication Cable 1 1Operation Manual 1 1Tubing Clip 0 2Boiling Tube (Not Illustrated) 30 30Fume Exhaust Tubing (5/16” Norprene) 1 1 (Not Illustrated)Reagent Waste Tubing (1/8” Teflon®) 1 1 (Not Illustrated)

Figure 1. Accessories

Innovators in Microwave Technology

Corporation

Vessel

CondenserRack

OperationManual

PowerCord

Fuse

ShieldVesselClamp

CommunicationCable

TubingClip

System

Installatio

n

6STAR System 2/6

600121Rev. 3

CEM Ltd. CEM GmbH CEM S.r.l.Unit 2 Middle Slade Carl-Friedrich-Gauss-Str. 9 Via Dell’Artigianato, 6/8Buckingham Ind. Park 47475 Kamp-Lintfort 24055 Cologno al Serio (Bg)Buckingham MK18 1WA Germany ItalyUnited Kingdom Tel: (49) 2842-719021 Tel: (39) 35-896224Tel: (44) 1-280-822873 Fax: (49) 2842-719539 Fax: (39) 35-891661Fax: (44) 1-280-822342Fax: (44) 1-280-812419

1. Inspect the instrument for cracks, dents or warping.

WARNING

If damage is noted, do not attempt instrument startup.

2. If the instrument has been damaged in shipping, contact thefreight carrier to report damage and to file a damage report. Con-tact the CEM Service Department or local subsidiary or distribu-tor to report damage and to request service information.

CEM CorporationService Department

P.O. Box 2003100 Smith Farm Road

Matthews, NC 28105-0200 USA

Within the continental United States(800) 726-5551

Outside the United StatesTelephone: (704) 821-7015

Fax: (704) 821-7894Telex: 802118

InstrumentInspection


InstrumentDescription

Figure 2. STAR System 2 (Front View)

Figure 3. STAR System 6 (Front View)

Vapor Collection/Reagent AdditionModule

MainInstrument

MainInstrument

Vapor Collection/Reagent AdditionModule

Display &Keyboard

Display &Keyboard

LightedWindowfor Cavity

LightedWindowfor Cavity

Vessel

Vessel

Condenser

Condenser

Vapor Collection/Reagent AdditionArm

Vapor Collection/Reagent AdditionArm

Shield

Shield

System

Installatio

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8STAR System 2/6

600121Rev. 3

34

12

Figure 4. STAR System 6 (Rear View)

Figure 5. STAR System (Side Views)

VaporCollectionPort

PrinterPort

ComputerPort

Power CordReceptacle

FuseHolder

On/OffSwitch

FacingInstrument

Left Side Right Side

Fitting for End of 3/16” TubingLabeled “Connect to VaporCollection Module”

Connection for End of 3/8”Tubing Labeled “Connect toVapor Collection Module”

ReagentTubing

Voltage SelectionSwitch


��

��

SpillTray

Figure 6. STAR System 2 (Front Panel Removed)

Vessel – holds the sample during a digestion

Cavity – positions the vessel and provides the microwave energy toperform the digestion

Condenser – condenses vapors and directs reagents to flow down thesides of the vessel

Vessel Clamp – clamps the condenser and the arm to create a seal

Vessel Liner – directs spillage into the spill tray

Shield – prevents contact with reagents should an event occur duringa digestion

Vapor Containment/Reagent Addition Arm – routes vapors fromvessel and directs reagent(s) to vessel

Vapor Containment System – removes vapors and routes them tothe fume hood during the digestion process (includes vapor collectionmodule and vapor scrubber)

Vapor Collection Module – directs fumes from the vessel to thevapor scrubber

Vapor Scrubber – contains solutions to neutralize vapors during thedigestion process

Reagent Addition (optional) – automatically adds reagents to thecavity in programmed quantities

Vacuum Pump – pulls vapors from vessel through the vapor collec-tion module and directs them into the fume hood

Arm- in-Position Sensor – prevents operation if the arm is in anupright position or over-extended in a downward position

Vessel-in-Position Sensor – prevents operation if the vessel is notinstalled

Spill Sensor – alerts operator with an error message when a spilloccurs and pauses all methods

Temperature Sensor – monitors the temperature during the diges-tion and provides feedback control

Spill Tray – collects any spillage from the cavity

Valve – opens and closes to permit the flow of the reagent

RFStub

System

Installatio

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10STAR System 2/6

600121Rev. 3

Select – permits selection of the applicable cavity for setup, editingand/or operation

Start/Pause – begins the method currently displayed on the selectedcavity screen or pauses the operation during any stage of the method

Stop – stops operation of method and returns to the cavity mainscreen

Edit – permits editing of parameters for the method displayed on theselected cavity

Home – returns the selected cavity to the main screen

Print – permits printing of method data, method program and/orsetup parameters

Setup – permits editing of system parameters

Change – incrementally increases or decreases current parameterdisplayed on selected cavity (upper case letters, lower case letters,numbers and symbols) or scrolls through selections such as methods,reagents, etc.

Next – advances to the next method parameter during editing orsetup menus

Back – returns to the previous screen during editing or setup menus

Keyboard

Figure 7. STAR System 2 Keyboard


1. Position the main instrument on the selected installation site(bench area if not using HF or inside a fume hood if using HF).

NOTE

Straps are positioned around the liner in each cavity ofthe main instrument to prevent breakage of the linersduring shipment. These straps must be removed prior toinstrument operation.

2. Carefully pull the straps extending from each cavity, one strap ata time, until all straps are removed. Retain straps for use iffuture shipment is required.

3. Ensure that the vessel support ring is properly installed andseated. Using an index finger, position the liner in each cavity sothat the opening in the bottom of the liner is positioned directlyabove the opening in the RF stub (figure 6, page 8).

Note: If liners are not installed, refer to “Vessel Liner Replacement,”page 75, for procedures for installing vessel liners.

Figure 8. Cavity Liner Protective Straps

4. Position the vapor collection/reagent addition module on top ofthe main instrument. While leaning the module toward the frontof the instrument, position the support brackets of the moduleinto the slots on the back of the top cover as illustrated in figure9. Ensure that the feet of the module are positioned and securedinto the tracks of the top cover.

ComponentInstallation

Figure 9. Vapor Collection/Reagent Addition Module Installation

System

Installatio

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12STAR System 2/6

600121Rev. 3

34

12

VaporCollectionPort

Figure 10. Back of Vapor Collection/Reagent Addition Module

5. Install the communications cable into the port labeled “Vapor Col-lection Port” on the main instrument and into the port of thevapor collection/reagent addition module.

6. If using the reagent addition option, proceed as follows. If notusing the reagent addition option, proceed to step 10.

WARNING

Proper precautions must be taken to avoid contact withreagents or reagent vapors. Protective gear should beworn as outlined in the user’s safety program for haz-ardous materials and the reagent manufacturer’s mate-rial safety data sheet. Refer to these guidelines forproper handling of the reagent.

7. Fill the reagent containers as required. Position the reagent tub-ing in the reagent containers. If necessary, tape the tubing to thecontainer to prevent the tubing from pulling free of the container.Ensure that the tubing is placed into the correct reagent con-tainer so that the proper reagent will be added to the sample asrequired. Reagent names can be changed in the Setup Menu.Default reagents are 1 - sulfuric, 2 - nitric, 3 - peroxide and 4 -hydrochloric.

NOTE

If reagent names have been or are to be changed duringsystem setup procedures, label reagent tubing with theappropriate reagent names, ensuring that they remainin the correct order. For example, if sulfuric is changedto water, the tubing installed in position #1 should belabeled water, etc.

WARNING

Do not use the automated reagent addition module forpumping HF.

AutomatedVacuumPumpAccessory(Optional)

Connection for End of 3/8”Tubing Labeled “Connect toVapor Collection Module”

Fitting for End of 3/16” TubingLabeled “Connect to VaporCollection Module”


34

12

Figure 11. Reagent Tubing and Containers

NOTE

CEM Corporation recommends using reagent containerswith covers which have a hole drilled through the coverto secure the tubing (figure 11), yet permit sufficient airinto container to prevent forming a vacuum during rea-gent uptake.

8. Place a waste bottle behind or on top of the main instrument to beused for the air/waste from the vapor collection/reagent additionmodule. This bottle is necessary to collect any residual reagentfrom the pump, valve, etc. Tubing should always be above liquidlevel.

WARNING

The tubing must be connected to the valve and routed tothe waste container to prevent escape of reagent duringoperation.

9. Connect the length of 1/8” Teflon® tubing in the left side of thevalve (facing instrument) on the reagent addition pump (figure12, page 14). Route the other end of the tubing to the bottle posi-tioned behind or on top of the main instrument in step 8. If neces-sary, secure the tubing to the flask to prevent the tubing fromescaping, permitting spillage of reagents.

10. If the instrument is installed on a work bench, place a beaker(flask) in the fume hood. If the instrument is installed in a fumehood, place a beaker (flask) in the fume hood for collection ofvapor residue.

11. Position the vapor scrubber module (three vapor containment cyl-inders) on the bench near the main instrument.

System

Installatio

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14STAR System 2/6

600121Rev. 3

12. Position the vacuum pump between the scrubber module and thefume hood or inside the fume hood, if preferred.

13. Using a flat blade screwdriver, pry the cap from each vapor scrub-ber cylinder. Add solutions to the cylinders as follows: #1 - deion-ized water to top of marbles (cylinder nearest main instrument),#2 - 25% NaOH (sodium hydroxide) to top of marbles (center cyl-inder), and #3 - deionized water one-half distance of marbles (cyl-inder nearest fume hood). (Refer to figure 13, page 17.)

14. Connect the end of the 3/8” tubing labeled “Connect to Vapor Col-lection Module” to the vapor collection/reagent addition module(figure 10, page 12). Connect the other end of the same tubinglabeled “Connect to First Scrubber Cylinder” to the inlet connec-tion on the first container of the scrubber.

CAUTION

During installation of the 3/8” tubing, verify that thetubing connector installed on the back of the vapor col-lection/reagent addition module is not broken orcracked.

To avoid condensation in the tubing which can lessenthe vacuum, the tubing between the vapor collection/reagent addition module and the first container of thescrubber should be as short as possible. If necessary,shorten tubing to avoid any loops.

WARNING

To avoid personal injury, remove any protective plasticplugs from the vacuum pump.

15. Connect the end of the 3/16” tubing labeled “Connect to VaporCollection Module” to the fitting on the back of the vapor collec-tion module (figure 10, page 12). Route the other end of the tubinglabeled “Secure Inside Lab Hood or Exhaust” to the flask placedin the fume hood in step 10. Place the tubing in the flask.

1.02.0

3.04.0

5.06.0

7.08.0

9.010.0

Figure 12. Air/Waste Tubing

Valve

Fitting

Air/WasteTubing


WARNING

Ensure that the tubing is installed correctly to avoid thepossibility of burns from exposure to reagents andvapors. The flow should be directed so that the vaporsare directed into the tubing that extends below the sur-face of the solution in the scrubber. The vapors are“cleansed” as they bubble to the surface.

16. Connect the end of the 3/8” tubing labeled “Connect to VacuumSide of Vacuum Pump” to the vacuum tubing connection (labeled“V”) of the vacuum pump. Connect the other end of the tubinglabeled “Connect to Last Scrubber Cylinder” to the outlet connec-tion of the third container of the scrubber.

17. Connect one end of the 3/8” tubing labeled “Connect to PressureSide of Vacuum Pump” to the pressure tubing connection (labeled“P”) of the vacuum pump. Route the other end of the tubinglabeled “Secure Inside Lab Hood or Exhaust” to the beaker (flask)positioned in the fume hood in step 10, page 13. Place the tubingin the flask.

18. Connect one section of 3/8” tubing labeled “Connect BetweenScrubber Cylinders” to the outlet of container one and to the inletof container two of the scrubber. Connect one end of the secondsection of tubing labeled “Connect Between Scrubber Cylinders”to the outlet of container two and the inlet of container three ofthe scrubber. (Refer to figure 13, page 17.)

19. If installing a STAR System 6 with a dual head vacuum pump(figure 23, page 80), install the white clips furnished in the acces-sory kit to secure the tubing to the pump fittings.

20. Install the shields in the shield holders of each cavity.

Note: Prior to operation, rotate the shields so that the plate is posi-tioned toward the front of the instrument.

21. If using a printer, connect the printer cable to the printer as out-lined in the printer literature. Connect the other end of theprinter cable to the printer port on the back of the main instru-ment (figure 4, page 8). Perform printer setup during the maininstrument setup procedures.

22. Ensure that the voltage selection switch (figure 4, page 8) is inthe proper position (setting) to parallel electrical line voltage (208/230V or 220/240V).

Note: System 2, 120V is not equipped with a voltage selection switch.

23. Plug the main instrument into a grounded, dedicated electricaloutlet as specified.

System

Installatio

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16STAR System 2/6

600121Rev. 3

24. Position the on/off switch of the main instrument in the “on” posi-tion. The following screen will appear.

TESTING FORREAGENT ADDITION

25. If the valve is not found, the following screen will appear.

VALVE MISSING

26. If the pump is not found, the following screen will appear.

PUMP MISSING

27. If the valve and pump are not found, the following screen willappear.

REAGENT ADDITIONNOT INSTALLED

28. If the valve and pump are found, the following screen will appear.

REAGENT ADDITIONINITIALIZED

29. Once the instrument determines whether or not the reagent addi-tion is installed, the method menu will appear.

METHOD X(XXXXXX)

30. If necessary, perform system setup procedures as outlined onpages 25 through 33. If not performing complete setup proce-dures, calibrate cavities as outlined on pages 30 through 33.

CAUTION

The STAR System 2 AND STAR System 6 must be cali-brated upon installation.

31. Ensure that the vacuum pump is plugged into an electrical outlet.Position the toggle switch of the vacuum pump in the “on” posi-tion. Ensure that the solutions in the scrubber containers arebubbling.

32. If using the reagent addition option, perform the prime method asoutlined on page 41 for each of the four reagent tubes. If a washreagent is selected, prime the wash reagent tubing first so thatthe wash option will be available for the remainder of the rea-gents.


Fig

ure

13.

ST

AR

Sys

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2 In

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on

Lab

ora

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Ben

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Fume Hood

Vap

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#1C

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DeionizedWater

25%NaOH

Sin

gle

Hea

dV

acu

um

Pu

mp

Air

/Was

teT

ub

ing

System

Installatio

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18STAR System 2/6

600121Rev. 3

Fig

ure

14.

ST

AR

Sys

tem

2 In

stal

led

in F

um

e H

oo

d f

or

HF

Use

Vap

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DeionizedWater

Mai

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stru

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Sin

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Pu

mp

Fu

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Safety

GeneralSafety

If the STAR System is installed inside a laboratory fume hood for useof hydrofluoric acid, other acids should not be stored inside the fumehood. Fumes from these acids may attack the electrical components ofthe system, resulting in possible damage and malfunctioning of thesystem.

Teflon vessels used in the STAR System will arc occasionally. Somearcing is normal when using Teflon vessels in conjunction with micro-wave energy.

Protective shields, which must be installed during initial instrumentsetup, are provided with the STAR systems. These shields must beinstalled with the plate positioned toward the front of the instrumentprior to performing any digestions.

Always use hot pads when removing vessels from the instrument cav-ity to avoid the possibility of burns.

Permit sample to cool prior to removal of vessel from the instrumentcavity to prevent reagent fumes in the laboratory.

Never insert anything into the instrument cavities other than themanufacturer approved vessels.

Never insert metal into an instrument cavity.

Hydrofluoric (HF) acid is unsafe when used with glass or quartz ves-sels. If using hydrofluoric acid, use Teflon® vessels.

Phosphoric acid (H3P04) should not be used with quartz or glass ves-sels. If using phosphoric acid, use Teflon® vessels.

Phosphoric acid can be used with Teflon vessels up to temperatures of250°C only. When the acid begins to break down, it forms salts thatcan adhere to the sides of the vessel, creating localized hot spots whichmay result in cracking of vessel.

CEM Corporation does not recommend the use of perchloric acid in theSTAR Systems because explosive perchlorates may be formed.

20STAR System 2/6

600121Rev. 3

WARNING

Acid decomposition of certain chemical compounds ortypes of samples constitutes unreasonable, hazardousmisuse of CEM microwave digestion systems. Theclasses of compounds listed below are unsuitable forclosed vessel microwave digestion because they arehighly reactive with oxidizing acids and/or may becomenitrated and potentially explosive. Absence of a particu-lar chemical compound from this list does nto implymicrowave acid decomposition of such a sample is safeunder all conditions. CEM will not be responsible fordamage to equipment and facilities or personal injuriesresulting from microwave digestion of such compounds/samples.

