Aquamax KF ECO Manual
Contents
1. gt seme S o a sm 55 9 gt 1 e 4 e e 9OHd 1N3 eidues NA O9OMSd LN3 oney M lt 9OYd LN3 vonnia 9SOMNd LN3 ATS lt WM JuDteAA C e 4 e 4 4 9OHd IN3 18101 lt SOMHd LN3 AIM 9 SOYd LNA 1 lt ejdues S9Oud IN3 9S A T anjea anjea e e e 6 0 pases gt gt gt gt gt gt dwad jxeu oj uo NWVHYDOYd 5584 t e YVATO WWHDOYUd e yJ e sipgodn lt sjequunu gt gt gt eumAue je AQVa3N 0 YWaTIO 55 gt gt gt gt gt e I3 11 ra TTT tty ty f Ip 1111 TT T 4 TIL 1111 1111 i 4 lt ynsey 4 gt gt gt gt gt m poujew md gt gt gt gt gt f 1 ed WVYDOYd 1 gt gt gt gt gt f gt gt gt gt f 1 1 lt pow deeg 1 gt gt gt gt 1 idi iiam gt gt gt gt gt gt 1 SUN2. Page 26 Page 26 PNOCESC OMICS pap UM Edu d Page 27 29 GRScientific 2 Aquamax KF ECO v 13 08 G R Scientific Ltd Tel 44 1525 404747 Fax 44 1525 404848 E mail info gerscientific com Website www grscientific com Correspondence Address Delivery Address Building 69 Building 69 Wrest Park Wrest Park Silsoe Silsoe Bedfordshire Bedfordshire 45 4 5 45 4 5 United Kingdom United Kingdom INTRODUCTION Key personnel at G R Scientific are recognised experts in coulometric Karl Fischer titration technology and electrochemisty They have designed and manufactured coulometric titrators since the early 1980 s and are widely regarded as some of the leading specialists in this technique The Aquamax is an economical entry level titrator which has single injection port glassware full numeric keypad for data entry results manager software for data storage and retrieval For use with generator electrodes either with or without frit This small footprint unit offers excellent value Aquamax KF 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 15 supplied in single shot bottles of 100ml No measuring of volumes required No mixing of other solvent
3. UW lt 1 gt gt gt 1 eum ejog HEIS WYYSOUd 1 gt gt gt gt gt gt 1 1 yug Wud ee gt gt gt gt gt gt T lt SPOW ud WVyoOHd ty l gt gt Bn 1 lt 16293 t 1 a l e e ONG edweg WyvuSOHd 1 4 4 4 C 4 4 14 Aquamax KF ECO v 13 08 PROGRAMMING A METHOD After the initial drift has been calculated in micrograms ug of water per minute the Aquamax 15 ready for operation It is now possible to step through the PROGRAM parameters and enter the required calculation data Ready 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 pre
4. cathode reagent are used When analysing Transformer oils Crude oils and other petroleum products Formula 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 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 reagent For your convenience these reagents are supplied in single shot bottles which contain 100ml so it 15 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 C reagent which are supplied in single shot 5 ml vials which havce safety 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 v
5. P GR Scientific User Manual Aquamax KF FCO 99 Data Capre and Retrieval Software UK Distribution by IMA Ltd Parkwell House Otley Road Guiseley West Yorkshire LS20 8BH England Tel 44 0 1943 878877 Email info ima co uk Website www ima co uk Aquamax ECO v 13 08 Aquamax KF ECO v 13 08 CONTENTS iroda ON MR T E Page 3 Principle of Measurement 0 cece cece cece cece cece eee Page 4 Technical SPCCHICAUONG Eod penso aired Page 5 Unpackine amp Farts LIS Page 6 Titration Cell Assembly Instructions ecce Page 7 8 Pulling amp Changing Reagerts Page 9 Front amp Rear Panel Description csse Page 10 Settimo Time amp Dl EEO EEO NRE Ud UN E TUNE Page 11 Connection amp Start Up Procedure 0 cece cece cece cece cece Page 12 Programming A Method sss Page 13 18 Example Methods amp Applications cccceeeeeeeeeeeeeeeeeeeeeas Page 19 21 How To Run A Test Examples V SG amp W w Page 22 23 Drift Compensation dada Page 24 Oa E o i EEE E EEE EEE E weeds ncaa wend E EEE Page 24 EL IC ERR Em Page 24 Cleaning the Glassware ccc cece cece cence cece cece mmm Page 25
6. Whilst in READY condition the Aquamax continually compensates for any drift caused by atmospheric moisture ingress or reagent decomposition and displays this information which 15 updated every 10 seconds If the drift value is above 25 minute the display will show High Drift XX This is a warning that the value 15 high however the instrument can still be used by simply pressing START to continue Provided the drift rate 1s 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 1s 60 ug minute but we recommend operating upto a maximum of 25 whenever possible If the drift value 15 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 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 t
7. For optimum performance use Aquamax KF Formula A reagent TURBINE LUBRICATING OILS For most Lube Oil applications a sample size of I ml is sufficient However if it is suspected that the water content is above 1 20 then a sample size of 0 2 to 0 5 ml is suggested 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 15 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 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 Powder sampler Aquamax KF ECO v 13 08 HOW TO RUN A 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 ECO with p
