User Manual
Contents
1. lt lt lt r r 14 GRScientific Aquamax KF Coulometric v08 10 PROGRAMMING A METHOD After the initial drift has been calculated in micrograms ug of water per minute the Aquamax KF is ready for operation It is now possible to step through the PROGRAM parameters and enter the required calculation data The Flow Chart on the previous page may prove helpful Press the PROGRAM key until the required option is displayed then simply follow the Flow Chart 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 decimal point key e until display shows Both then press ENTER and CLEAR to return to Ready SAMPLE ID NUMBER Press PROGRAM Y Display will show Y Key upto 8 numbers Y Press ENTER PROGRAM Sample ID No Sample ID No ENTER 12345678 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 Y Display will show Result Format PROGR2. Page 28 D Reagent Life 6 D D D Page 28 Y Y Y Y Cleaning the Glassware Page29 Y Y Troubleshooting Page 30 Warranty Page 30 Accessories Paee 31 Aquamax KF Coulometric v08 10 G R Scientific Ltd Tel 44 1525 404747 Fax 44 1525 404848 E mail info O erscientific com Website www erscientific com Correspondence Address Delivery Address P O Box 242 Building 69 Ampthill Wrest Park Bedfordshire Silsoe MK45 5AQ Bedfordshire United Kingdom MK45 4HS United Kingdom INTRODUCTION Key personnel at G R Scientific are recognised experts in coulometric Karl Fischer titration technology They have designed and manufactured coulometric titrators since the early 1980G and are widely regarded as some of the leading specialists in this technique The Aquamax KF Coulometric has a small footprint is easy to use and supplied complete with a specifically designed low drift cell which is also suitable for outdoor use The built in battery and optional carry case provide the versatility required by the laboratory and also the ease of use and portability required by the field engineer
3. Cou Lo Formula reagents have been specially formulated for use with Aquamax KF titrators Formula A anode reagent is suitable for most routine applications and is especially useful for water content determination of oil samples e g transformer oils crude oils etc This anode reagent 19 supplied in single shotO bottles of 100ml T No measuring of volumes required T No mixing of other solvents required Cathode reagent Formula C is supplied in Psingle shotO 5ml vials which have fafety snappers pre fitted thereby reducing risk to the operator Where appropriate G R Scientific products include traceable calibration certificates and are backed up by a five year warranty These titrators are used by many leading companies in the oil petrochemical gas pharmaceutical biotechnology automotive and power generation industries For a list of users typical applications or details of our network of international distributors please visit our website www grscientific com or contact G R Scientific Ltd on Tel 44 1525 404747 Fax 44 1525 404848 E mail info grscientific com To obtain the full benefits that this instrument can offer it 1s recommended that you read this user manual before assembling the unit Cou Lo and Aquamax KF are registered trade marks of G R Scientific Ltd ACE control system is patented technique owned by G R Scientific Ltd All Aquamax KF power supplies are double insulated units that do not need an earth
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5. 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 optional Low Drift Cell LDC 0101 complete with gas analysis kit LDC 0121 1 Fit the gas inlet and outlet adapters in place of the injection septa Remove the drying tube and seal the top of electrode using the injection port septa and screw cap Connect outlet adapter to wet gas flow meter Flush the sample lines and allow instrument to stabilise et ge oe 39 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 Calculation G x 273 t x 22 4 W W moisture content V x 273 x 18 G microgram count V gas volume litres t water temperature of wet gas flow meter C Gas sample adapter Fitted to vessel sy S Aquamax KF Coulometric v08 10 HOW TO RUNA TEST Please read the section PROGRAMMING A METHOD then use the PROGRAMMING FLOW CHART before running any samples Example Transformer oil sample by V SG Program the Aquamax KF 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 Confirm that Aquamax KF is in f
6. ground connection These units are sealed and conform to CSA LR84459 UL listings and CE requirements Aquamax KF titrators only require a low voltage 15V input to the electronic control circuitry The moulded plastic casing of the instrument also provides additional insulation Aquamax KF Coulometric v08 10 PRINCIPLE OF MEASUREMENT Karl Fischer titration is simply a means to measure water content of samples Modern instruments such as the Aquamax 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 For further information visit www grscientific com and download the PDF article titled Recent Advances y 802 l2 S024 3C5H5N H20 gt 2C5H5N HI C5H5 N O SO2 p SO4CH3 CH30H gt C5 H5 N SS CsHsN 2 2e gt l2 Using the latest pulse current technology and our patented ACEO control system Patent No GB2370641 the Aquamax KF automatically selec
