Aquamax KF Coulometric v1.12
Contents
1. Water temperature of wet gas flow meter C 6 2 Water Standard Test In principle standardization of a Coulometric Karl Fischer is not necessary since the water titrated is a direct function of the coulombs of electricity consumed However it is recognised that reagent performance can deteriorate with use over time and it is recommended that the titrator is regularly monitored by introducing a known quantity of water that is representative of the typical range of water concentrations being determined in samples Several of the ASTM methods for water content of crude oil and petroleum products suggest injecting between 1 0 ul and 10 ul distilled water to check reagent performance Each of these methods requires that the result be recorded in micrograms of water not as a calculated ppm or percentage The ug check button on every Aquamax KF Coulometric Titrator enables this check to be done without the need to reprogram the calculation mode Simply press ug check and the display will prompt add standard Introduce 10ul of distilled water as required by ASTM methods by syringe and the display and print out will be in micrograms water This only applies to a single analysis as the titrator will then revert back to the programmed calculation mode for subsequent runs 6 3 How to Run a Test Note Read Chapter 5 4 Programming a Method then use Chapter 5 5 Programming Flow Chart before running any samples Example Transformer oil sample by2. have not been reached then it is possible to switch off the titrator and allow the oil to separate from the reagent The oil can then be siphoned off and the instrument switched on again After this operation it may take up to 30 minutes before the instrument settles down to a stable baseline If it takes longer than 30 minutes then it is advisable to clean the cell and recharge with fresh reagents Turbine Lubricating Oils For most Lube Oil applications a sample size of 1ml is sufficient However if itis suspected that the water content is above 1 96 then a sample size of 0 2 to 0 5 ml is suggested Some lubricating oils contain additives which can react with the KF reagents interfering with the chemical reaction For these applications we suggest using the Aquamax KF PLUS in conjunction with an oil evaporator such as the Aquamax KF model 510000 as per ASTM D6304 Ketones and Amines These can react with the Methanol present in most Coulometric reagents resulting in inaccurate results and in extreme conditions titration end point being unattainable For samples containing Ketones amines or Aldehydes the use of specially formulated Coulometric reagents for Ketone samples is recommended Powder Samples One of the main advantages of the Coulometric technique is that reagents do not have to be replenished after every analysis therefore the introduction into the titration cell of solid samples which do not dissolve is not recommended Three
3. please visit our website www grscientific com SCHEMATIC OF TYPICAL TITRATION ELECTROLYSIS CURRENT DETECTOR SIGNAL 1 3 Instrument Connections Various ports are located on the back plate of the instrument Below is a list of ports that can be found 1 Power Supply Port The power supply port is for connecting to a 18V mains power supply using the supplied power adaptor 2 RS232 Port For updating titrator software connecting to other equipment for remote controlling software specific protocols to be provided 3 USB A Port For exporting results data to a Removable Flash Drive memory stick when running sample tests in the field or remote locations and subsequent transfer to PC at a later date for loading onto Results Manager files 4 USB B Port For connecting directly to PC to export data to Results Manager and enable results to be saved on files for future reference See Results Manager User Manual section Chapter 2 Safety Information 2 1 General Safety Points CE ROHS COMPLIANT GR Scientific products are in conformity with the EU Directives 2004 108 EC and 2006 95 EC This is based upon the compliance of the products with the harmonised standards BS EN 61000 4 2 2009 BS EN 61010 2 030 2010 and BS EN 61326 1 2013 GR Scientific products are manufactured in accordance to ROHS following the EU Directive 2011 65 EU it does not contain any of the restricted substances in concentrations and applica
4. 1ug 200mg Water Typical 1ug 10mg Water 1ppm 100 Water 0 1ug 2 24mg per minute 400ma Automatically Controlled 10 100ug 3ug 100ug 1mg 3ug above 1mg 0 3 0 30 minutes user selectable 0 30 minutes user selectable Weight weight W w Weight Dilution Ratio W K Volume Density V SG Volume volume V v User Programmable ug mg kg ppm ug mg kg ppm Max Mean Min values up to 99 runs 10 User Programmable Methods User Programmable Microprocessor Controlled User Selectable Multi Languages User Selectable Analysis Time amp Date Print Out USB amp RS232 Ports Flash Drive memory stick 18 Key Touchpad 40 Character Alphanumeric Backlit LCD 42 Character High Speed Thermal Printer 90 264V AC 47 63Hz 290 x 255 x 130 mm 3kg 10 2 PORTABLE Model Titration Method Electrolysis Control End Point Detection End Point Indication Titration Vessel Measuring Range Moisture Range Max Sensitivity Max Titration Speed Max Current Drift Compensation Precision Start Delay Time End Delay Time Calculation Modes Display Format Print Format Statistics Method Storage Sample ID Number Stirrer Speed Languages Calendar Clock Battery Low Indicator Data Outputs Removable Data Storage Data Entry Display Printer Protective Sleeve Carrying Handle Power Supply Unit Dimensions Weight Coulometric Karl Fischer Titration Patente
5. Power Adaptor 503052 Glassware Set LDC Twin Port Comprises of 503053 Titration Vessel LDC 503054 Detector Electrode LDC 503055 503056 Generator Electrode frit LDC 503057 Electrode Lead x2 503058 Desiccant Tube LDC amp Cap 503059 Pack Injection Septa 10 pack 503070 Molecular Sieve 503071 Stirrer Bar 503072 Polypropylene Funnel 503160 Paper Roll Thermal Single x3 503164 Luer Needle 19 Gauge Screw Fit 503063 Gas Tight 1 0ml Syringe All the following parts are not included as standard with the PLUS model but can be purchased as optional extras 201004 Carry Case 503062 Gas Tight 0 25ml Syringe 11 2 PORTABLE Model Part No 101016 All the following parts are included as standard with the PORTABLE model but can be purchased as single tems 101005 Results Manager Software Package Comprises of 102026 Results Manager Software CD 101009 Interface Cable 101010 512MB USB Flash Drive Memory Stick 201004 Carry Case 301203 Vessel Sleeve 401424 In Car Adaptor 401511 Power Adaptor 503046 Glassware Set Single Port Comprises of 503047 Titration Vessel 5030468 Detector Electrode 503049 503050 Generator Electrode frit 503051 PTFE Sleeves 10 pack 503057 Electrode Lead x2 503058 Desiccant Tube LDC amp Cap 503059 Pack Injection Septa 10 pack 503070 Molecular Sieve 503071 Stirrer Bar 503072 Polypropylene Funnel 503160 Paper Ro
6. V SG Program the Aquamax KF titrator with parameters for the analysis For Transformer Oil samples these parameters are usually Result Format mg kg or ppm Calculation Mode V SG Sample Volume 1 0 ml Sample SG 0 875 Other parameters such as Sample ID number Printer Mode etc are optional Analysis Method 1 Confirm that Aguamax KF titrator is in Ready mode 2 Flush 1 0ml syringe several times minimum 6 times with sample 2 3 Fit luer needle and flush through with sample 4 Draw sample into syringe beyond the 1 0ml marking 5 Invert syringe so that any air bubbles can be ejected through the needle and adjust syringe plunger to the 1 0 ml mark 6 Wipe off excess sample from outside of needle using a clean dry tissue or paper towel Pierce needle through injection septa of titration vessel 1 2 cm Press START Push needle into anode reagent and inject sample 0 Withdraw needle from titration vessel 1 Read result in mg kg ppm water on display and printout 2 Repeat steps 2 11 if duplicate result required Example Powder sample by W w Program the Aquamax KF titrator with parameters for the analysis 1 Analysis Method 1 Confirm that the Aquamax KF titrator is in Ready mode 2 Place a suitable amount of sample in the powder sampler and seal with stopper provided 3 Weigh sampler 4 Press PROGRAM until Calculation Mode is displayed then select W w 5 Enter t