8. 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 placed in a low temperature oven at 40 50 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 ECO should be ready for operation within 5 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 Aquamax KF ECO v 13 08 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 f
9. character alphanumeric backlit LCD 90 264V AC 47 63 Hz 12V DC car adapter internal battery 250 x 245 x 120 mm 3 5kg Aquamax KF ECO v 13 08 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 CO titrator is located underneath the glassware case along with the mains power pack Remove all of these items and check that they have arrived undamaged After unpacking your Aquamax KF ECO check that the glassware accessories pack contains Item Description Single Port Cell 1 pce Titration Vessel single port 503047 1 pce Detector electrode 503048 pce Generator electrode 503049 pack PTFE sleeves 5 each size 503051 1 pce Desiccant tube amp cap 503058 pack Injection septa 10 503059 1 pce I ml Gas Tight syringe 503063 1 pce Luer needle Pair 17 amp 19 gauge 503067 1 bottle Molecular sieve 503070 1 pce Stirrer bar 503071 1 pce Funnel 503072 ACCESSORIES pce Mains power pack 401607 GRScientific 6 Aquamax KF ECO v 13 08 AQUAMAX KF TITRATION CELL STEP BY STEP ASSEMBLY INSTRUCTIONS Position titration vessel on Aquamax KF titrator Place the PTFE sleevses on ground glass Joints of each electrode Position electrodes on titration vessel It 15 not necessary to overtighten these screw joints Connect leads to generator and detector electrodes then connect the leads to the titrator Generator electro
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11. 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 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 LANGUAGE The Aquamax can be programmed to show all display prompts and print outs in various languages Use the decimal point key e to select language then press ENTER GENERATOR ELECTRODE The Aquamax 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 O 9 and ENTER 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 Method When this pro
12. R 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 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 ANALYSIS METHOD 2 1 Confirm that Aquamax is in Ready mode 2 Placea suitable amount of sample in the powder sampler p n 503069 and seal with stopper provided 3 Place sampler on balance and tare to zero 4 Press PROGRAM until Calc Mode displayed then select W w 5 Enter the sample weight as 0 0 gram 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 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 Aquamax KF ECO v 13 08 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 in memory This ensures that the displayed result is corrected for any ingress of atmospheric moisture during the titration period
13. ach 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 90 microgram count bl xK W where W weight of sample dissolved gm K total volume of diluent sample volume 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 K 20ml 200 100ul bl microgram count of 100ul injected volume diluent GRScientitic 16 Aquamax KF ECO v 13 08 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 Vx SG where volume of sample ml SG specific gravity 4 Volume V v Result volume microgram count Vx 1 0 where V volume of sample ml This is essentially the same as V SG mode except that the sample S G 1s fixed at 1 0 DELAY TIMES The Aquamax KF ECO has been programmed to accept two d
14. ans 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 1odine so that 1 milligram of water is equivalent to 10 71 coulombs of electricity Combining the coulometric technique with Karl Fischer titration Aquamax 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 502 l2 S02 3C5H5N H20 gt 265 5 5 5 N 0n O SO2 SO4CH3 gt C5 5 Tus a C5H5N ie H 21 2e gt l2 Using the latest pulse current technology and our patented ACE control system Patent No GB2370641 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 please
15. arameters 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 are optional ANALYSIS METHOD l Confirm that Aquamax 15 in Ready mode 2 Flush 1 0ml syringe several times minimum 6 times with sample 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 T Pierce needle through injection septa of titration vessel 1 2 cm 8 Press START 9 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 11 if duplicate result required Aquamax KF ECO v 13 08 Example Powder sample by W w Program the Aquamax with parameters for the analysis ANALYSIS METHOD 1 1 Confirm that Aquamax KF ECO is in Ready mode 2 Placea suitable amount of sample in the powder sampler p n 503069 and seal with stopper provided 3 Weigh sampler 4 Press PROGRAM until Calculation Mode displayed then select W w 5 Enter the sampler weight when prompted by display then press ENTE
16. ases 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 Aquamax KF ECO v 13 08 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 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
