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1. Figure 3 11 Model 9000F Sub pan Rear View C o Ki qa ahane td ar EA 8 a o Y n o a dre E gt 4 O 00 Ae c ao CR E ee 88 oo o2 PETO i Es M KEE Hi 2 gt o ES E i o 8 o O e o O O 9 I i E 1 Relay Output Board Controls Model 734 735 2 Detector Board converts Reference and Sensing Electrode signals for computer 3 Flowmeters and Connections controls gases to pyrolysis tube 4 Furnace Temperature Controller Connector operates 12 combustion furnace 22 ANTEK 9000F USER S MANUAL 3 3 Computer NOTE See computer Operator s Manual for more detail i do The computer mouse Figure 3 13 controls the screen pointer or cursor Cursor shapes include I beam Figure 3 12 Rear View POWER KEYBOARD MOUSE MONITOR 50 PIN RIBBON CABLE
2. 69 5B Board Computer Interface Board Ribbon Cable Distribution Board Ribbon Cable Connection from Computer Reagent A Feed supplies Reagent A to Valve A Gas Supplies gases to flowmeters Waste Connections to waste bottles Fans Rear Panel Main Board power distribution O GFN OU PWN Reagent B Input supplies Reagent B to Reagent B Pump 21 ANTEK 9000F USER S MANUAL Figure 3 10 Model 9000F Pan Fans 2 Furnace Oxidation Furnace 3 Dual Head Peristaltic Pump pumps Receiving Solution A into the Receiving Vessel and out to Rear Panel Waste Furnace Controller controls furnace temperature 5 5 VDC Power Supply supplies voltage to signal boards and SSRs
3. GASEOUS 3 2 Model 9000F Figure 3 2 Access points To remove instrument panels loosen the two locking screws slide the top cover back one inch lift up on the cover and set the cover aside Next loosen the four locking screws located on each of the side panels and remove side covers by lifting straight up with the panels CAUTION Remove the right panel slowly so that accidental breakage of the pyrolysis tube will not occur 17 ANTEK 9000F USER S MANUAL Figure 3 3 Model 9000F Front Panel P ANTEK E D ak li e SEE se I WA ojisilo S l To openthe front door Loosen the locking screws and the door will hinge out ofthe way Figures 3 4 3 11 provide an instrument overview Figure 3 4 Model 9000F Chemistry Section TEMPERATURE CONTROLLER O ELECTRODES e e e REFERENCE FLUORIDE PYRO 02 INLET 02 CARRIER
4. O il AI MO MA na DIL O II FIERI AT m O pu AI N IMA N Mn DIL Locate the Ion Specific Electrode ISE flow cell as shown in Figure 2 11 2 3 4 1 Installing the lon Specific Reference Electrode 1 Locate and remove the Reference Electrode P N 71315 from the 9000F Accessory Kit The electrode 1s stored in a protective holder with a moist sponge to keep it from drying out Figure 2 13 Reference Electrode PROTECTIVE POLI SHED CASE MEMBRANE ELECTRODE SPONGE BODY 2 Remove and inspect the Reference Electrode for damage particularly the membrane which forms the sensing end of the Electrode Body 3 Ifthe level of Potassium Chloride KCI Solution is low and or has abubble of air in it larger than 0 1 ml remove the Electrode from its body and fill with the provided Potassium Chloride KCI Solution P N 37120 as shown in Figure 2 13 11 ANTEK 9000F USER S MANUAL Figure 2 13 Filling Reference Electrode ELECTRODE C O RING ELECTRODE BODY OVERFILL TO A LEVEL THAT ASSURES MINIMUM AIR BUBBLE FORMATION 4 Carefully insert the Reference Electrode into the ISE Cell Body and finger tighten Figure 2 14 Installing Reference Electrode Reference Electrode O Ring 5 Carefully place the Sensing Electrode P N 71314 into the ISE Cell Body snap into place and finger tighten the nut Figure
5. 1 4 Teflon Ferrules Cl KCI Solution for filling the reference electrode AUA aiad High Temperature Septa 1 2 Diameter urbc E I RA ISE Cell TR Fluoride lon Specific Electrode A Reference Electrode A T Dual Head Peristaltic Pump 10 2 Glassware 10 2 1 10 2 2 Part Number Description 00 TE Receiving Vessel rank H ED Direct Injection Pyrotube Glassware for use with MultiMatrix Model 740 Part Number Description dC X MultiMatrix Model 740 Pyrotube e kaja Quartz Boats High Wall 6 Pk SUI IERI I Quartz Weigh Boats 6 Pk UL ii air Weigh Boat Carriers 6 Pk Fac P MultiMatrix Model 740 Model 734 Pyrotube Combo For use with Gas LPG Sampling System Model 734 Part Number Description FINZI a Inline filter Nupro 0 5 micron A D sample line kit 10 3 Consumables Part Number Description ocn UH 25 uL syringe WI d ees Reagent A solution 4 gal case CO RR URN Reagent B solution 4 gal case c PE Organic fluoride standards fluorohexane in isooctane iros Blank 1 5 25 50 100 250 and 500 ppm F kit 37049 ENTER Inorganic fluoride standards NaF in water ti Blank 1 5 25 50 100 2
6. 2 3 8 Computer Install the computer monitor keyboard and mouse interface as described in the computer s Operator s Manualandasshownin Figure 2 20 Follow closely the guidelines set outin the computer s Operator s Manual 2 3 9 Solution Reagent Bottles Fill and install the Reagent Bottles as shown in Figure 2 22 WARNING Severe damage will be caused to the Model 9000F if incorrect solutions are used Check all labels prior to filling of the Reagent Bottles Figure 2 22 Installing Reagent Bottles SL ES OASIS PRA N 3 S e REAGENT A REAGENT B WASTE 15 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK SECTION 3 SYSTEM OVERVIEW 3 1 Introduction Before installing accessory equipment and or proceeding to the primary testing section of the installation procedure become familiar with the locations and various features ofthe Antek Model 9000F Fluoride Analyzer Figure 3 1 System Overview REAGENT A REAGENT B
7. Active Method Af2461 mth A ANTEK Model 9000F Elemental Analyzer Edit Method Run Calibration Initialization complete Instrument running 6 6 02 3 39 PM 30 ANTEK 9000F USER S MANUAL 5 3 Furnace Power Up WARNING Furnace operates at a temperature in excess of 1000 C and can serve as an ignition source and cause severe burns To heatthe combustion furnace perform the following steps The furnace controller is located on the front panel ofthe Antek 9000F NOTE The furnace controller contains no user serviceable parts Warranty is void if controller shows evidence of tampering Figure 5 3 Furnace Controller Action Result 1 Press to view setpoint 2 Press 96 to increase setpoint 3 Press 96 to decrease setpoint 4 Adjust forasetting of 1050 C 5 Press together to reset alarm or reset fault message 6 If alarm persists discontinue operations and disconnect power Contact local Antek Representative or Antek Service Department 7 Note the temperature indication of the furnace as it heats to verify proper operation 5 4 Reagent Pumps CAUTION Do not allow the pumps to operate without a filled reagent bottle being attached Running the pump dry for extended periods of time can cause the pump to fail and can cause damage to the pyrolysis tube if an injection occurs without Reagent B being present in the pyrotube 31 ANTEK 9000F USER S MANUAL 5 4 1 Reagent A
8. 5 Letthe instrument equilibrate Load the calibration file and the method file you want to use with your samples To do this enter edit method and open the file you wish to use Method files have mth file extensions and are saved under c 19000f methods directory Go to Run Calibration screen and open the calibration file you want to use or if you want to create a new calibration curve see the next section 6 3 Building a Calibration Curve 1 Select Run Calibration from the Main Screen 2 Press Editand press New and name this file Select your display preferences by pressing display preferences under the Edit button Be sure to save this new cal file once you have created it The calibration files are saved under c 9000F cals directory Calibration files all have the cal extension after their file name NOTE A detailed description of software operation is given in Section 8 3 Press File and select Save File As Type in the name with the cal extension and then press OK 33 ANTEK 9000F USER S MANUAL 4 Run afew blanks to be sure that the baseline is quiet and stable You can include this data in the calibration if you choose NOTE Avoid cross contamination Be sure to clean the syringe out thoroughly Draw a sample with the syringe the same way each and every time This ensures good precision 5 Torunastandard select the Run menu Press Standard Fill out the information about the standard
9. USER S MANUAL 2 2 Cautions WARNING The furnace of the Antek 9000F Fluoride Analyzer operates at temperatures above 1000 C and can serve as an ignition source The instrument must be located in a non explosive atmosphere WARNING Do not power up equipment All activities described in Section 2 Installation do not require electrical power 2 3 Physical Installation 2 3 1 Gases Connect gases as shown in Figure 2 4 Figure 2 4 Gas Connections su iii e Using the copper gas lines supplied with the 9000F system connect the supply gases to the proper gas inlet fittings Refer to Figure 2 6a for the recommended assembly procedure for the swage type compression fittings included in the accessory kit Figure 2 5a Compression Fittings m Insert tubing through nut Slide ferrule over tubing Insert tubing with ferrule until tubing bottoms in fitting Secure nut finger tight plus one turn ANTEK 9000F USER S MANUAL Figure
10. clockwise all gas control valves CAUTION Do not shut control valve off hard Turn clockwise only until slight resistance is felt Over tightening may damage the control device 2 Setthe supply pressure ofthe oxygen to the recommended level as outlined in previously The normal oxygen pressure levelis 2 75 bar 40 psig CAUTION Unless specifically stated the supply pressure of gases used with the Antek 9000F should not exceed 4 0 bar 60 psig 3 Theflow rate may be estimated by observing the flow meter ball and comparing the reading to Figure 7 1 4 Carefully turn ON counterclockwise the Inlet Oxygen control valve Adjustthe oxygen flow to the desired rate asindicated by the flow meter ball Optimum oxygen flow rates for specific application s will be determined by experience 38 ANTEK 9000F USER S MANUAL 7 1 4 Pyro Oxygen WARNING Oxygen is a strong ozidizer and greatly accelerates combustion This is the main oxygen supply to the high temperature oxidative portion ofthe pyrotube Normally 350 to 450 mL min Pyro oxygen flow is required to maintain a safe excess of oxygen and ensure complete oxidation ofthe sample CAUTION Do not attempt to analyze samples without an adequate supply of oxygen to the oxidative zone This may result in incomplete combustion and the formation of fine carbon particles coking The coking may cause irreversible reduction or complete loss of sensitivity by the detector 1 Turn OFF c