7. fully functional and to ensure that it meets all of the requirements that the instrument supports 13 3 Customer Support and Service We want you to maximise the return on your equipment through a service program tailored to your requirements from when you purchase our equipment which includes e Support and Repair Maintenance and Calibration raining and Installation Quality Assurance and Certification Our dedicated service staff are on hand to help in the unlikely event that your equipment develops a fault Please contact us using the details provided to discuss the next step 13 4 Warranty Under the conditions of our warranty all faults which are proved to be due to material construction or manufacturing defects which occur within 24 months of the delivery date will be repaired or replaced at our discretion free of charge at our premises Freight costs will be chargeable along with any inspection work which was not necessitated by manufacturing or material defects Breakages of glassware or electrodes are not covered by this guarantee In the event of instrument failure during the warranty period written authorisation must be obtained from the manufacturer prior to shipping 41 GR Scientific Building 69 Wrest Park Silsoe Bedfordshire UK MK45 4HS tel 44 0 1525 404747 fax 44 0 1525 404848 info grscientific com www grscientific com GRS cientific
8. options available Powder samples which readily dissolve in the Anode reagent can be introduced using the optional powder sampler part no 503069 Calculation mode W w Powder samples which cannot be dissolved in the Anode reagent should be extracted or dissolved in a suitable solvent and then an aliquot injected Calculation mode W K f neither of above methods are suitable you may need to use a solids evaporator system in conjunction with the Aquamax KF PLUS titrator Gas Samples Gas samples can be introduced by fitting a needle onto the gas sampling cylinder and selecting Calculation mode W w Alternatively gas samples can be bubbled through the titration vessel and the passed volume measured For this method we suggest using the gas analysis kit 5030 4 and a wet gas flow meter connected to the outlet of the titration vessel 1 Fit the gas inlet and outlet adapters in place of the injection septa 2 Remove the drying tube and seal the top of electrode using the injection port septa and screw cap 3 Connect outlet adapter to wet gas flow meter 4 Flush the sample lines and allow instrument to stabilise 5 Press START and allow gas sample to flow through the cell at an approximate flow rate of 0 5 litres minute 6 Turn off gas flow and allow titration to reach end point 23 24 Calculation EXI EDO W Vx27 3x18 Where W Moisture content G Microgram count V Gas volume litres t
9. should always be taken when handling them and when cleaning the glassware Whenever possible this should be done in a safe area e g inside a fume Cupboard Reagents should not be recharged while the titration cell is still attached to the titrator Under normal circumstances the titration cell can be used for a large number of samples before having to replenish the reagents The glassware only requires simple cleaning procedure normally just rinsing with solvent drying and then re charging with fresh reagent Once the reagents have been exhausted or when the titration cell maximum volume has been reached it should simply be necessary to 1 DISASSEMBLE titration cell disconnect leads from titrator 2 EMPTY the titration cell and generator electrode 3 RINSE all parts with methanol Do not use brush on electrodes 4 DRY all parts 5 REASSEMBLE glassware 6 RECHARGE with fresh reagents If the cell is heavily contaminated then it may be necessary to clean it more thoroughly For oil samples cleaning with chloroform or xylene is suggested whilst for salt deposits a water wash may be required Use whichever solvent is most suited for the sample type The titration vessel can even be cleaned with hot soapy water and a bottle brush However after cleaning with suitable solvent all glassware parts MUST be rinsed inside and out with methanol They can then be dried with a warm air blower such as a domestic hair dryer place
10. titrator and connect the electrode leads onto the appropriate sockets There are some bi products formed in the cathode chamber which can react with the iodine in the anode chamber and this can cause longer preconditioning times It is advisable to have the cathode reagent 2 3mm lower than the anode reagent when first charging the titration vessel to speed up preconditioning The Aquamax KF titrator is now ready to be switched on 11 12 4 4 Loading the Printer 1 To load the paper into the printer first open the paper roll holder lid above the print head and remove the old roll 2 Insert the paper roll into the compartment Note To avoid damage to the printer mechanism it is advisable to only use the correct thermal paper rolls see Chapter 10 Parts and Accessories 3 Gently pull the paper roll so it hangs over the printer edge 4 Close the printer lid and remove the excess paper 4 5 Connecting a USB Device To use the memory store insert Flash Drive into USB port A titrator will see it and a symbol will appear on the display The symbol will appear blacked out while the drive is being written to and then clear when idle The drive should only be removed when in the idle mode To read data saved on drive insert it into PC USB port Start Results Manager load selected file and then save in the format you require Note See Chapter 8 for full instructions on Results Manager Chapter 5 Basics of O
11. to print out the titration parameters being used at that time Simply scroll through the options using until the required mode is displayed then press ENTER Options available Off No result print out Every Result Will print result after every titration first result also prints all calculation input data Full Report Will print results after every titration and then print out statistical data after a selected number of titrations Statistics Print The Aquamax KF titrator can be programmed to print out the statistical data from a series of results when using Full Report print mode If no number has been selected the Aquamax will automatically clear after 99 runs If 3 or more runs have been selected the Aquamax will print out the minimum maximum and mean values Print Drift The Aquamax KF titrator can be programmed to print out the drift value for each titration This is a useful indicator of titration cell stability If drift is above 25 ug minute print will show XX This is a warning that a high drift value was present at start of the titration Delay Times The Aquamax KF titrator has been programmed to accept two different types of delay times one at the start of titration and one at the end as a minimum titration time Start Delay Time The Aquamax KF titrator has a preset delay of five seconds which allows samples to be dispersed into the reagents before the titration starts Some samples particularly powders
12. 1 2 Checks Once you have received the instrument immediately check to make sure that there is no damage and no parts are missing A delivery note will be included within the package to use to compare with the shipment Ensure that inside the shipment has a calibration certificate for the instrument if not please request this from the manufacturer 4 1 3 Location Locate the instrument within the work area where it is free from excessive vibrations direct sunlight contamination from chemicals explosive environments corrosive atmospheres major temperature fluctuations 4 2 Connecting the Power Supply The Aquamax KF Coulometric is powered by an external mains source with a power pack to ensure this connection is the correct voltage of 18V DC for the instrument Damage may occur beyond repair and the user may be subjected to electric static shocks if the incorrect power is supplied Note Refer to Chapter 2 for more safety information To avoid risk of electrocution make sure the I O switch is set to OFF before connecting the power supply 4 3 Setting Up the Glassware 4 3 1 Glassware Assembly Generabor N Drying Tube Electrode Cap assembly D Ring TEN d Screw Cap Generator Electrode Injection Port Cap Septa O Detector Electrode Titration Vessel Stimer Bar 4 3 2 Connecting to the Aquamax KF Coulometric Note This is sho