• Explosives (TNT, Nitrocellulose, etc.)• Propellants (Hydrazine, Ammonium Perchlorate, etc.)• Pyrophoric Chemicals• Hypergolic Mixtures (Nitric Acid and Phenol, Nitric Acid and

Triethylamine, Nitric Acid and Acetone, etc.)• Animal Fats (Esters of glycerol capable of nitration and the

formation of nitroglycerin or other nitrated organic compounds)• Aviation Fuels (JP-1, etc.)• Acetylides• Glycols (Ethylene Glycol, Propylene Glycol, etc.)• Perchlorates (Ammonium, Potassium, etc.)• Ethers (Cellosolve - Ethylene Glycol Phenyl Ether, etc.)• Lacquers• Alkanes (Butane, Hexane, etc.• Ketones (Acetone, Methyl Ethly Ketone, etc.)

CompoundsUnsuitable forOpen CavityMicrowaveDigestion


SystemCautions

Do not pump samples with the reagent pump in the automated rea-gent addition module.

Do not pump hydrofluoric acid (HF) with the automated reagent addi-tion module.

If the plunger of the syringe on the reagent pump in the automatedreagent addition on top of the main instrument is removed from thebarrel, it should be rinsed with deionized water and thoroughly driedprior to replacement.

The vacuum pump is 100% oil free and does not require lubrication.All bearings are sealed and permanently lubricated.

The vacuum pump should be used to pump air or gas, not liquids.

To avoid personal injury, remove any protective plastic plugs from thevacuum pump.

The vacuum pump should be operated for a few minutes to permitwarmup prior to pumping saturated or nearly saturated vapors.

Prior to turning the vacuum pump off after use, permit the pump tooperate for approximately 2 minutes to purge any droplets of conden-sation which might have formed on the inside of the pump. This pre-vents crystallization and/or absorption of liquids by the pumpmaterials.

Only plastic (not metal) fittings should be threaded into the head(s) ofthe vacuum pump.

Safety

22STAR System 2/6

600121Rev. 3


24STAR System 2/6

600121Rev. 3


The Setup Menu permits entry (edit) of system parametersincluding reagent volume (amount of reagent available in supplysource), printer functions, method delete, printer setup, rea-gent names, date/time, wash option, calibration, overtimesetup and software version. To access a specific function within thesetup procedure, refer to the software chart on pages 23 and 24.

METHOD X(XXXXXX)

1. From the main screen, press the “SETUP” key on the keyboard.The following screen will appear.

1 - REAGENTVOLUME

2. Press the “NEXT” key. The following screen will appear.

SELECT REAGENT(XXXXXXXX)

3. Press the “+” and/or “–” Change keys to select the desired reagent(1 - Sulfuric, 2 - Nitric, 3 - Peroxide, 4 - Hydrochloric, etc).

Note: If reagent names are to be changed, refer to page 27.


XXXXXXXX VOLUMEXX.XXL

5. Enter the volume of selected reagent (step 3) available in theinstrument supply source. During operation, the instrument willintake reagent from the supply source. Based on method parame-ters, if sufficient reagent is not available in the supply source, theinstrument will not permit operation when the “Start” key ispressed. The instrument screen will toggle between “InsufficientReagent” and “Go to Setup Menu Item 1.”

6. Use the “+” and/or “–” Change keys to enter or edit the number.

7. Press the “NEXT” key and the “+” and/or “–” Change keys to enteror edit digits of the volume (50 liters maximum).

8. Once the volume has been entered, press the “NEXT” key toreturn to the following screen.

1 - REAGENTVOLUME

9. Press the “+” Change key. The following screen will appear.

2 - AUTO PRINT

InstrumentSetup

Setu

p

ReagentVolume

Auto Print

26STAR System 2/6

600121Rev. 3

Note: Auto Print permits entry of print parameters to enable or dis-able automatic printing of the method and/or data after each test.Examples of printouts are included in Appendix B.


PRINT METHOD(ON)

11. Press the “+” and “–” Change keys to toggle between “on” and“off.”


PRINT DATA(ON)

13. Press the “+” and “–” Change keys to toggle between “on” and“off.”

14. Press the “NEXT” key to return to the following screen.

2 - AUTO PRINT


3 - CLEAR METHOD

16. To clear (erase) a method’s parameters, press the “NEXT” key.The following screen will appear.

. SELECTED:METHOD XX

17. To select the particular method (1 - 20) for which the parametersare to be erased, press the “+” and “–” Change keys. Once theselected method is displayed, press the “NEXT” key. The followingscreen will appear.

‘START’ TO CLEARMETHOD XX

18. Press the “START” key for the selected cavity. The followingscreen will appear.

‘START’ IF YOU ARESURE!!!

Note: The previous screen permits the operator to choose not to erasethe method parameters.

Clear Method


19. If erasure is not desired, continue to press the “BACK” key untilthe “Clear Method” screen is displayed. If erasure is desired, pressthe “START” key. The method parameters and name will beerased from memory. The following screen will appear.

3 - CLEAR METHOD

Note: Once cleared, the method name will revert to the originalnumeric number.


4 - PRINTER SETUP


SELECT PRINTER(XXXXXX)

22. Press the “+” and “–” Change keys to select the desired printer(IBM, ASCII, Epson or HP). Laser printers are not compatible.

23. Press the “NEXT” key to return to the “Printer Setup” screen.

4 - PRINTER SETUP


5 - CHANGE REAGENTNAME


SELECT REAGENTXXXXXXXX*

NOTE

Default reagents are 1 - Sulfuric, 2 - Nitric, 3 - Peroxideand 4 - Hydrochloric.

26. Use the “+” and/or “–” Change keys to select the reagent to bechanged.

Note: If a reagent name is changed in any way, the instrument auto-matically deletes the volume of the reagent programmed in the firstsection of the system setup. If reagent name(s) is changed, the usermust return to section No. 1 of the Setup procedure and program avolume for the newly named reagent(s). (Refer to page 25.)

Setu

p

Printer Setup

Change ReagentName

Setu

p

28STAR System 2/6

600121Rev. 3


Reagent PumpSpeed (S low)*

Note: A slow pump speed should be selected for a highly viscous rea-gent such as sulfuric and phosphoric, and a fast pump speed should beselected for a non-viscous reagent. However, if adding reagent in ali-quots of 5mL or more, the instrument will automatically default to aslow pump speed, regardless of this selection.

28. Use the “+” and/or “–” Change keys to toggle between a slow andfast reagent pump speed.


XXXXXXXX*

30. Use the “+” and/or “–” Change keys to enter or edit the first letter.

31. Continue to press the “NEXT” key and the “+” and/or “–” Changekeys to enter or edit each letter of the custom reagent (8 charac-ters maximum).

32. Press the “BACK” key until the “5 - Change Reagent Name”screen is displayed.


6 - WASH OPTION

Note: The wash option can be used to help prevent any minute mixingof reagents within the reagent pump syringe barrel. If the wash optionis activated, one of the four available reagents must be selected as thewash reagent. It is then used to wash the syringe barrel before andafter addition of any of the remaining three reagents which areselected. CEM Corporation recommends using deionized water as thewash option reagent. Once the wash option is activated, it becomesactive for each cavity and for each method which utilizes the selectedreagent(s).


WASH REAGENTXXXXXXXX

35. Use the “+” and/or “–” Change keys to select the reagent to beused as the wash option reagent.

Note: Only one (1) reagent can be selected as a wash reagent.

Wash Option



WASH VOLUMEXXmL

Note: The instrument defaults to 2mL.

37. Press the “+” and/or “–” Change keys to enter or edit the numberof milliliters of wash reagent to be used for washing the syringebarrel before and after the addition of the selected reagent(s). Themaximum number of milliliters which can be entered is 10.


REAGENTX. XXXXXXXX

39. Use the “+” and/or “–” Change keys to select the reagent(s) forwhich washing is required (1 - Sulfuric, 2 - Nitric, 3 - Peroxide,4 - Hydrochloric, etc).


WASH XXXXXXXX(YES)

41. Press the “+” and/or “–” Change keys to toggle to “Yes.”

Note: If the wash option is to be used for additional reagent(s), pressthe “Back” key to return to the following screen.

REAGENTX. XXXXXXXX

42. Once desired reagents are selected to be preceded and followed bythe wash option, press the “NEXT” key to return to the followingscreen.

6 - WASH OPTION


7 - SET CLOCK


(XX) HOUR FORMATXX:XX

45. Press the “+” and “–” Change keys to toggle between “12” and “24”hour format.

Set Clock

Setu

pS

etup

30STAR System 2/6

600121Rev. 3

Note: If the 12-hour format is selected, the time will be followed byeither “a.m.” or “p.m.” as applicable.

46. To set or correct the time, press the “NEXT” key. The followingscreen will appear.

1 0 Jan 961 0 : 3 0

Note: The above screen is an example only. The screen will providethe actual date, etc. (if entered) or zeros.

47. Use the “+” and/or “–” Change keys to enter or edit the day of themonth.

48. Press the “NEXT” key to position the cursor on the month. Usethe “+” and/or “–” Change keys to enter or edit the month.

49. Press the “NEXT” key to position the cursor on the year. Use the“+” and/or “–” Change keys to enter or edit the year.

50. Press the “NEXT” key to position the cursor on the hour. Use the“+” and/or “–” Change keys to enter or edit the hour.

51. Press the “NEXT” key to position the cursor on the minutes. Usethe “+” and/or “–” Change keys to enter or edit the minutes.

52. Once the time is properly set, continue to press the “BACK” keyuntil the “6 - Set Clock” screen is displayed.


8 - CALIBRATETEMPERATURE

Note: Each cavity must be calibrated. During calibration procedures,no other operation of any cavity is possible.


SELECT VESSEL(XXXXXX)

CAUTION

Teflon vessels must be selected if using hydrofluoricacid.

55. Use the “+” and/or “–” Change keys to select either quartz/glassvessels or Teflon vessels.

CalibrateTemperature


NOTE

This calibration procedure is based on using nitric acid(quartz/glass vessels) or deionized water (teflon vessels)as the low boiling point reagent and sulfuric (quartz/glass vessels) or nitric acid (teflon vessels) as the highboiling point reagent. To determine the proper low andhigh calibration values, boil 50mL of each reagent on ahot plate, and, with a certified thermometer, measurethe temperature of the reagent while boiling. CEM Cor-poration recommends using the above reagents for ini-tial temperature calibration and calibration verification;however, reagents other than those listed may be uti-lized, if desired.

56. Ensure that the liner is positioned so that the opening in the bot-tom of the liner is positioned directly above the opening in thespill tray assembly. To promote even boiling, place a CEM boilingtube in the vessel, ensuring that the tube extends below the sur-face of the reagent. Place a clean vessel containing 20mL of nitricacid (quartz/glass vessel) or water (Teflon vessel) in the selectedcavity. Place a condenser on the vessel. Lower the vapor collectionarm and install a vessel clamp. Ensure that the shield is posi-tioned with the plate toward the front of the instrument. Positionthe toggle switch of the vacuum pump in the “on” position. Note:The CEM boiling tube is constructed of a special Teflon materialand enhances the boiling action.

CAUTION

If calibration of multiple cavities is required, CEM rec-ommends calibration of the low boiling point of each cav-ity, one at a time, followed by calibration of the highboiling point of each cavity, one at a time.


CARE CALIBRATIONWILL CHANGE!!!


LO CAL TEMP XXXPRESS START

Note: The default value is “121” for quartz/glass vessels and “100” forTeflon vessels.

59. If necessary, use the “+” and/or “–” Change keys to edit the “lo cal”temperature value.

60. Press the “START” key. The following screen will appear.

BOILING? (STOP)CAL DATA XXX

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32STAR System 2/6

600121Rev. 3

61. Wait for the “cal data” of the reagent in the vessel to rise. Oncethe “cal data” is constant, press the “STOP” key. The followingscreen will appear.

HI CAL TEMP XXXPRESS START


62. If necessary, use the “+” and/or “–” Change keys to edit the “hi cal”temperature value.

63. Remove the vessel with the lo-cal reagent. Place 15mL of sulfuricacid (quartz/glass vessels) or nitric acid (Teflon vessels) in a clean,dry vessel. Place a CEM boiling tube in the vessel, ensuring thatthe end of the tube is below the surface of the reagent and theother end is above the surface of the reagent. Place the vessel inthe selected cavity. Place a condenser on the vessel. Lower thevapor collection arm and install a vessel clamp. Ensure that theshield is positioned with the plate toward the front of the instru-ment. Note: Do not use sulfuric acid which has been open to theatmosphere because the acid will absorb water.



65. Wait for the “cal data” of the reagent in the vessel to rise. Oncethe “cal data” is constant and a rolling boil is observed for four (4)minutes, press the “STOP” key. The following screen will appear.

CELL XCALIBRATED

Note: If the instrument fails to calibrate correctly, the new calibrationdata will not be saved and the instrument will revert to the previouscalibration values. One of the following screens will appear.

INCORRECTCALIBRATION

or

CELL XNOT CALIBRATED

66. Press the “NEXT” key. The instrument will return to the followingscreen.



67. Select each cavity and repeat calibration procedures.


9 - SET OVERTIME

Note: An overtime can be entered into the instrument, permitting theinstrument extra time to reach the ramping parameter, if not met dur-ing programmed ramping time.


OVERTIME0 HRS 10 MINS

Note: The instrument defaults to a 10-minute overtime. Maximumtime which can be entered into the overtime screen is 10 hours, 59minutes.

70. To enter or edit the number of hours, use the “+” and/or “–”Change keys.

71. Press the “NEXT” key to position the cursor on the minutes. Usethe “+” and/or “–” Change keys to enter or edit the minutes.

72. Press the “NEXT” key to return to the “9 - Set Overtime” screen.


10 - SFTW VERSIONXXXXXX-XX

Note: The above screen is an information screen and cannot be edited.

74. Press the “HOME” key to end the Setup menu and return to theMain Screen.

METHOD X

Setu

p

Software Version

Set Overtime

34STAR System 2/6

600121Rev. 3

METHOD X* (XXXXXX)*

UPDATE ANOTHER REAGENT (N0* )

IN ALIQUOTS OF 0.0* ML

UPDATE ANOTHER REAGENT (YES)*

ADD AT START OF STAGE (YES)*

IN ALIQUOTS OF 0.0* ML

TOTAL VOLUME XXXXXXXX 0.0* ML

REAGENT (XXXXXXXX)*

ADD REAGENT (YES)*

TIME AT TEMP XX MINS 00* SECS

TIME AT TEMP 0* MINS 00 SECS

TEMPERATURE TARGET 0*

RAMP TIME XX MINS 00* SECS

RAMP TIME 0* MINS 00 SECS

STAGE (ACTIVE)*

UPDATE INITIAL REAGENT (YES)*

METHOD X STAGE 8

TOTAL VOLUME XXXXXXXX X.X* mL

REAGENT XXXXXXXX*

METHOD X* (XXXXXX)*

CHANGE METHOD NAME (YES)*

METHOD X* (XXXXXX)*

NEXT

METHOD X* (XXXXXX)*

NEXT

NEXT

METHOD X* (XXXXXX)*

BACK

ADDITION 1*

ADDITION 2*

METHOD X STAGE 1

EDIT

METHOD X STAGE 2

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

NEXT

METHOD X* (XXXXXX)*

BACK

BACK

BACK

BACK

NEXT

NEXTNEXT

NEXT

*Use + (plus) and/or – (minus) Change Keys to Make Selection

BACK

NEXT

SELECT VESSEL (XXXXXX)*

NEXT

Program/Edit Menu


Program/EditMethod

The Program/Edit Menu permits entry and storage of method parame-ters for a variety of sample types and digestions using the storedmethods. A total of 20 methods, each with up to 40 stages, can bestored. To enter, store and edit methods, follow procedures outlinedbelow. To access a specific function within the program/edit procedure,refer to the software chart on page 34.

1. Select the cavity to be utilized.

METHOD X(XXXXX)

Note: The instrument defaults to the last method utilized.

2. To select a particular method (1 - 20), press the “+” and/or “–”Change keys.

3. Press the “Edit” key. The following screen will appear.


4. Press the “+” and “–” Change keys to select either quartz/glassvessels or Teflon vessels.


CHANGE METHODNAME (YES)

6. Press the “+” and “–” Change keys to toggle between (yes) and(no).


METHOD X

8. Use the “+” and/or “–” Change keys to enter or edit the letter(upper case or lower case letter, symbol or number).

9. Press the “NEXT” key and the “+” and/or “–” Change keys to enteror edit each letter, symbol and/or number of the method name (32characters maximum).

10. Once the complete method name has been entered, press the“BACK” key until the “Change Method Name” screen is displayed.