7. local representatives just contact Telephone 44 0 1525 404747 Fax 44 0 1525 404848 Email info grscientific com Web www grscientific com es di
8. 0 EXAMPLE COULOMETRIC METHODS Water Determination of Electrical Insulating Oils by Coulometric Karl Fischer Titration Water Determination of Crude Oils by Coulometric Karl Fischer Titration Water Determination of Petroleum Products by Coulometric Karl Fischer Titration Water Determination of Crude Oils by Coulometric Karl Fischer Titration Water Determination of Petroleum Products by Coulometric Karl Fischer Titration Water Determination of Insulating Liquids Oil Impregnated Pressboard by Coulometric Karl Fischer Titration Water Determination of Natural gas by Coulometric Karl Fischer Titration Water Determination of Crude Petroleum by Coulometric Karl Fischer Titration Water Determination of Petroleum Products by Coulometric Karl Fischer Titration ny Aquamax KF Coulometric v08 10 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 19 recommended that the smallest representative amount of sample be used to ensure fastest titration speed and maximum sample throughput before reagents have to be replenished Supplied as standard with every Aquamax KF titrator is a Iml syringe and luer needle These are suitable for injection of oil samples and water standards Other volume syringes are commercially available from
9. AM Ug 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 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 decimal point key lt until the required format is displayed then press ENTER to store this in memory and PROGRAM to move onto the next prompt If you have selected a result format in ppm mg kg or the instrument will prompt you for the necessary calculation mode and data values Result Format Calculation Mode ENTER PROGRAM V SG The display shows the calculated water content according to the programmed Result Format and Calculation Mode program settings ie whatever has been chosen to be shown printed at the end of the titration The only exception to this 1s 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 start to show the calculated result in ppm mg kg or water ny Aquamax KF Coulometric v08 10 CALCULATION MODE The Aquamax KF has 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 o
10. GRS cientific Mquamax KFO Coulometric User Manual Aquamax KF v 08 10 Aquamax KF Coulometric v08 10 CONTENTS Y Y Introduction 6 6 6 CEE Page 3 Principle of Measurement 6 Page4 Specifications amp Features 6 Pages Unpacking amp Parts List Page6 Titration Cell Assembly Instructions Page7 8 Filling 8 Changing Reagents Page9 Front amp Rear Panel Description Pagel Setting Time amp Date Pagell Connection amp Start Up Procedure Page 12 Programming A Method Page 13 19 Example Methods amp Applications Page 20 23 How To Run A Test Examples V SG amp W w Page 24 25 Printer Loading the paper Page 26 Example Print Out Page 27 Drift Compensation _ Page 28 Overtitration
11. ReadyO mode Flush 1 0ml syringe several times minimum 6 times with sample Fit luer needle and flush through with sample Draw sample into syringe beyond the 1 0ml marking a oe A as Invert syringe so that any air bubbles can be ejected through the needle and adjust syringe plunger to the 1 0 ml mark 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 1 2 cm Press START SR 2 SS Push needle into anode reagent and inject sample 10 Withdraw needle from titration vessel 11 Read result in mg kg ppm water on display and printout 12 Repeat steps 2 1 11 if duplicate result required ny u Aquamax KF Coulometric v08 10 Example Powder sample by W w Program the Aquamax KF with parameters for the analysis ANALYSIS METHOD 1 I E t n a D zA Confirm that Aquamax KF is in AReady mode Place a suitable amount of sample in the powder sampler p n 2000 9511 and seal with stopper provided Weigh sampler Press PROGRAM until Calculation Mode displayed then select W w Enter the sampler weight when prompted by display then press ENTER CLEAR 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 Reweigh the sampler The net weight of sampler can be entered either during the titration by pressing PROGRAM or w
12. aiting until the end of titration when display will prompt TARE Weight Enter the weight then press CLEAR ANALYSIS METHOD 2 l Fe oy et A 2 Confirm that Aquamax KF is in AReady mode Place a suitable amount of sample in the powder sampler p n 2000 9511 and seal with stopper provided Place sampler on balance and tare to zero Press PROGRAM until Calc Mode displayed then select W w Enter the sample weight as 0 0 gram then press ENTER CLEAR 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 Reweigh the sampler 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 ny Aquamax KF Coulometric v08 10 LOADING THE PRINTER To load the paper into the printer first open the paper roll holder lid above the print head and remove the old roll and rollers Now fit rollers to new paper roll LDC 0119 load as shown and insert the paper into the slot at the rear of the print head As soon as the printer sees the paper it will automatically load it To avoid damage to the printer mechanism it is advisable to only use the correct part number LDC 0119 thermal paper rolls Cut the end of the paper roll at a slight angle as shown This will make it easier to feed