13. Aquamax KF Coulometric User Manual Edition 1 1 July 2015 Contents Chapter 1 Chapter 2 Chapter 3 Chapter 4 Chapter 5 Chapter 6 MONOT O MENS RS 3 1 1 Instrument Description 9 1 2 Principle of Measurement lic a 3 1 3 Instrument Connections russia rige 4 3231617 VIO II 01 ii 5 2 1 General Safety Points essere 5 2 2 Electrical SOTO ro 5 2 3 Solvent and Chemical Safety sss 5 2 4 Recycling and Disposal saan 5 Instrument DVBIVIBM csi 6 3 1 PLUS MdG sarisin aier sense Sa 6 SS FONT A ire E e 6 3 2 2 Rear Panel e 6 S PORTABLE Modol srta 7 3 2 1 Front Panel ouo Eom a T S27 Rear PINE orde eia S EEEE T DO VOCE EN E E IA A E AA OO 8 Merom SEID rar 9 4 1 Receiving an Aquamax KF Coulometric sss 9 4 1 1 Packaging MEN m m T 9 9 A120 eR S Sei y A e o o DE OE DOTT 9 4 2 Connecting the Power Supply esee 9 4 3 Setting Up the Glassware 10 4 3 1 Glassware Assembly sese 10 4 3 2 Connecting to the Aquamax KF Coulometric 10 4 3 3 Filling and Changing Reagent sss 11 4 4 Loading the Printer eese eene 12 4 5 Connecting a USB Device esset 12 Basilios of OPES ON PR 13 5 1 Swit hing ON and OFF pende 15 5 2 Set
14. Windows directory and file dialog box to allow you to choose the location and filename for the saved data Files are stored in XML format eXtensible Markup Language which is a standard format widely used to store information in a flexible manner and provide interchange between applications The extension xml is used to identify XML files and will be added automatically to the file name Load The Load button allows you to load a set of results previously saved to disk using the Save button or transferred from a titrator through some other means Again it opens the standard windows directory and file dialog box to allow you to find the directory and file you require and is configured to display files with the xml extension Loading a set of results from file will replace the ones currently held in Results Manager so if these have not yet been saved you will be asked whether you wish to do so before loading them Export Although many applications can read the XML results files some cannot The Export button provides the ability to save the results currently loaded as a text file that can be read by applications such as Microsoft Excel Again the standard directory and file dialog allows you to choose the location and name for the file the results will be stored in CSV format Comma Separated Values with the csv extension Print The Print button allows the current set of results to be printed on any printer connected and supported by Wind
15. and viscous samples may need additional time to fully dissolve By selecting the start delay program you can increase this time by up to 30 minutes Aquamax KF Coulometric Display shows Select required time delay and press ENTER Whilst a delay time is in operation the display will show add sample and the clock counter will show the time remaining before the start of titration A start delay can be overridden by simply pressing START Minimum Titration Times For some applications such as certain gas samples or when using the Aquamax KF titrator combined with an oil evaporator or solids evaporator system it can prove useful to delay the end point of the titration By selecting this parameter you can increase the minimum titration time by up to 30 minutes Aquamax KF Coulometric Display shows Select required minimum time and press ENTER 19 20 End Sensitivity The sensitivity of detector signal as the end point is approached can be set from O 9 seconds The default value is 3 seconds and there are very few occasions when this may need to be altered Decreasing this value can prove useful if samples cause interference e g some Lube Oil samples Beep Mode Four options are available for the audible alarm beeper and they can be scrolled through using until the required one is displayed Then press ENTER The options are Off Beeper inactive Key Press Beep once every time a key is pre
16. d ACE Control System GB2370641 AC Polarisation Visual Display Print Out Acoustic Beep Low Drift Cell Design no grease or PTFE sleeves required Possible 1ug 200mg Water Typical 1ug 10mg Water 1ppm 100 Water 0 1ug 2 24mg per minute 400ma Automatically Controlled 10 100ug 3ug 100ug 1mg 3ug above 1mg 0 3 0 30 minutes user selectable 0 30 minutes user selectable Weight weight W w Weight Dilution Ratio W K Volume Density V SG Volume volume V v User Programmable ug mg kg ppm ug mg kg ppm Max Mean Min values up to 99 runs 10 User Programmable Methods User Programmable Microprocessor Controlled User Selectable Multi Languages User Selectable Analysis Time amp Date Print Out Display amp Print Out Indication USB amp RS232 Ports Flash Drive memory stick 18 Key Touchpad 40 Character Alphanumeric Backlit LCD 42 Character High Speed Thermal Printer Included Included 90 264V AC 47 63Hz 12V DC Car Adaptor Internal Battery 290 x 255 x 130mm Not including carrying handle or protection cage 5kg 3f 38 Chapter 11 Parts List 11 1 PLUS Model Part No 101001 All the following parts are included as standard with the PLUS model but can be purchased as single items 101005 Results Manager Software Package Comprises of 102026 Results Manager Software CD 101009 Interface Cable 101010 512MB USB Flash Drive Memory Stick 401511
17. d in a low temperature oven at 40 50 C or left in a desiccator After being fully dried reassemble the titration cell and charge with fresh reagents THE MORE THOROUGHLY THAT THE TITRATION CELL IS CLEANED AND DRIED THE FASTER THE INSTRUMENT WILL STABILISE READY FOR OPERATION AFTER RECHARGING REAGENTS Under normal conditions the Aquamax KF titrator should be ready for operation within 5 10 minutes after reassembly however it could take considerably longer before to completely stabilise if the drying procedure has not been properly carried out Generator Electrode Acid Wash Procedure If the frit of the generator electrode has become blocked or severely stained with samples such as crude oils then it may occasionally be necessary to use an acid wash procedure 2 Place the electrode in a 250ml conical flask ensure the electrode is suspended and not resting on the Rinse the empty generator electrode with Xylene or other suitable solvent platinum mesh Add 10ml Xylene to the inner cathode chamber and leave to stand for 10 minutes Remove the Xylene 3 Repeat using 10ml of Methanol then gently swirl to remove residual solvent and remove 4 Add 10ml deionised water to inner cathode chamber and allow to stand for 30 minutes 5 Remove any remaining water add 10ml 50 50 HCL and allow to stand for 1 hour Top up any loss of HCL through the frit After 1 hour carefully pour the acid into a flowing water st
18. do not want to recall a method press PROGRAM to view the next prompt 5 6 Program Flow Chart 22 Chapter 6 Running a Test 6 1 Example Applications Liquid Samples Liquid samples are usually introduced into the titration vessel by using a syringe The greater the amount of water introduced into the titration cell will cause the titration to take longer and also consume the reagents more quickly It is recommended that the smallest representative amount of sample be used to ensure fastest titration soeed and maximum sample throughput before reagents have to be replenished Optional gas tight syringes and luer needles are available from GR Scientific With volumes of 0 25 1 0 and 5 0ml these are suitable for injection of oil samples and water standards Other volume syringes are commercially available from various suppliers Please ensure that the needle is long enough to reach into the anode reagent This guide may be of assistance when selecting injection volume of samples Expected Water Content Suggested Sample Size From To From To 1 ppm 10 ppm 1 0 ml 2 0 ml 10 ppm 100 ppm 1 0 ml 2 0 ml 100 ppm 500 ppm 0 5 ml 1 0 ml 500 ppm 1000 ppm 0 5 ml 1 0 ml 0 001 0 01 1 0 ml 2 0 ml 0 01 DIES 1 0 ml 2 0 ml 0 1 0 5 0 5 ml 1 0 ml 0 10 0 fn 1 0 ml 1 0 96 5 0 78 0 2 ml 0 2 ml 50 More Than Less Than 0 1 ml Note These volumes are only a guide You may wish to experiment with sample size to determine the optim