17. d allow the instrument to precondition equilibrate microgram count Aquamax XXXX 4 Precondition detector signal titration speed At the end of the precondition period the display will show XXXX 1g Drift Test After the initial drift has been calculated in micrograms of water per minute the Aquamax 15 ready for operation The background drift value will usually slowly decrease with time as the titration vessel becomes drier and more stable Although it 15 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 Aquamax KF ECO v 13 08 PROGRAM FUNCTIONS When the Aquamax ECO displays Ready you can enter titration parameters recall or edit existing methods enter new method files etc by using the PROGRAM ENTER CLEAR and 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 Plus will return to the Ready condition 2 If you have started to enter an incorrect value press CLEAR and the Aquamax KF Plus will display the previou
18. de lead connects to socket marked GENERATOR detector electrode lead connects to socket marked DETECTOR 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 filled It is recommended that the titrator 15 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 Aquamax KF ECO v 13 08 AQUAMAX KF ECO TITRATION CELL Drying Tube assembly Prensa Cus MI Le lt T Ring s IUE Generator Electrode Injection Detector Electrode Titration Vessel Stier Aquamax KF ECO v 13 08 FILLING amp CHANGING REAGENTS The Aquamax KF ECO has been designed to operate with all major coulometric Karl Fischer reagents however optimum performance can be obtained by using Aquamax KF Formula reagents which have been specifically formulated for use with these instruments For most routine applications 100ml of Formula A anode reagent and 5ml of Formula
19. essel 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 titrator is now ready to be switched on Cathode Reagent Anode Reagent Aquamax KF ECO v 13 08 DESCRIPTION Front Panel Keypad Display panel Stirrer speed Rear Panel Power Jack Nominal 18v DC 45w Supply Input Fuse 3 15amp T type Time delay RS232 Standard 4 wire RS232 Input Output RS232 Port 15vDC 40 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 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
20. est 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 Iml syringe and luer needle 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 1 10 ppm or2 ml 10 100 1 or 2 ml 100 500 ppm 0 5orl ml 500 1000 ppm 0 5orl ml 0 001 O90 1 or 2 ml x Oel 1 or 2 ml PLE ee ese 0 5 or 1 ml 0 3 TO 0 5 or 1 ml s0 e 50 0 2 ml above PO m 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 out and contaminate the electrodes requiring more frequent and thorough cleaning of the glassware Th
21. he display will read OVERTITRATION SEE INSTRUCTION MANUAL 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 60 mls of sample to be added For the analysis of most liquid samples e g solvents the Aquamax KF CO 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 A will analyse upto 1 gm water whilst a 5 ml charge of Cathode reagent Formula will analyse upto 250 mg water Considering that the injected sample volume is normally small and also that the analysis 15 usually for the determination of low levels of water these water capacity values are not normally a limiting factor 5 Similar to all other Karl Fischer reagents coulometric reagents will deteriorate when exposed to sunlight and with incre
22. ifferent 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 ECO 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 OO secs 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 TIME For some applications such as certain gas samples or when using the Aquamax KF Plus 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 upto 30 minutes Display shows Min Titration Time 00 mins 15 secs Select required minimum time and press ENTER Aquamax KF ECO v 13 08 END SENSITIVITY The sensitivity of detector signal as the end point is approached can be set from 0 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
23. is problem can be reduced by using Cou Lo Formula A 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 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 Aquamax KF ECO v 13 08 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 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
24. mpt 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 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 EXAMPLE APPLICATIONS Raw Materials Inorganic and organic salts oxides peroxides and carbonates Pharmaceutical Tablets Salves and creams Drugs Vitamins Cosmetics Soaps shower gels and shampoos Dental Care and mouth rinse products Sprays Beverages Dairy and Meat Products Honey Molasses and Sugars Tobacco products Animal Feed Biological Proteins and gelatins Hormones and steroids Dried plant material Vaccines Petrochem Hydrocarbons Lubricating motor oil and greases Hydraulic insulating and transformer oils Mineral oils Plastics Surfactants Paints lacquers and solvents Leather paper and textiles Agriculture Aquamax KF ECO v 13 08 19 Aquamax KF ECO v 13 08 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 small