13. avily 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 placed in a low temperature oven at 40 1 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 should be ready for operation within 5 1 10 minutes after reassembly however it could take up to 20 minutes before to completely stabilise if the drying procedure has not been properly carried out ny Aquamax KF Coulometric v08 10 TROUBLESHOOTING OVERTITRATION Detector senses too much Iodine Usually caused by old reagents or stirrer switched off Check stirrer speed Add 3 5 microlitres 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 c
14. d 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 sy i Aquamax KF Coulometric v08 10 AQUAMAX KF TITRATION CELL Generator e Drying Tube Electrode Lap assembly U Ring _ Screw Lap generator _ Electrode I Detector Electrode Injection Port Lap Septa Titration Vessel Stirer Bar Aquamax KF Coulometric v08 10 FILLING amp CHANGING REAGENTS The Aquamax KF has been designed to operate with all major coulometric Karl Fischer reagents however optimum performance can be obtained by using Cou Lo Formula reagents which have been specifically formulated for use with these instruments For most routine applications 100ml of Formula NAO anode reagent and 5ml of Formula FCO cathode reagent are used When analysing Transformer oils Crude oils and other petroleum products Formula NAO is especially suited as it contains other solvents to improve sample miscibility and solubility 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 and
15. e injected into Cou Lo Aquamax bl micrograms of water for same injected volume of diluent ug e g Accurately weigh approximately 2 gm of sample into a 20ml stoppered graduated flask Make upto 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 2 gm K 20ml_ 200 100ul bl microgram count of 100ul injected volume diluent ny Aquamax KF Coulometric v08 10 3 Volume Specific Gravity V SG The most widely used technique for liquid samples However care must be taken to ensure removal of all air bubbles from the syringe Result ppm or microgram count V x SG where V volume of sample ml SG specific gravity 4 Volume V v Result volume microgram count V x 1 0 where V volume of sample ml This is essentially the same as V SG mode except that the sample S G is fixed at 1 0 PRINTER MODES Selecting this program allows the printer to be turned ON or OFF It also enables you to print out the titration parameters being used at that time Simply scroll through the options using the decimal point key e 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 t
16. electrodes are removed from the instrument whilst this procedure is performed to avoid reagent spillage onto the instrument casing 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 upto the lower line with Formula MAO reagent For your convenience these reagents are supplied in Psingle shot bottles which contain 100ml so it is not necessary to measure any volumes simply pour in the complete bottle Also using the funnel charge the inner chamber of the generator electrode with Formula FCO reagent which are supplied in single shot 5 ml vials which havce fsafety snappers pre fitted thereby reducing risk to the operator 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 titrator and connect the electrode leads onto the appropriate sockets The colours of anode and cathode reagent are only an illustration to show that there are two different liquids These are not necessarily the exact colours of the reagents being used The Aquamax KF titrator is now ready to be switched on Cathode Reagent Anode Reagent Aquamax KF Coulometric v08 10 DESCRIPTION Front Panel Printer Display pa
17. ess ENTER Choose from English Francais Espanol Portugues Deutsch amp Magyar GENERATOR ELECTRODE The Aquamax KF can be operated using generator electrodes with or without frit diaphragm Use the decimal point key e 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 ENTER All titration parameters printer mode beeper mode etc are stored automatically Display then shows Save Method Done 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 Methodo 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 do not want to recall a method press PROGRAM to view the next prompt ny E ASTM D 1533 ASTM D 4928 ASTM D 6304 IP 386 IP 438 IEC 60814 BS EN 60814 ISO 10101 3 ISO 10337 ISO 12937 Aquamax KF Coulometric v08 1