19. ger so a failure to connect to the titrator is most likely to be caused by selecting the wrong serial port when clicking the Connect button Other possible causes of a connection failure are as follows Incorrect titrator software The serial port functionality is fully implemented in version 2 6a and above of titrator firmware and previous versions may not work reliably or establish a connection at all Contact GR Scientific or your local agent in order to obtain an upgrade to your titrator firmware Note The firmware version is displayed on the titrator immediately after the unit is switched on Chapter 13 Conformity and Warranty 13 1 Declaration of Conformity GR Scientific products are in conformity with the EU Directives e 2004 108 EC Electromagnetic Compatibility Directive e 2006 95 EC Low Voltage Directive This is based upon the compliance of the products with the harmonised standards BS EN 61000 4 2 2009 Electromagnetic Compatibility Generic immunity standard Residential commercial and light industry e BS EN 61010 2 030 2010 Safety requirements for electrical equipment for measurement control and laboratory use Particular requirements for testing and measuring circuits BS EN 61326 1 2013 Electrical equipment for measurement control and laboratory use EMC requirements General requirements 13 2 Quality Control The Aquamax KF Coulometric is adequately and professionally Quality Controlled to ensure that it is
20. ght Dilution ratio W K Note Use this method if you need to dissolve a sample in another solvent Suitable for samples which will not dissolve in the anode reagent or which might interfere with the KF reaction microgram count bl Result ppm or 96 WxK Where W Weight of sample dissolved gm de Total volume of diluent sample Volume injected into Aquamax KF bl micrograms of water for same injected volume of diluent pig e g Accurately weigh approximately 2 gm of sample into a 20ml stoppered graduated flask Make up to the volume line with suitable solvent diluent Using appropriate syringe inject 100ul of diluted sample into the titration cell Calculation parameters for this example would be W 2gm 20ml 100yul bl microgram count of 100pl injected volume diluent 3 Volume Specific Gravity V SG Note The most widely used technique for liquid samples However care must be taken to ensure removal of all air bubbles from the syringe microgram count Result ppm or 96 V x SG Where V volume of sample ml SG specific gravity 4 Volume V v microgram count Result volume E ee See V x 1 0 Where V volume of sample ml This is essentially the same as V SG mode except that the sample SG is fixed at 1 0 Printer Modes Selecting this program allows the printer to be turned ON or OFF lt also enables you
21. he sampler weight when prompted by display then press ENTER CLEAR 6 Remove the injection septa port press START and pour the sample inside the titration vessel ensuring that sample does not stick to the inside of the vessel wall Replace injection septa port 7 Reweigh the sampler 8 The net weight of sampler can be entered either during the titration by pressing PROGRAM or waiting until the end of titration when display will prompt TARE Weight Enter the weight then press CLEAR 2 Analysis Method 1 Confirm that Aguamax KF titrator is in the Ready mode 2 Place a suitable amount of sample in the powder sampler and seal with stopper provided 3 Place sampler on balance and tare to zero 4 Press PROGRAM until Calculation Mode displayed then select W w 5 Enter the sample weight as 0 0 grams then press ENTER CLEAR 6 Remove the injection septa port press START and pour the sample inside the titration vessel ensuring that the sample does not stick to the inside of the vessel wall Replace injection septa port 7 Reweigh the sampler 8 The weight difference of sampler can be entered either during the titration by pressing PROGRAM or waiting until the end of titration when display will prompt TARE Weight Enter the weight then press CLEAR 6 4 Drift Rate Compensation At the start of any titration the drift value in the top left corner of the screen in micrograms per minute is stored
22. ientific directly Chapter 3 Instrument Overview 3 1 PLUS Model 3 1 1 Front Panel 1 Printer 5 Detector BNC Connector 2 Display 6 Vessel Holder 3 Keypad 7 Vessel Retaining Thumb Screw 4 Generator BNC Connector 3 1 2 Rear Panel o 1 hl 2 emu 711623 3 4 5 6 1 18VDC Power Input 4 USB B Port 2 Fuse 5 I O Switch 3 RS232 Port 6 USB A Port 3 2 PORTABLE Model 3 2 2 Front Panel 1 2 3 E 08 8 BEEM i ec 90 ros s EL GRs 1 Carry Handle 5 Generator BNC Connector 2 Printer 6 Detector BNC Connector 3 Display 7 Vessel Holder 4 Keypad 8 Vessel Retaining Thumb Screw 3 2 2 Rear Panel 1 2 3 4 5 6 1 18VDC Power Input 4 USB B Port 2 Fuse 5 I O Switch 3 RS232 Port 6 USB A Port 3 3 Keypad Na Ww Mg Check 2 Alphanumeric 0 9 Decimal Point 1 2 3 Clear 4 5 Stirrer 6 Start 7 Programme 8 Enter 9 9 Stirrer Chapter 4 Instrument Set Up 4 1 Receiving an Aquamax KF Coulometric 4 1 1 Packaging The Aquamax KF Coulometric is packaged in suitable protective packaging to ensure that no damage occurs during transit only this packaging is suitable for the safe transportation during transit Please keep this packaging as transit of the instrument may need to occur in the future 4
23. in memory This ensures that the displayed result is corrected for any ingress of atmospheric moisture during the titration period Aquamax KF Coulometric Whilst in the Ready condition the Aquamax KF titrator continually compensates for any drift caused by atmospheric moisture ingress or reagent decomposition and displays this information which is updated every 10 seconds If the drift value is above 30 ug minute the display will show Drift Warning START to continue This is a warning that the value is high however the instrument can still be used by simply pressing START to continue Provided the drift rate is stable then it usually acceptable to continue operation The Aquamax titration cell design can provide drift values down to less than 5 ug minute but can also operate at much higher values The maximum drift value is 60 ug minute but we recommend operating up to a maximum of 25 whenever possible 20 26 If the drift value is above 60 ug per minute the display will read EXCESS DRIFT SEE INSTRUCTION MANUAL Most common causes of excess drift are Titration vessel not properly sealed check septa amp fittings Reagents almost depleted clean amp recharge the cell Sample introduced before pressing START key Trace moisture on cell walls If excess drift occurs switch the instrument off remove titration cell from clamp gently swirl the anode reagent around the cell walls replace cel
24. l in clamp switch instrument on and allow to precondition 6 5 Overtitration If the detector electrode senses too much lodine in the titration cell usually caused by instrument being left unoperated for a long period the display will read OVERTITRATION SEE INSTRUCTION MANUAL Aquamax KF Coulometric simply add 3 5 microlitres of water or a small amount of a known wet sample until the detector signal bars on bottom left of display are activated Then the instrument will automatically carry out its precondition Chapter 7 Results 7 1 Printout Explanation Aquamax KF Titrators allow you to select different print modes If you choose to have the printer on you will receive a hard copy of the result obtained together with the selected parameters for that particular titration every time a titration is performed Options Available Off No result print out Every Result Will print result after every titration first result also prints all calculation input data Full Report Will print results after every titration and then print out statistical data after a selected number of titrations The Aquamax KF titrator automatically increments the next run number every time you press the start button The run counter is reset to zero when power is switched off and back on again A duplicate set of results can be printed out simply by holding down the start button for 3 seconds Results memory is cleared after du