11. Aa PURO aa 6 es go o AMP o A o 6 Lol Cieli nr 6 2 3 2 rio o MAMMA A UU AR EANET sS 7 dio CACA EU pais 10 2 34 25010401 LCI CO ZOTE ia 10 2 3 4 1 Installing the Ion Specific Reference Electrode 11 20 00 IDRA PUD WI 13 O Clan 14 29 DIA CIN AAA 15 DNE COMINO nni 15 ll o o A 15 SECTION 3 SYSTEM OVERVIEW 11100 rr 17 Sl WAUA UONI AA u m 17 3 2 Model 9000F IA 17 5 3 COIDULGI ac eae amme E oi 22 SECTION 4 ACCESSORY EQUIPMENT onu nan nn annan anne nn nan annan nene annan rr rr rra 25 4 1 Model 735 Controlled Rate Sample Drive cuore 25 41 osta 60 oo vo i Gps A 25 A ea 26 4 2 MODEL 734 GAS LIQUID INLET SYSTEM i 27 42 Rd 27 400 Vaia 27 SECTION 5 PRIMARY TESTIS lilla 29 De E es UR AA III Wa 29 SO MULE POWEFUD Aa 29 DO PUA BO WMU iii 31 is A S E ee ees 31 kl iu sqq uic Aa 32 242 A A mmm 32 5 5 Installation and Startup neci TT 37 ANTEK 9000F USER S MANUAL SECTION 6 SIAR FOP BASICS ai 33 61 Startup MOr te Very St SET IT TTL 33 6 2 UDI IA AAA 33 63 BAAG a E rO CUIVE ia 33 Aca tire kaaa aaa 34 SES REA 34 SECTION 7 APPLICATIONS amp ANALYTICAL PROCEDURES rr aannnnannnnnannnnnannnnnnne 37 A LOOK BASIC p 37 AM deb 37 F E A O e o II A 37 RN MERE SI e 38 e O MAA 39 7 1 5 Reagent B Deionized Water sanee 40 Fil
12. Calibration and be sure your calibration curve appears If it does not use the File and Open commands toload the correct curve 2 Clickon Run Sample 3 In this menu click on Run and then Sample Fill out the information regarding the sample completely and correctly Be sure to enter 1 for Multiplication Dilution Factor and enter aSample Weight or Volume 4 The analysis begins once you press OK The data is collected and when the analysis is complete the baseline is drawn the maximum mV is noted and the area counts displayed Whenthe run is finished click OK and this data will now be displayed on the sample table If you do not want to save the data click on cancel and abort the run 5 Besuretosave the file once you have all your data displayed in the sample table The file names have sam extensions They are saved in the c 19000f samples directory 6 5 Shutdown Daily Shutdown Procedure 1 Turnoffthe Reagent B 2 Turnoffthe flow of TISAB Reagent A on the drive controller 3 Turnoffthe gasesatthe rotometers Carefully turn these knobs clockwise to turn off the flow of gases 4 Turnoffthe monitor only Leave the PC on 34 ANTEK 9000F USER S MANUAL To shutdown the instrument for along periodoftime jn 2 3 Turn off the Reagent B pump Turn down the furnace to 500 C Turn off the gases at the rotometers Carefully turn these knobs clockwise to turn off the flow of gases Turn off the flow
13. SYSEM FOW CCODSIOETHIOFPIS AI 40 Eo FUNGA TED AA ETE TOT 42 7 4 Sample Handling SIPENDI 42 7 4 1 Liquid Sample Materials riada ete 42 7 4 2 Gas and Liquefied Gas LPG Sample Materials eene 42 Tavo WANA WA ET 43 7 5 Ka AA c e o CO 43 7 0 Gaseous and HIGQUCHEC GAS ANAIYSIS ma a 44 JN SONGS ASS ata 44 SECTION 8 SOFIWARE mai 45 AA PPP 45 964 RUN 85119 72 14 07 7 inicio 46 SECTION 9 TROUBLESFIOOTING acicate eb 51 SECTION 10 PARIS Ge CONSUMABLES cipal AA iu 53 A A 53 192 HS nn e A A 53 10 2 1 Glassware for use with MultiMatrix Model 740 i 53 10 2 2 For use with Gas LPG Sampling System Model 734 eene 53 0 9 CONSUNADI na paa aaa 53 TOC 3 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK TOC 4 MATERIAL SAFETY DATA SHEET ELECTRODE FILL SOLUTION Section Product Identification Product Name Electrode Fill Solution Supplier s Name PAC Emergency Phone Number 800 365 2143 713 580 0339 Address 300 Bammel Westfield Road Houston Texas 77090 3508 Date Prepared June 1 2004 Hazardous Shipment Labeling Testing by Bureau of Explosives has indicated this is not an Oxidizer Section ll Hazardous Ingredients Identity Information Hazardous Components Potassium Chloride KCI USIA PRL od None ACGIH TLV None PID ae ie 100 mg Kg IVNCat De ionized Water H20 CONO asa 132183 lama 90 0 OSHA PEL con
14. The Model 734 is available in different configurations for various analytical requirements Model Description or ananas Gas liquefied gas sampling system 7984 1 A Automated gas liquefied gas sampling system o Gas sampling system 734 2A Automated gas sampling system Foo CORE Liquefied gas sampling system 34 BA Automated liguefied gas sampling system The following text will focus on the general aspects ofinstallation and operation For complete details of Model 734 installation and operations refer to the Model 734 Operations Manual Installation Depending on the configuration of the 9000F system and the pyrotube being used the Model 734 may be interfaced differently Figure 4 4 illustrates a common interface configuration Interface to 71156 Direct Injection 4 2 2 Operation Once the Model 734 is properly installed the following steps should be taken to place the system in Service 1 Place the main power switch to the Model 734 in the ON position 2 Allow the Model 734 to warm up for at least Y hour prior to sample injection 3 Using the appropriate Model 734 controls assure that the valves are fully functional 27 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK 28 SECTION 5 PRIMARY TESTS 5 1 Pressure Leak Tests The following procedure will only a
15. cap tightly sealed to protect product integrity NFPA Rating Scale 0 4 HI o 1 LI ma 1 A UL MAMA 0 DDOGIBIC iaa None MSDS 10 ANTEK 9000F MANUAL Material Safety Data Sheets Section VIII Control Measures Respiratory Protection NotApplicable Volar Not applicable Protective Gloves None Eye Protection esarresaresacamentasss Safety Glasses Other protective clothing None Work Hygienic Practices Emergency eye wash should be available The information contained herein is furnished without warranty of any kind Users should consider these data only as a supplement to other information gathered by them and must make independent determinations of the suitability and completeness of the information from all sources to assure proper use and disposal of these materials and the safety and health of employees and customers MSDS 11 ANTEK 9000F MANUAL Material Safety Data Sheets THIS PAGE INTENTIONALLY BLANK MSDS 12 SECTION 1 GENERAL INFORMATION 1 1 INTRODUCTION The Antek 9000F Fluoride Measurement System is a powerful development for rapid analysis of materials containing fluoride compounds Solid liquid gaseous or LPG samples may be analyzed with ease usually in less than fifteen minutes 1 1 1 Principle of Operation The automated method of analysis involves a high temperature oxidation of the
16. entire sample converting any fluorine containing compounds to hydrogen fluoride HF The HF then preferen tially reacts with a proprietary carrier andis then transferred to a buffered receiving solution in which itis decomplexed The Fluoride Ion F is then measured in a temperature controlled manner with an Ion Specific Electrode ISE Since the fluoride induced millivolt change is proportional to the amount of fluoride in the sample quantitation is greatly simplified The chemical reactions involved may be summarized as follows Reaction Chemistry by Pyrohydrolysis ISE RF H20 02 45 HF Oxides HF Buffers NaF Hs0 Detection as disassociated F ions by ISE 1 1 2 System Components Basic System Model 9000F Fluoride Analyzer Accessories for liquid analysis Computer System with Integrated software Package Starter Chemicals and Reagent Storage Rack 1 1 3 Optional Equipment Model 735E Syringe Drive Model 734 Gas LPG Inlet System Model 738 Autosampler Model 740 MultiMatrix NOTE Installation and use of the Basic System are covered in this manual Installation and use of other optional equipment will be covered in other manuals or addenda to this manual 1 1 4 Materials Required But Not Supplied In order to install and operate the System 9000F the following additional materials are required e Smallset of screw drivers e Smallset of open end wrenches including 7 16 1 2 and 9 16 e Small adjustable wrench e Needle nose plier
17. not attempt to operate the system until all of the setup procedures set forth in the previous sections of this manual have been thoroughly read understood and completed 7 1 Important Basics 7 1 1 7 1 2 Regardless ofthe application in which the Antek 9000F is employed there are certain conditions that must be present in order to obtain predictable analytical performance Itis also important that the operator understand the basic principles and instrument functions utilized Gas and Carrier Flows WARNING High pressure gases should be handled with extreme care Ensure that all relevant safety precautions are carefully followed and all gas lines regulators gas purifiers etc are specified for the intended use Inlet Argon Argon or helium is used as a carrier gas to sweep the volatilized sample from the inlet and into the high temperature oxidative portion of the pyrotube Normally 75 to 140 mL min argon flow is required to provide an even sweep of the sample inlet Helium is also acceptable NOTE For certain applications inlet argon may not be necessary or desirable In these cases proceed to Section 7 1 2 Inlet Oxygen 1 Turn OFF clockwise all gas control valves CAUTION Do notshut control valve off hard Turn clockwise only until slight resistance is felt Over tightening may damage the control device 2 Setthesupply pressure of the argon to the recommended level as outlined previously The normalargon pressu
18. of TISAB Reagent A on the drive Take the bottle cap and line that are affixed and inside the TISAB gallon reservoir and affix it to a gallon jug filled with high purity de fluorinated water ASTM Type I water Turn the dual head peristaltic pump on and flush the instrument lines out with water Flush atleast a half of a gallon through the instrument When you are through turn off the flow of water to the instrument The middle position on the controller is OFF Exit the fluoride software Turn offthe PC and monitor 6 Turnoffany peripherals Turn off the 9000F 35 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK 36 SECTION 7 APPLICATIONS amp ANALYTICAL PROCEDURES The Antek 9000F is capable of rapid precise quantitative analysis of fluorine content in solid liquid or gaseous matrices Thissection will attempt to provide the Antek 9000F user with a broad spectrum of information on the finer details of various recommended analytical procedures and instrument applications Included are procedures and suggestions with particular emphasis on as flows furnace temperature sample handling and preparation calibration and sample analysis NOTE The following procedures and suggestions are meant for informational purposes The optimum parameters and procedures for any particular application and sample type will best be determined by experience or consultation with ANTEK applications specialists CAUTION Do