18. g 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 La Aquamax KF Coulometric v08 10 CLEANING 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 BRUSH TO CLEAN INSIDE ELECTRODE AS THIS COULD DAMAGE CONNECTIONS Coulometric reagents are flammable and toxic so care 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 See page 11 on charging procedure Under normal circumstances the titration cell can be used for a large number of samples before having to replenish the reagents 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 pA 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 he
19. he glass frit of the generator electrode These problems can be reduced by modifying the Anode reagent with 20 1 40 volume Chloroform If difficulties continue contact G R Scientific Ltd for further information 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 options available e Powder samples which readily dissolve in the Anode reagent can be introduced using the optional powder sampler part no 2000 9511 Calculation mode W w e 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 e If neither of above methods are suitable you may need to use a ADP 511 oven in conjunction with the Aquamax KF titrator Powder sampler ADP 511 Evaporator sy gt Aquamax KF Coulometric v08 10 GAS SAMPLES Gas samples can be introduced by fitting a needle onto the gas sampling bomb and selecting
20. hen print out statistical data after a selected number of titrations STATISTICS PRINT The Aquamax KF 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 mean SD amp CV values PRINT DRIFT The Aquamax KF 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 g minute print will show XX This is a warning that a high drift value was present at start of the titration ny Aquamax KF Coulometric v08 10 DELAY TIMES The Aquamax KF 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 has a preset delay of five seconds which allows samples to be dispersed into the reagents before the titration starts Some samples particularly powders and viscous samples may need additional time to fully dissolve By selecting the start delay program you can increase this time by upto 30 minutes Display shows Start Delay Time 00 mins 00 secs Select required time delay and press ENTER Whilst a delay time is in operation the display will show add sampleOand the clock counter will show the t
21. hilst in READY condition the Aquamax KF 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 25 g minute the display will show High Drift XX 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 g minute but can also operate at much higher values The maximum drift value is 60 Eg minute but we recommend operating upto a maximum of 25 whenever possible If the drift value is above 60 ug per minute the display will read EXCESS DRIFT SEE INSTRUCTION MANU ALO Most common causes of excess drift are Titration vessel not properly sealed check septa amp fittings Reagent 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 cell in clamp switch instrument on and allow to precondition OVERTITRATION If the detector electrode senses too much Iodine in the titration cell usually caused by instrument being left unoperated for a long period the display wi
22. icrograms of water per minute the Aquamax KF is ready for operation 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 20 ug 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 es Aquamax KF Coulometric v08 10 PROGRAM FUNCTIONS When the Aquamax KF displays Ready you can enter titration parameters recall or edit existing methods enter new method files etc by using the PROGRAM ENTER CLEAR and e keys Key Functions PROGRAM press PROGRAM key to scroll through menus listed ENTER allows parameter values for the displayed menu to be entered Into memory this key has two functions 1 If you have finished entering data press CLEAR and the Aquamax KF will return to the Ready condition 2 If you have started to enter an incorrect value press CLEAR and the Aquamax KF will display the previously stored value you can now select the correct value and press ENTER CLEAR decimal point key allows scroll through of individual parameters in each menu When the required parameter is displayed press ENTER to store it ei MENU LIST Sample ID Number upto 8 digits Result Format ug ppm mg kg or water Ca
23. ied to the battery It 1s therefore recommended that the instrument is used from mains power supply whenever possible so that the battery is kept fully charged Maximum battery operating time is 8 hours continuous use This may be reduced if repeated high water contents are being determined or if the printer is being continually used sy k Aquamax KF Coulometric v08 10 SETTING THE DATE AND TIME Switch on the Aquamax KF and wait for it to display the following 7 Aa r p NTA a DC J d T ee Use the E decimal point key to move the cursor across the screen Use the numerical keys to set alter the required number When completed press the ENTER key to save the changes and exit es S Aquamax KF Coulometric v08 10 CONNECTION amp START UP PROCEDURE Assemble glassware see Assembly Instructions Charge vessel and generator electrode with reagents see Filling amp Changing Reagents Locate assembled titration vessel onto the Aquamax Connect electrode leads Connect mains lead power cord Switch ON using switch on rear panel and wait for display to show an u m If required adjust the stirrer speed using the black toggle switch on the front of the Instrument 7 Press START and allow the instrument to precondition equilibrate microgram count detector signal titration speed At the end of the precondition period the display will show After the initial drift has been calculated in m
