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A subsidiary ofKARL FISCHER REAGENTS

What is the Karl Fischer Method?As shown in Formula (1) below, the Karl Fischer method uses Karl Fischer reagent, which reacts quantitativelyand selectively with water, to measure moisture content. Karl Fischer reagent consists of iodine, sulfur dioxide,a base and a solvent, such as alcohols.I2+SO2+3Base+ROH+H2O2BaseHI+BaseHSO4R 1As described below, this method can be used in both volumetric and coulometric titration systems.ElectrolysiselectrodesAnodechamberDrying tubeCathode chamberSample injection capSample injection portDetection electrodeDrain cockRotor DiaphragmCoulometric TitrationWith coulometric titration, the sample is added to anelectrolytic solution, the main constituents of which areiodide ions, sulfur dioxide, a base, and a solvent (suchas alcohol). Electrolytic oxidation causes the productionof iodine, as shown inFormula (2), resulting in animmediate Karl Fischer reaction.2I - 2eI2 2According to Faraday's laws, the iodine is produced inproportion to the quantity of electricity. This means thatthe water content can be determined immediately fromthe coulombs required for electrolytic oxidation.1mg of water = 10.71 CoulombsAs shown in Figure 1, two types of coulometricreagents are required: an anolyte, which is placed in theanode chamber of the electrolysis cell, and a catholyte,which is placed in the cathode chamber. Coulometricreagents do not need assessment. Another advantage isthat they can be used repeatedly.Figure1Electrolysis cell of Coulometric Moisture MeterSample injection portDetection electrodeControl/display systemDetectionunitData processingunitControl unitMeasurement systemAutomaticswitchingvalveTitrationPiston buretPulse motorVolumetric TitrationA dehydrating solvent suitable for the sample is placedin a flask. Titrant is used to remove all moisture fromthe solvent. The sample is then added. Titration iscarried out using a titrant, the titer (mgH2O/mL) ofwhich has previously been determined. The moisturecontent of the sample is determined from the titrationvolume (mL). The end point is detected using theconstant-current polarization voltage method. Figure 2shows the components of typical commerciallyavailable automatic volumetric titration system.Titration bath flaskTitration nozzleFigure2Volumetric Moisture MeterMitsubishi Chemical Group API Corporation started inOctober, 2002, and succeeded to the KF reagents business.We provide excellent reagents, services and technicalsupport for our customer satisfaction.Our KF reagents, AQUAMICRON ® is manufactured atMitsubishi Chemical Corporation Kashima Plant whichhave quality systems that adhere to the requirements of ISO9001 and have recieved third party accreditation.AQUAMICRON ® is a registered trademark of Mitsubishi Chemical Corporation.1

Scope of Applications for Karl Fischer MethodThe Karl Fischer method can be used with a wide range of substances. However, the method depends on a kindof iodometry based on t he reaction between the Karl Fischer reagent and water. The results will therefore show apositive error if the sample includes substances that react with iodine, and a negative error if the sample includessubstances that produce iodine by oxidizing iodide compounds. The following tables list substances that can betitrated directly with Karl Fischer reagents, substances t hat cannot b e titrated directly but can be titrated bymeans of adjustments based on appropriate chemical reactions or processes, and substances t hat react with KarlFischer reagents and are therefore unsuitable for direct titration. Even if a substance cannot be titrated directly,its moisture content can be measured by indirect means, such as the water vaporization method. Please contactmcckf.com for further information.Compounds that can be titrated directlyOrganic compoundsHydrocarbons(saturated, unsaturated compounds)Alcohols, Polyhydric alcohols, Phenols, EthersInert ketones(diisopropyl ketone, et al)Inert aldehydes(formaldehyde, chloral, et al)Organic acids, Hydroxylic acids, amino acidsAcid anhydridesEsters, Lactones, Inorganic acid estersAmines(