19. preferred However an unbreakable plastic container is recommended for the collection of waste fluids if plumbing to a drain is not possible Place waste container where it can be easily monitored at a level below the Model 9000F Analyzer NOTE These aqueous waste materials are high in salt content Routine disposal with water dilution is permissible 1f compatible with your laboratory sewer system and local regulations 1 2 2 Electrical Requirements The Antek Model 9000F Fluoride System and computer utilizes stable 115 VAC 50 60 Hzor 230 VAC 50 Hz A 15ampcircuitisrequiredfor 115 VAC and an 8 amp for 230 VAC A good ground is necessary for each component The basic system requires seven 7 electrical outlets Check Optional Equipment for additional electrical requirements WARNING A poor ground may present a severe shock hazard 115VAC 230VAC Outlets Amperes Amperes Required Model 734 2 0 1 0 Model 735 1 0 0 5 1 Model 9000F 15 0 8 0 1 Computer System 2 Circulating Baths 1 Peristaltic Pumps 1 ANTEK 9000F USER S MANUAL 1 2 3 1 2 4 1 2 5 Gas Reguirements Chromatographic grade argon and chromatographic grade oxygen are required to operate the Antek Model 9000F Fluoride System These gas streams must be regulated at 40 psig and in line gas dryers are suggested OIE anos 3 0 bar 40 psig 99 75 maximum moisture 5 ppm A 3 0 bar 40 psig 99 75 maximum moisture 5 ppm Helium may be substituted for argon as a car
20. pyrotube This pyrotube isintended for the analysis of gas and liquid samples only This pyrotube may be used in conjunction with microliter syringes Model 734 Gas Liquid Inlet System or Model 735 Sample Drive Refer to Figure 2 6 and Figure 2 7 for access location and orientation information NOTE It may be desirable to perform a SAVE file information as described in Section 8 before system shutdown This will preserve all analytical parameters calibration data and sample data for later use or reference ANTEK 9000F USER S MANUAL In the eventa P N 71156 pyrotube needs to be installed or replaced the following steps should be taken 1 To allow the furnace to cool turn the main power switch of the 9000F Furnace Module to the OFF position and unplug the power cord from the power source WARNING Ensure that the power cord has been unplugged from the power source before continuing If poweris applied while servicing internal components a severe electric shock hazard may exist 2 Remove the side panels as shown in Figure 2 6 This should provide adequate space for installation ofthe pyrotube 3 If a pyrotube is currently installed in the furnace carefully remove the receiving vessel remove the gas fittings remove the spring clamp loosen the ceramic endplates and remove the used pyrotube 4 Ensure that the furnace is free of any materials which will obstruct the insertion of the new pyrotube 5 Carefully clean the ex
21. sufficiently pressurized to provide adequate sample volume and pressure Particularly LPG sample containers should have at least 12 bar 200 psig pressure Solid Sample Materials Solid sample materials are easier to handle and less likely to be contaminated or altered However solid materials are subject to contamination by various means and care should be taken to prevent analytical error Some solid materials may be contaminated by their container or by exposure to liquids or vapors Many solid matrices are extremely hygroscopic Therefore many variables must be considered when analyzing solid sample materials The following are some suggestions which will help in reducing analytical error 1 Trace Fluorine Extreme care must be taken notto contaminate the sample Trace amounts offluorine in a sample material may be changed by the slightest mistakes in sample handling The sample may have to be refrigerated and all glassware syringes and any other apparatus used should be clean and free of fluorine compounds to avoid possible contamination If trace fluorine analysis is to be accurate the highest level of analytical technique should be used 2 Volatile Fluorine If a solid sample material contains volatile fluorine compounds the sample should be refrigerated and tightly capped while waiting for analysis This will prevent loss of fluorine and erroneous results 3 Hygroscopic Matrix Most solid sample materials are hygroscopi
22. 2 15 Sensing Electrode MEME j N DO NOT OVERTIGHTEN O RING 12 ANTEK 9000F USER S MANUAL 6 Connectthe ISE Sensing Electrode P N 71314 the ISE Reference Electrode and ground as shownin Figure 2 16 Figure 2 16 ISE Flow Call REFERENCE Figure 2 17 ISE Cell Body Flow Path 7 Make sure the Receiving Solution flowpath is clear as shown in Figure 2 17 FLOW PATH 2 3 5 Dual Head Peristaltic Pump Locate the Dual Head Peristaltic Pump as shown in Figure 2 18 Figure 2 18 Dual Head Peristaltic pump 13 ANTEK 9000F USER S MANUAL Confirm that the Peristaltic tubing P N 30258 is properly locked in position as shown in Figure 2 19 Figure 2 19 Peristaltic Pump Tubing THUMB SCREW TUBING ROUND NOT CRIMPED OR FLATTENED 2 3 6 Cables Install the Control Interface connections as shown in Figure 2 20 Power cords may be attached to equipment CAUTION Do not apply power See Section 2 3 8 regarding computer Figure 2 20 Control Interface Connections POWER CORD 2101010 1 0 PORT ANTEK 9000F USER S MANUAL 2 3 7 Drain and Vent Install the drain and vent as shown in Figure 2 2 1 Waste fluids can be collected in one single container or directly plumbed to a drain Figure 2 21 Drain and Vent REAGENT A REAGENT B
23. 2 5b Glass to Metal Fitting 2 3 2 Figure 2 6 sa Position 4 nut first then slide Teflon ferrule over glass arm Insert male fitting until glass arm bottoms outin base of male fitting Secure finger tight Back out glass arm tip Imm so that bevel inside male fitting does not chip glass arm tip Tighten until male nutthreads are nearly covered Do not over tighten Installation of Pyrotubes To install the pyrolysis tube remove the side panels To remove the side panels loosen the four locking screws located on each panel and remove side covers by lifting straight up with the panels as shown 1n Figure 2 6 Ifnecessary the instrument cover may be removed by loosening the two locking screws and sliding back one inch and lifting up CAUTION Remove the right panel slowly so that accidental breakage of the pyrolysis tube if present will not occur ANTEK 9000F USER S MANUAL Figure 2 7 Pyrotube 71156 Installation Figure 2 8 Pyrotube 71191 Installation 1 Receiving vessel 2 Ceramicendplates 3 Pyro oxygen gas fitting 4 ReagentBfitting 5 Inlet gas fitting 6 Spring Clamp The following isa step by step procedure for the installation of the P N 71156
24. 3 300 Bammel Westfield Road Houston TX 77090 Phone 281 580 0339 800 444 TES T 8378 Fax 281 580 0719 THIS PAGE LEFT BLANK Installation Problem Report Company Installation Date Contact Installed By Address PAC Representative Sales Order City St Zip Country Territory Fax or e mail complete report to Service Manager Phone Fax fax 281 580 0719 4 e mail service paclp com E mail Purchase Date SN Model Install Date Problem s Model S N Part Description of Problem Model S N Part Description of Problem Model S N Part Description of Problem Type of Problem Appearance Broken Electronic Missing Off Spec Wrong Assembly Electric Leak Mechanical Non function SS AAA For more information please contact us E mail sales expotechusa com Website www ExpotechUSA com
25. 50 and 500 ppm F kit A Fuse 1 Amp A AE OA Fuse 3 Amp 220g 2 SE Fuse 15 Amp c 25 uL syringe with replaceable needles WI T a TEEN needle replacements 5 pk ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK 54 OPAC Except as noted ANTEK INSTRUMENTS a subsidiary of PAC hereinafter referred to as ANTEK hereby warrants its products against failure due to defects in material and workmanship for a period of one 1 year from the date of delivery when the products are used under appropriate conditions and in accordance with the manufacturer s operating instructions Notwithstanding the foregoing photomultiplier tubes and UV lamps are warranted for ninety 90 days Primary furnaces are warranted for six 6 months ANTEK does not warrant products that are not manufactured by ANTEK except to the extent of the warranty ANTEK may actually pass through or assign from the manufacturer Buyer s sole and exclusive remedies shall be limited to the repair and or replacement of defective parts at the sole discretion of ANTEK All product warranties are F O B Houston Texas LIMITED WARRANTY OF PAC Warranty covers parts and labor only Warranty will not be granted for removal and installation of parts components or accessories or for normally required maintenance functions including but not limited to minor repairs gasket or seal replac
26. LOW O HIGH a GAIN MEDIUM O Ee O OO I HEDHII gt al al el al eel d O PUMA AY al al al al al lola VENT TO WASTE 1 Sub Panel Access Screws 5 2 Furnace Temperature Controller 3 Flowmeters a Oxygen To Pyrolysis Tube b Oxygen To Pyrolysis Inlet c Argon To Pyrolysis Inlet ANTEK 9000F USER S MANUAL 4 Fluoride Detector ISE Figure 3 5 Model 9000F General Plumbing Diagram TO BOTTOM ARM INLET GAS CARRIER 02 MIX TO TOP ARM TISAB PUMP WATER PUMP IN 1 2 OF PUMP REAGENT A PYROLYSIS TUBE 71156 COOL WATER OUT TO PUMP LLER 68007 E fr u w gt 2 5 e o e CH INLET GAS CARRIER 02 MIX O2 IN CARRIER IN LIQUID HEATED WATER IN or OUT DET CELL ELECTRODE REFERENCE ELECTRODE Wx A MN RECEIVING VESSEL HEATER 68006 TISAB PUMP WASTE 1 2 OF PUMP A 1 2 OF PUMP HEATED WATER IN or OUT Figure 3 6 Rear Panel Plumbing Connections CLA ZA SS e PE ASA n REAGENT B n REAGENT A LT x ES AS 5 e 0980 WASTE 19 ANTEK 9000F USER S MANUAL Figure 3 7 Pyrolysis Tube Plumbing gas liquid only Combusted sample to Furnac
27. Model 9000F Fluoride Analyzer Installation Operation Service Manual For more information please contact us E mail sales expotechusa com Website www ExpotechUSA com ANTEK 9000F USER SMANUAL THIS MANUAL CONTAINS CONFIDENTIAL AND PROPRIETARY INFORMATION Which is the property of PAC This manual and all information disclosed herein shall not be used to manufacture construct or fabricate the goods disclosed herein shall not be exploited or sold shall not be copied or otherwise reproduced in whole or in part and shall not be revealed or disclosed to others or in any manner made public without the express written permission of PAC REVISION HISTORY A First release B Updates to format and content October 2004 10 27 04 CE DECLARATION OF CONFORMITY Equipment Fluoride Analyzer Model 9000F Date of Issue April 12 1996 Manufacturer Antek Instruments 300 Bammel Westfield Road Houston TX 77090 3508 USA This equipment complies with the following standards EN 55011 Limits and Methods of Measurement of Radio Disturbances Characteristics of Industrial Scientific and Medical ISM Radio Frequency Equipment IEC 801 2 IEC 1000 4 2 Cenelec 60801 2 Electromagnetic Compatibility for Industrial Process Measurement and Control Equipment Part 2 Electrostatic Discharge Requirements IEC 801 3 IEC 1000 4 3 Cenelec 50140 Electromagnetic Compatibility for Electrical and Electronic Equipment Pa