UPDATE INITIALREAGENT (YES)

12. Press the “+” and “–” Change keys to toggle between (yes) and(no).

Pro

gram

/Ed

it

Select Vessel

Update InitialReagent

Change MethodName

36STAR System 2/6

600121Rev. 3

13. Press the “NEXT” key.

Note: If “Yes” is selected and the automated reagent option module isnot installed, the following screen will appear.

REAGENT ADDITIONNOT INSTALLED

Note: If using HF or if the automated reagent module is not being uti-lized, proceed to step 21.

Note: If “Yes” is selected and a reagent option is installed, the follow-ing screen will appear.

ADDITION 1

14. Press the “+” and “–” Change keys to edit the reagent additionnumber (10 maximum).


REAGENTXXXXXXXX

Note: The instrument defaults to the last selected reagent.

16. Press the “+” and/or “–” Change keys to select the desired reagent(None, Sulfuric, Nitric, Peroxide, Hydrochloric, Etc.).


TOTAL VOLUMEXXXXXXXX X.X mL

18. Press the “+” and/or “–” Change keys to edit the total amount ofreagent to be added. The number of milliliters increase ordecrease in increments of 0.5mL.


IN ALIQUOTSOF 0.0 mL

20. Press the “+” and/or “–” Change keys to edit the size of the ali-quots (amounts) in which the reagent will be added. The numberof milliliters increase or decrease in increments of 0.5mL, with amaximum of 10.0mL.


UPDATE ANOTHERREAGENT (YES)

Reagent Volume


22. Press the “+” and “–” Change keys to toggle between “yes” and“no.”

23. Press the “NEXT” key.

Note: If “Yes” was selected in step 22, repeat steps 12 through 20 foradditional reagent addition(s).

Note: If “No” is selected in step 22, the following screen will appear.

METHOD XSTAGE 1

24. If necessary, press the “+” and/or “–” Change keys to edit or enterparameters for the stage (up to 40 stages available).


STAGE (ACTIVE)

26. Press the “+” and “–” Change keys to toggle between “active” and“inactive.” The instrument defaults to “inactive.”

Note: If a stage is changed to “inactive,” that particular stage will not oper-ate during the digestion, and the stages will be renumbered on the display.


RAMP TIME0 MINS 00 SECS

Note: Ramp time is the defined time in which the instrument is toreach the target temperature. It ensures that a linear temperaturerise is calculated once the Start key is pressed. If the method ispaused and restarted, the software compares the current temperaturewith the programmed temperature and applies microwaves asrequired, based on the new starting temperature.

28. Press the “+” and/or “–” Change keys to edit the number of min-utes for ramp time (0 - 99).


RAMP TIMEXX MINS 00 SECS

30. If applicable, press the “+” and/or “–” Change keys to edit thenumber of seconds for ramp time (0 - 59).

Note: A minimum time of one (1) second is required for the ramp timein Stage 1.

Pro

gram

/Ed

it

Stage

Ramp Time

38STAR System 2/6

600121Rev. 3

TemperatureTarget


TEMPERATURETARGET 30

32. Press the “+” and/or “–” Change keys to edit or enter the targettemperature to be reached within the ramp time (30 - 430°C).


TIME AT TEMP0 MINS 00 SECS

34. Press the “+” and/or “–” Change keys to edit the number of min-utes to maintain the target temperature (0 - 99).


TIME AT TEMPXX MINS 00 SECS

36. Press the “+” and/or “–” Change keys to edit the number of sec-onds to maintain the target temperature (0 - 59).

37. Press the “NEXT” key. If the instrument is not equipped with areagent option, the Stage 2 screen will appear. If the instrumentis equipped with a reagent option, the following screen willappear.

UPDATE REAGENT(YES)

Note: If a reagent is not to be utilized, press the “+” and/or “–” Changekeys to toggle to “Yes,” then select reagent “None.”


REAGENT(XXXXXXXX)

39. Press the “+” and/or “–” Change keys to select the desired reagent(None, Sulfuric, Nitric, Peroxide, Hydrochloric, Etc.).


TOTAL VOLUMEXXXXXXXX 0.0 mL

41. Press the “+” and/or “–” Change keys to edit the total amount ofreagent to be added.

Time atTemperature

UpdateReagent

Reagent Volume



IN ALIQUOTSOF 0.0 mL

43. Press the “+” and/or “–” Change keys to edit the size of the ali-quots (amounts) in which the reagent will be added. The numberof milliliters increase or decrease in increments of 0.5mL, with amaximum of 10.0mL.


ADD AT START OFSTAGE (NO)

45. Press the “+” and “–” Change keys to toggle between “yes” and“no.”

Note: If “Yes” is selected, reagent will be added at the beginning of thestage. If “No” is selected, the total volume of reagent will be added inselected aliquots at equal intervals of the total time at parameter.


METHOD XXSTAGE XX

Note: Repeat steps 26 through 46 to enter or edit parameters for eachadditional stage of the method.

47. If no additional stages are required for the method, press the“Home” key one (1) time or the “Back” key two (2) times to returnto the main screen.

METHOD X

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/Ed

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40STAR System 2/6

600121Rev. 3

SELECT REAGENT XXXXXXXX*

PRIME

Prime Menu

METHOD X* (XXXXXX)*

EDIT

+ / –

PRIME COMPLETED XXC

PRIME

HOME

START


The instrument must be primed prior to first-time use and if reagenttubing must be purged. Each reagent tube must be primed separately.

METHOD X(XXXXX)

1. From the main screen, press the “+” and/or “–” Change keys untilthe following screen appears.

PRIME

2. Ensure that the selected cavity contains a vessel and condenser,that a clamp is installed to reinforce the seal between the con-denser and arm, that a shield is installed, that reagent tubing isplaced in the reagent containers, that the ends of the tubing arebelow the top level of the reagents, and that each container con-tains the proper reagent.

Note: If reagent tubing is to be purged, refer to Routine Maintenance,“Reagent Pump Flush,” page 51.

3. Press the “EDIT” key. The following screen will appear.

SELECT REAGENTX. XXXXXXXX

4. Press the “+” and/or “–” Change keys to select the desired reagentto be primed (1. Sulfuric, 2. Nitric, 3. Peroxide, 4. Hydrochloric).

NOTE

If reagent names have been changed during the setupprocedure, the instrument will uptake 4mL of the spe-cific reagents being utilized.

5. Press the “HOME” key to return to the main screen.

PRIME

6. Press the “START” key. The instrument will uptake 4mL of theselected reagent to prime the tubing. The following screen willappear.

PRIMECOMPLETED XXXC

7. Repeat the preceding procedures to prime each of the remainingthree reagents to be utilized.

WARNING

Do not use hydrofluoric acid (HF) to prime the pump.The reagent pump installed in the automated reagentaddition module is not suitable for pumping HF.

PrimeMethod

Prim

e

42STAR System 2/6

600121Rev. 3

METHOD X* (XXXXXX)*

REAGENT ADDITION UPTAKE XXXXXXXX

TEMP XX STAGE X RAMP XX:XX:XX

TEMP XX STAGE X OVTM XX:XX:XX

TEMP XX STAGE X COOL DOWN TO TAP

TEMP XX STAGE X TAP XX:XX:XX

TEMP XX STAGE X UPTAKE XXXXXXXX

TEMP XX STAGE X TAP XX:XX:XX

METHOD X COMPLETED XXC

Run Menu

START

*Use + (plus) and/or – (minus) Change Keys to Make Selection

1 ‘PRINT’ SELECTED METHOD

PRINT

PRINTING METHOD


1. Press “Select” for the cavity to be utilized.

METHOD X(XXXXX)


2. To select a particular method (1 - 20), press the “+” and/or “–”Change keys.

NOTE

If one or more cavities are in the calibration method,even if calibration is completed, additional cavities willnot perform a method.

WARNING

Do not fill the vessel above the fill line nor place morethan 200mL of solution in a glass/quartz vessel or 65mLin a Teflon vessel for digestion. Overfilling the vesselcan cause microwave leakage.

3. Place the vessel containing the sample into the selected cavity.

WARNING

Ensure that the type of vessel (quartz/glass or Teflon)entered when programming or editing the method isplaced into the cavity. Temperature of the cavity is cali-brated based on vessel type.

4. Install the condenser in the vessel. Slightly turn the condenser

clockwise to form a “seal.”

5. Position the vapor collection/reagent addition arm so that the tipof the arm is resting in the top of the condenser. Install the vesselclamp to reinforce the seal between the vessel condenser and thearm.

6. Ensure that the shield is installed in the shield holder. Rotate theshield to position the plate outward toward the front of the instru-ment.

WARNING

The shield should always be installed and properly posi-tioned prior to performing a method to prevent potentialinjury should an event occur.

7. Position the toggle switch of the vacuum pump in the “on” posi-tion.

8. Press the “Start” key for the selected cavity.

InstrumentOperation R

un

Pause Method

44STAR System 2/6

600121Rev. 3

Note: If the “START/PAUSE” key for the selected cavity is pressedwhile performing a method, the method is paused until the “START/PAUSE” key is pressed to resume the method. The following screenwill flash during the pause.

TEMP XX STAGE XMETHOD PAUSED

Note: If the “STOP” key is pressed while performing a method, thedisplay will flash the method name, aborted, and the temperature..

METHOD XABORTED XXXC

Note: If insufficient reagent for satisfying method parameters isdetected by the instrument, the following screens will toggle on thedisplay:

INSUFFICIENTREAGENT VOLUME

GO TO SETUP MENUITEM 1

9. If an initial reagent is not programmed, proceed to step 13.

WARNING

The vacuum pump must be operating continuously dur-ing manual addition of reagent. For instrumentsinstalled on laboratory work benches, provisions mustalso be made to handle any fumes which escape duringmanual reagent addition.

WARNING

If using hydrofluoric acid (HF), the acid must be addedmanually. The automated reagent addition module isnot designed or equipped to pump HF.

WARNING

If using hydrofluoric acid (HF), Teflon vessels must beused.

WARNING


Stop Method

InsufficientReagent

Manual ReagentAddition(Must Use for HF)


10. To add the reagent manually, press the “Pause” key to pause themethod; remove the clamp; lift the arm; slowly and carefully addthe reagent through the top of the condenser; quickly replace thearm; replace the clamp; and press the “Start” key to continue themethod.

WARNING

Avoid breathing reagent vapors. For work-benchinstalled instruments, if fumes are detected risingthrough the condenser, immediately replace the armand clamp and wait until the reaction has subsided andthe fumes have dissipated prior to completion of themanual reagent addition.

11. If an initial reagent is programmed, the following screen willappear.

REAGENT ADDITIONUPTAKE XXXXXXXX

12. Once initial reagent(s) has been added to the sample, the follow-ing screen will appear.

TEMP XX STAGE XRAMP XX:XX

13. As the temperature increases, the entered ramping time willcount down on the above screen. If desired temperature is reachedduring the entered ramping time, proceed to step 18, page 46.

14. If the desired temperature is not reached during the enteredramping time, the instrument will access the overtime phase, andthe following screen will appear.

TEMP XX STAGE XOVTM XX:XX:XX

Note: Overtime is the defined period of additional time for the instru-ment to reach the temperature parameter if, for some reason, it couldnot be reached during the ramp time.

15. The entered overtime will appear on the screen, and will begincountdown as the temperature increases. Once the temperatureparameter is reached, the overtime phase will end.

Note: Often during overtime, the temperature will slightly bypass thedesired temperature parameter. If this happens, the following screenwill appear.

TEMP XX STAGE XCOOL DOWN TO TAP

Note: TAP is defined as time at parameter.

Ru

n

46STAR System 2/6

600121Rev. 3

16. The instrument will pause until the sample cools to the targettemperature.

17. When the temperature parameter is reached, the following screenwill appear.

TEMP XX STAGE XTAP XX:XX:XX

18. The entered “time at parameter” (TAP) will be displayed, and thetime will begin countdown.

Note: If additional reagents or additions of aliquots of reagent are tobe added, the following screen will appear.

TEMP XX STAGE XUPTAKE XXXXXXXX

Note: Once the reagent addition is complete, the display will return tothe following screen.

TEMP XX STAGE XTAP XX:XX:XX

19. Once the “time at parameter” is complete, indicating that thestage is complete, the test will continue with additional stages orreturn to the Main Screen.

20. Upon completion of the test, the display will flash the methodname, completed, and the temperature.

METHOD XCOMPLETED XXXC

21. To print the selected method, the data from the test performed, orthe method setup parameters, press the “Print” key. The followingscreen will appear.

1 - ‘PR INT ’SELECTED METHOD

22. If needed, press the “+” and/or “–” Change keys to select the otheravailable printing functions.

2 - ‘PRINT’ DATAFROM LAST RUN

or

3 - ‘PRINT’ SETUPPARAMETERS

MethodCompleted

Print


23. Once the appropriate print function is selected, press the “Print”key. Based on the print function selected, one of the followingscreens will appear:

PRINTINGMETHOD

PRINTINGDATA

PRINTINGSETUP

24. Remove the vessel(s) containing the digested sample from theinstrument as follows:

WARNING


25. Remove the vessel clamp from the arm and condenser.

26. Lift the arm approximately 1” (2.5cm) from the top of the con-denser and lightly strike it two or three times on the condenserfrom this height to ensure that all reagent residue is removedfrom the small tube extending from the arm.

WARNING

To avoid burns, use hot pads when removing the vesselfrom a cavity.

WARNING

To prevent reagent vapors in the laboratory, always per-mit the sample to cool prior to removing the vessel fromthe instrument cavity.

27. Lift the vessel and condenser from the instrument cavity. Removethe condenser from the vessel. Cap the vessel to prevent reagentvapors from escaping into the laboratory.

NOTE

If a spill occurs during a test, a “Spill Detected” errormessage will occur. All cavities will pause operation.Refer to page 73 and remove spill. Replace liner if neces-sary. Once spill is removed, press the “Start/Pause” keyof each cavity which was in operation to resume thetest(s).

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48STAR System 2/6

600121Rev. 3

NOTE

Methods can be started at any stage. To begin a methodat a particular stage, access the “Program/Edit Menu.”Use the “+” and/or “–” Change keys to advance to thebeginning of the desired stage. Press the “Start” key. Ifthe desired stage is programmed “Inactive,” the displaywill indicate that the stage is inactive. Use the “+” and/or “–” Change keys to change the stage to “Active.”Then, press the “Start” key.

NOTE

If the STAR System 2/6 is idle for 10 minutes, it willautomatically turn off all lights and fans in the instru-ment.


This section covers routine maintenance, troubleshooting and basicservice instructions. For detailed instructions concerning service andrepair, contact the CEM Service Department or the nearest subsidiaryor distributor.

WARNING

If operation and maintenance instructions are notstrictly followed, serious injury and/or damage to theSTAR System 2 or 6 could result. CEM Corporation can-not accept responsibililty for unsatisfactory performanceor damage resulting from failure to comply with instruc-tions or safety practices.

WARNING

This instrument utilizes high voltages and microwaveradiation. Instrument service and repair should be per-formed only by technicians trained in repair and main-tenance of high voltages and microwave power systems.

WARNING

To avoid possible electrical shock or exposure to micro-wave energy, disconnect instrument from electrical out-let prior to any disassembly procedures.

WARNING

After performing any service to or inspection of theSTAR System 2 or 6 which requires removal of the frontor top cover or replacement of components in the micro-wave generation system, perform a microwave leakagemeasurement, page 52, prior to instrument operation.

WARNING

Proper precautions must be taken to avoid contact withreagents or reagent vapors. Protective gear should beworn as outlined in the user’s safety program for haz-ardous materials and the reagent manufacturer’s mate-rial safety data sheet. Refer to these guidelines forproper handling of the reagent

RoutineMaintenance,Troubleshooting,and Service

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50STAR System 2/6

600121Rev. 3

Routine maintenance should be performed on the instrument to pro-long the life of the instrument and minimize downtime. Routine main-tenance procedures should be performed as described below.

NOTE

Failure to properly maintain the STAR System 2 orSTAR System 6 will nullify the instrument warranty.

WARNING

Proper precautions must be taken to avoid contact withreagents or reagent vapors. Protective gear should beworn as outlined in the user’s safety program for hazard-ous materials and the reagent manufacturer’s materialsafety data sheet. Refer to these guidelines for properhandling of the reagent

Frequency Action

Daily Clean and inspect vessels for cracks or other damage.Ensure that all tubing on the reagent addition moduleis primed and that all connections are tight.Verify proper volume of liquids in scrubber (Refer to page14, item 13).Using tissue paper, ensure suction at the balljoint of thevapor collection system.Monitor liquid level in scrubber cylinders. Liquid levelshould remain below 2” (5cm) from top of cylinder. Emptyand replace scrubber solutions as required.