25. nments All products within the E chem series cover a wide range of applications in areas including food and beverage water environmental power and petrochemical industries E chem electrodes buffers standards We offer a range of combined pH glass epoxy tough and reference electrodes for every application and budget of our electrodes are manufactured in the UK so you are guaranteed Uncompromised quality and fast delivery For accurate pH and conductivity measurements we offer certified standards traceable to NIST and are tested using ISO 17025 accredited method Our conductivity standards have an accuracy of 1 0 and their shelf life is valid regardless of when the bottle was first opened provided good laboratory practice 15 adhered to Our pH Buffers are manufactured to exacting specifications according to NIST with an extended shelf life Temperature dependence data is printed on the labels as are lot numbers and expiry dates GR Scientific 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 Support and repair Maintenance and calibration Training 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 below to discuss the next step For furthe
26. 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 Aquamax KF ECO v 13 08 OTHER PRODUCTS IN THE GR SCIENTIFIC RANGE Aquamax Plus This is the truly versatile model which includes a built in battery and printer to enable use in areas where the power supply is irregular Low Drift Cell twin port glassware results manager software and accessories are supplied as standard As well as being a stand alone instrument the Aquamax KF Plus can be combined with our Oil Evaporator and soon a new 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 Aquamax KF Portable Designed primarily for the oil and power industries this titrator is the only model on the market with a carry handle attached directly to the unit It also features a protective stainless steel cage built in printer and single button operation for water standards analysis using either distilled water or water pellets Specially designed Low Drift Cell twin port glassware avoids the need for PTFE sleeves or grease on the electrodes to seal titration cell from moisture invasion Aquamax KF OPS Workstation Also available is a carry case for transportation in the field and an OPS Workstation which includes everything the
27. r information about any of our products pricing or details about local representatives just contact Telephone 44 0 1525 404747 Fax 44 0 1525 404848 Email info grscientific com Web www grscientific com GRScientific 20
28. rom 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 Call G R Scientific Ltd or your local dealer for suggestions on sampling technique for your application E mail info Q grscientific com TEL 44 1525 404747 FAX 44 1525 404848 INSTRUMENT CARE Although the instrument casing 1s 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 36 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
29. s excellent stability for non aqueous titrations microTAN OPS Workstation Everything you need in one footprint and transportable The MicroTAN workstation is an organised workspace containing all equipment and chemicals required to run your samples MicroTAN unit chemicals and accessories are contained in a sturdy outer case with a firm foam lining in an ergonomic arrangement Optional accessories include a bottle top dispenser for dedicated dispensing of titration solvent and a mini thermal printer TitraMax Titrator Is a simple versatile yet robust potentiometer for measuring TAN TBN mercaptan sulphur and analysis of petroleum products Pre programmed methods that conform to ASTM standards and an interchangeable burette system with intelligent volume recognition are key features of the Titramax In addition each unit is supplied with bespoke UK manufactured electrodes for optimum performance and reproducible results GRScientific 28 Aquamax KF ECO v 13 08 E chem pH amp Conductivity meters The E chem range of pH conductivity benchtop meters have been developed to provide cost effective robust and simple to use solutions for your needs The E512 pH meter offers research grade specifications with a comprehensive range of features and functions ideal for general laboratory QC and GLP based applications Producing rapid and reliable results that are accurate and reproducible are paramount in all field and laboratory enviro
30. s required Cathode reagent Formula C 15 supplied in single shot 5ml vials which have safety 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 three year parts and labour 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 is 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 ground connection These units are sealed and conform to CSA LR64459 UL listings and CE requirements Aquamax KF titrators require a low voltage 15V input to the electronic control circuitry The moulded plastic casing of the instrument also provides additional insulation Aquamax KF ECO v 13 08 PRINCIPLE OF MEASUREMENT Karl Fischer titration 1s simply a me