28. Pump Reagent A TISAB is added to the receiving vessel via a Masterflex dual head peristaltic pump found on the left hand side ofthe Antek 9000F Make sure that a bottle containing TISAB is connected to the Reagent A port Turn on the flow atthe drive controller by setting the switchto FWD and the speed to 3 0 Verify that flow is advancing from the bottle to the receiving vessel through the ISE and out the liquid vent 5 4 2 Reagent B Pump CAUTION The Reagent B pump should not be turned on until the furnace is at least 800 C Reagent Bisintroduced to the pyrotube via a Masterflex peristaltic pump Turn the Reagent B pump switch on on is the up position the middle position is off Turn the speed dial to the 3 o clock position for a rate of 1 ml min Visually ensure that Reagent Bis being pumped to the entrance ofthe pyrotube 5 5 Installation and Start up Checklist The following is a checklist that can be used to assure that the Model 9000F is ready to enter routine operation __ System located properly Accessories ifany installed Gas lines with specified pressures and flows installed Waste line and vents installed __ Pyrotube properly installed Leak check pressure check performed Reagent reservoirs filled and pumps primed Furnace atoperating temperature Computer operational with integrated software 32 SECTION 6 START UP BASICS This chapter contains a detailed description of the procedures needed to
29. S 5 Section Product 19 EAMETSA Ia MSDS 5 Section UI e Hazardous a reales MSDS 5 Section IA ads n MSDS 5 Section IV Fire and Explosion Hazard Data annan enne na nne MSDS 5 SECTION Y ROACH ADELA 0200000 5 00 0 2 aa MSDS 6 Section VI Health Hazard Dala cuore Tm MSDS 6 section Vi Fhe CAO irradia ira mu m MSDS 6 Section VIII Control Measures iii MSDS 7 MATERIAL SAFETY DATA SHEET REAGEN TE qc MSDS 9 Section Product IdentificatiON w wmwwmanwwanamwwnanwwananwa Een wwa MSDS 9 Section Il Hazardous Ingredients identity Information cee MSDS 9 SEAN BIS WAA e c iia MSDS 9 Section IV Fire and Explosion Hazard Data anat ia MSDS 9 SECUORN Y KAVU Ab AAA MSDS 10 sector Yi HELA Hazard NI aatatel ateismi la oro MSDS 10 Section VII uices acm m Um MSDS 10 Section VIII Control Measures consi IU rare Cs DIM PIER UM MO MSDS 1 1 SECTION 1 GENERAL INFORMATION 5 e ais an 1 NM IDUHeAs5qeIP e 1 NE Suo 61 ONO n 1 LL PIREO 1 11 5 Ooo KA E aA ias 1 1 1 4 Materials Required But Not Supplied 1 TOC 1 ANTEK 9000F USER S MANUAL MEAE POG CINCY AES i m 2 1 2 1 Environmental Requirements ia 2 L22 EI e 1001 RITA 2 MED UN na 3 182 PRODI WI AA e o E A 3 1 2 5 Telecoms RICO alla 3 SECTION 2 INSTALLATION ar AA 5 A eise LOCATION NO mm 5 KUA
30. TERNATIONAL SALE OF GOODS In accordance with Article 3 2 of the Convention on the Limitation Period in the International sale of Goods ANTEK and Buyer hereby agree that they have expressly excluded the application of the Convention from their Agreement as set forth herein including all terms obligations requirements and duties which may be said to exist or arise from such convention This warranty does not cover and ANTEK will not assume any liability or responsibility in connection with this warranty in the event any fire suppression agents including ABC style or dry powder fire extinguishers other than gases CO2 Halon or FM200 are used directly or indirectly upon the ANTEK products Buyer should be aware that these types of powders are corrosive to electronics and may cause permanent damage to all circuit boards and connections Likewise if any residue from any ABC style or dry powder extinguisher is found in the instrument during the course of an otherwise warranted repair ANTEK will have no liability or responsibility under the warranty and all such repairs will be performed at the ANTEK standard rate for parts and labor Further if upon ANTEK s inspection and review ANTEK determines that the condition of the products is not caused by a defect in ANTEK s material and workmanship but 1s the result of some other condition including but not limited to the use of any dry powder extinguisher the Buyer shall be liable for all direct expen
31. are correct and properly fitted 15 Ifreplacing a used pyrotube conduct a leak test as described in Section 5 before resuming normal operations During initial start up installation a leak test will be performed later in Section 5 ANTEK 9000F USER S MANUAL 2 3 3 Reagent Pump Locate and inspect the Reagent B Pump as described in Figure 2 9 Figure 2 9 ReagentPump YA lt DNA Make sure that the connections of the tubing leading to and from the Reagent B Pump are secure and tight 2 3 4 Absorption Detection Zone Open the front door of the Antek Model 9000F Fluoride analyzer by loosening the two locking screws on the door and it will open outward to the left as shown in Figure 2 10 Figure 2 10 Door Open Q ANTEK ww D AA O ETEA O TU ANTEK 9000F USER S MANUAL The Front Panel is shown in Figure 2 11 Figure 2 11 Chemistry Section TEMPERATURE CONTROLLER e
32. arranty of any kind Users should consider these data only as a supplement to other information gathered by them and must make independent determinations of the suitability and completeness of the information from all sources to assure proper use and disposal of these materials and the safety and health of employees and customers MSDS 7 ANTEK 9000F MANUAL Material Safety Data Sheets THIS PAGE INTENTIONALLY BLANK MSDS 8 MATERIAL SAFETY DATA SHEET REAGENT B Section Product Identification Product Name Fluoride Carrier Reagent B Supplier s Name PAC Emergency Phone Number 800 365 2143 281 580 0339 Address 300 Bammel Westfield Road Houston Texas 77090 3508 Date Prepared June 1 2004 Hazardous Shipment Labeling Testing by Bureau of Explosives has indicated this is not an Oxidizer Section ll Hazardous Ingredients identity Information Hazardous Components Deionized Water H20 CASNO ia 100 516 JA RENATE 99 95 OSHA PE droits None ACGIH TLV Tn None 629 mg Kg OrlDog Section Ill Physical Data Boiling POMME ma 100 C PECCAINO POINT siii 0 C SDeoIH6 GLA VIL lora 1 00 Vapor PLESSULE serna Not applicable DEL 2500 aa eben 5 5 7 5 Solubility in Watel naa Miscible Volatiles by Wt ceeeeeees Notapplicable Evaporation Rate sra Not applicable Y apor Density miwa Not applicable APPIANO aan Odorless Liquid Section IV Fire and Explosion Hazard Data Flash POSTE audiens tense Not ap
33. arrow and hand Figure 3 13 Mouse Main Operator Button Right Button E NY There are fourbasic mouse techniques Pointing Clicking Double Clicking Dragging Position the cursor Activating Selecting Highlights and opens the file Selecting and repositioning an icon to a new location 23 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK 24 SECTION 4 ACCESSORY EOUIPMENT The Antek 9000F Fluoride Analyzer utilizes several accessories to enhance overall performance This section contains guidelines that can be used along with the Operator s Manuals for the following equipment 4 1 Model 735 Controlled Rate Sample Drive 4 1 Figure 4 1 1 The Model 735 Controlled Rate Sample Drive provides an accurate reproducible method of sample introduction into the furnace of the ANTEK 9000F system The Model 735 may be used in conjunction with a syringe for liquid or with a Model 740 MultiMatrix and a quartz sample boat for liquid and solid samples See the Model 735 Operations Manual for detailed instructions before attempting to operate the inlet system Installation The Model 735 should be located on the right side of the ANTEK 9000F system Depending on the configuration of the 9000F system and the pyrotube being used the Model 735 may be interfaced differently Figures 4 1 and 4 2 illustrate two common interface configurations and physical layouts Interface to 71156 D
34. c Many variables must be considered when analyzing liquid sample materials The following are some suggestions which will help in reducing analytical error 1 TraceFluorine Extreme care must be taken not to contaminate the sample Trace amounts offluorinein a sample material may be changed by the slightest mistakes in sample handling The sample may need tobe refrigerated and all glassware syringes and any other apparatus used should be clean and free offluorine compounds to avoid possible contamination Iftrace fluorine analysis is to be accurate the highest level of analytical technique should be used 2 Volatile Fluorine If aliquid sample material contains volatile fluorine compounds the sample should be refrigerated and tightly capped while waiting for analysis This will preventloss of fluorine and erroneousresults 3 Volatile Matrix Most liquid sample materials are volatile to some extent However samples of volatile organic matrices should be keptin a sealed container and refrigerated prior to analysis Evaporation ofsolventis a major cause of analytical error in elemental analysis 4 Reactive Fluorine or Matrix Some fluorine compounds and some matrices may be reactive Extreme care should be taken when choosing a container for these materials Use only inert sample containers to preventanalytical errors Asageneral rule liquid sample materials require very little pre analysis preparation Some materials may need di
35. c to some extent These sample materials should be kept in a sealed container or possibly a desiccator prior to analysis Absorption of water is a major cause of analytical error in weighing 4 Reactive Fluorine or Matrix Some fluorine compounds and some matrices may be reactive Extreme care should be taken when choosing a container for these materials Use only inert sample containers to prevent analytical errors In order to obtain the most accurate and repeatable results solid sample materials must be very homogeneous Therefore solid materials of a heterogeneous nature must be mixed or homogenized This canbe accomplished by grinding or mixing the solid material Extreme care shouldbe taken not to contaminate or chemically alter the solid materialin any way After grinding the solid material should be remixed to eliminate any stratification of the smaller particles 7 5 Liquids Analysis In order to analyze liquid syringe able materials a method with the following characteristics should be utilized Furnace Temperature Reagent B Injection Rate Sample Injection Rate 900 1100 C sample dependent 1 0 1 5 pl minute concentration dependent 1 0 1 5 ul second Sample Size Sample dependent Sample Injection Point See Figure 7 3 or 7 4 9000F Gas Flow Settings 11605 A 4 5 Inlet Og in 2 5 Aries 8 5 43 ANTEK 9000F USER S MANUAL 7 6 Gaseous and Liguefied Gas Analysis In order to analyze gaseous or liguefied gases