Weekly Inspect reagent addition tubing for damage.Verify pH levels of scrubber solutions. Replace as required.Inspect O-rings on scrubber containers and replace asrequired.Remove vacuum tubing and check for condensation orblockages.Perform a Quick Temperature Calibration.

Monthly Clean fan grills and fans with soft bristle brush or othercleaning tool capable of removing lint and build-up.Clean instrument cavity openings with damp cloth.Perform microwave leakage test.Inspect reagent pump syringe seal and replace as required.Inspect reagent pump syringe for rust or corrosion andreplace syringe as required.Inspect reagent pump tubing connections and tighten orreplace as required.Clean reagent valve stator and rotor and replace as required.

Annually Replace all vapor containment tubing.

As Required Lubricate reagent pump lead screw (every 1,000,000strokes of the syringe).

RoutineMaintenance

RoutineMaintenanceSchedule


WARNING


1. Remove all four reagent tubes from the reagent containers. Placethe reagent tubing into a clean suitable waste container. Select acavity and perform the prime method one (1) time for each of thefour reagent tubes. (Refer to Prime Method, page 41.)

2. Place all four reagent tubes into a container of deionized water.

3. Ensure that a vessel and condenser are properly positioned in theselected cavity and that a clamp is installed on the condenser andarm.

4. Perform the prime method on the selected cavity two (2) times foreach of the four reagent tubes.

5. Remove the reagent tubing from the container of water.

6. Perform the prime method on the selected cavity one (1) time foreach of the four reagent tubes using air only.

7. Position reagent tubing in reagent containers in accordance withlabeling for proper position.

8. Perform the prime method on selected cavity one (1) time for eachof the four reagent tubes to prime the reagent pump tubing withappropriate reagents. If a wash reagent is selected, prime thewash reagent tubing first so that the wash option will be availa-ble for the remainder of the reagents.

WARNING


1. Using a flat blade screwdriver, pry the cap from each scrubbercylinder.

2. Inspect both O-rings for distortion, cracks or other damage.Replace O-rings as required.

3. Empty and discard solution in accordance with material safetydata sheet for applicable reagent(s) being utilized and/or regula-tory requirements.

ReagentPumpFlush

ScrubberSolutionReplacement

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52STAR System 2/6

600121Rev. 3

4. Add solutions to scrubber cylinders: #1 - deionized water to top ofmarbles, #2 - 25% NaOH (sodium hydroxide) to top of marbles,and #3 - deionized water one-half distance of marbles.

NOTE

Ensure that sodium hydroxide is placed in the same cyl-inder each time it is replaced.

1. With instrument operating, use a federally approved microwaveleakage detector such as Holaday Model HI-1500 and measuremicrowave leakage around keyboard and display, fans on sides ofinstrument, and around individual panels of instrument.

2. Leakage should not exceed 5mW/cm2. If instrument shows exces-sive microwave leakage, do not attempt further operation. Con-tact CEM Service Department or local subsidiary or distributor.

NOTE

Microwave test meters are available from CEM Corpora-tion. CEM does not recommend use of inexpensivemeters available in electronics stores because they lackthe necessary sensitivity to properly test an instrumentfor microwave leakage.

WARNING


1. Remove all four reagent tubes from the reagent containers. Placethe reagent tubing into a clean suitable waste container. Select acavity and perform the prime method one (1) time for each of thefour reagent tubes. (Refer to Prime Method, page 41.)

2. Place all four reagent tubes into a container of deionized water.

3. Ensure that a vessel and condenser are properly positioned in theselected cavity and that a clamp is installed on the condenser andarm.

4. Perform the prime method on the selected cavity two (2) times foreach of the four reagent tubes.

5. Remove the reagent tubing from the container of water.

6. Perform the prime method on the selected cavity one (1) time foreach of the four reagent tubes.

MicrowaveLeakageMeasurement

Reagent PumpSyringeReplacement


7. Position the instrument on/off switch in the “off” position. Unplugthe instrument from the electrical outlet.

8. Remove the communications cable from the back of the vapor col-lection/reagent addition module.

9. Disconnect the two sections of black tubing from the back of thevapor collection/reagent addition module. Place the ends of thetubing into a suitable waste container.

10. Using Kimwipes or paper towels, remove any residual reagentfrom the ends of each of the vapor collection/reagent additionarms. Lift the vapor collection/reagent addition module from thetracks in the top of the instrument and tilt the module toward thefront of the instrument until the support brackets on the moduleare free from the slots in the instrument top cover. Remove themodule from the instrument.

GearPulley

Figure 15. Reagent Pump Gear Pulley

SupportBracket

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1.02.0

3.04.0

5.06.0

7.08.0

9.010.0

SyringeBarrel

Figure 16. Reagent Pump Syringe

SyringePlunger

Pin

11. Rotate the gear pulley of the reagent pump, located on the bottomof the pump, in a clockwise direction to lower the syringe suffi-ciently to permit removal of the syringe barrel.

12. Remove the pin from the base of the plunger. Loosen the screw inthe syringe clamp.

SyringeClamp

54STAR System 2/6

600121Rev. 3

13. While pulling down slightly, carefully unscrew the glass syringebarrel from the luer lock fitting.

NOTE

Rotate the gear pulley of the pump in a counterclock-wise direction to raise or clockwise direction to lower thesyringe shaft as necessary during syringe installation.

14. Place the plunger of the new syringe on the plunger shaft. Alignthe barrel with the luer lock fitting.

CAUTION

Installation of the syringe barrel requires pushingupward during installation to avoid stripping thethreads on top of the barrel.

15. While pushing upward, carefully screw the syringe barrel into theluer lock fitting.

16. Install the pin in the base of the plunger. Tighten the screw in thesyringe clamp.

17. Position the vapor collection/reagent addition module on top ofthe main instrument. Position the support brackets of the moduleinto the slots on the back of the main instrument top cover.Ensure that the feet of the module are positioned and secured intothe tracks of the top cover.

18. Connect the communications cable from the main instrument tothe vapor collection/reagent addition module.

19. Install the ends of the two sections of black tubing labeled “Con-nect to Vapor Collection Module” on the back of the vapor collec-tion/reagent addition module.

20. Position the four reagent tubes into the proper reagent contain-ers. If necessary, secure the tubing to the containers to avoid anyspillage of reagents.

21. Plug the instrument into the electrical outlet, and position the on/off switch in the “on” position. Perform the prime method one (1)time for each of the four reagent tubes to prime the reagentpump. If a wash reagent is selected, prime the wash reagent tub-ing first so that the wash option will be available for the remain-der of the reagents.


WARNING


1. Perform steps 1 through 10 of “Reagent Pump Syringe Replace-ment,” page 52.

2. Rotate the gear pulley of the reagent pump, located on the bottomof the pump (figure 14), in a clockwise direction to lower thesyringe to its lowest point.

3. Remove the pin from the base of the plunger. Slightly rotate theplunger away from the barrel, and remove the plunger from theshaft.

4. Using pliers, grip the seal approximately one-third of the waydown and remove the seal from the plunger.

5. Remove the O-ring from the top of the plunger. If necessary, useneedle nosed pliers to assist in removal of the O-ring.

6. Install the new O-ring on the top of the syringe plunger, usingcaution to avoid distortion or damage to the O-ring. If necessary,use needle nosed pliers to assist in the installation of the O-ring.

7. Wet the plunger tip and the O-ring with deionized water.

8. Place the seal on a flat surface with the open end facing upward.Firmly press the tip of the plunger into the open end of the sealuntil it snaps into position.

Reagent PumpSyringe SealReplacement

Figure 17. Reagent Pump Syringe Plunger with Seal

O-Ring

O-Ring

Seal Seal

Plunger Plunger

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600121Rev. 3

9. Lay the plunger on a solid flat counter with the tip of the plunger(from the O-ring outward) hanging over the edge of the counter.Slowly roll the plunger along the edge of the counter while press-ing firmly on the portion of the seal below the O-ring. Rotate theplunger three (3) complete turns to ensure that the sharp, raisededge of the plunger bites into the seal for a secure fit.

10. Wet the seal with deionized water.

11. Install the plunger on the shaft, and install the pin in the base ofthe plunger.

12. Rotate the gear pully counterclockwise sufficiently to insert theplunger into the glass syringe barrel.

13. Perform steps 17 through 21 of “Reagent Pump Syringe Replace-ment,” page 54.

WARNING


CAUTION

Only the lubrication available from CEM Corporationshould be used to lubricate the reagent pump leadscrew. Other lubricants can cause the pump to malfunc-tion. Lubrication of the reagent pump lead screw is usu-ally needed only after approximately 1,000,000 strokesof the syringe. If lubrication is needed more frequently,attempt to identify a cause.

1. Remove all four reagent tubes from the reagent containers. Placethe reagent tubing into a clean suitable waste container. Select acavity. Ensure that a vessel and condenser are properly placed inthe selected cavity. Perform the prime method one (1) time foreach of the four reagent tubes.

2. Place all four reagent tubes into a container of deionized water,and perform the prime method on the selected cavity two (2)times for each of the four reagent tubes.

3. Remove all four reagent tubes from the container of water andperform the prime method on the selected cavity one (1) time foreach of the four reagent tubes. (Refer to Prime Method, page 41.)

4. Remove the communications cable from the back of the vapor col-lection/reagent addition module. Remove the two sections of blacktubing from the back of the vapor collection/reagent addition mod-ule. Place the tubing into a suitable waste container.

Reagent PumpLead ScrewLubrication



6. Using Kimwipes or paper towels, remove any residual reagentfrom the ends of each of the vapor collection/reagent additionarms. Lift the vapor collection/reagent addition module from thetracks in the top of the instrument and tilt the module toward thefront of the instrument until the support brackets on the moduleare free from the slots in the instrument top cover. Remove themodule from the instrument.

7. Using the appropriate lubrication from CEM Corporation, lubri-cate the lead screw.

8. Position the vapor collection/reagent addition module on top ofthe main instrument. Position the support brackets of the moduleinto the slots on the back of the main instrument top cover.Ensure that the feet of the module are positioned and secured intothe tracks of the top cover.

9. Connect the communications cable from the main instrument tothe vapor collection/reagent addition module. Install the ends ofthe two sections of black tubing labeled “Connect to Vapor Collec-tion Module” on the back of the vapor collection/reagent additionmodule.

10. Position the four reagent tubes into the proper reagent contain-ers. If necessary, secure the tubing to the containers to avoid anyspillage of reagents.

11. Plug the instrument into the electrical outlet, and position thepower switch in the “on” position. Perform the prime method one(1) time for each of the four reagent tubes to prime the reagentpump. If a wash reagent is selected, prime the wash reagent tub-ing first so that the wash option will be available for the remain-der of the reagents.

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58STAR System 2/6

600121Rev. 3

1.02.0

3.04.0

5.06.0

7.08.0

9.010.0

Figure 18. Reagent Valve Tubing

Valve

Connector

WARNING


1. Remove all four reagent tubes from the reagent containers. Position allfour tubes into a clean, suitable waste container. Select a cavity. Place avessel and condenser in the selected cavity. Install a vessel clamp. Per-form the prime method one (1) time, with air only, for each of the fourreagent tubes.

2. Place the reagent tubing into a container of deionized water. Performthe prime method on the selected cavity two (2) times for each of thefour reagent tubes.

3. Remove the reagent tubing from the container of deionized water. Per-form the prime method on the selected cavity one (1) time for each ofthe four reagent tubes.

4. Remove the vessel clamp. Lift the vapor collection arm approximately 1”(2.5cm) from the top of the condenser and lightly strike it two or threetimes on the condenser from this height to ensure that all reagent resi-due is removed from the small tube extending from the arm. Using Kim-wipes or paper towels, remove any remaining residual reagent from theends of each of the vapor collection/reagent addition arms.

5. Position the instrument on/off switch in the “off” position. Unplug theinstrument from the electrical outlet.

6. Ensure that all arms of the vapor collection/reagent addition module areraised. Remove all shields, vessels and condensers from the instrument.

7. Using a small flat blade screwdriver, remove the communications cablefrom the back of the vapor collection/reagent addition module.

8. Lift the vapor collection/reagent addition module, with black tubinginstalled, from the tracks in the top of the main instrument and tilt themodule toward the front of the instrument until the support brackets onthe module are free from the slots in the instrument top cover. Removethe module from the instrument.

Cleaning ofReagent ValveRotor & Stator

9. Tilt the module backward and,using a dispensing bottle, ejectdeionized water into the tips ofthe module arms to removeany residual reagent from thearms. Permit the water todrain from the black tubing.

10. Disconnect the two sections ofblack tubing from the back ofthe vapor collection/reagentaddition module.

11. Disconnect the tubing connec-tor from the right side (facingmodule) of the reagent pumpvalve.


Bolts

Face Plate

Spacer

Body

Stator

Figure 19. Reagent Valve

21. Remove the rotor from the rotor housing.

22. Using deionized water, clean the rotor and stator, ensuring that allshavings are removed

CAUTION

Do not use water to clean the valve rotor and/or stator wheninstalled in the valve. Residual moisture can collect in thelubricated areas and cause corrosion of the valve parts.

23. Install the rotor in the rotor housing with the slotted side facingupward.

24. Install the stator on the pins of the rotor with the convex side down-ward. Ensure that the alignment mark is positioned for proper installa-tion.

25. Install the spacer on the valve head, ensuring that the alignment markis positioned for proper installation.

26. Carefully install the face plate on the valve head. Use caution to avoidcrimping any tubing or pulling any tubing from fittings or installed posi-tion. Using an Allen wrench, install the screws in the face plate of thevalve.

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Valve HeadScrew

12. Using a 5/16” box wrench, remove thescrews and rear metal plate from the mod-ule. Position the rear plate to the side ofthe module to permit access to the valve.

13. Remove the Keps nuts from the manifold.Slide the manifold down tubing away fromvalve and instrument.

14. Using a pencil or marking device, markthe face plate, spacer and body of thevalve to establish proper installed positionduring assembly.

15. Using a 9/64” Allen wrench, remove thevalve head screw from the valve. Care-fully lift the valve head from the valveand out of the module.

16. Using a 7/64” Allen wrench, remove thebolts from the face plate of the valve.

17. Remove the metal face plate of the valve,using caution to avoid pulling any tubingfrom its proper installed position or crimp-ing any of the tubing.

18. Remove the spacer from the valve head.

19. Using a pencil or marking device, markthe stator to establish proper installedposition during assembly.

20. Remove the stator from the pins.

60STAR System 2/6

600121Rev. 3

27. Install the assembled valve head on the valve body. Using a 9/64” Allenwrench, install the screw in the valve head.

28. Slide the manifold down the tubing and position and install it on theside of the module.

29. Route the reagent tubing from the valve through the front of module andconnect it to the right side of the reagent pump valve.

30. Install the metal rear plate on the module, using caution to avoid crimp-ing any wiring or tubing.

31. Carefully lift the vapor collection/reagent addition module to the top ofthe main instrument. While leaning the module toward the front of theinstrument, position the support brackets of the module into the slots onthe back of the top cover. Ensure that the feet of the module are posi-tioned and secured into the tracks of the top cover.

32. Install the communications cable between the main instrument and thevapor collection/reagent addition module. Connect the two sections ofblack tubing to the vapor collection/reagent addition module.

33. Install the four reagent tubes in the reagent containers, ensuring thattubing is placed in the proper container.

34. Perform the prime method for each of the four reagent tubes to primethe tubing with the proper reagent.

1. Select the cavity to be calibrated.

NOTE:

Each cavity must be calibrated.

2. Press the “SETUP” key. Press the “+” key seven (7) times or untilthe following screen appears.




CAUTION

Teflon vessels must be selected if using hydrofluoricacid.

4. Use the “+” and/or “–” Change keys to select either quartz/glassvessels or Teflon vessels.

QuickTemperatureCalibration


NOTE

The following calibration procedure is based on usingnitric acid (quartz/glass) vessels) or deionized water (tef-lon vessels). If the boiling point of the reagent is known,use the appropriate data for calibration. If the boilingpoint is not known, boil 50mL of either nitric acid orwater (based on type of vessel used) on a hot plate, and,with a certified thermometer, measure the temperatureof the reagent while boiling. CEM Corporation recom-mends using nitric acid for the quick temperature cali-bration procedure for quartz/glass vessels unless themajority of target temperatures are approximately100°C. For temperatures of approximately 100°C, CEMrecommends using deionized water to perform the quickcalibration procedure for quartz/glass vessels, also. Rea-gents other than nitric or deionized water may be uti-lized, if desired, based on type of vessel used.