25. lation Mode W K Prm 1 Prm 2 amp Prm 3 columns show weight Blank value Dilution ratio Flags If a letter appears in this column click the question mark for an explanation Help on Result Flags This column may show one or more letters to indicate possible problems with the measurement as Follows A ACE system was activated during this measurement B Low battery condition was detected D Drift warning was given and ignored E Calibration error Calibration has expired LU Calibration error No calibration present 8 5 Closing and Uninstalling Closing Results Manager The standard close button the X in the top right corner will close the application If results have been downloaded but not yet saved you will be prompted to save them before closing Uninstalling Results Manager If you no longer require the application it may be removed from your PC using the Add Remove Programs utility in the Windows Control Panel Scroll down the list of applications to the Results Manager entry and click the button to delete the application 33 34 Chapter 9 Maintenance 9 1 Reagent Life There are three main factors which govern the life of reagents and therefore the frequency of cleaning and recharging the titration cell 1 The physical size of the titration cell allows for 50 60mL of sample to be added For the analysis of most liquid samples e g solvents Aquamax KF titrators normally
26. ll Thermal Single x3 503164 Luer Needle 19 Gauge Screw Fit 503062 Gas Tight 0 25ml Syringe 503063 Gas Tight 1 0ml Syringe 39 40 Chapter 12 Troubleshooting Overtitration Detector senses too much lodine Usually caused by old reagents or stirrer switched off Check stirrer speed Add 3 5 micro litres of water until detector bars activate and allow to precondition Excess Drift Indicates excess moisture ingress or condensation on cell walls Switch OFF Remove titration cell from clamp and gently swirl anode reagent around the cell walls Reconnect switch ON and allow to Precondition Long Preconditioning Time Normally caused by glassware not being sufficiently dried before assembly Re clean glassware and electrodes dry thoroughly and charge with fresh reagents Progressively Lower Results for Same Sample Moisture contamination of syringe Flush syringe and needle with sample several times before beginning new test Poor Repeatability for Same Sample Sample size probably too small or moisture contamination of syringe Increase sample size and flush syringe and needle several times before beginning new test Warning Letters on Print Out Warning letters will be printed after time of each analysis to signify the following Uncalibrated E Calibration expired B Battery level low A ACE system active Results Manager The serial port parameters are set automatically by Results Mana
27. ode reagent When analysing Transformer oils Crude oils and other petroleum products we recommend using specially formulated anode reagents which contain other solvents to improve sample miscibility and solubility There are also single Coulometric reagents available for use with fritless generator electrodes Note When analysing samples of Ketones amines or others which may interfere with the reaction it is advisable to use specialised reagents which can be obtained from various suppliers Although reagents can be poured into the titration vessel whilst it is located on the titrator we recommend that the vessel electrodes and electrode leads are removed from the instrument whilst this procedure is performed to avoid reagent spillage onto the instrument casing Note Any spillage onto the instrument casing should be wiped off immediately to avoid damage or staining Remove the drying tube and injection septa Using the funnel supplied charge the titration vessel with 100ml anode reagent this is approximately to the lower line on the vessel Also using the funnel charge the inner chamber of the generator electrode with 5ml of cathode reagent This is not required if using fritless generator electrode Note It is not necessary to clean the funnel between reagents Reconnect the drying tube and injection septa so that the titration vessel is sealed from ingress of atmospheric moisture Locate the complete titration vessel onto the
28. only requires a few micro litres to be injected therefore the maximum volume of 50 60mL should not become a limiting factor Oil samples are an exception and are dealt with elsewhere in this manual 2 The total amount of water that can be analysed before saturation of the reagents varies slightly from one reagent manufacturer to another Typically a 100 ml charge of Anode reagent will analyse up to 1 gm water whilst a 5 ml charge of Cathode reagent will analyse up to 250 mg water Considering that the injected sample volume is normally small and also that the analysis is usually for the determination of low levels of water these water capacity values are not normally a limiting factor 3 Similar to all other Karl Fischer reagents Coulometric reagents will deteriorate when exposed to sunlight and with increases in temperature Placing the instrument in direct sunlight or near to a heat duct can decrease the reagent life As reagents age the titration speed will reduce and the drift value will increase 9 2 Cleaning the Glassware IMPORTANT The platinum mesh and wires of the electrodes are fragile and can be easily bent or broken Extreme care MUST be taken when disassembling cleaning and reassembling the titration cell The generator electrode is the most expensive part of the Aquamax KF glassware DO NOT USE A BRUSH TO CLEAN INSIDE ELECTRODE AS THIS COULD DAMAGE CONNECTIONS Coulometric reagents are flammable and toxic so care
29. ort Status Dia conn nected Model c Our em Aquam mx 2 d Serial 71006 Calibrated 7 DOE Date 15 Mey 2006 Results 4 Result Format ppm Calculation Mode V s L Result for Sample ID 001 EN Bor Pos jUnw esk f ane 1 0000 ET hos L hx homn pum Min 10 1 ppm LE GRS Results Manager Sielta GRScientific Results Manager CONNECT EXPORT 1 PRINT Status Disconnected Model Cou Lo Aquermnax2 4f Se a 71006 Calibrated 09 05 2006 Dale 15 May 2006 Results 4 Result Format Calculation Mode e Cr puta lor E sample ID 002 EJ Samp Wt Mesut Flags Time Oh Net 1 esso ese peser tre patr Ron 09 34 27 zara inaasa iness maaa mor M oa 3616 O0 290 50 10 1487 0 3969 0 0752 _ 200 58 Mean 01 El SD 0 00 Cw 1 03 E GRS Results Manager E Ie Ir S NN Results Manager CONNECT EXPORT Status Discornected Model Cou Lo Aquamex 24 Serial 71006 Se al 71006 Calibrated 06 05 2005 ee Date 15 May 2006 Resulis 3 Resul Formal Calculation Mode WK Results for Sample ci 003 E Sson 13002 20 000 25 0000 0 8929 58 ee ee ine brem e Min 1 0 Mean 1 0 SD 000 Cv 010 Result Calculated result in the selected format Example Calculation Mode V SG Prm 1 amp Prm 2 columns show Volume amp Density values Example Calculation Mode W w Prm 1 Prm 2 amp Prm 3 columns show Total weight Tare weight amp sample Example Calcu