36. city Not found Signs and symptoms of exposure Dizziness nausea weakness no serious acute or chronic affects with either external or inhalation exposure Medical conditions generally aggravated by exposure kidney or heart problems Emergency and first aid procedures SEIL adt CV CS ra wash with large amounts of water for 15 minutes IU EO EDO versa idea consult physician MSDS 2 ANTEK 9000F MANUAL Material Safety Data Sheets Section VII Precautions Steps to be taken if material is released or spilled Pick up and wash down drain with excess water Waste Disposal Method Notregulated Precautions to be taken in handling and storing Store atroom temperature and keep cap tightly sealed to protect productintegrity NFPA Rating Scale 0 4 Health 2 PI makku MAR I Reactivity n 0 SPEC sicari None Section VIII Control Measures Respiratory Protection 5 tns Not Applicable Venta tod uno Not applicable Protective COV CS aid Optional Eye PEOLE CON sotana Safety glasses Other protective clothing None required Work Hygienic Practices Emergency eye wash should be available Wash hands throroughly before eating or drinking Theinformation contained herein 1s furnished without warranty of any kind Users should consider this data only as a supplement to other information gathered by them and must make independent determinations of the suitab
37. completely and correctly For example if you were using a 1 ppm organic fluoride enter 1 ppm F std as the name enter the volume you are going to inject 20 pL and then enter 1 for the concentration amount Draw 20 pL of afluoropentane in xylenes or similar organic standard into a syringe Place the syringe through the septa and mountit onto the Model 735 Controlled Syringe Drive or in a quartz boat in the Model 740 multi matrix The Fluoride software sends a signalto the Model 735 Controlled Rate Syringe Drive after you press OK The analysis begins when the OK button is pressed At each level of the calibration do multiple injections To run another injection right after the other anotherinjection ofthesame sample press Run and select Standard and highlight the sample you are injecting again Press Insert After This sample islabeled with the same name followed by a dash and a number The numbers denote the individual injections 6 Touseornotusea particular injection press Edit Select Name s I D s and Uses and highlight the particular injection to use or not use To not use this injection click on the green X box This clears that box and this data will not be included in the calibration calculations To use a particular injection be sure that the green X box is activated You will see a green box with an X in it 6 4 Running Samples 1 Besure that the calibration curve that you want to use is loaded To be sure of this click on Run
38. e Reagent B condenser Thermocouple top E Carrier Mix bottom Pyrotube 71156 Pyro 02 Ceramic Inserts Sample to ISE Figure 3 8 Rear External View e cn e Hv L 1ALSA 1ALSA FF POWER TEMP SUPPLY cor 1 Oxygen Argon Mix Feeds carrier mixture to pyrotube 2 Reagent B Feed supplies Reagent B to the Reagent B Pump 3 PowerSwitch applies power to 9000F 20 ANTEK 9000F USER S MANUAL 4 Power Connection links power cord 5 Fuse Tray containing Fuses Fuse Rating 115 v Fuse Rating 230 v LI 15 amp 8 amp L2 15 amp 8 amp 6 Fansand Peristaltic Pump Transformer lamp Power Supplies lamp Furnace Controller lamp Furnace 12 amp 7 Drains waste exit to containers 2 8 Carrier Supply argon or helium 9 Oxygen Supply 10 Reagent A from Reagent A supply bottle 11 Computer Interface 50 pin ribbon cable 12 Remote Control Cable Connectors for Model 734 735 Figure 3 9 Model 9000F Rear Internal View O
39. ed to septa fittings screws fuses pyrolysis tubes dryer tubes scrubber tubes sample boats inlet heater elements SIC Auto Sampler or Leap Tech Buyer expressly understands and agrees that all invoices must be paid in full prior to any obligation of ANTEK to issue or perform any warranty service as set forth herein Page 2 of 3 300 Bammel Westfield Road Houston TX 77090 Phone 281 580 0339 800 444 TEST 8378 Fax 281 580 0719 OPAC No employee representative or agent of ANTEK is authorized to either expressly or impliedly modify extend alter or change any of the warranties expressed herein Further Buyer acknowledges that no such employee representative or agent of ANTEK has in any way attempted either verbally or in writing to change alter modify any terms and conditions of this warranty either express or implied ANTEK and Buyer agree that the internal laws of the State of Texas shall govern the rights and duties of the parties under this agreement and jurisdiction and venue is fixed in Harris County Texas ANTEK and Buyer further agree that the choice of law jurisdiction and venue as set forth herein are material terms and conditions to this agreement and but for such agreement ANTEK would not enter the agreement for the consideration as set forth between the parties Buyer agrees that ANTEK s prices reflect an analysis of the elimination of uncertainty regarding the Jurisdiction for any dispute Page 3 of
40. ements inspection requirements adjustments etc DISCLAIMER OF ALL OTHER EXPRESS OR IMPLIED WARRANTIES IT IS EXPRESSLY AGREED THAT BUYER S REMEDIES EXPRESSED IN THIS WARRANTY ARE BUYER S EXCLUSIVE REMEDIES FURTHER ANTEK MAKES NO WARRANTY EXPRESS OR IMPLIED AS TO THE DESIGN SALE INSTALLATION OR USE OF ITS PRODUCTS ANTEK MAKES NO OTHER WARRANTY WHATEVER EXPRESS OR IMPLIED AS TO THE MERCHANTABILITY OR FITNESS FOR ANY PARTICULAR PURPOSE OF THE PRODUCTS SOLD UNDER THIS AGREEMENT AND ANTEK S LIABILITY SHALL BE LIMITED TO THE WRITTEN WARRANTY SPECIFIED HEREIN LIMITATIONS AND EXCLUSIONS TO WARRANTY BUYER AGREES THAT ANTEK SHALL NOT BE LIABLE FOR ANY DIRECT INCIDENTAL OR CONSEQUENTIAL DAMAGES WHETHER BUYER S CLAIM BE BASED IN CONTRACT TORT WARRANTY STRICT LIABILITY OR OTHERWISE WHICH BUYER MAY SUFFER FOR ANY REASON INCLUDING REASONS ATTRIBUTABLE TO ANTEK EXCLUSION OF APPLICATION OF UNITED NATIONS CONVENTION ON CONTRACTS FOR THE INTERNATIONAL SALE OF GOODS In Accordance with article 6 of the United Nations Convention on Contracts for the International Sale of Goods ANTEK and Buyer hereby exclude the application of the convention including all terms obligations requirements and duties which may be said to exist or arise from such convention Page 1 of 3 300 Bammel Westfield Road Houston TX 77090 Phone 281 580 0339 800 444 TEST 8378 Fax 281 580 0719 EXCLUSION OF CONVENTION ON THE LIMITATION PERIOD IN THE IN
41. establish basic operation upon instrumentstart up CAUTION Do not attempt to operate the Model 9000F system until all installation and setup procedures outlined in the previous sections of this manual have been successfully completed CAUTION Become familiar with the location and use of all controls indicators connections and accessories and carefully read all instructions prior to operating any portion of the system 6 1 Start up for the very first time To power up the instrument for the first time or when power has been lost Itis important to follow this start up procedure step by step You are establishing communication between the instrument peripherals and the PC 1 Turnonthe 9000F instrument first The on off switch is on the back of the instrument located in the lower right hand comer as you look at the front of the 9000F 2 Turnonany peripherals 735 734 or 740 3 Turnon the computer Start the Fluoride software 6 2 Obtaining a Stable Baseline 1 Turn on the gases argon or helium and oxygen Set the rotometers to 4 0 3 0 and 2 0 on the front panel of the instrument Flows may be sample dependent 2 Turnontheflow of TISAB Reagent A on the separate drive controller Set this switch to FWD 3 Setthe furnace controller to 1050 C This procedure is described in detail in Section 5 3 4 Turnonthe Reagent B pump up is the on position the middle position is off after the furnace reaches 800 C
42. ggravated by exposure Respiratory ailments persons with sensitive skin may be affected Emergency and first aid procedures skin and eyes irrigate with plenty of water RI acoso Dilute with large amounts of water Do not induce vomiting Consult physician Section VII Precautions Steps to be taken if material is released or spilled Vacuum up and set aside for waste disposal Waste Disposal Method Dilute neutralized solution down drain with excess water Observe all federal state and locallaws Precautions to be taken in handling and storing Keep away from oxidizers and caustics Store atroom temperature and keep cap tightly sealed Acetic acid is a CERCL hazard and is subject to Section 3 04 of SARA Title III Other Precautions Always wash hands thoroughly with soap and water after working with this material MSDS 6 ANTEK 9000F MANUAL Material Safety Data Sheets NFPA Rating Scale 0 4 AA 1 T EDE arteria I Reactivity A 0 SPEC naa None Section VIII Control Measures Respiratory Protection ria Not Applicable Ventilation siria local exhaust Protective Gloves Yes Eye Protectio wa Safety Goggles Other protective clothing Lab coat Work Hygienic Practices Emergency eye wash should be available Wash hands throroughly before eating or drinking The information contained herein is furnished without w
43. h in the ON position 2 Allow the Model 735 to stand with the power ON for atleast five minutes to ensure accurate drive speeds 3 Drive the push block in the forward and reverse directions using the forward and reverse push buttons and the speed control At this point the forward and reverse stop positions may be adjusted using the knob adjustments on the left and right sides ofthe Model 735 rear panel NOTE For use with a microliter syringe the forward stop should allow the push block to completely eject all liquid from the syringe and the reverse stop should allow the push block to be in a position as to not interfere with the syringe For use with a quartz boat the forward stop should allow the push block to completely insert the boat into the furnace and the reverse stop should position the boat under the septum of the pyrotube or the access port of the multi matrix sampler 4 Consult the 735 Operator s Manual for a complete review of installation procedures 5 Ensure that the 9000F system can control the Model 735 and that all necessary timed events have been programmed 6 Section 5 Primary Tests of this manual contains a testing procedure to confirm control of the Model 735 26 ANTEK 9000F USER S MANUAL 4 2 MODEL 734 GAS LIQUID INLET SYSTEM 4 2 1 Figure 4 4 The Model 734 Gas Liquid Inlet System is intended for the introduction of gases and liquefied petroleum gases into the furnace ofthe ANTEK 9000F system