5. Ensure that the liner is positioned so that the opening in the bot-tom of the liner is positioned directly above the opening in thespill tray assembly. To promote even boiling, place a CEM boilingtube in the vessel, ensuring that one end of the tube extendsbelow the surface of the reagent and the other end is above thesurface. Place a vessel containing 20mL of nitric acid (quartz/glassvessels) or deionized water (Teflon Vessels) in the selected cavity.Place a condenser on the vessel. Lower the vapor collection armand install a vessel clamp. Ensure that the shield is positionedwith the plate toward the front of the instrument. Position thetoggle switch of the vacuum pump in the “on” position.


CARE CALIBRATIONWILL CHANGE!!!


LO CAL TEMP XXXPRESS START


8. If necessary, use the “+” and/or “–” Change keys to edit the “lo cal”temperature value based on the vessel type, the reagent used and/or the reagent boiling point determined above.



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600121Rev. 3

10. Wait for the “cal data” of the nitric acid in the vessel to rise. Oncethe “cal data” is constant, press the “STOP” key. The followingscreen will appear.

HI CAL TEMP XXXPRESS START

11. Press the “HOME” key to return to the following screen.

METHOD X(XXXXX)

12. If desired or required, verify quick temperature calibration as out-lined below.

1. Ensure that overtime is programmed for 10 minutes in the instru-ment setup procedures.

2. Select the cavity to be utilized.

METHOD X(XXXXX)


3. To select a particular method (1 - 20), press the “+” and/or “–”Change keys. Select a method which is not programmed or whichcan be edited for calibration verification.


CHANGE METHODNAME (YES)

5. Press the “+” and “–” Change keys to toggle to “yes.”


METHOD X(XXXXX)

7. Use the “+” and/or “–” Change keys to enter or edit the first letter(upper case or lower case letter, symbol or number).

8. Press the “NEXT” key and the “+” and/or “–” Change keys to enteror edit each letter, symbol and/or number of the method name (24characters maximum).

9. Once the complete method name has been entered, press the“BACK” key until the “Change Method Name” screen is displayed.

Verification ofQuickTemperatureCalibration



UPDATE INITIALREAGENT (YES)

11. Press the “+” and “–” Change keys to toggle to “no.”


METHOD XSTAGE 1


STAGE (INACTIVE)

14. Press the “+” and “–” Change keys to toggle to “active.”


RAMP TIME0 MINS 00 SECS


RAMP TIMEXX MINS 00 SECS

17. Press the “+” key to enter 1 second of ramp time.


TEMPERATURETARGET 30

19. Press the “+” and/or “–” Change keys to enter a target tempera-ture 200°C.

20. Press the “Home” key. The following screen will appear.

METHOD X(XXXXX)

21. Place a vessel containing the 20mL of nitric acid (quartz/glass ves-sels) or deionized water (Teflon vessels) used for “Quick Tempera-ture Calibration” in the selected cavity. Place a CEM boiling tubein the vessel, one end above the surface and the other below thesurface of the reagent. Place a condenser on the vessel. Lower thevapor collection arm and install a vessel clamp. Ensure that theshield is positioned with the plate toward the front of the instru-ment. Position the toggle switch of the vacuum pump in the “on”position.

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600121Rev. 3

22. Press the “Start” key for the selected cavity. Because the instru-ment is unable to reach the target temperature of “200°C” in theramp time of 1 second, the instrument will access the overtimephase, and the following screen will appear.

TEMP XX STAGE 1OVTM 10:00:00

23. Once the reagent reaches a rolling boil and the temperaturebecomes constant, press the “Stop” key.

24. The temperature in step 23 should be the temperature deter-mined when boiling the nitric acid or water on a hot plate asdescribed on page 56 or 121°C (boiling temperature of nitric acidat STP) ± 3°C or 100°C (boiling temperature of water at STP)±5°C. If verifying the high calibration value with sulfuric acid(quartz/glass vessels) or nitric acid (Teflon vessels), the tempera-ture in step 23 should be 330°C or determined boiling point (±5°C) for sulfuric or 121°C or determined boiling point (± 5°C) fornitric.


TroubleshootingChart

Symptom Possible Cause Remedy

Instrument Inoperative Power cord not plugged into Plug power cord into electrical(No Power) electrical outlet outlet

Blown fuse(s) Replace fuse(s)

Loose connections * Verify all connections

Blown power supply fuse * Replace power supply fuse

Faulty power supply * Replace power supply

Intermittent or No Loose or faulty connectors in * Tighten/replace connectorsPower to Instrument power inlet

Power cord not properly Remove and reinstall power cordinstalled

Loose DC connector * Tighten DC connector

Cell Inoperative Vapor containment/reagent Position vapor containment/addition arm not down reagent arm in down position

No vessel in cavity Place vessel in cavity

Vessel-in-position sensor Replace vessel support ring assy.

Insufficient reagent indicated Check and fill reagent container(s)by software as required. Enter reagent volume

(Setup)

No Microwaves Faulty high voltage * Replace triac, magnetron, filamentcomponent(s) transformer, high voltage trans-

former, and/or capacitor as required

Disconnected temperature * Connect temperature sensorsensor

Slot fails to open * Verify operation of motor and slot

Low Microwave Power Line voltage below required Increase line voltage to specificationin One Cell specification

Faulty slot * Replace slotFaulty motor * Replace motorFaulty high voltage * Replace high voltage component(s)component(s)

Low Microwave Power Line voltage below required Increase line voltage to specificationInstrument (All Cells) specification

Faulty magnetron cooling fan * Replace fanFaulty magnetron * Replace magnetronFaulty high voltage * Replace high voltage component(s)component(s)

Intermittent Microwaves Faulty magnetron cooling fan * Replace fanFaulty magnetron thermal * Replace switchswitchFaulty high voltage wires * Replace high voltage wiringFaulty high voltage * Replace high voltage component(s)component(s)

No Control of Microwave Faulty motor or PC board * Replace motorPower in Individual Cell * Replace PC board

No Control of Microwave Faulty triac or PC board * Replace triacPower in instrument * Replace PC board

*Requires a technician trained in repair and maintenance of high voltages and microwave powersystems.

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Fuse Blows During Faulty high voltage * Replace high voltage component(s)Operation component(s)

Faulty triac * Replace triac

Faulty power supply * Replace power supply

Blank Display on Loose or faulty connection on Verify/replace connectionIndividual Cavity display

Blank Displays on Power cord not connected to Plug power cord into electricalInstrument (All Cavities) electrical outlet outlet

Fuse drawer not installed Install fuse drawer

Blown fuse or fuse not Install fuse or replace faulty fuseinstalled

Blown power supply fuse * Replace power supply fuse

Loose connection on display * Tighten all connections on displayboard board

Loose connection on CPU * Verify all connections on CPUboard board

Faulty display board * Replace display board

Faulty CPU board * Replace CPU board

Faulty power supply board * Replace power supply board

Keyboard Inoperative Loose or damaged cable from Connect/tighten/replace cablekeyboard to control board

Faulty keyboard * Replace keyboard

Faulty control board * Replace control board

Fan(s) Inoperative Loose or faulty connection on * Tighten/replace connection onfan(s) fan(s)

Faulty fan(s) * Replace fan(s)

Faulty PC board * Replace PC board

No Cavity Lighting Faulty light bulb * Replace light bulb

Loose or faulty light * Tighten/replace connectionsconnection(s)

Faulty PC board * Replace PC board

Thermal Overload Cooling fan not operating Check for blockage of air inletMessage areas

Turn instrument off, wait for 10minutes, retry operation

* Verify fan connections

* Replace fan as required.

Faulty magnetron thermal * Replace switchswitch

Inaccurate Temperature Cell(s) not properly calibrated Perform temperature calibrationReadings of cavity(s)

Cavity insulator improperly * Replace insulatorpositioned

Inoperative fan(s) * Replace faulty fan(s)




No Reagent Addition Reagent module not installed Install reagent addition module

Cable not connected Connect cable between maininstrument and reagent additionmodule

Empty reagent container(s) Fill reagent container(s)

Inoperative syringe pump Call CEM Service Department

Reagent addition tubing Route reagent tubing through tipincorrectly routed of arm

Faulty reagent addition module Replace reagent addition module

Faulty valve Replace valve

Noisy Reagent Pump Dirty motor lead screw Clean and lubricate lead screw

Frequent Syringe Stalls Dirty motor lead screw and/or Clean encoder with airencoder Clean and lubricate lead screw

Incorrect Volume of Tubing dirty, crimped or Straighten, clean or replace tubingReagent Delivered frayed

Loose or faulty connection Tighten/replace connection

Syringe not tightened on valve Tighten syringe

Dirty syringe Clean/replace syringe

Damaged seal Replace seal

Damaged valve fittings Replace valve

Insufficient reagent Fill reagent container

Reagent Dispensed Into Faulty valve motor Verify valve movement and thatReagent Container encoder changes position with eachRather Than Vessel valve movement.

Faulty valve Replace valve

Bubbles in Reagent Loose fittings Tighten or replace fittingsAddition Syringe

Fluid Leakage from Temperature of reagent too Permit reagent to warm to roomBottom of Syringe low temperature

Dirty, blocked or crimped Straighten, clean or replace tubingtubing

Damaged seal Replace seal

Variable or Moving Dirty, blocked or crimped Straighten, clean or replace tubingAir Gap tubing

Loose or damaged connections Tighten/replace connections

Syringe incorrectly installed Remove and reinstall syringe

Faulty valve Replace reagent pump valve

Bubbles in Reagent Loose syringe and/or fittings Inspect tubing connections andtighten as required

Inspect syringe and tighten asrequired


Tro

ub

lesho

otin

g

68STAR System 2/6

600121Rev. 3


Reagent Addition Pump Tubing not in reagent Position tubing in correct reagentLoses Prime container(s) containers

Loose fittings Verify that all fittings on valveand module are tight

Crimped tubing Check all tubing for crimps

Suction in reagent tubing Ensure that reagent containers arenot airtight.

Vapors in Laboratory Vapor containment module Install vapor containment modulenot installed

Loose or damaged connections Tighten/replace connectionson vapor containment module

Vacuum pump not turned on Turn vacuum pump on

Vent hose to fume hood not Install vent hose in fume hoodinstalled

Scrubber solution(s) losing Verify effectiveness of solutionsefficiency with pH paper and replace any

solution that is neutral or acidic

Scrubber Not Removing Scrubber solution(s) losing Verify effectiveness of solutionsVapors efficiency with pH paper and replace any

solution that is neutral or acidic

Loose or damaged connections Tighten/replace connectionson scrubber or vacuum pump

Clean scrubber and tubing



ErrorMessages

Error Message Symptom/Cause Remedy

PIC LATCH ERROR All methods paused. Press “Home” key to clear error.Any unidentified error will Operator can either resume or stopbe displayed with this error methods.message. * Possible faulty control board if

error continues.

THERMAL OVERLOAD All methods paused. Press “Home” key to clear error.Magnetron has overheated. Operator can either resume or stop

methods.* Replace fan, magnetron and/oroverload switch if error continues.

PIC COMM TIMEOUT All methods paused. Press “Home” key to clear error.Communication failure Operator can either resume or stopbetween PIC Processor and methods.main processor. * Replace control board if error

continues.

PIC COMM CRC ERR All methods paused. Press “Home” key to clear error.Incorrect CRC calculated on Operator can either resume or stopcommunication from PIC methods.Processor. * Possible faulty control board if

error continues.

PIC COMMAND All methods paused. Press “Home” key to clear error.ERROR Command not recognized by Operator can either resume or stop

PIC Processor. methods.* Possible faulty control board orother hardware if error continues.

PIC CRC ERROR All methods paused. Press “Home” key to clear error.CRC error calculated by Operator can either resume or stopPIC Processor. methods.

* Possible faulty control board iferror continues.

VALVE INIT ERROR All methods paused. Press “Home” key to clear error.Valve could not be initialized. Operator can either resume or stop

methods.* Possible faulty valve, encoder orcable on reagent pump.

VALVE HOME All methods paused. Press “Home” key to clear error.ERROR Valve could not find home. Operator can either resume or stop


VALVE LOST All methods paused. Press “Home” key to clear error.System does not know reagent Operator can either resume or stopvalve position and cannot methods.position valve. * Possible faulty valve, encoder orEncoder problem. cable on reagent pump.

ENCODER ERROR All methods paused. Press “Home” key to clear error.Valve encoder error detected. Operator can either resume or stop


PIC UNKNOWN All methods paused. Press “Home” key to clear error.ERROR Error displayed by HEX Operator can either resume or stop

number. Error will not equate methods.with any known error Record HEX number and contactcondition. CEM Service Department.


Erro

r Messag

es

70STAR System 2/6

600121Rev. 3


REAGENT PUMP Reagent pump initialize error. System will attempt to reinitializeINIT ERROR Pump will not accept pump prior to aborting method. If

commands until it has been successful, method will continue. Ifproperly initialized. unsucccessful, method will abort.

Turn instrument off and back on.

REAGENT PUMP System is stopped. Turn instrument off and back on toINVALID CMD Incorrect command issued. clear error.

REAGENT PUMP System is stopped. Turn instrument off and back on toINVALID OPR Invalid parameter given with clear error.

command.

REAGENT PUMP System is stopped. Turn instrument off and back on toINVALID SEQUENCE Incorrect command structure clear error.

or communications protocol.

REAGENT PUMP Reagent pump not initialized. System will attempt to initializeNOT INITIALIZED pump prior to aborting method. If

successful, method will continue. Ifunsuccessful, method will abort.Turn instrument off and initializepump to clear error.

REAGENT PUMP Pump syringe plunger loses System will attempt to initializePLUNGER OVLD steps. pump prior to aborting method. If

successful, method will continue. Ifunsuccessful, method will abort.Turn instrument off and initializepump to clear error.

REAGENT PUMP Valve drive loses too many System will attempt to initializeVALVE OVLD steps. pump prior to aborting method. If

successful, method will continue. Ifunsuccessful, method will abort.* If error continues, replace reagentpump.

REAGENT PUMP System is stopped. Turn the instrument off and backPLUNGER ERR Plunger movement commands on to clear error.

not allowed when valve is inbypass or throughput position.

REAGENT PUMP System is stopped. Turn the instrument off and backCOMMAND OVFL Pump buffer contains too many on to clear error.

characters to permit commandto be executed.

REAGENT PUMP System is stopped. Turn the instrument off and backRETRY ERROR Reagent pump not responding on to clear error.

to commands and retry timeris timing out.

SPILL DETECTED Cavity operation is stopped. Turn instrument off.TURN UNIT OFF All other methods are paused. Clean spill as required.

CELL Cell operation is stopped. Calibrate temperature in cellNOT CALIBRATED Cell (cavity) will not operate (cavity).

because temperature valuesare unavailable.

TIME ERROR No time programmed in stage Program minimum of 1 second ramp1 of method. time in first stage of method.




REAGENT ADDITION Reagent Addition not installed Turn system off. Ensure that NOT INSTALLED or system unable to detect/ Reagent Addition and cables

initialize pump or valve. are properly installed.

INSUFFICIENT Cavity inoperable. If necessary, fill reagent containers.REAGENT VOLUME Insufficient reagent volume to Enter reagent volume for system

perform method. in Setup menu.

VESSEL NOT IN Cavity operation is paused. Place vessel in cavity and press thePOSITION System detects that no vessel “Start/Pause” key.

is in cavity.

ARM NOT IN Cavity operation is paused. Place vessel and condenser inPOSITION System detects that arm is cavity. Lower arm. Press “Start/

not properly positioned. Pause” key.

EE Prom Calibration Press “Home” key to clear error.Data Error Messages Turn the instrument off.

EE ERROR 1 Error verifying LoCalTemp * Replace EE Prom on the control EE ERROR 2 Error verifying HiCalTemp board.EE ERROR 3 Error verifying RawCalLoEE ERROR 4 Error verifying RawCalHiEE ERROR 5 Error verifying CalTimeEE ERROR 6 Time out reading EE Prom

busybitEE ERROR 7 Error verifying MagPower 1EE ERROR 8 Error verifying MagPower 2EE ERROR 9 Error verifying MagPower 3EE ERROR 10 Error verifying MagPower 4EE ERROR 11 Error verifying MagPower 5EE ERROR 12 Error verifying MagPower 6EE ERROR 13 Error writing EE Prom

PRINTER Printer is turned off. Ensure that printer is plugged inand turned on.

Printer is out of paper. Ensure that printer has paper.Busy flag stays active for >11seconds after reset is issued.

ISR FAILURE All methods paused. Call CEM Service DepartmentTURN UNIT OFF System lost Interrupt Service

Routine. Hardware failure.


Erro

r Messag

es

72STAR System 2/6

600121Rev. 3

WARNING

This instrument utilizes high voltages and microwaveradiation. Instrument service and repair should be per-formed only by technicians trained in repair and main-tenance of high voltages and microwave power systems.