24. ime remaining before the start of titration A start delay can be overridden by simply pressing START MINIMUM TITRATION TIME For some applications such as certain gas samples or when using the Aquamax KF combined with a solid sample vaporiser unit such as the ADP 511 1t can prove useful to delay the end point of the titration By selecting this parameter you can increase the minimum titration time by upto 30 minutes Display shows Min Titration Time 00 mins 15 secs Select required minimum time and press ENTER END SENSITIVITY The sensitivity of detector signal as the end point is approached can be set from O 1 9 seconds The default value 1s 3 seconds and there are very few occasions when this may need to be altered Decreasing this value can prove useful 1f 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 the decimal point key e until the required one is displayed Then press ENTER The options are Off beeper inactive Keypress beep once every time a key is pressed End titration beep three times at the end of a titration Both beep after every keypress and three times at the end of a titration ny Aquamax KF Coulometric v08 10 LANGUAGE The Aquamax KF can be programmed to show all display prompts and print outs in various languages Use the decimal point key lt to select language then pr
25. into the printer The mechanism has optical sensors which detect the paper and will auto feed Schematic of paper feed Fit rollers onto both sides of paper roll Locate paper roll in to compartment K Aquamax KF Coulometric v08 10 PRINT OUTS The Aquamax KF allows 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 1s 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 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 duplicate print out or when power is switched off PRINT OUT EXPLANATION EXAMPLE OF V SG CALCULATION Aquamax KF V XXXX Serial No 71000 Calibrated DD MM YYYY Run Date Titrator model Software version Titrator serial number Date titrator calibrated Date sample run Run number amp time of analysis F generator electrode with frit Nett micr
26. lamp 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 U Uncalibrated E 1 Calibration expired B Battery level low A 1 ACE system active Call G R Scientific Ltd or your local dealer for suggestions on sampling technique for your application E mail info grscientific com TEL 44 1525 404747 FAX 44 1525 404848 INSTRUMENT CARE Although the instrument casing is highly resistive to most solvents care should be taken to ensure that any spillage is wiped off immediately to avoid staining or possible damage to the paint surface WARRANTY Under the conditions of our warranty all faults which are proved to be due to material construction or manufacturing defects which occur within 60 months of the delivery date will be repaired o
27. lculation Mode V SG W W W K or V v Printer Mode off every result or full report Statistics Print upto 99 runs will print min max mean SD amp CV Print Drift on or off Start Delay Time upto 30 minutes Min Titration Time upto 30 minutes End Sensitivity 0 1 9 seconds Beep Mode Off keypress end titration or both Language select language Generator Electrode with frit without frit Save Method store upto 10 methods See PROGRAMMING A METHOD for an explanation of each Menu List parameter ny Aquamax KF Coulometric v08 10 PROGRAMMING FLOW CHART nm tr ote al e e gt gt O gt k gt UVA19 NVYDOYA e e e ee ee e e ee e rt e lt lt e e e e e gt gt gt Sa Ss gt gt gt T YVATO AVIDOYA gt e e e ee e e enfeA e ygJiNJ ueg rt e e 4 Doo 1 Ett YVA19 NVY9DOHd gt gt t e ee ww4V3I NWVHSOHd gt gt gt gt e wWV3TO WVdOOHd gt gt gt A T tt YVI19 WVY 90Nd gt gt gt Lt YVETO INNWHDOUd gt gt gt e YV319 NVH9OMd gt gt gt gt a gt e ee YV319 NVY90Nd gt gt gt T e YVeTO WYYDOUd gt gt gt gt gt 3IN3 SUnJ 66 ojdn iuuq SONSHEJS equinu Jajua a D 2
28. ll read FOVERTITRATION SEE INSTRUCTION MANUALO 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 instrument will automatically carry out its precondition REAGENT LIFE There are three main factors which govern the life of reagents and therefore the frequency of cleaning and recharging the titration cell l The physical size of the titration cell allows for 50 1 60 mls of sample to be added For the analysis of most liquid samples e g solvents the Aquamax KF normally only requires a few microlitres to be injected therefore the maximum volume of 50 60 mls 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 Formula MAO will analyse upto 1 gm water whilst a 5 ml charge of Cathode reagent Formula FCO will analyse upto 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 Placin