30. ows It will open the standard printer dialog allowing you to choose the printer and set options such as paper type and location The printout should scale automatically to fit the page although obviously it has not been possible to test this on every different combination of printer and paper size 3 4 Display Explanation Status Disconnected Model Cou Lo Serials Calibrated Status Titrator and computer are connected or disconnected Model Manufacturer model and software version Serial Instrument serial number Calibrated Last date titrator calibrated Date 15 May 2006 Results 4 ResultFormat ppm Calculation Mode V SG Date Date analysis recorded Results Total number of results recorded Result Format Selected result format ug ppm mg kg or water Calculation Mode Selected calculation mode V SG W w W K V v Results for Sample ID 001 Results for Sample ID Samples identification number Flags _ Run Sequential count of analysis runs Time Time analysis recorded Drift Titrator background drift value during analysis Nett The nett microgram count for analysis after drift deducted 31 32 Prm1 Prm 2 amp Prm 3 The sample data used for the calculation These parameters change depending on calculation mode being used Examples of the three main calculations are shown 18 GRS Results Manager cene Results Manager connect 32 A Exp
31. peration 5 1 Switching ON and OFF The Aquamax KF Coulometric has one l O switch and is powered by either a mains power supply using an adaptor or a built in battery for power Note Refer to Chapter 4 2 for power supply connections To avoid risk of electrocution make sure the I O switch is set to OFF before connecting the power supply 5 2 Setting the Date and Time 1 Switch on the Aquamax KF titrator and wait for it to display the following Aquamax KF Coulometric 2 Hold down the START key until the Aquamax KF titrator displays Aquamax KF Coulometric 3 Use the to move the cursor across the screen 4 Use the numerical keys to set alter the required number 5 When completed press the ENTER to save the changes and exit 13 14 5 3 Preconditioning 1 Assemble glassware see Assembly Instructions 2 Charge vessel and generator electrode with reagents see Filling amp Changing Reagents 3 Locate assembled titration vessel onto the Aquamax KF titrator 4 Connect electrode leads 5 Connect mains lead power cord 6 Switch ON using switch on rear panel and wait for display to show Aquamax KF Coulometric Note If required adjust the stirrer speed using the arrow keys on the front of the instrument 7 Press START and allow the instrument to precondition equilibrate Aquamax KF Coulometric Microgram Count Detector Signal Titration Speed 8 At
32. plicate print out or when power is switched off Print Out Examples Example of V SG Calculation Aquamax KF V XXXX Serial No 71000 Calibrated DD MM YYYY Run Date Run 1 Run Time Nett Count Drift 00 Result Format 06 Calculation Mode V SG Volume 1 0000 ml Density 1 0000 Res 0 000096 Run 2 14441 ia Nett Count 0 0 ug Drift 00 Res 0 0000 Titrator model Software version Titrator serial number Date titrator calibrated Date sample run Run no and time of analysis F generator with frit Nett microgram count after drift correction Drift value at start of titration Result format selected Calculation mode selected Sample volume Sample density Calculated result water content Subsequent runs of the same sample and calculation parameters show run number run time nett count Drift value and calculated result 27 28 Example of W w Calculation Aquamax KF V Serial No 71000 Calibrated DD MM YYYY Run Date Run 1 Run Time Nett Count Drift 00 Result Format Calculation Mode W w Total Weight 0 0000 gm Tare Weight 0 0000 gm Sample Weight 0 0000 gm Res 0 0000 Run number amp time of analysis N generator no frit Nett microgram count after drift correction Drift value at start of titration Result format selected Calculation mode selected Weight of syringe plus sample Weight of syringe after sample injected Weight of sample analysed Calc
33. ption Key personnel at G R Scientific are recognised experts in Coulometric Karl Fischer titration technology and electrochemistry They have designed and manufactured Coulometric titrators since the early 1980 s and are widely regarded as one of the leading specialists in this technique The Aquamax KF PLUS is a small foot print titrator with a full numeric keypad for data entry and results manager software for data storage and retrieval Suitable for use with generator electrodes either with or without frit This titrator is a truly versatile model which includes a printer to enable use in areas where connection to a PC isn t available Low Drift Cell twin port glassware and accessories are supplied as standard As well as being a stand alone instrument this titrator can be combined with accessories such as an Oil Evaporator or a Solids Evaporator system Suitable for a wide range of applications the Aquamax KF PLUS can be used to determine water contents of liquids gases and solids An optional carry case for transportation can also be included Designed primarily for the oil and power industries the Aquamax KF PORTABLE is the only model on the market with a carry handle attached directly to the unit It also features a protective cage built in printer and single button operation for water standards analysis Specially designed Low Drift Cell glassware avoids the need for PTFE sleeves or grease on the electrodes to seal titration cell from moist
34. ream in the sink ensuring that the breather hole midway down the side of the electrode is positioned at the top when pouring acid out 6 Thoroughly rinse the electrode using a wash bottle containing deionised water Add 10ml deionised water to the inner chamber and allow to stand for 30 minutes 7 Remove any remaining water add 10ml Methanol and allow to stand for 10 minutes Ensure that the outer surfaces of the electrode do not come in contact with waste solution gathering in the bottom of the vessel 8 Drain remaining solvent from inner chamber and dry electrode Note Wear safety goggles and protective gloves when handling acid 35 36 Chapter 10 Technical Specifications 10 1 PLUS Model Titration Method Electrolysis Control End Point Detection End Point Indication Titration Vessel Measuring Range Moisture Range Max Sensitivity Max Titration Speed Max Current Drift Compensation Precision Start Delay Time End Delay Time Calculation Modes Display Format Print Format Statistics Method Storage Sample ID Number Stirrer Speed Languages Calendar Clock Data Outputs Removable Data Storage Data Entry Display Printer Power Supply Unit Dimensions Weight Coulometric Karl Fischer Titration Patented ACE Control System GB2370641 AC Polarisation Visual Display Print Out Acoustic Beep Low Drift Cell Design no grease or PTFE sleeves required Possible
35. rint Drift Start Delay Time Min Titration Time End Sensitivity Beep Mode Language Generator Electrode Save Method up to 8 digits method number 1 9 ug ppm mg kg or water V SG W w W K or V v off every result or full report up to 99 runs will print min max and mean on or off up to 30 minutes up to 30 minutes 0 9 seconds off key press end titration or both select language with frit without frit store up to 10 methods Note See Chapter 5 4 Programming A Method for an explanation of each Menu List parameter 15 16 5 5 Programming a Method After the initial drift has been calculated in micrograms ug of water per minute the Aquamax KF titrator is ready for operation It is now possible to step through the PROGRAM parameters and enter the required calculation data Aquamax KF Coulometric Press PROGRAM until the required option is displayed then simply follow the Flow Chart in Chapter 5 5 to enter the specific data values Pressing PROGRAM will move you on to the next prompt pressing CLEAR will return to Ready condition It is not necessary to step through all of the programme functions for every method for example if you only require to change the Beep Mode from Off to Both simple press PROGRAM until display shows Beep Mode press the until display shows Both then press ENTER and CLEAR to return to Ready Sample ID Number Press PROGRAM Display will