WARNING

To avoid possible electrical shock or exposure to micro-wave energy, disconnect instrument from electrical out-let prior to any disassembly procedures.

WARNING


WARNING


WARNING

Prior to troubleshooting or replacement of any compo-nent in the high voltage section of the System 2/6, theinstrument must be switched off and unplugged fromthe electrical outlet. Permit instrument to sit idle for atleast two minutes. Using a well insulated screwdriver,touch the end of the screwdriver between terminals ofthe high voltage capacitor to discharge all residual volt-age from the instrument.

Service

Figure 20. Discharge of Residual Voltage from High Voltage Capacitor

HighVoltageCapacitor


If a spill occurs, the spill tray must be removed, emptied and cleaned.To remove spillage, proceed as follows:

WARNING


1. Turn the instrument off and unplug it from the electrical outlet.Remove the vessel clamps. Ensure that all arms of the vapor col-lection/reagent additon module are raised. Remove all vessels andcondensers. Remove shield holders from each cavity.

2. Remove the communications cable from the back of the vapor col-lection/reagent addition module. Remove the two sections of blacktubing from the back of the vapor collection/reagent addition mod-ule. Place the ends of the tubing into a suitable waste container.

3. Using Kimwipes or paper towels, remove any residual reagentfrom the ends of each of the vapor collection/reagent additionarms.

WARNING

Dispose of contaminated Kimwipes or paper towels inaccordance with user’s safety program for hazardousmaterials and the reagent manufacturer’s materialsafety data sheet.

4. Lift the vapor collection/reagent addition module from the tracksin the top of the instrument and tilt the module toward the frontof the instrument until the support brackets on the module arefree from the slots in the instrument top cover. Remove the mod-ule from the instrument and place it on the counter or workbenchusing extreme caution to avoid pulling the reagent tubing fromthe reagent containers.

CAUTION

Use caution when removing the front panel to avoidbreaking the glass panel installed on the front cover.

5. Using pliers or a flat blade screwdriver, remove the screw covers.Remove the screws from the bottom of the instrument front panel.Pull the front panel down until its tabs are free from the slots inthe top cover and remove the front panel.

6. Remove the screws and remove and position the top cover, withthe display cable installed, to the back of the main instrument.Use caution to avoid disconnecting the display cable.

SpillRemoval

Service

74STAR System 2/6

600121Rev. 3

7. Loosen the setscrew and remove the vessel support ring assemblyfrom the cavity. Remove the liner from the cavity and check theliner for cracks or damage. Replace the liner as required.

CAUTION

If using hydrofluoric acid, the liner must be replaced.

WARNING

Proper precautions must be taken to avoid contact withreagents or reagent vapors. Protective gear should beworn as outlined in the user’s safety program for haz-ardous materials and the reagent manufacturer’s mate-rial safety data sheet. Refer to these guidelines forproper handling of the reagent. Based on type of rea-gent, neutralization may be necessary prior to removalof spill tray.

Note: For neutralization of HF, CEM Corporation recommends a 20%solution of magnesium sulfate (20 g of salt crystals mixed with 80 g ofdeionized water). To neutralize the HF spill, fill a dispensing bottlewith approximately 200mL of the magnesium sulfate solution. Slowlyadd approximately 10mL of the solution to the spill tray. The reactionwill produce a vapor. Once the spill tray is emptied in step 10 below,rinse the tray with the remainder of the magnesium sulfate; thenrinse it with deionized water.

8. Loosen the clamp securing the channel of the spill tray to the RFstub of the cavity.

9. Slide the spill tray down and away from the RF stub, using cau-tion to avoid damage to the sensor board and cable installed onthe bottom of the tray.

��

��

SpillTray

Clamp

RFStub

Figure 21. Spill Tray


10. Empty the spill tray into a suitable reagent waste disposal con-tainer and rinse any residual material from the tray. Dry the spilltray with suitable acid wipes.

11. Neutralize any other liquid present in the cavity with magnesiumsulfate and wipe up with acid wipes. Dispose of wipes in accor-dance with user’s safety program for hazardous materials andreagent manufacturer’s material safety data sheet.

Note: If necessary, replace the spill tray.

12. Install the spill tray on the RF stub, using caution to avoid dam-age to the sensor board and cable installed on the bottom of thetray. Push the tray up on the RF stub until the lip of the channelis against the bottom of the RF stub.

13. Install the clamp on the channel of the spill tray and tighten itsecurely to prevent the spill tray from moving freely. Install cableconnections.

14. Install the liner in the cavity, ensuring that the opening in thebottom of the liner is properly aligned with the opening in thespill tray assembly.

15. Install the vessel support ring assembly on the cavity. Secure thering with the setscrew.

16. Install the instrument top cover, and secure it with screws, ensur-ing that the display cable is routed away from the vessel supportrings. Install the instrument front cover, ensuring that the tabs atthe top of the cover engage the slots in the top cover. Install thescrews and screw cover bases to secure the front cover.

17. Position the vapor collection/reagent addition module on top ofthe main instrument using extreme caution to avoid pulling thereagent tubing from the reagent containers. Position the supportbrackets of the module into the slots on the back of the maininstrument top cover. Ensure that the feet of the module are posi-tioned and secured into the tracks of the top cover.

18. Connect the communications cable from the main instrument tothe vapor collection module. Install the ends of the two sections ofblack tubing labeled “Connect to Vapor Collec-tion Module” on theback of the vapor collection/reagent addition module.

19. Plug the instrument into the electrical outlet, and position thepower switch in the “on” position.

20. Ensure that the selected cavity contains a vessel and a condenserand that a clamp is installed on the condenser and arm. Performthe prime method one (1) time for each of the four reagent tubesto prime the reagent pump. If a wash reagent is selected, primethe wash reagent tubing first so that the wash option will beavailable for the remainder of the reagents.

21. Carefully install all screw covers.

Service

76STAR System 2/6

600121Rev. 3

WARNING


WARNING


1. Remove the vessel clamps. Ensure that all arms of the vapor col-lection/reagent addition module are raised. Remove all vesselsand condensers. Remove shield holders from each cavity.


3. Remove the communications cable from the back of the vapor col-lection/reagent addition module. Remove the two sections of blacktubing from the back of the vapor collection/reagent addition mod-ule. Place the ends of the tubing into a suitable waste container.

4. Using Kimwipes or paper towels, remove any residual reagentfrom the ends of each of the vapor collection/reagent additionarms. Lift the vapor collection/reagent addition module from thetracks in the top of the instrument and tilt the module toward thefront of the instrument until the support brackets on the moduleare free from the slots in the instrument top cover. Remove themodule from the instrument and place it on the counter or work-bench using extreme caution to avoid pulling the reagent tubingfrom the reagent containers.

CAUTION


5. Using pliers or a flat blade screwdriver, remove the screw covers.Remove screws and screw cover bases from the front cover. Pullthe front cover of the main instrument down and away from theinstrument.

6. Remove screws and lift and position the top cover, with displaycable installed, to the back of the main instrument. Use caution toavoid disconnecting cable.

7. Loosen the setscrew and vessel support ring assembly from thecavity.

VesselLinerReplacement


8. Remove the liner from the cavity and check the liner for cracks ordamage.

9. Install the liner in its appropriate cavity, ensuring that the open-ing in the bottom of the liner is properly aligned with the openingin the spill tray assembly.

10. Install the vessel support ring assembly on the cavity. Secure thering with the setscrew.

11. Install the instrument top cover, and secure it with screws, ensur-ing that the display cable is routed away from the vessel supportrings. Install the instrument front cover, ensuring that the tabs atthe top of the cover engage the slots in the top cover. Install thescrews and screw cover bases to secure the front cover.

12. Position the vapor collection/reagent addition module on top ofthe main instrument using extreme caution to avoid pulling thereagent tubing from the reagent containers. Position the supportbrackets of the module into the slots on the back of the maininstrument top cover. Ensure that the feet of the module are posi-tioned and secured into the tracks of the top cover.

13. Connect the communications cable from the main instrument tothe vapor collection/reagent addition module. Install the ends ofthe two sections of black tubing labeled “Connect to Vapor Collec-tion Module” on the back of the vapor collection/reagent additionmodule.

14. Plug the instrument into the electrical outlet, and position thepower switch in the “on” position.

15. Ensure that the selected cavity contains a vessel and a condenserand that a clamp is installed on the condenser and arm. Performthe prime method one (1) time for each of the four reagent tubesto prime the reagent pump. Carefully install all screw covers. If awash reagent is selected, prime the wash reagent tubing first sothat the wash option will be available for the remainder of thereagents.

16. Perform a microwave leakage measurement, page 52.

Service

78STAR System 2/6

600121Rev. 3

WARNING


1. Remove one of the four reagent tubes from the reagent container.Place the tubing into a clean suitable waste container. Select acavity.

2. Ensure that a vessel and condenser are properly placed in theselected cavity and that a clamp is installed on the condenser andarm. Perform the prime method for the tubing of the selected rea-gent one (1) time with air only to remove the reagent from thetubing

3. Place the tube in a container of deionized water. Replace the ves-sel in the selected cavity with a clean, dry vessel. Select theappropriate cavity and perform the prime method.

4. Remove the vessel from the cavity. Pour the contents of the vesselinto a 10mL graduated cylinder. If a total of 4mL is not dis-pensed, refer to the Troubleshooting Chart, “Incorrect Volume ofReagent Delivered.”

5. Remove the tube from the container of deionized water and placeit into the waste container.

6. Repeat steps 1 through 5 to verify the volume of each of the fourreagent tubes.

7. Install the four reagent tubes in the reagent containers, ensuringthat the tubing is placed in the proper container. Perform theprime method for each of the four reagents to prime the tubingwith reagents. If a wash reagent is selected, prime the wash rea-gent tubing first so that the wash option will be available for theremainder of the reagents.

WARNING


1. Remove all four reagent tubes from the reagent containers. Placethe tubing into a clean suitable waste container. Select a cavity and perform the prime method one (1) time for each of the fourreagent tubes.

ReagentDeliveryConfirmation

Reagent PumpValveReplacement


2. Place all reagent tubing into a container of deionized water, andperform the prime method on the selected cavity two (2) times foreach of the four reagent tubes.

3. Remove the reagent tubing from the container of water and per-form the prime method on the selected cavity one (1) time for eachof the four reagent tubes.


5. Loosen fittings and remove the tubing from valve. Loosen the twoscrews and remove the valve.

6. Install the new valve, ensuring that the flat side of the keyedshaft of the valve is aligned with the hole in the encoder and thatthe alignment pins on the valve are aligned with the bores of theframe. Install the two screws to secure the valve.

7. Install the tubing and tighten the fittings finger tight. Do not usetools to tighten the fittings.

8. Plug the instrument into the electrical outlet and position the on/off switch in the “on” position.

9. Position the reagent tubing in the reagent containers. Secure thetubing, if necessary. Perform the Prime method for each of thefour reagent tubes to prime the reagent pump. If a wash reagentis selected, prime the wash reagent tubing first so that the washoption will be available for the remainder of the reagents.

1.02.0

3.04.0

5.06.0

7.08.0

9.010.0

Figure 22. Reagent Pump Syringe

Valve

Fitting

Fitting

Service

80STAR System 2/6

600121Rev. 3

1. Unplug the vacuum pump from the electrical outlet. Label anddisconnect the vacuum and pressure tubing from the vacuumpump fittings.

2. Using a pencil or marking device, mark the pump housing, inter-mediate plate, and headplate to establish proper installed posi-tion during assembly.

3. Remove the four (4) capscrews and washers from the headplate.Remove the headplate.

4. Label the valveplate for installed position in relation to the valveports on the intermediate plate. Remove the valveplate and theintermediate plate.

5. Remove the four (4) screws and the housing cover.

6. Using both hands, turn the diaphragm counterclockwise andunscrew it from the connecting rod, using caution to avoid losingthe shims (spacers) on the threaded stud of the diaphragm.

7. Place the shims (spacers) removed in step 6 with the diaphragm(or the exact quantity of new shims) on the threaded stud of anew diaphragm.

8. Using both hands, carefully screw the new diaphragm clockwiseinto the connecting rod. Tighten the diaphragm firmly usinghands only. Do not use tools. When the diaphragm is tight, lift theedge of the diaphragm and ensure that the stud is completelyinserted into the connecting rod. If a gap is noticed between thediaphragm stud head and the connecting rod, tighten the dia-phragm until there is no gap.

9. Turn the counterweight until the connecting rod is centered.

10. Position the intermediate plate on the housing, ensuring that themarks made in step 2 above are aligned.

11. Position the valveplate on top of the intermediate plate in accor-dance with labeling attached during removal (step 4).

12. Carefully position the headplate on the intermediate plate, ensur-ing that the marks made in step 2 above are aligned.

CAUTION

Do not crimp or damage the valveplate during installa-tion of the headplate.

13. Install and tighten the four (4) socket screws uniformly in a criss-cross fashion in the headplate.

14. Turn the counterweight by hand to ensure that the pump turnsfreely.

15. Install the housing cover and secure it with the four (4) washersand capscrews.

DiaphragmReplacement –Single HeadVacuum Pump


Figure 23. Single Head Vacuum Pump (Exploded View)

Diaphragm

Headplate

Valveplate

IntermediatePlate

HousingCover

SocketScrew

Counterweight

Connecting Rod

DiaphragmStud Head

DiaphragmStud

Service

82STAR System 2/6

600121Rev. 3

NOTE

When using twin-head pumps, always replace the dia-phragm and valves in both heads at the same time.

1. Unplug the vacuum pump from the electrical outlet.

2. Label and disconnect the vacuum and pressure tubing from thevacuum pump. Label the interconnecting tubing and fittings forproper installed position. Remove the white clips (System 6 only)and carefully remove the tubing from the fittings. Using a 20 mmwrench, remove the nuts and fittings.

3. Using a pencil or marking device, mark the pressure plate, pumphead and pump case to establish proper installed position duringassembly.

4. Label the vacuum and pressure valves for proper installed posi-tion.

5. Using a 4 mm socket key, remove the six (6) socket screws andthe two (2) valve clamp rings.

6. Using a 27 mm socket wrench, unscrew the valve bodies with O-rings from the pump. Remove the valve disks from the valve cavi-ties. Remove any residual Teflon® tape from the threads of thevalve bodies and bores of the pump head to avoid clogging thenew valves when the system is assembled.

7. Remove and discard the O-rings from both valve bodies.

8. Remove the four (4) screws and washers and housing cover.

9. Remove the four (4) socket screws with disc springs from the pres-sure plate. Remove the pressure plate and pump head as anassembly, maintaining their relative installed position.

10. Using both hands, turn the diaphragm counterclockwise andunscrew it from the connecting rod, using caution to avoid losingthe shims (spacers) on the threaded stud of the diaphragm.

11. Place the shims (spacers) removed in step 10 with the diaphragm(or the exact quantity of new shims) on the threaded stud of anew diaphragm.

12. Using both hands, carefully screw the new diaphragm clockwiseinto the connecting rod. Tighten the diaphragm firmly usinghands only. Do not use tools. When the diaphragm is tight, lift theedge of the diaphragm and ensure that the stud is completelyinserted into the connecting rod. If a gap is noticed between thediaphragm stud head and the connecting rod, tighten the dia-phragm until there is no gap.

13. Turn the counterweight until the diaphragm is in mid-position(flat across).

Diaphragm& ValveReplacement –Dual HeadVacuum Pump

Service


��

��

Diaphragm

Figure 24. Dual Head Vacuum Pump (Exploded View)

Screw

Spacer Ring

SocketScrew

ClampRing

ClampRing

Nut

Fitting Nut

Fitting

Disk

Disk

InletValveBody

OutletValveBody

PressurePlate

PumpHead

PressurePlate

PumpHead

DiscSprings

Sleeve

Sleeve

O-Ring

HousingCover

Counterweight

DiaphragmStud Head

DiaphragmStud

ConnectingRod

Service

Beveled EdgeOn Top

84STAR System 2/6

600121Rev. 3

14. Carefully align and seat the bead of the diaphragm in the grooveof the spacer ring.

15. Position the pressure plate and pump head on the housing, ensur-ing that the marks made in step 3 are aligned. Install and tightenthe four (4) socket screws until the disc springs are flattened. Donot over tighten the screws.

16. Turn the counterweight by hand to ensure that the pump turnsfreely.

17. Install the housing cover and secure it with the four (4) washersand screws.

18. Apply a single layer of Teflon® tape centered around the threadsof each valve body, ensuring that it is smooth, overlapped andapplied in a clockwise direction so that it will adhere when thevalve bodies are screwed into the headplate.