29. nel Keypad Stirrer speed Rear Panel b Power Jack Nominal 15v DC 40w Supply Input 4 15vDC 40w Fuse 3 15amp T type Time delay RS232 Standard 4 wire RS232 Input Output RS232 Port USB B Direct cable to PC Results Manager Port USB A Removable Flash Memory Store Port RS232 Port For updating titrator software connecting to other equipment for remote controlling software specific protocols to be provided USB B Port 1 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 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 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 as 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 see Results Manager user manual for full instructions There is a separate power ON OFF switch on the rear panel Whilst connected to mains power supply a trickle charge is continuously appl
30. o gt gt gt gt gt gt NA L 1 TT raf tT Ty Lf rT Ta TT 14 11111 ta TE Ty Ty Pre j 111 tty TTT 4 rT Ts gt SOYd 1N3 1 MM apo 989 DOYA LN3 SS A H gt gt gt duroJd peu o uo SAQUI 01 WYHOON SS 1d syBip g oy dn si quunu 19 ua n lt lt lt e y WO lt lt HAINT lt 6 0 Jequuinu pajeg lt A L y Ig 1 4 l t tg Ty TTT gt gt pouJen SAES gt gt gt adA 10je190Ua5 gt gt gt oBenSue gt o gt gt gt o _ d pow desg co gt gt gt Ayanisuasg pug gt gt gt SUI uonenu UN gt gt o aut Aejaq Les gt gt gt o gt YU Wid DTO gt gt gt gt poW I8JULA ooo 6n yi Jeuo y Bubu ynsey wdd asooyo Po0OUBMW II gt gt gt ON GI adwes gt gt Too dai kisa gt 1 wvsooud gt t wit Sasa gt 1 q m mg u t gt i i sd gt gt T ic abg of ddar ss gt gt t pant S gt T t NVyIDOYdA lt gt k t diii aig gt T 1 kus adla Apeey
31. ogram count after drift correction Drift 00 Drift value at start of titration Result Format G Result format selected Calculation Mode V SG Calculation mode selected Volume 1 0000 ml Sample volume Density 1 0000 Sample density Run 1 Run Time F Nett Count 0 0 ug Res 0 0000 Calculated result water content Subsequent runs of the same sample and calculation parameters show run Run 2 Run Time number run time nett count Nett Count 0 0 ug Drift value and calculated result Drift 00 Res 0 0000 EXAMPLE OF W w CALCULA TION Aquamax KF V XXXX Serial No 71000 Calibrated DD MM Y Y Y Y Run Date Run 1 Run Time N Nett Count 0 0 ug Drift 00 Result Format Calculation Mode W w Total Weight 0 0000 gm Tare Weight 0 0000 gm Sample Weight 0 0000 gm Run number amp time of analysis N generator electrode without 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 Res 0 0000 Calculated result water content ny Aquamax KF Coulometric v08 10 DRIFT RATE COMPENSATION At the start of any titration the drift value in the top left corner of the screen in micrograms per minute 1s stored in memory This ensures that the displayed result is corrected for any ingress of atmospheric moisture during the titration period W
32. r 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 The Cou Lo Safe Warranty Registration Form must be returned so that we can register your details Kr x Aquamax KF Coulometric v08 10 ACCESSORIES CARRY CASE Optional Carry case provides the portability required by the field engineer The Aquamax KF can be transported complete with glassware assembled ready for immediate use on arrival at destination Power cords syrlnges etc can all be carried inside the carry case Hd which has a special compartment for this purpose Part no 201109 COU LO FORMULA REAGENTS Specially formulated to ensure optimum performance our uniquely packaged reagents provide improved sample miscibility and solubility Packaged in Psingle shot 100ml bottles and 5ml feasy snap O vials Cou Lo Formula reagents are safer to use and safer to store OTHER PRODUCTS IN THE AQUAMAX RANGE AQUAMAX KF VOLUMETRIC AQUAMAX TAN TITRATOR GAS TIGHT OIL SYRINGE water content determination total acidity number 1 0ml with white markings For further information about any of our products pricing or details about
33. tions Weight weight Volume density Volume volume Weight Dilution ratio ug mg kg ppm ug count plus calculated mg kg ppm water Upto 99 runs user programmable 10 programmable methods Sample ID number Printer Stirrer speed Battery life Charging time User programmable 42 character high speed thermal printer Microprocessor controlled 8 hours running time from fully charged Fully charged 14 hours Battery low indication Dimensions Weight Carry case Calendar clock Display print out indication 10 x 9 x 5 inches 250 x 245 x 120 mm 6 pounds 3 kg Optional Analysis time date print out Aquamax KF Coulometric v08 10 UNPACKING amp PARTS LIST Inside the shipping carton you will find a plastic case which contains the glassware and accessories pack and the user manual The Aquamax KF titrator is located underneath the glassware case or inside the optional carry case if ordered The mains power lead power pack and in car adapter are inside the carry case lid compartment Remove all of these items and check that they have arrived undamaged After unpacking your Aquamax KF check that the glassware accessories pack contains Item Description Low Drift Cell 1 pce Titration Vessel 71 0102 1 pce Detector electrode 71 0103 1 pce Generator electrode 71 0104 1 pce Desiccant tube amp cap 71 0106 1 pack Injection septa 10 71 9507 1 pce Iml Gas Tight s