44. he baseline without actually starting a run It shows the baseline of the electrode furnace temperature or chiller temperature Please select the samples or injections you would like to use Figure 8 7 Comparison Strip chart Fiesse solectihe samples ormjectians v u would ike to Using the shift key and the left mouse button severalindividualinjections may be compared Figure 8 8 Comparison Strip chart gt View Comparison Chart vi i 100 35 e S42 i r 0 e 9 A AR EE mV 100 i Time each tic mark 30 seconde 2 Hot 47 ANTEK 9000F USER S MANUAL Figure 8 9 Injection Chart Please select the samples or injections you would like to D B m D 3 n O gt D 3 k k Figure 8 10 View Injection Chart gt View Imecton Chart vi Det MEE Sample 4 inecbon 2 1500 pom wanah MI 110 i i 90 c i 1 lk e 0 20 Im 44 _ 20 2 410 soo sio 064 73 820 sio 1000 SETE 48 ANTEK 9000F USER S MANUAL Figure 8 11 Run Standard gt Get New Run Type vi What would you like to do with this run ID 1 1 500 ppm 1 Replace Injection IL 2 1 100 ppm 1 ID 2 2 100 ppm 2 ID 3 1 500 ppm 1 Insert After gt gt D 3 2 500 ppm 2 D 3 3 500 ppm 3 B 3 4 500 ppm 4 3 5 500 ppm 5 lt lt Insert Before D 4 1 1500 ppm 1 O 4 2 1500 ppm 2 New Sample This is the screen that appears when the Standard b
45. ility and completeness of the information from all sources to assure proper use and disposal of these materials and the safety and health of employees and customers MSDS 3 ANTEK 9000F MANUAL Material Safety Data Sheets THIS PAGE INTENTIONALLY BLANK MSDS 4 MATERIAL SAFETY DATA SHEETSHEET RECEIVING Section Product Identification Product Name Receiving Solution Reagent A Supplier s Name PAC Emergency Phone Number 800 365 2143 281 580 0339 Address 300 Bammel Westfield Road Houston Texas 77090 3508 Effective Date Jasnuary 1 2004 Hazardous Shipment Labeling Testing per NACE TM 0169 has shown this product to be non corrosive Section ll Hazardous Ingredients Hazardous Components CAS No Yo OSHA PEL ACGIH TLV LD Acetic Acid C H 02 64 19 7 1 25 mg m 25 mg ml 1 200 Orl Rbt Sodium Acetate C2H 3NaO 127 09 3 8 None None 1 300 IVN Rbt Sodium Chloride NaCI 7647 14 5 6 None None 8 000 Orl Rbt Trans 1 2 Diamino Cyclohexane 150 Tetraacetic Acid CDTA 482 54 2 lt 1 None 1PR Mouse Deionized Water H 20 130 185 gt 84 None None 690 000 Orl Dog Section Ill Physical Data BOIS PA ia 100 C Freezing Poi a 6 C Pecos 1 07 Vapor Pressure oe ti Not applicable PLO UU sai ama 5 0 5 5 Solubility in Water Miscible Volatiles by Wt Not applicable Evaporation Rate Notapplicable Vapor Density Notap
46. ir bubble trapped on outside surface of electrode membrane Poor connections inside electrode plug Membrane leaking Excessive leakage from reference electrode junction Presence of an interfering ion in a constant concentration swamping the selected ions Electrode aged Restrictions in line Tygon tubing around the peristaltic pump is compressed Air bubble trapped on inside of membrane Reference electrode not filled Poor connections inside electrode plugs Solution Check outside of membrane and tap electrode to release bubble Open plug and check wiring Replace electrode Replace reference electrode Check performance with fresh standards and TISAB Replace electrode Check for restrictions in the line Check all fittings and lines from receiving vessel out to waste Replace the Tygon tubing Shake electrode with membrane facing downwards to release air bubble Fill reference electrode with KCI solution Open plugs and check wiring ANTEK 9000F USER S MANUAL SECTION 10 PARTS amp CONSUMABLES 10 1 Hardware Part Number Description A A Size 14 Pump Head 5 0 0 6 PRE E RARIT 1 8 Teflon Tubing o0 Tubing for Reagent B Pump 020 A White Square Plastic Union A P Tygon Tubing Size 16 So A Black Barbed Fitting A TENE EIEE assed TE ETY Tubing for Size 14 Pump Head SALO
47. irect Injection Figure 4 2 Interface to Multi Matrix using PIN 71191 Pyrotube In order to install the Model 735 the following guidelines should be followed 1 Locate the Model 735 as shown in Figure 4 1 or 4 2 2 Attach all electrical power and electronic connections Refer to Figure 4 3 for the location of all controls and connections 3 To have the 9000F control the movement of the Model 735 utilize the Remote Control Cable P N 20058 Connectthe five prong adaptor to the Remote Inlet on the Model 735 rear panel Connect the plug to the desired External Timed Events port on the 9000F rear panel 25 ANTEK 9000F USER S MANUAL Figure 4 3 Model 735 Front amp Rear Panel Connections REVERSE LIMIT FORWARD LIMIT I 7 I O 3 REMOTE A S N TAG WARNING aL Ii sa FUSES ARE 280VAC J5 T TYPE ONLY REPLACE FUSES WITH SAME RATING TYPE THE 4 1 2 Operation Once the Model 735 is properly installed the following steps should be taken to place the system in service 1 Place the main power switc
48. lockwise all gas control valves CAUTION Do not shut control valve off hard Turn clockwise only until slight resistance is felt Over tightening may damage the control device 2 Setthe supply pressure of the oxygen to the recommended level as outlined previously The normal oxygen pressure level is 2 75 bar 40 psig CAUTION Unless specifically stated the supply pressure of gases used with the ANTEK 9000F Analyzer should not exceed 2 75 bar 40 psig 3 The flow rate may be estimated by observing the flow meter ball and comparing the reading to Figure 7 2 4 Carefully turn ON counterclockwise the Pyro oxygen control valve Adjust the oxygen flow to the desired rate as indicated by the flow meter ball Optimum oxygen flow rates for specific application s will be determined by experience Figure 7 2 Pyro Oxygen Flowmeter Curve BALL SETTING Note This chart demonstrates approximate flows and should be used only as a guideline 39 ANTEK 9000F USER S MANUAL 7 1 5 Reagent B Deionized Water This is the supply of Reagent B into the inlet area of the pyrotube Furnace temperature must be greater than 800 C before turning the pump on Recommended flow injection rate is normally 1 to 1 5 mL minute This flow rate is sample and concentration dependent WARNING Do not apply Reagent B to the pyrotube until all gas connections have been completed and leak checked If gas connections are not complete and leak free Reage
49. lows The argon carrier supplies only the Inlet Argon flow meter Oxygen supplies the Inlet Oxygen and Pyro Oxygen flow meters The carrier gases Inlet Argon and Inlet Oxygen are mixed at the exitofthe flow meter assembly and routed to the Carrier Loop 4 on the rear panel From the Carrier loop the now mixed carrier gas is transferred to the pyrolysis tube 5 to sweep the sample into the heated combustion zone Oxygen from the Pyro Oxygen flow meter is also routed to the pyrolysis tube 5 This large supply ofoxygen provides for the complete combustion ofthe sample All combustion products including Reagent B exit the pyrolysis tube via a Receiving vessel 6 There the sample is then mixed into the Receiving Solution Reagent A The dual headed peristaltic pump feeds in Reagent A through the top of the Receiving Vessel and pulls the sample Reagent A mixture from the Receiving Vessel through the Ion Selective Electrode ISE Flow cell 7 and then pumps it out to waste The Ion Specific Sensing Electrode 8 in conjunction with its Reference Electrode 9 senses the change in millivolt potential due tothe change in fluoride concentration and this data is collected by the computer The software using the Nernst Equation calculates the concentration of fluoride based upon the potential mV reading and the calibration curve being used 41 ANTEK 9000F USER S MANUAL 7 3 Furnace Temperature The function of the pyro furnace is to pro
50. lution or filtration but generally no sample preparation is necessary 7 4 2 Gas and Liquefied Gas LPG Sample Materials Gas sample materials are extremely easy to contaminate or alter for a variety ofreasons Some gaseous matrices are reactive and some are extremely hygroscopic Many variables must be considered when analyzing gas sample materials The following are some suggestions which will help in reducing analytical error 1 Trace Fluorine Extreme care mustbe taken notto contaminate the sample Trace amounts offluorine in asample material may be changed by the slightest mistakes in sample handling All glassware syringes high pressure sample containers and any other apparatus used should be clean and free of fluorine compounds to avoid possible contamination If trace fluorine analysis is to be accurate the highest level of analytical technique should be used 42 ANTEK 9000F USER S MANUAL 7 4 3 2 Volatile Fluorine and Matrix Since all gas samples and all gaseous fluorine compounds are difficult to contain the sample should be kept in a leak free sample container before analysis This will preventloss of fluorine and erroneous results 3 Reactive Fluorine or Matrix Some fluorine compounds and some gaseous matrices may be reactive Extreme care should be taken when choosing a container for these materials Use only inert sample containers to prevent analytical errors All gas and LPG sample containers should be
51. n Screen The Main Screen is shown in Figure 8 2 This screen allows the operator to select from three options Edit Method Run Calibration and Run Sample In the upper left hand corner the main screen always shows the active method being used Figure 8 2 Main Screen ES 90001 vi r Active Method A Model 9000F i ene Li Standy Edit Method Run Calibration Initialization complete Instrument running 45 ANTEK 9000F USER S MANUAL 8 2 Run Calibration When the Run Calibration button is selected from the Main Screen Figure 8 2 or the Method Selection Box upper left of every screen the screen below will be displayed Figure 8 3 Run Calibration Screen gt View Comparison Chail vi 3 nao gt MAA m In this example the name of the calibration file that is currently active is Example cal Figure 8 4 Calibration Table HEEL ACI CI OMS NN CTA E E E Figure 8 5 Calibration Chart 2c00 0400 gt 00 2000 0 4000 0 6000 0 8000 0 10000 0 12000 0 14000 0 16000 0 ppm Concentration ppm F This is the chart of the used data If any calibration points are not used the Calibration Chart will change accordingly 46 ANTEK 9000F USER S MANUAL Figure 8 6 View Trends amp View Tienda vi Fumace Temperature C Updare Fata Chiler Temperature C E 15 second Electrode Detector mivat Me aw This screen allows the operator to view t