31. sed 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 Aquamax KF ECO v 13 08 CALCULATION MODE The Aquamax 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 out 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 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 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 e
32. sly 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 JM MENU LIST sample ID Number upto 8 digits Result Format ug ppm mg kg or water Calculation Mode V SG W W W K or V v start Delay Time upto 30 minutes Min Titration Time upto 30 minutes End Sensitivity 0 9 seconds 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 Aquamax KF ECO v 13 08 PROGRAMMING FLOW CHART 6 6 4 5 4 4 6 06 e c c c c e 2 t 1 lt e gt gt UV3 19 e e eee e e ee gt gt 4 e gt e e enieA 4 4 lt e e MHulN3 _ gt gt gt gt gt gt gt suondo JO 5 0 1 lt e 4 Auvdlo WvVHOOHd H3IN3J lt 6 0 5 lt
33. ss ENTER and CLEAR to return to Ready SAMPLE ID NUMBER Press PROGRAM Display will show Key upto 8 numbers 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 Display will show Result Format PROGRAM Hg Results can be selected in ppm mg kg or 96 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 e 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 4o the instrument will prompt you for the necessary calculation mode and data values Result Format Calculation Mode 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 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 u
34. titrator will see it and 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 GRScientific 10 Aquamax KF ECO v 13 08 SETTING THE DATE AND TIME 1 Switch on the Aquamax ECO and wait for it to display the following Aquamax KF ECO Press START 2 Hold down the START key until the Aquamax displays Set Date Time DD MM YYYY 55 3 Usethe decimal point key to move the cursor across the screen 4 Usethe numerical keys to set alter the required number 5 When completed press the ENTER key to save the changes and exit Aquamax KF ECO v 13 08 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 E d ur dim Aquamax KF ECO Press START If required adjust the stirrer speed using the black toggle switch on the front of the instrument 7 Press START an
35. user needs such as syringes standards reagents etc all in one footprint for ultimate efficiency Aquamax KF Oil Evaporator For combined operation with the Aquamax KF Plus titrator to determine water content of additives lube oils base oils automatic transmission fluids hydrocarbon solvents and other petroleum products Aquamax KF Solids Evaporator For combined operation with the Aquamax KF Plus titrator to determine water content of solids such as plastics nylons paper powders etc Aquamax KF ECO v 13 08 Aquamax KF Volumetric An adaptable titrator capable of titrating with superior accuracy and precision even for samples with low moisture content Dual syringes enable the operator to dispense titrant and standard automatically eliminating cell opening which may introduce moisture to the system The Aquamax KF Volumetric comes equipped with a solvent handling system to reduce cell conditioning time and can be connected directly to your laboratory balance via serial interface Choose from four pre programmed methods or develop a custom method for almost any application or sample type microTAN Zitrator An innovative micro system for measuring Total Acid Number which enables the user to save up to 7596 of organic solvent per sample analysis compared to standard potentiometers Supplied with an optimized titration vessel and micro combination electrode that regenerates to optimum efficiency in minutes and offer
36. visit our website www grscientific com SCHEMATIC OF TYPICAL TITRATION ELECTROLYSIS CURRENT DETECTOR SIGNAL Technical Specifications Titration Method Electrolysis Control Titration vessel End Point Detection End point indication Measuring range Moisture range Max sensitivity Max titration speed Max current Drift compensation Precision Start delay time End delay time Calculation modes user programmable Display format Method storage Sample ID number Stirrer speed Languages Data outputs Removable Data storage Data Entry Display Power supply Dimensions Weight Aquamax KF ECO v 13 08 Aquamax KF ECO Coulometric Karl Fischer titration Patented ACE control system GB2370641 Robust single injection port glassware design AC polarisation Visual display print out acoustic beep Possible lug 200 mg water Typical lug 10mg water Ippm 100 water 0 lug 2 24 mg per minute 400 ma Automatically controlled 10 100ug 3ug 100ug I1mg 3ug above Img 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 ug mg kg ppm 96 10 user programmable methods stored plus multi method via pc link User programmable Microprocessor controlled Multi languages user selectable USB and RS232 ports Flash drive memory stick 15 key touchpad 40
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