CAUTION

The manufacturer recommends that the Teflon® tapenot be used in excess and that no substitute tape be uti-lized.

19. Install a new O-ring on the outlet valve body. Ensure that thesleeve is positioned with the beveled side facing upward and thatit is flat on the bottom of the valve cavity.

NOTE

The beveled side of the valve sleeve is difficult to see. Ifnecessary, place the sleeve under a magnifying glass todetermine the beveled side.

20. Install the new valve disk in the valve cavity. Carefully threadthe outlet valve body into the pump head and tighten the valvebody. Do not over tighten the valve.

21. Install a new O-ring on the inlet valve body. Ensure that the ser-rated airgate is positioned on the bottom with the grooves up andthat the sleeve is correctly positioned with the beveled side up.

NOTE

The beveled side of the valve sleeve is difficult to see. Ifnecessary, place the sleeve under a magnifying glass todetermine the beveled side.

22. Install the new valve disk in the valve cavity. Carefully threadthe inlet valve body into the pump head and tighten the valvebody. Do not over tighten the valve.

23. Install and securely tighten the clamp rings with the six (6)socket screws.


24. Carefully apply three (3) layers of Teflon® tape around each tub-ing fitting. Using a 20 mm wrench, install the nuts and fittings.

25. Install the interconnecting tubing and fittings per the labelingattached during disassembly.

26. Connect the vacuum and pressure tubing, ensuring that the tub-ing is installed per the labeling attached during pump disassem-bly. Install the white clips to secure the tubing to the fittings(System 6 only).

Service

86STAR System 2/6

600121Rev. 3


SystemRemoval

System

Rem

oval

WARNING


1. Turn the instrument off and unplug it from the electrical outlet.Remove the communications cable from the back of the vapor col-lection/reagent module.

2. Raise all arms of the vapor collection/reagent addition module.Using HF resistant spill wipes, remove any residual reagent fromthe ends of each of the arms.

WARNING

Dispose of contaminated wipes in accordance with theuser’s safety program for hazardous materials and thereagent manufacturer’s material safety data sheet.

3. Empty the solution from cylinder #1 of the vapor scrubber as out-lined below. If necessary, empty and replace the solution in cylin-ders 2 and 3. Liquid level should remain near the height of themarbles in the cylinder.

3a. Using a flat blade screwdriver, pry the cap from the scrub-ber cylinder.

WARNING

Solutions should be discarded in accordance with theuser’s safety program for hazardous materials, the rea-gent material safety data sheet, and/or regulatoryrequirements.

3b. Empty and discard the solutions from the cylinders.

3c. Cylinder #1 should remain empty of solution for the follow-ing procedure. If cylinders #2 and #3 are emplied, add solu-tions to the cylinders: #2 - 25% NaOH (sodium hydroxide) totop of marbles, and #3 - deionized water one-half distance ofmarbles.

3d. Inspect both O-rings for distortion, cracks or other damage.Replace the O-rings if necessary.

3e. Install the caps on the cylinders.

4. Place an empty vessel and condenser in each cavity of the system.Install vessel clamps on each condenser and arm. Position eachshield so that the plate is outward toward the front of the instru-ment.

88STAR System 2/6

600121Rev. 3

CAUTION

If hydrofluoric acid (HF) has been used in the system,Teflon vessels should be used for the entire system.

WARNING

Vessels and condensers must be placed in each cavity toavoid any possible spillage of and/or contact with con-taminated fluids.

5. Disconnect the 3/16” tubing labeled “Connect to Vapor CollectionModule” from the top fitting on the back of the vapor collection/reagent addition module. Use caution to ensure proper handlingand disposal of any reagent droplets or residue and cleaningmaterial.

6. Connect the 3' length of 3/16” tubing supplied in the instrumentaccessory kit to the fitting from which the tubing was removed instep 5.

7. Place a 250mL beaker filled with sodium bicarbonate solution(10% concentration) near the instrument. Position the open end ofthe tubing installed in step 6 in the beaker of sodium bicarbonatesolution.

8. Turn the vacuum pump on. The system will suction the sodiumbicarbonate solution and back-flush the vapor containment/reagent addition module. Permit the system to suction the entire250mL of solution.

9. Using deionized water instead of sodium bicarbonate, repeatsteps 7 and 8 two times.

10. Fill a 100mL beaker with sodium bicarbonate solution (10% con-centration).

11. Remove the vessel clamp and slightly raise the vapor collectionarm for cavity #1.

12. Position the beaker filled with sodium bicarbonate solution underthe vapor collection arm of cavity #1. Permit the instrument tosuction approximately 50mL of the solution from the beaker.

13. Lower the vapor collection arm of cavity #1; install the vesselclamp, and slightly raise the vapor collection arm of cavity #2.

14. Refill the beaker with sodium bicarbonate solution. Repeat steps12 and 13 for cavity #2. For a System 6, repeat steps 12 and 13 forcavities #3 through #6. Once this procedure is completed for eachcavity, ensure that each vapor collection arm is in the down posi-tion.

15. Repeat step 3 to empty the solutions from the vapor scrubber cyl-inders. Note: Cylinder #1 should be empty for the following proce-dure.


WARNING

Vessels contain neutralized acid and/or complexed fluo-ride ion (hazardous waste). Waste should be handled inaccordance with the user’s safety program for hazardousmaterials and the reagent material safety data sheet.

16. Using 100mL of water instead of sodium bicarbonate, repeat steps10 through 14 a minimum of two times.

17. Based on system design, if necessary, remove the reagent tubingwith fittings from the manifold on the back of the vapor collection/reagent addition module. Fittings are installed finger tight only.Do not use tools to remove fittings.

18. Remove the air/waste tubing from the bottle behind or on top ofthe main instrument, ensuring that all residue is drained fromthe tubing. Remove the other end of the tubing with installed fit-ting from the valve of the reagent pump. Rinse the tubing withtap water several times to remove any reagent residue

19. Remove all tubing from the back of the vapor collection/reagentaddition module. Place the tubing into a suitable waste container.

20. Using a flat blade screwdriver, pry the cap from each scrubbercylinder. Empty and discard the solution in accordance with thematerial safety data sheet for the applicable reagent(s) being uti-lized and/or regulatory requirements. Completely rinse the scrub-ber cylinders with deionized water.

21. Disconnect all tubing from the scrubber cylinder caps and the vac-uum pump. Rinse all tubing several times with deionized water toremove any reagent residue.

22. Install the caps on the scrubber cylinders.

23. Remove the shields from each cavity.

24. Carefully remove all four reagent tubes from the reagent contain-ers. Rinse the ends of the tubing. Place the four tubes into a suita-ble acid waste container.

25. Position the instrument on a workbench or in a fume hood so thatthe back of the instrument is accessible for service or remove thevapor collection/reagent addition module from the main instru-ment as outlined below.

a. Remove the 3/8” tubing from the fitting on the back of thevapor collection/reagent addition module. Facing the front ofthe instrument, disconnect the tubing on the right side ofthe module (tubing extends from the reagent pump valveinto the module).

b. Lift the vapor collection/reagent addition module from thetracks in the top of the main instrument and tilt the module

System

Rem

oval

90STAR System 2/6

600121Rev. 3

toward the front of the instrument until the support brackets onthe module are free from the slots in the instrument top cover.Remove the module from the instrument.

26. Remove the screws and rear metal plate from the module. Posi-tion the rear plate to the side of the module to permit access tothe valve.

27. Remove the Keps nuts from the manifold. Slide the manifold offthe reagent tubing.

28. Loosen the setscrew and lift the valve head with installed tubingfrom the valve.

29. Using a 7/64” Allen wrench, remove the screws from the face plateof the valve. Permit any residual reagents to drain from the tub-ing into a waste container.

30. Position all the vapor collection arms in an upward position.Using pliers, carefully remove the screw covers from the screws inthe top cover of the vapor collection/reagent addition module.Remove the screws.

31. Carefully lift the cover off the vapor collection/reagent additionmodule, using caution to avoid damage to the arms as the over islifted over them.

WARNING


32. Remove the reagent tubing from the vapor collection arms bypulling the tubing from the arm assemblies.

33. Place the valve face plate with the installed tubing into a sink oftap water to rinse away any residual reagents.

34. Remove the valve rotor and rinse it to remove any residual rea-gents. Replace the rotor in the valve.

35. Once the valve face plate and tubing are completely rinsed, installthe face plate with the tubing on the valve using three screws.Position the valve head on the valve, and tighten the setscrew.

36. Coil the reagent tubing and place the valve and tubing into aplastic bag for shipment with the instrument.

37. Install the top cover on the vapor collection/reagent addition mod-ule. Install the manifold on the module using the Keps nuts.Install the rear metal plate on the module.


38. Disconnect all tubing from the scrubber cylinder caps and vacuumpump.

39. Remove the shields from each cavity of the instrument.

40. Install the straps removed from each cavity during system instal-lation (figure 8, page 8 of the Operation Manual) by following theprocedures outlined below in either step 41a or 41b.

CAUTION

If the straps were not saved during system installation,to avoid breakage, the vessel liners must be shipped sep-arately, not installed in the cavities of the instrument.

40a. Slide the loose ends of the straps removed during systeminstallation down the sides of the cavities and under theliners.

40b. Remove the liners and install the straps as follows:

CAUTION


(1) Using pliers or a flat blade screwdriver, remove thescrew covers from the instrument cover. Remove thescrews from the bottom of the instrument front panel.Pull the front panel down until the tabs are free fromthe slots in the top cover and remove the front panel.Remove the screws and the top cover from the maininstrument, using caution to avoid disconnecting thedisplay cable.

(2) Loosen the setscrew and remove the vessel support ringassembly from each cavity. Remove the liner from eachcavity.

(3) Position the straps removed during system installationbetween the inside of the cavities and the vessel linerswith the loose ends positioned through the opening inthe bottom of the liner. Install each liner with strapsinto each cavity. (Refer to figure 8, page 8 of the Opera-tion Manual.)

(4) Install the vessel support ring assembly on each cavity.Secure the ring to the cavity with a setscrew.

(5) Install the instrument top cover, and secure it with thescrews. Install the instrument front cover, ensuringthat the tabs at the top of the cover engage the slots inthe top cover. Install the screw bases and screws tosecure the front cover. Install the screw covers.

System

Rem

oval

92STAR System 2/6

600121Rev. 3

41. Package each component of the system in the appropriate con-tainer for shipment.

NOTE

Once the instrument is repaired, residual sodium bicar-bonate must be removed from the instrument prior touse. Create a method with the following parameters: ini-tial reagent - 4mL sulfuric acid, stage #1 ramp time - 5minutes, target temperature - 250°C, time at tempera-ture - 5 minutes, add reagent - 10mL nitric acid in ali-quots of 1mL . Perform this method in each cavity.


Specifications

STAR System 2 STAR System 6

Dimensions (WxDxH)Main Instrument 18” x 13.15” x 14” 29.5” x 13.13” x 14”

45.72 cm x 33.4 cm x 35.5 cm 74.93 cm x 33.4 cm x 35.5 cmVapor Collection/Reagent Addition Module 6.5” x 9” x 12” 20.5” x 9” x 12”

16.54 cm x 22.86 cm x 30.48 cm 52.07 cm x 22.86 cm x 30.48 cm

Weight (Main Instrument) 48 lbs. (21.77 kg) 67 lbs. (30.39 kg)

Program Storage 20 Methods 20 Methods

Power Requirements 120 ±10% VAC, 60 Hz 208/230 ±10% VAC, 60 Hz220/240 ±10% VAC, 50 Hz 220/240 ±10% VAC, 50 Hz

Operating Temperature Ambient - 500 °C Ambient - 500 °C

Readout Temperature Ambient - 430 °C Ambient - 430 °C

Temperature Control Individual feedback per cavity Individual feedback per cavity

Temperature Sensors 2 6

Vessel-in-Position Sensors 2 6

Arm-in-Position Sensors 2 6

Vessel Capacity, Each 250, 100, 50mL 250, 100, 50mL

No. of Vessels Maximum 2 Maximum 6

No. of Staggered Start Times Maximum 2 Maximum 6

Vapor Containment Module Standard Standard

Automatic Reagent Additon Optional OptionalMaximum 4 reagents

Keyboard Type Membrane Membrane

Printer Port Parallel Parallel

Communications Port RS232 RS232

CEM STAR Systems Patents Pending

Sp

ecification

s

94STAR System 2/6

600121Rev. 3

E®

Certified toCAN/CSA C22.2 No. 1010.1

Emission and Safety Approvals

U.S. and CanadaEmissions – Complies with FCC part 18 (47 CFR part 18 Industrial,

Scientific and Medical Equipment).Safety – ETL* approved to UL standard 1262 (Laboratory Equipment).

CSA** approved to standard CAN/CSA C22.2 No. 1010.1 (LaboratoryEquipment).

European CommunityEmissions – Conforms to EC standard EN 55011 (Emissions for

Industrial, Scientific and Medical Equipment).Conforms to EC standard EN50082-1 (Electromagnetic Compatability- Part 1).

Safety – Conforms to EC standard IEC 1010-1 (Safety Requirements for Electrical equipment for measurement, control and laboratory use -Part 1).

*ETL and UL are equivalent NRTL’s (Nationally Recognized Testing Laboratories)**CSA is approved testing laboratory by the Standards Council of Canada

CE

CConforms to UL Std. 3101

78355

®


What Is Covered:CEM Corporation warrants that the instrument will be free of any defect inparts or workmanship and will, at its option, replace or repair any defectivepart (excluding consumables) or instrument.

For How Long:This warranty remains in effect for 365 days from date of delivery to theoriginal purchaser.

What Is Not Covered:This warranty does not cover parts or workmanship which have been dam-aged due to:• Neglect, abuse or misuse,• Damage caused by or to test samples,• Damage incurred during instrument relocation,• Damage caused by or to any attached equipment,• Use of incorrect line voltages or fuses,• Fire, flood, "acts of God" or other contingencies beyond the control of CEM

Corporation,• Improper or unauthorized repair, or• Any other damage caused by purchaser or its agents.

Responsibilities of Purchaser:To ensure warranty coverage, the purchaser must:• Use the instrument according to directions,• Connect the instrument properly to a power supply of proper voltage,• Replace blown fuses,• Replace consumables and• Clean the instrument as required.

How to Get Service:Purchaser should contact the Service Department of CEM Corporation oryour distributor for return authorization and for proper crating andshipping instructions to return instrument, freight prepaid, for service. On-site repairs by an authorized service technician are available through theCEM Service Department. Travel costs will be charged to the purchaser foron-site repairs.

Within the U.S. Outside the U.S.CEM Corporation CEM Corporation3100 Smith Farm Rd. 3100 Smith Farm Rd.Matthews, NC 28105-5044 Matthews, NC 28105-5044(800) 726-5551 (704) 821-7015Fax: (704) 821-4368 Fax: (704) 821-4368

Warranty Disclaimer:CEM Corporation hereby excludes and disclaims any warranty ofmerchantibility or fitness for any particular purpose. No warranty,express or implied, extends beyond the face hereof. CEM Corpora-tion shall not be liable for loss of use of instrument or other inci-dental or consequential costs, expenses or damages incurred by thepurchaser or any other user.

Purchaser's Rights under State Law:This warranty gives the purchaser specific legal rights, and the purchasermay also have other rights which vary from state to state.

Warranty Warran

ty

96STAR System 2/6

600121Rev. 3

1

Appendix A

Method Development

Four methods are factory programmed into the STAR System 2 and STAR System 6instruments: 1) Mild Digest (HNO3, H2O2), 2) Moderate Char (H2SO4, HNO3,H2O2), 3) Rigorous Char (H2SO4, HNO3, H2O2) and 4) Super Char (H2SO4, HNO3,H2O2). These methods are provided as guidelines only.

The methods were developed for sample sizes of 1-2g. For larger or smaller samplesizes, reagent volumes and time at parameter should be adjusted accordingly.

The following guidelines should be used to adapt the factory programmed methods ifa sample does not digest to requirements or for method development:

1. Add additional charring stages as required. For example, after oxidation bynitric acid at 250°C, ramp the sample to 280°C, immediately followed with a200°C peroxide oxidation.

2. Increase the time for nitric acid and peroxide oxidations, increasing the amountof reagent in proportion to the amount of additional time. For each 1mL of rea-gent added in excess of the time at parameter (TAP) in a stage, increase thetime by 30 seconds.

2

Mild Digest (HNO3, H2O2)

This method is designed for digestions for which the use of higher boiling point rea-gents, such as sulfuric acid, or temperatures above 120°C are not desirable.

This method was developed for a sample size of 1-2g. For larger or smaller samplesizes, reagent volumes and time at parameter should be adjusted accordingly.