34. ts 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 please visit our website www grscientific com SCHEMATIC OF TYPICAL TITRATION ELECTROLYSIS CURRENT DETECTOR SIGNAL Al START END START END Titration method Electrolysis control End point detection End point indication Display Measuring range Moisture range Max sensitivity Max titration speed Max electrolysis current Drift compensation Start delay time Min titration time Power supply Precision Calculation modes Display format Print format Statistics Method storage Aquamax KF Coulometric v08 10 SPECIFICATIONS amp FEATURES Aquamax KF Coulometric Coulometric Karl Fischer Titration Patented ACE control system GB2370641 AC polarisation Visual display print out acoustic beep 40 character alphanumeric backlit LCD lpg 10 mg water 1 ppm 100 water r T ya 2 mg per minute 400 ma Automatically controlled 0 30 minutes user programmable 0 30 minutes user programmable 90 264 VAC 47 63 Hz 12V DC car adapter internal battery 10 100ug 3ug 100ug 1 mg 5 ug above 1 mg 0 5 User programmable calcula
35. ut in either ppm or percentage of water Press the decimal point key e to scroll through the options 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 This is the most accurate calculation and is suitable for almost all types of samples powders liquids gases etc Result ppm or microgram count 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 1s 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 2 Weight Dilution ratio W K 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 Result ppm or microgram count bl TTT _ x K w where W weight of sample dissolved gm K total volume of diluent sample volum
36. 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 LL Z 7 FS Z Z Z Z 1 10 ppme ee eee lor2ml 10 100 ppm lo2m 100 500 ppm 0 5 orl m 500 1000 ppm 0 50or1ml 0 001 0 01 l or 2 ml 0 01 0 1 H 1 or 2 ml 0 1 0 5 0 5 or lm 0 5 1 0 0 5 or lm 1 0 5 0 0 2 ml above 5 0 HT 0 1 ml or less Please note that these volumes are only a guide You may wish to experiment with sample size to determine the optimum 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 outO and contaminate the electrodes requiring more frequent and thorough cleaning of the glassware This problem can be reduced by using Cou Lo Formula AO 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 ppm water 100 ppm Sulphides
37. would show as approximately 50 ppm 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 ny Aquamax KF Coulometric v08 10 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 1 40 ppm it 19 usually necessary to inject sample volumes of 1 ml This means that upto 50 samples would fill the titration cell Provided that the other criteria governing reagent life total water titrated and reagent age 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 upto 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 For optimum performance use Cou Lo Formula AOreagent TURBINE LUBRICATING OILS For most Lube Oil applications a sample size of Iml is sufficient However if it is suspected that the water content is above 1 then a sample size of 0 2 to 0 5 ml is suggested Some lubricating oils contain additives which can coat the detector electrode or block t
38. yringe 71 9508 GT 1 pce Luer needle 71 9509 1 bottle Molecular sieve 71 9512 1 pce Stirrer bar 71 9514 pce Funnel 71 9515 pce Thermal paper roll 71 0119 ACCESSORIES pce Mains lead 71 4014 18 19 20 UK EU US pce Mains power pack 71 401607 pce In Car Adapter 71 401421 pce User Manual 71 9517 pce Dust cover 71 301301 pce Carry case optional 71 201109 sy Aquamax KF Coulometric v08 10 AQUAMAX KF TITRATION CELL STEP BY STEP ASSEMBLY INSTRUCTIONS Position titration vessel on Aquamax KF titrator The glass joints do not require Teflon sleeves or grease The special screw fittings seal the vessel from ingress of moisture from the atmosphere and are easily released even after several weeks Position electrodes on titration vessel It is not necessary to overtighten these screw joints Connect leads to generator and detector electrodes then connect the leads to the titrator Generator electrode lead connects to socket marked AGENERATORO 1 detector electrode lead connects to socket marked ADETECTORO Place stirrer bar inside titration vessel Fit injection septa into plastic screw cap connectors and locate onto injection ports of titration vessel Fill drying tube with molecular sieve and locate on top of generator electrode 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 fille
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