52. nlet tubing e Septum 6 Once the system is deemed leak free remove plugs adjust regulator to 40 psi and return flow meters to desired settings 5 2 Computer PowerUp Before proceeding with further testing it will be necessary to activate the computer control system WARNING The computer Assembly and Installation procedure located in the Quick Setup pamphlet of the computer s installation package must have been completed before proceeding with the section Turn on the power to the CPU and monitor After the computer has gone through its start up routine double click on the 9000F icon on the desktop to initialize the Fluoride software The screen in Figure 5 1 will come up as shown 29 ANTEK 9000F USER S MANUAL Figure 5 1 Initial Screen with Standby Dialog Box Opened E 3000f vi Active Method Af2461 mth Instrument Hardware Status Edit Aulosamplers Present Methoc prit ANTEK Mirtel QOO b AA pino AM OO ME Run sample E sit Program sell al The Standby Dialog Box will appear If the furnace and the cooler temperatures are 10 of the preset temperature noted in the loaded method a green status bar will be shown If not a red status bar will be displayed Press OK to close the dialog box The Main Screen will now be accessible as seen in Figure 5 2 Using the mouse one ofthree function screens can be selected Edit Method Run Calibration and Run Sample Figure 5 2 Main Screen
53. nt B may leak out and present a hazard 1 When furnace is at temperatures greater than 900 C turn on the Reagent B Pump Note audible rhythmic pulse 2 Confirm Reagent B introduction to the pyrotube by observing for the formation of a steam like mist 7 2 System Flow Considerations The following is a discussion ofthe system flow ofthe Antek 9000F Figure 7 3 and Figure 7 4 illustrates allinterconnecting tubing and the general location of each flow related component Refer to Figure 7 4 for the components described in the following flow system description Figure 7 3 9000F Direct Inject TO BOTTOM ARM O INLET GAS P To OP AR j est A WATER PUMP IN 1 2 OF PUMP REAGENT A COOL WATER OUT TO PUMP COOL WATER IN FROM PUMP RECEIVING VESSEL CHILLER 68007 GAS WENT o pis i INLET GAS CARRIER 02 MIX 02 CARRIER IN LIQUID WENT DET CELL ELECTRODE A T E REFERENCE LECTRODE O A RS NDA lt KW RECEIVING VESSEL HEATER 68006 TISAB PUMP WASTE 1 2 OF PUMP ra 40 ANTEK 9000F USER S MANUAL Figure 7 4 9000F Boat Inject System Carrier gas 1 Oxygen 2 are supplied to the system atthe rear panel ofthe Furnace Module and are routed to the flow meter assembly 3 on the front panel ofthe Furnace Module These flow meters and their associated needle valves provide for control and monitoring of all system gas f
54. plicable APPOATAMGEE adan Colorless liquid vinegar like odor Section IV Fire and Explosion Hazard Data Psh Poi eer Not applicable Atttolenition Temperalures ria Not applicable Flammable LIS Seas Not applicable Extinguishing Media Carbon dioxide dry chemical alcohol foam or mist Special Fire Fighting Procedures Use self contained breathing apparatus Fire and Explosion Hazards suse Not applicable MSDS 5 ANTEK 9000F MANUAL Material Safety Data Sheets Section V Reactivity Data Stability ii Stable Conditions to Avoid Heator flame Incompatibilities Strong oxidizers HNOs chromic acid sodium peroxide contact with strong caustics can cause spattering Hazardous Decomposition Products toxic gases such as carbon monoxide may be released during a fire Hazardous Polymerization ios eor dts will not occur Section VI Health Hazard Data Routes of Entry AO a No SI PERE OR CORRO No TAGES OA ai YES Health Hazards AUS M EET Ingestion may cause nausea breathing difficul ties and damage to stomach and digestive tract Low hazard for skin and inhalation CHIODI AWEKA MANA can cause anemia nephritis and methemoglobinernia Carcinogenicity Notfound Signs and symptoms of exposure Irritation in respiratory tract upset stomach or nausea irritation of eyes nose throat Medical conditions generally a
55. plicable Auto Ignition Temperature Not applicable Flammable Limits Not applicable Extinguishing Media Any Special Fire Fighting Procedures Not applicable Fire and Explosion Hazards Not applicable MSDS 9 ANTEK 9000F MANUAL Material Safety Data Sheets Section V Reactivity Data Stability isesi Stable Conditions to Avoid Storing near heat or incompatible chemicals Incompatibilities None Hazardous Decomposition Products None Hazardous Polymerization will not occur Section VI Health Hazard Data Routes of Entry Is ia No A No Ingestion Yes Health Hazards None Carcinogenicity Not found on these lists Signs and symptoms of exposure No serious acute or chronic affects with either external or inhalation exposure Medical conditions generally aggravated by exposure None Emergency and first aid procedures skin did Eyes rin washoff with large amounts of waterfor 15 minutes o A induce vomiting consult physician Section VII Precautions Steps to be taken if material is released or spilled Wash down drain with excess water Waste Disposal Method Vacuum and or wash down drain with excess water Observe all federal state and local laws Precautions to be taken in handling and storing Store at room temperature and keep
56. pply if there are no other instruments using the same gas supply 1 Turn all flow meter control needle valves clockwise to zero CAUTION Donotforce valve closure as damage to flow meter can occur Turn clockwise only until slight resistance is felt 2 Apply pressure 40 psi toinstrumentby turning the gas on atthe oxygen cylinder regulator Pressure will be seen on the regulator 3 Turnoffthe cylinder valve and ensure that the pressure does not drop 4 Ifthe pressure does not drop there are no leaks between the regulator and the instrument If pressure does drop check all fittings between the gas supply outlet and the flow meters Repeat procedure for Argon or Helium Once the pressure test has been completed successfully an instrument leak check must be performed 1 Reduce the oxygen supply to lt 5 psi either at the cylinder regulator or with an in line regulator 2 Ensure that there is a septum in the injection port of the pyrotube or the Model 740 MultiMatrix 3 Open the Pyro O flow meter to half of full scale 4 Plug both the gas vent and the liquid vent on the back of the instrument 5 Ifthere are no leaks the ball in the flow meter will fall to zero Ifit does not drop check all fittings to ensure that they are tight and secure Fittings to check include Pyrotube ball joint O ring and receiving vessel clamp a b Pyrotube T Reducing union for Reagent B inlet tubing d Reducing union for Carrier gas i
57. re levelis 2 75 bar 40 psig When using certain accessories the argon fine pressure may need to be increased to 4 0 bar 60 psig CAUTION Unless specifically stated the supply pressure of gases used with the Antek 9000F should not exceed 4 0 bar 60 psig 3 Theflow rate may be estimated by observing the flow meter ball and comparing the reading to Figure 7 1 37 ANTEK 9000F USER S MANUAL 4 Carefully turn ON counterclockwise the Inlet Argon control valve Adjust the argon flow to the desired rate as indicated by flow meter ball Optimum argon flow rates for specific application s will be determined by experience Figure 7 1 Inlet Argon or Inlet Oxygen Flowmeter Curve E gt Inlet Argon or Oxygen Tube A 125 7 with Glass Ball 2 E 4 s 6 BALL SETTING Note This chart demonstrates approximate flows and should be used only as a guideline 7 1 3 Inlet Oxygen Oxygen is often mixed with the argon carrier to improve the volatilization and provide a smooth ignition for the sample In certain applications and with certain types of samples oxygen may be completely substituted for the inlet argon carrier i e aqueous samples soil samples etc Normally 50 to 75 mL min inlet oxygen flow is required WARNING Extreme care should be taken when using inlet oxygen in the analysis of volatile flammable samples such as benzene crude oil toluene LGD naphtha etc This may present an explosion hazard 1 Turn OFF
58. rier gas Plumbing Requirements Dual Stage Regulators provide stable pressures that do not vary from day to day and help provide consistent and reproducible results Telecommunication Requirements e Telephone jack suitable for use in FAX modem service e PCAnywhere32 software ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK SECTION 2 INSTALLATION 2 1 Instrument Location Position the Antek 9000F Fluoride Analyzer computer and accessories on a level surface as shown in the following figures Alternate arrangements are possible Consult this Operators Manual or your local Antek Representative Waste fluids can be collected in one single container or plumbed directly to a drain Figure 2 1 Model 9000F with Model 735 Figure 2 2 Model 9000F with Model 740 Figure 2 3 Model 9000F with Model 734 ANTEK 9000F
59. rotube and or lines to receiving vessel owitch off for Reagent B pump Reagent B is the fluoride carrier Leaks in the system Electrodes aged or damaged Are there any blockages in the system 51 SECTION 9 TROUBLESHOOTING Solution Clean or change out pyrotube Be sure to use UHP gases and Type H20 Check reference electrode and fill with KCI solution if necessary Perform a leak check Check and be sure that the 9000F is grounded to the PC chassis After you turn everything on let the system equilibrate for approximately 45 minutes Check and be sure that everything is set properly Check for any blockages in the lines and fittings Replace the pyrotube and lines if necessary Perform a leak check If anything has changed recently check and see if that is the source of the problem Test the electrodes See separate section on the Maintenance and Testing of the Electrodes Clean and or change out the pyrotube and recalibrate Turn on switch on Reagent B pump Let the system equilibrate Perform a leak check Visually inspect the electrodes Test the electrodes Check lines and fittings Ensure that the TISAB sample solution flow is clear and free from any blockages ANTEK 9000F USER S MANUAL Problem Wildly erratic readings spikes Steady continuous drift in one direction Electrode slope less than 3 mv Decade Pumps too slow Over range reading Possible Cause s A