36. rt to show the calculated result in ppm mg kg or water Calculation Mode Aquamax KF Titrators have four standard calculation modes in memory Each of these allow the instrument to divide the microgram count by the gram weight of sample introduced so that the calculated result can be printed out in either ppm or percentage of water Press to scroll through the options that are available Select the calculation mode required and press ENTER The display will prompt you with the appropriate parameters Enter the numerical value for each parameter and press ENTER The four standard calculations are 1 Weight difference W w Note This is the most accurate calculation and is suitable for almost all types of samples powders liquids gases 6 microgram count Result ppm or 96 2 W w Where W Total weight of sampler sample gm w Tare weight of empty sampler gm After entering the total weight W the instrument will return to the Ready condition The Tare weight w can be entered at any time during the titration by pressing PROGRAM or at the end of titration For ease of operation it is possible to enter the Total weight W as 0 0000gm then place the full sampler on the balance and tare to zero Thereafter it is only necessary to enter the weight difference tare weight w for each titration This procedure reduces potential data entry errors 17 18 2 Wei
37. send the next record and causes it to indicate that connection has been established using a special character on its display The receiving application may also send a negative response to reset the serial interface causing the entire current set or results to be retransmitted Results Manager Package Comprises of Part No 102026 Results Manager Software CD Part No 101009 Interface Cable connects titrator to computer USB port Part No 101010 512MB USB Flash Drive Memory Stick 8 2 Installation IIE DVD RW Drive E Results Manager When the Results Manager CD is inserted it will automatically open an AutoPlay screen in order to install the application General options Note PCs must have Windows 7 or higher to run the application ems N FF 0 FB Bg C3 x z Select setup from the options and dotnetfx driver ResultsMana windowsinsta autorun readme ResultsMana follow the process to carry out the ger 1305 ler31 ger installation of the application lt gt ResultsMana test ner 1 3 n 5 Once this has completed Results Manager will open automatically The application can be used as many times with the CD inserted To use Results Manager without inserting the CD copy all of the files from the CD to a folder in My Documents 29 30 8 3 Running Results Manager With the application running five buttons across the top of the screen allows the user to carry out the functions tha
38. show Key up to 8 numbers Press ENTER Aquamax KF Coulometric Aquamax KF Coulometric If you do not want to enter any further parameters simply press CLEAR to go back to the Ready condition Press PROGRAM if you want to continue entering other parameters Result Format Press PROGRAM Display will show Aquamax KF Coulometric Results can be selected in ug ppm mg kg or water If you want to select the format already stored in memory and shown on the display press PROGRAM and the instrument will go to the next prompt If you want to change format to give results in ppm mg kg or you can scroll through these options by pressing until the required format is displayed and then press ENTER to store this in memory and PROGRAM to move onto the next prompt If you have selected a result format in pom mg kg or the instrument will prompt you for the necessary calculation mode and data values Aquamax KF Coulometric Aquamax KF Coulometric The display shows the calculated water content according to the programmed Result Format and Calculation Mode program settings e whatever has been chosen to be shown printed at the end of the titration The only exception to this is in the W w mode when the Tare Weight has not yet been entered In this case the display will show the ug count The PROGRAM key can be used to enter the Tare Weight at any time during the titration once this has been done the display will sta
39. ssed End Titration Both Beep after every key press and three times at the end of a titration Beep three times at the end of a titration Language The Aquamax KF titrator can be programmed to show all display prompts and print outs in various languages Use to select language then press ENTER Generator Electrode The Aquamax KF titrator can be operated using generator electrodes with or without frit diaphragm Use to select either with or without frit then press ENTER The titration electrolysis current settings are automatically adjusted for each style of generator and appropriate reagents Save Method If you want to save a method for future use this can be done by pressing a numerical key 0 9 and then ENTER All titration parameters printer mode beeper mode etc are stored automatically Aquamax KF Coulometric Display then shows Then press CLEAR and the instrument will revert back to the Ready condition Recall Method If any methods have been saved to memory then the first prompt before Sample ID number will be Recall Method When this prompt is displayed simply press the number of the method file you wish to recall and press ENTER There are 10 method files available numbered from O to 9 The titration parameters etc will all be automatically recalled Press PROGRAM to view the recalled method parameters or press CLEAR and the instrument will go back to the Ready condition If you
40. t it provides as follows CONNECT SAVE LOAD EXPORT PRINT Connect To establish a connection to a titrator linked to the USB port on your PC click the Connect button The first time you do this after running the application you will be asked to choose the serial port used to make the connection Desktop PCs will normally have COM1 and perhaps COM2 fitted while laptops usually have only COM1 to provide functionality on machines without serial ports these are normally installed in the range COM4 to COMB although this may usually be changed using the Windows Device Manager Once connection has been established the Status display on the screen will change to Connected and the text on the Connect button will change to Disconnect Clicking it again will disconnect the titrator from the PC While connected Results Manager will download any test results it finds and display them and will continue to load the results of any further tests that are carried out as long as it remains connected Because the files that it uses contain single sets of results when the user starts a new set of measurements on the titrator i e a new sample ID is entered titration parameters are changed or the end of a fixed run is reached Results Manager will orompt the user to save the previous set of results before discarding them and loading the new set Save The Save button allows you to save the current set of results to a file on disk It opens the standard
41. the end of the precondition period the display will show Aquamax KF Coulometric 9 After the initial drift has been calculated in micrograms of water per minute the Aquamax KF is ready for operation Aquamax KF Coulometric The background drift value will usually slowly decrease with time as the titration vessel becomes drier and more stable Although it is possible for the titrator to be used at high drift values it is advisable to wait until the drift value is below 20ug minute and stable before commencing especially for low water content samples in the ppm ranges The lower and more stable the drift the more accurate the result 5 4 Program Functions When the Aquamax KF titrator displays Ready you can enter titration parameters recall or edit existing methods enter new method files etc by using PROGRAM ENTER CLEAR and KEY FUNCTION PROGRAM Press PROGRAM to scroll through menus listed ENTER Allows parameter values for the displayed menu to be entered into memory CLEAR 1 If you have finished entering data press CLEAR to return to the Ready condition 2 11 you have started to enter an incorrect value press CLEAR to return to the previously stored value Scrolls through individual parameters in each menu When the required parameter is display press ENTER to store it Menu List Sample ID Number Recall Method Result Format Calculation Mode Printer Mode Statistics Print P