Samples*

Agricultural: Apple (Red Delicious), asparagus, blueberry, carrot, celery, cherry,cherry (sour), citrus #3, cotton, cranberry, cucumber, grapefruit, grapes (Concord),kidney beans (red), orange, peach, pear (Bartlet), pear (Boso), pepper (Bell), pineneedles SRM 1575, plum (Empress), plum (Friar), raspberry, rice flour, rice flourSRM 1568, strawberry, yew

Biological: Liver (bovine SRM 1577B), lobster hepatopancreas TORT 2, muscle(bovine SRM 8414), and oyster tissue SRM 1566A

Environmental (leaches): soils, sludges, soil (Montana SRM 2710), and soil (Montana2711)

Other: Paper

*Sample types listed are examples only of the types that can be used. Other sampletypes may be used with this method depending upon reagents used and analytesrequired.

Example:

(Date, Time)

METHOD NAME: MILD DIGESTHNO3/H2O2

INITIAL REAGENT ADDITION

ADDITION REAGENT VOLUME ALIQUOTS

1 NITRIC 10.0mL 10.0mL

METHOD STAGE

RAMP TARGET TIME AT ADD ATSTAGE TIME TEMP. TEMP. REAGENT VOLUME ALIQUOTS START

1 03:00 110C 10:00 NONE 00.0mL 0.0mL NO 2 00:01 110C 05:00 PEROXIDE 10.0mL 1.0mL NO

Note: This method specifies no sulfuric; therefore, it is more susceptible to changes in boiling point caused by thedecomposition of organic samples. When digesting plant materials, the evolution of gases, etc. from 1g of samplewill decrease the boiling point to approximately 116°C until the sample is almost digested. The Mild Digest wasdesigned to digest a wide variety of samples with minimal risk of boiling a vessel dry due to boiling point changeswhich are sample dependent. In addition, final acid matrixes are more predictable due to the fact that none of thenitric acid that is initially added to the sample is boiled away during the digest. The target temperature can be mod-ified by determining the characteristic boiling temperature of the sample and setting the target temperature param-eter to approximately 2 - 3°C below that boiling temperature. If nitric acid is liberated from the digestion vesselduring stage one of the digest, the nitric acid reagent may be added to the sample at the rate at which it is boiledaway. Times at temperature may be modified according to the length of time required to digest the sample.

3

Moderate Char (H2SO4, HNO3, H2O2)

This method is designed for digestions for which the sample composition requiresonly moderate charring to facilitate shorter digestion times and more complete oxi-dation of organic material than that provided by the mild method.


Samples*

Agricultural with use of sulfuric acid: Apple (Red Delicious), asparagus, blueberry,carrot, celery, cherry, cherry (sour), citrus #3, cotton, cranberry, cucumber, grape-fruit, grapes (Concord), kidney beans (red), orange, peach, pear (Bartlet), pear(Boso), pepper (Bell), pine needles SRM 1575, plum (Empress), plum (Friar), rasp-berry, rice four, rice flour SRM 1568, strawberry, yew

Biological with use of sulfuric acid: Liver (bovine SRM 1577B), lobster hepatopan-creas TORT 2, muscle (bovine SRM 8414), oyster tissue SRM 1566A

Light oils: food samples with fat/oil content, peanut butter

Foods: milk powder, whole milk, mayonnaise, cereal

Plastics: samples that are readily digested such as PCR

Environmental: wastewater, emulsions, hazardous waste, filters

Other: paints, solvents


Example:

(Date, Time)

METHOD NAME: MODERATE CHARH2SO4/HNO3/H202



1 NITRIC 10.0mL 10.0mL 2 SULFURIC 5.0mL 5.0mL

METHOD STAGE


1 03:00 120C 01:00 NONE 0.0mL 0.0mL NO 2 03:00 250C 05:00 NITRIC 10.0mL 1.0mL NO 3 00:00 200C 10:00 PEROXIDE 20.0mL 1.0mL NO

4

Rigorous Char (H2SO4, HNO3, H2O2)

This method is designed for digestions for which the sample composition requires asevere char using sulfuric acid in the initial stages to break down highly stableorganic structures so that subsequent oxidation by nitric and peroxide can provide acomplete digest.


Samples*

Oils: Oil SRM 1634, motor oil, residual fuel oil, Pliogrip (synthetic rubber)

Polymers/Plastics: Arofene (epoxy hardener), Aroset (epoxy hardener), Hetron(epoxy hardener), polycarbonate, polycarbonate resin, polycarbonate resin with car-bon black, polycarbonate resin with additive, polyether ether ketone (PEEK), poly-propylene, polypropylene with additive, polythalamide with carbon fibers, RTPgreen, flame retardants

Other: Resins, solvents, adhesives, organic chemicals, asphalts, fuels


Example:

(Date, Time)

METHOD NAME: RIGOROUS CHARH2SO4/HNO3/H202




METHOD STAGE


1 03:00 120C 01:00 NONE 0.0mL 0.0mL NO 2 03:00 250C 00:10 NITRIC 2.0mL 2.0mL NO 3 01:00 280C 00:00 NONE 0.0mL 0.0mL NO 4 00:00 250C 10:00 NITRIC 20.0mL 1.0mL NO 5 00:00 200C 10:00 PEROXIDE 20.0mL 1.0mL NO

For extremely difficult samples requiring charring, repeat char step #3 as manytimes as required between nitric step #4 and peroxide step #5.

5

Super Char (H2SO4, HNO3, H2O2)

This method is designed for digestions of samples larger than 2 grams* and/or sam-ples that tend to dry out during the initial stages of the Rigorous Char DigestionProcedure. This method is designed with nine (9) stages, five of which can be acti-vated or deactivated (stages 2-6), based on the digestion characteristics of the sam-ple.

Samples*

Oils: Oil SRM 1634, motor oil, residual fuel oil, Pliogrip (synthetic rubber)

Polymers/Plastics: Arofene (epoxy hardener), Aroset (epoxy hardener), Hetron(epoxy hardener), polycarbonate, polycarbonate resin, polycarbonate resin with car-bon black, polycarbonate resin with additive, polyether ether ketone (PEEK), poly-propylene, polypropylene with additive, polythalamide with carbon fibers, RTPgreen, flame retardants

Other: Resins, solvents, adhesives, organic chemicals, asphalts, fuels


Example:

(Date, Time)

METHOD NAME: SUPER CHARH2SO4/HNO3/H202




METHOD STAGE


1 03:00 120C 01:00 NONE 0.0mL 0.0mL NO 2 01:30 150C 05:00 NITRIC 10.0mL 1.0mL NO 3 01:30 175C 05:00 NITRIC 10.0mL 1.0mL NO 4 01:30 200C 05:00 NITRIC 10.0mL 1.0mL NO 5 01:30 225C 05:00 NITRIC 10.0mL 1.0mL NO 6 01:30 250C 05:00 NITRIC 10.0mL 1.0mL NO 7 02:00 280C 00:00 NITRIC 1.5mL 1.5mL YES 8 00:00 250C 10:00 NITRIC 20.0mL 1.0mL NO 9 00:00 200C 10:00 PEROXIDE 20.0mL 1.0mL NO

The objective of the Super Char method is to heat the sample to the char temperature (280°C) using theleast amount of time and reagent possible. It does not require all stages for completion of the digestion.Stage 1 is required; stages 2 through 6 are optional; and stages 7 through 9 are required. However,ramp times, times at temperature, reagent volumes, and aliquots can be edited to meet sample require-ments. For example: Begin the digestion with stage 1. Continue to stage 2. If no reaction is observed orif the sample does not go into solution, deactivate stage 2 and continue to stage 3. If the sample goesinto solution in stage 2, stages 3 through 6 can be deactivated. If required, continue the digestionthrough stage 3 through 6 until the sample goes into solution, deactivating any unnecessary stages.Then, continue with stages 7 through 9 for method completion, editing parameters as required. Usethe Edit Menu for stage deactivation or editing parameters.

*Sample size dependent upon sample type

6

1

Appendix B

Examples of Method, Data, Temperature and Instrument Setup Parameters Printouts

The following examples of printouts are programmed in Setup, no. “2 - Autoprint.”

Method

23 Apr, 96 12:58

METHOD NAME: METHOD 9

INITIAL REAGENT ADDITIONNONEMETHOD STAGE

RAMP TARGET TIME AT ADD ATSTAGE TIME TEMP. TEMP. REAGENT VOLUME ALIQUOTS START 1 00:01 30C 00:01 NONE 0.0mL 0.0mL NO 2 01:00 31C 00:00 NONE 0.0mL 0.0mL NO

Data

23 Apr, 96 12:58

METHOD NAME: METHOD 9

CELL 1

TEMP. MAX.STAGE SET POINT HIT TEMP. 1 30C PASS 41C 2 31C PASS 41C

*STAR System 2 example

2

The following examples are printouts of Instrument Setup Parameters accessed withthe “PRINT” key.

Instrument Setup Parameters

Quartz/Glass Vessels

23 Apr. 96 12:58

INSTRUMENT SETUP PARAMETERS

REAGENT VOLUME REMAINING PRINT EACH RUN PRINTERSULFURIC 09.93L PRINT METHOD (ON) IBMNITRIC 09.74L PRINT DATA (ON)PEROXIDE 09.80LH2O 09.97L

CALIBRATIONLOW HIGH LOW HIGH

CELL TEMP TEMP DATA DATA LAST CAL DATE1 121C 330C 371 2301 23 Apr, 962 121C 330C 378 2288 23 Apr, 96

LINE FREQUENCY 60 HZ

SOFTWARE VERSION: V 2.48/1.02

Teflon® Vessels

15 Nov. 96 15:48

INSTRUMENT SETUP PARAMETERS

REAGENT VOLUME REMAINING PRINT EACH RUN PRINTERSULFURIC 00.00L PRINT METHOD (0FF) IBMNITRIC 00.00L PRINT DATA (OFF)PEROXIDE 00.00LH2O 00.00L

CALIBRATIONLOW HIGH LOW HIGH

CELL TEMP TEMP DATA DATA LAST CAL DATE1 100C 121C 400 500 23 Apr, 962 100C 121C 400 500 23 Apr, 96

LINE FREQUENCY 60 HZ

SOFTWARE VERSION: HF-001/1.03

1

Appendix C

Chemical Elements and Their Symbols

Element Symbol Element SymbolActinium Ac Mercury HgAluminum Al Molybdenum MoAmericium Am Neodymium NdAntimony Sb Neon NeArgon Ar Neptunium NpArsenic As Nickel NiAstatine At Niobium NbBarium Ba Nitrogen NBerkelium Bk Nobelium NoBeryllium Be Osmium OsBismuth Bi Oxygen OBoron B Palladium PdBromine Br Phosphorus PCadmium Cd Platinum PtCalcium Ca Plutonium PuCalifornium Cf Polonium PoCarbon C Potassium KCerium Ce Praseodymium PrCesium Cs Promethium PmChlorine Cl Protactinium PaChromium Cr Radium RaCobalt Co Radon RnCopper Cu Rhenium ReCurium Cm Rhodium RhDysprosium Dy Rubidium RbEinsteinium Es Ruthenium RuErbium Er Samarium SmEuropium Eu Scandium ScFermium Fm Selenium SeFluorine F Silicon SiFrancium Fr Silver AgGadolinium Gd Sodium NaGallium Ga Strontium SrGermanium Ge Sulfur SGold Au Tantalum TaHafnium Hf Technetium TcHelium He Tellurium TeHolmium Ho Terbium TbHydrogen H Thallium TlIndium In Thorium ThIodine I Thulium TmIridium Ir Tin SnIron Fe Titanium TiKrypton Kr Tungsten WLanthanum La Uranium ULawrencium Lr Vanadium VLead Pb Xenon XeLithium Li Ytterbium YbLutetium Lu Yttrium YMagnesium Mg Zinc ZnManganese Mn Zirconium ZrMendelevium Md

2

1

APPENDIX D

Conversion Tables

Volume Equivalents

meter3 foot3 gallon liter quart inch3 cc1 35.31 264.2 1000 1056.8 61023 1x106

28.317x10-3 1 7.4822 28.317 29.92 1728 28.317x103

3.785x10-3 0.1337 1 3.785 4 231 37851x10-3 0.03531 0.2642 1 1.057 61.023 1000

9.463x10-3 0.03342 0.25 0.9463 1 57.75 946.251.638x10-5 5.787x10-4 43.29x10-4 0.01639 0.01732 1 16.387

1x10-6 35.31x10-6 2.642x10-4 1x10-3 10.568x10-4 0.06102 1

Temperature Equivalents

°F - 32° 1.8

°F = 1.8 (°C) + 32°

°K = °C + 273.15°

°C =

Fractional Units of Measure Conversion Data

Prefix Factor Fraction

centi 10-2= 1/100 part per hundred

milli 10-3= 1/1,000 part per thousand

micro 10-6= 1/1,000,000 part per million (ppm)

nano 10-9= 1/1,000,000,000 part per billion (ppb)

pico 10-12= 1/1,000,000,000,000 part per trillion (ppt)

femto 10-15= 1/1,000,000,000,000,000 part per quadrillion (ppq)

atto 10-18= 1/1,000,000,000,000,000,000 part per quintillion

Percent Parts/Million Parts/Billion Parts/Trillion

.001% = 10 ppm

.0001% = 1 ppm = 1000 ppb = 1,000,000 ppt

.00001% = .1 ppm = 100 ppb = 100,000 ppt

.000001% = .01 ppm = 10 ppb = 10,000 ppt

.001 ppm = 1 ppb = 1,000 ppt

.0001 ppm = .1 ppb = 1,000 ppt

.01 ppb = 100 ppt

.001 ppb = 1 ppt

2

1

APPENDIX E

Concentrated Reagents and Their Uses

HNO3: All common metals except aluminum and chromium. Tin, Tungsten or antimonymay precipitate out as hyrated oxides.boiling point - approximately 121°C

H2SO4: Partly effective because of its high bp. Organic compounds, most metals and manyalloysboiling point - approximately 330°C to 340°C

H2O2: Speeds oxidation of organic material when mixed with mineral acids

HCl: Metal oxides and metals more easily oxidized than hydrogenboiling point - approximately 110°C

Aqua Regia: Contains various reactive and very powerful oxidation products which dissolve thenoble metals

H3PO4: Non oxidizing, occasionally used to dissolve sulfidesboiling point - approximately 158°C (85% H3PO4)

2

1

APPENDIX F

Examples of Aqua Regia, Reverse Aqua Regia Additionsand Multiple Char Methods

The following examples are not complete methods, only the pertinent stages.

Aqua Regia

Stage Ramp Target T TAP Reagent Aliquots At Start1 3 Min. 120°C 1 Min. None No2 3 Min. 250°C 2 Min. 4.0mL HNO3 1mL No3 1 Sec. 225°C 0 3.0mL HCl 3mL Yes4 2 Min. 250°C 0 1.0mL HNO3 1mL Yes5 1 Sec. 250°C 5 Min. 5.0mL HNO3 1mL No

Reverse Aqua Regia

Stage Ramp Target T TAP Reagent Aliquots At Start1 3 Min. 120°C 1 Min. None No2 3 Min. 250°C 2 Min. 4.0mL HNO3 1mL No3 1 Sec. 225°C 0 3.0mL HNO3 3mL Yes4 2 Min. 250°C 0 1.0mL HCl 1mL Yes5 1 Sec. 250°C 5 Min. 5.0mL HNO3 1mL No

Multiple Char A

Stage Ramp Target T TAP Reagent Aliquots At Start1 3 Min. 120°C 1 Min. None No2 3 Min. 250°C 3 Min. 6.0mL HNO3 1mL No3 2 Min. 280°C 0 1.0mL HNO3 1mL Yes4 0 250°C 2 Min. 4.0mL HNO3 1mL No5 2 Min. 280°C 0 1.0mL HNO3 1mL Yes6 0 250°C 2 Min. 4.0mL HNO3 1mL No

Multiple Char B

Stage Ramp Target T TAP Reagent Aliquots At Start1 3 Min. 120°C 1 Min. None No2 3 Min. 250°C 3 Min. 6.0mL HNO3 1mL No3 2 Min. 280°C 0 1.0mL HNO3 1mL Yes4 0 250°C 2 Min. 4.0mL HNO3 1mL No5 0 200°C 2 Min. 4.0mL H2O2 2mL No6 2 Min. 280°C 0 1.0mL HNO3 1mL Yes7 0 250°C 2 Min. 4.0mL HNO3 1mL No

Note: If a sample turns black when H2O2 is added at the end of the Multiple Char Method A, use MultipleChar Method B. Add additional charring stages as required.

2

Documents

STAR System 2â„¢ - CEM Distributor Support