60. rt 3 Immunity to Radiated Radio Frequency Electromagnetic Fields IEC 801 4 IEC 1000 4 4 Electromagnetic Compatibility for Industrial Process Measurement and Control Eguipment Part 4 Electrical Fast Transient Burst Reguirements IEC 801 6 IEC 1000 4 6 Electromagnetic Compatibility for Electrical and Electronic Equipment Part 6 Immunity to conducted disturbances induced by radio frequency fields EN 50082 2 Electromagnetic Compatibility Generic Immunity Standard Part 2 Industrial Environment This certifies that the aforementioned equipment conforms with the protection requirements of Council Directive 89 336 EEC on the approximation of the laws of the Member States relating to Electromag netic Compatibility Signature of the Manufacturer Y Jay Szinyei VP of Research amp Development ANTEK 9000F USER SMANUAL THIS PAGE INTENTIONALLY BLANK CONTENTS MATERIAL SAFETY DATA SHEET ELECTRODE FILE SOLUTION cuenta ae MSDS 1 Section Product Identification isso ra cn MSDS 1 Section Il Hazardous Ingredients Identity Information ee MSDS 1 alo a T MSDS 1 Section IV Fire and Explosion Hazard Data arena Oer MSDS 2 Seele RECH 1 aas a a a MSDS 2 Section 4 Am 532100 Hazard Dala pu roads MSDS 2 SECCION VU Precautions RT MSDS 3 section Wl CONTO Measures i mei isana kaani aaa i esses aa MSDS 3 MATERIAL SAFETY DATA SHEETSHEET RECEIVING sees MSD
61. s e Argon or Helium supply dry regulated to 40 psig e Oxygen supply dry regulated to 40 psig e Flow meter to measure up to 750 cc min e One narrow mouth plastic liquid waste storage container ANTEK 9000F USER S MANUAL CAUTION Become familiar with all modules and accessories and carefully read all instructions before attempting to operate the system 1 2 Reguirements 1 2 1 Environmental Reguirements 1 Ambient Temperature Operational stability requires a reasonably constant room tem perature 2 Corrosive or Dusty Atmosphere A corrosive atmosphere will in time cause problems with solderjoints electrical contacts Dust and dirt that may be sweptin by cooling fans may collect and retain moisture thus causing corrosion and short circuits Dust may also collect on heat transfer surfaces causing reduced radiation and resulting in component damage 3 Space Requirements Approximately 72 inches 183 cm x 30 inches 76 cm of bench space is required for the Fluoride System The bench should be capable of supporting atleast 350 pounds 159 kg Adequate air space should be provided on both sides top and behind the instrument 4 Ventilation Flammables Reasonable ventilation associated with a typical modern laboratory environment is normally acceptable WARNING Furnace operates at a temperature in excess of 1000 C and can serve as an ignition source 5 Fluid Drain Plumbing the waste line directly to a drain is
62. ses incurred by ANTEK to conduct the inspection and review Further this warranty does not cover and ANTEK shall not be liable for either direct or consequential damage caused either directly or indirectly as a result of any act of God including but not limited to natural disaster such as floods earthquakes or tornadoes damages resulting from or under the conditions of strikes or riots war damages or improper operation due to intermittent power line voltage frequency electrical spikes or surges unusual shock or electrical damage accident fire or water damage neglect corrosive atmosphere or causes other than ordinary use Additionally ANTEK shall not be responsible for any loss of use to Buyer or for any damage which may be caused by or attributable to the ANTEK products Buyer agrees these limitations of ANTEK s liability are reasonable Buyer further agrees that these limitations of ANTEK s liability is part of the consideration for this agreement and is reflected in the amounts charged by ANTEK for its products The obligations of ANTEK under this warranty are limited to the repair or replacement at ANTEK s option of any part component or instrument which in the sole opinion of ANTEK is defective and which has been returned at the buyer s expense to the factory or service center as may be designated by ANTEK during the one 1 year warranty period This warranty does not cover certain expendable items such as but not limit
63. sista None AC A None DD p 629 mg Kg OrlDog Section lil Physical Data BO Pollina 100 C Freezing POLGU ia 4 C SPELL Gravity ascnass tessesprseuseses 1 06 MADOLPEESSUTE erica Notapplicable DIA it 5 5 7 5 Solubility in Water Miscible Volatiles by Wt assonanza Not applicable Evaporation Rate psn Not applicable Vapor Density wi Not applicable Appearance waa Odorless Liquid MSDS 1 ANTEK 9000F MANUAL Material Safety Data Sheets Section IV Fire and Explosion Hazard Data Flash P IE nica Notapplicable Adttoleniton Lompetabiites centra Not applicable Flammable LIMItS sordas Not applicable Extinguishing Media Any Special Eire Fighting Procedures irrita Notapplicable Fire and Explosion Hazards Not applicable Section V Reactivity Data Stability Stable Conditions AVI anat Storing near heat or incompatible chemicals Iucompatibilities ai BrF3 anything incompatible with water Hazardous Decomposition Products None Hazardous Polymerization will not occur Section VI Health Hazard Data Routes of Entry Japala Hon aaa No A No A AA Yes Health Hazards A SA KUOA ANA Large amounts taken internally may be fatal or cause dizziness cramps convulsions vomiting weakness and collapse CO ciao can cause anemia nephritis and methemoglo binemia Carcinogeni
64. such as LPG materials a method with the following characteristics should be utilized Furnace Temperature Reagent B Injection Rate Sample Injection Rate Sample Size Sample Injection point 9000 Gas Flow Settings Injection valve position timing 7 7 Solids Analysis 900 1100 C sample dependent 1 0 1 5 pl minute concentration dependent 25 mL minute Model 734 carrier gas setting Liquid LPG 15 pL 10 mL See Model 734 Operator s Manual Pyro O9 sicuri 4 5 alet Op arena 0 0 MERA conside 5 0 Remain in inject position for atleast 3 minutes In order to analyze solid or viscous materials a method with the following characteristics should be utilized Furnace Temperature Reagent B Injection Rate Sample Weights Sample Introduction 9000 Gas Flow Settings 900 1100 C sample dependent 1 0 1 5 pl minute concentration dependent Sample dependent Use a series of holds if necessary to control combustion Pyro Og sila 4 5 Inlet Og in 2 5 A A 3 5 44 ANTEK 9000F USER S MANUAL SECTION 8 SOFTWARE When the Antek 9000F program is started from Windows the first screen to appear is Figure 8 1 Verify that the furnace temperature is sufficient to continue If itis sufficient click on Cancel Figure 8 1 Instrument Hardware Status Instrument Hardware Status Fumace Temp KIE c Cooler Temp REGA c Autosamplers Present l Syringe Drive 8 1 Mai
65. terior of the new pyrotube with fluoride free high purity 1sopropyl alcoholto remove any materials which may damage the tube when heated 6 Dry the tube completely taking care notto touch the pyrotube as fingerprints can leave oils that will damage the tube when heated 7 Inserta new septum into the pyrotube with the Teflon side in 8 Remove o ring if present from the new pyrotube and carefully insert the pyrotube into the right side of the furnace as shown in Figure 2 7 9 Install the ceramic endplates as illustrated in Figure 2 7 and secure with the spring clamps on both ends of the furnace 10 Adjustthe orientation ofthe pyrotube as illustrated in Figure 2 7 or 2 8 WARNING The proper attachment of the gas inlet tubes side arms is critical If not hooked up properly an explosion hazard may exist 11 Locate and attach the inlet gas line from outside the rear panel and the pyro oxygen line from the flow meter assembly inside the front panel to the proper pyrotube side arms with 4 nuts and Teflon ferrules 12 Locate and attach the Reagent B feedline to its inlet as shown in Figure 2 7 or 2 8 CAUTION Care should be taken when assembling the metal Teflon quartz connections The quartz tube is fragile and may be broken easily See Figure 2 5 13 Replace the o ring seal and install the receiving vessel on the left exit side of the pyrotube and secure with the joint clamp 14 Ensure that all gas connections
66. utton is chosen from the Run popup menu Replace Injection will overwrite existing highlighted data with the new injection Insert After gt gt and lt lt Insert Before inserts the new injection in the same concentration level as the highlighted injection New Sample adds the next injection as a new standard concentration Figure 8 12 New Sample Please enter the new standard s information Name Cal Std 5 Oper ID Multiplication ay 100 Sample pM Dilution Factor 2 Weight Volume E 3 Concentration El 0 00 ppm Injections Vial El 1 Position El 1 49 ANTEK 9000F USER S MANUAL THIS PAGE INTENTIONALLY BLANK 50 ANTEK 9000F USER S MANUAL Problem Noisy baseline Saw toothed pattern baseline Wavy pattern baseline Baseline changing more than 1 2 mV min Baseline not the same in mV as the day before greater than 10 mV change Low Sensitivity Possible Cause s Contaminated pyrotube Contaminated H20 and or gases Air bubble inside the reference electrode Leak in the system 9000F not grounded to PC chassis Electrodes not properly equilibrated Is Reagent B pump turned on Are all the flows set to the correct settings gases Reagent B and Reagent A Are there any blockages in the system Any visible evidence of sooting or contamination of the lines or pyrotube Possible contamination from gases TISAB or Reagent B Electrode damaged or aged Carbon in py
67. vide the thermal energy to completely oxidize any material to be analyzed by the Antek 9000F The pyro furnace is intended to operate at extremely high isothermal temperatures The temperature set points are entered via the Furnace Controller as described in Section 5 ofthis manual All temperatures are in degrees centigrade C Most analyses may be successfully accomplished ata pyrofurnace temperature of 1050 C however temperatures up to 1000 C are common for aqueous or inert materials Some special applications may be conducted atlower furnace temperatures Asa general rule the furnace temperature need not be changed on a regular basis 7 4 Sample Handling 4 Preparation The concentration of fluorine in the sample and the chemical and physical composition ofthe sample matrix itself will greatly determine the amount of care necessary in handling and preparing samples prior to analysis with the Antek 9000F Improper sample handling and preparation may yield results which are nonrepeatable and inaccurate For example touching injection needles or sample boats may introduce fluorine compounds into the system and produce erroneous results 7 4 1 Liquid Sample Materials Liquid sample materials are among the easiestto contaminate or alter for a variety ofreasons Most potential contaminates are soluble in some liquids and the liquid sample may be placed in almost any container Some liquid matrices are volatile and some are extremely hygroscopi

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