42. ting the Date and Time eese 13 5 3 6010111011111 cito onala 14 5 4 Program Functions csi 15 5 5 Programming a Method anna 16 5 6 Program Flow Cha Einicio 21 Fonning a TESTE AMA ner Mu UE nist mn nn ne pent ane ery ayer er 22 64 Example Applications sir dedicacion 22 6 2 Water Standard Tests rt 24 6 3 HOW to Run a TES 24 6 4 Drift Rate Compensation 25 6 5 UTA OP NN 26 Chapter 7 Chapter 8 Chapter 9 Chapter 10 Chapter 11 Chapter 12 Chapter 13 Results duna diia 27 7 1 Printout m do igr iio pp T 27 Results MANAGED sas 29 81 16501112 sais riada 29 A 2 be O 29 8 3 Running Results Manager 33 30 8 4 Display Explanation aaa 31 8 5 Closing and Uninstalling srt 33 MAIRENA MOS aE RR 34 9 1 Reagent ET 34 9 2 Cleaning the Glassware 34 Technical Specifications 36 10 1 PLUS Model ise iia 36 102 PORTABLE Model Suess 36 Pare E m M H 38 111 CNU EE eT 38 11 2 PORTABLE Model susana ira 38 TIO UDS ROO UNA sesionar 40 Conformity and Warranty 41 13 1 Declaration of Conformity esses 41 T32 QUAN CONTO aterra 41 13 3 Customer Support and Service ess 41 a RU 41 Chapter 1 Introduction 1 1 Instrument Descri
43. tions banned by this directive 2 2 Electrical Safety The Aquamax KF Coulometer complies with the international standard IEC 61010 Only operate this instrument within the mains voltage supply that is specified on the back the instrument an incorrect mains Supply can damage the instrument Never open the housing of the instrument only GR Scientific personnel who are trained to service the instrument can open the housing There is risk of electrocution if live components are touched Always ensure the instrument is disconnected from the mains power supply when connecting or disconnecting cables from the back of the instrument as electrostatic discharge can build up 2 3 Solvent and Chemical Safety When using flammable or irritant solvents and chemicals follow suitable safety measures to protect yourself and others around Always use the instrument in a well ventilated area clean up spilled fluids immediately and keep flame sources away from the work area Always follow the safety instructions of the chemical manufacturer and apply the correct countermeasures that are required 2 4 Recycling and Disposal This instrument is covered by the WEEE Waste Electronic and Electrical Equipment Directive 2012 19 EU to prevent the negative and harmful effects on the environment and public health For more information on how to dispose of the instrument safely please contact your local authority your local waste disposal company or GR Sc
44. ulated result water content Chapter 8 Results Manager 3 1 Description Results Manager is a Windows application that allows you to view and print sets of results created by the Coulometric family of Karl Fischer Titrators lt can download results directly from the titrators through a serial port connection or open result files previously saved to disk The Coulometric family of titrators provide a serial interface for the download of test results to our own PC software package Results Manager or to third party software running on any equipment with a serial port capable of running at 9600 bps in asynchronous mode The titrator serial port is configured as a DTE so connection to a standard PC serial port is achieved using a crossover or null modem cable The titrator serial port is activated by raising the DCD input pin this would normally be carried out under control of the software package at the remote end of the link Data is transmitted by the titrator in plain ASCII text with records terminated by a Carriage Return CR character Each record starts with a letter to identify the record type e g Product type and version Configuration parameter or Result data a number to identify the exact information contained and one or more items of actual information Records must be acknowledged by the receiver using a simple positive response record or they will be retransmitted after a timeout delay this allows the titrator to move on and
45. um balance between repeatability reagent depletion and speed of analysis Crude Oils IP 386 amp 438 ASTM D1533 D4928 D6304 API MPMS Chapter 10 9 ISO 10337 amp 12937 Most Coulometric reagents contain Methanol as the main solvent and as such it is possible that waxy deposits from crude oils can drop out and contaminate the electrodes requiring more frequent and thorough cleaning of the glassware This problem can be reduced by using Coulometric KF Anode Reagent which has been specially formulated for this application The most common interference in crude oil samples is usually caused by Mercaptans or Sulphides Samples containing alkyl groups will react stoichiometrically so that 100 ppm Mercaptans would show as approximately 30 pom water 100 ppm Sulphides would show as approximately 50 pom water In normal practice oils containing less than 500 ppm Mercaptans or sulphides are regarded as having no appreciable effect Repeatability problems are usually caused by sampling inaccuracies or improper homogenisation of the sample Transformer Insulating Oils ASTM D 1533 BS EN 60814 IEC 60814 Due to the viscosity of these samples and the fact that typical water content levels are in the range 5 40 ppm it is usually necessary to inject sample volumes of 1 ml This means that up to 50 samples would fill the titration cell Provided that the other criteria governing reagent life total water titrated and reagent age
46. ure invasion A sturdy carry case for transportation in the field is also included 1 2 Principle of Measurement Karl Fischer titration is simply a means to measure water content of samples Modern instruments such as the Aquamax KF use the Coulometric principle whereby the water present in the sample is coulometrically titrated to a predefined end point at which there is a minute excess of free iodine present Stoichiometrically 1 mole of water will react with 1 mole of iodine so that 1 milligram of water is equivalent to 10 71 coulombs of electricity Combining the Coulometric technique with Karl Fischer titration Aquamax KF titrators determine the water content of the sample by measuring the amount of electrolysis current necessary to produce the required iodine This is an absolute technique which does not require calibration of the reagents SO S50 3C5H5N H20 gt 2C5H5N HI C5H5 N SO SO CH3 CsHsN CH30H gt Cs Hs ani 2 2e gt p Using the latest pulse current technology and our patented ACE control system Patent No GB23 0641 the Aquamax KF automatically selects the appropriate titration speed dependent upon the amount of water present in the sample The titration speed is reduced as the end point is approached and when the titration is completed the instrument prints out and displays the results For a more detailed explanation of the technique and a comparison with volumetric Karl Fischer titration
47. wn without the protective cage and carry handle but the same procedure applies 1 Position the titration vessel on the titrator 2 Connect the generator and detector leads to the electrodes Note The glass joints do not require PTFE sleeves or grease The special screw fittings seal the vessel from the atmosphere and are easily released even after several weeks 3 Position the electrodes on the titration vessel and tighten by hand 4 Connect the generator and detector leads to the BNCs 5 Position the drying tube with desiccant and tighten by hand 6 Place the stirrer bar inside the titration vessel 7 Fit injection septas into the injection port caps and screw tightly by hand onto the injection ports The assembled titration cell is now ready to be charged with reagents prior to use Please be sure to assemble correctly every time the cell is cleaned or re filled It is recommended that the titrator is NOT switched on until after the titration vessel has been charged with reagents This will avoid damage being caused to the electrodes by the stirrer bar Avoid twisting the electrode leads otherwise they may become damaged 4 3 3 Filling and Changing Reagents Aquamax KF Coulometric Titrators have been designed to operate with all major Coulometric Karl Fischer reagents For most routine applications generator electrodes with frit diaphragm are used in conjunction with 100ml of anode reagent and 5ml of cath
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