Coulometric ReagentsThere are two types of coulometric reagents: the anolyte (generating solution),which is placed in the anodechamber of the electrolysis cell, and the catholyte (counter electrolyte), which is placed in the cathode chamber.There are also special anolyte for use with ketones, lower carboxylic acids and silicone oils. AQUAMICRON ®can be used in coulometric moisture measurement systems sold by various companies, and it has a worldwidereputation for excellent performance.AQUAMICRON ® SeriesProduct name Code No.Specification Package Main solvent UseAQUAMICRON ®AXIAXAX01ASAKXCXUFLSXAMIXAMAXAMA01SAMAAKXCXUFLSMoisturemaximum 0.15mgH2O/mLMoisturemaximum 0.15mgH2O/mLMoisturemaximum 0.15mgH2O/mLMoisturemaximum 0.6mgH2O/mLMoisturemaximum 0.15mgH2O/mL500mLglass bottle100mLglass bottle500mLglass bottle500mLglass bottle5mL ampulex 10/case500mLglass bottleMethanol,PropylenecarbonateFor OilsMethanol, ChloroformNaphtha, Gasolone, Diesel oil, Electrical insulation oil, etc.Propylenecarbonate,DiethyleneglycolemonoethyletherMethanolMethanol,Propylenecarbonate*AXI For frit or fritless type cell, equivalent to FLS*AXI, AX & AX01For General-useOrganic solvents, Inorganic chemicals, Oiles,Petroleum products, Virious kind of gases, etc.For KetonesKetones. Silicone oils. Low carboxylic acids, etc.CatholyteBoth AX and AS and AKX available to combine withFor fritless type cellOrganic solvents, Inorganic gases, etc.AQUAMICRON ® AXI/CXU or AX/CXUUse:General samplesCharacteristics:Minimal environmental contaminationWide range of applicationsHigh quality, high performanceEasy to useAQUAMICRON ® AS/CXUUse:General samplesCharacteristics:Wide range of applicationsHigh quality, high performanceEasy to useAQUAMICRON ® AKX/CXUAQUAMICRON ® AXI or FLSDoes not include carbon tetrachloride or chloroformSuitable for petroleum productsCan be used with moisture vaporization method(When using AQUAMICRON ® AXI or AX in a moisture vaporization method, replenish thevaporized portion with methanol.)Excellent reputation for accurate moisture measurement and end-point stability Approximately800mg of moisture can be measured per 100mL of AQUAMICRON ® AXI or AX, and approximately150mg per 5mL of AQUAMICRON ® CXUThese products can be used in the existing coulometric moisture measurement system.Especially suitable for oils, petroleum productsExcellent reputation for accurate moisture measurement and end-point stability.Approximately 800mg of moisture can be measured per 100mL of AQUAMICRON ® AS, andapproximately 150mg per 5mL of AQUAMICRON ® CXU.These products can be used in the existing coulometric moisture measurement system.Use:Ketones, lower carboxylic acids, some aldehydes (aromatics)Characteristics:Minimal environmental contamination Does not include chloroform or methyl cellosolveWide range of applicationsSuitable for ketones, lower carboxylic acids and some aldehydesHigh quality, high performance Accurate moisture measurement, good end-point stabilityApproximately 300mg of moisture can be measured per 100ml of AQUAMICRON ® AKX, andapproximately 100mg per 5mL of AQUAMICRON ® CXU (when used with AQUAMICRON ®AKX).Easy to useThese products can be used in the existing coulometric moisture measurement system.Use:Suitable for alcohols, esters, benzene, toluene, inorganic gases, etc.Characteristics:Easy to useAQUAMICRON ® AXI or FLS is a single-solution type reagent. It should be used in single-solutionelectrolytic cells without diaphragm, fritless type cell.Can be used with moisture vaporizati on method(When using AQUAMICRON ® AXI or FLS in amoisture vaporization method, replenish the vaporized portion with methanol.)Easy maintenanceCeramic diaphragm is not used, therefore it is easy to maintain electrolytic cell in good condition.3

Examples of sample measurement using AQUAMICRON ® AXI/CXU or AX/CXU.Sample NameAQUAMICRON ® AXI/CXUAQUAMICRON ® AX/CXUMeasured Moisture RSD, % Measured Moisture RSD, %TolueneHexaneEthyl acetate1-PropanolEthylene glycolN-Methyl pyrrolidoneForm amide82.41min33.80.7min2271.3min8341.5min2271.3min6701.6min5361.5min0.270.50.521.20.680.30.6184.033.92278312226715331.21.70.190.61.90.260.42Solid water standard(KF-oven method)3.76%14-17min0.663.76%14-15min1.5Instrument: CA-200 Moisture Meter (Mitsubishi Chemical Analytech) Sample size: 0.7-1.7g, 0.08g at KF-oven methodReagent: AQUAMICRON ® AXI or AX 100mL, AQUAMICRON ® CXU 5mLAverage value for n=3 Unit: ppm unless noted as %Examples of sample measurement using AQUAMICRON ® AKX/CXU.Sample NameAQUAMICRON ® AKX/CXUMeasured MoistureFormic acidunable to measureAcetic acid153Propionic acid659Acetone0.166%Acetyl acetone270Methyl ethyl ketone771Methyl isobuthyl ketone626Cyclohexanone3303-Phenyl propion aldehyde0.226%Chloral249Benzaldehyde483Salicylaldehyde0.116%Instrument: CA-200 Moisture Meter (Mitsubishi Chemical Analytech)Reagent: AQUAMICRON ® AKX 100mL, AQUAMICRON ® CXU 5mLAverage value for n=3 Unit: ppm unless noted as %Sample size: 0.5-1.0gExamples of sample measurement using AQUAMICRON ® AXI or FLSSample NameAQUAMICRON ® AXIAQUAMICRON ® FLSMeasured Moisture RSD, % Measured Moisture RSD, %MethanolEthanolTolueneHexaneEthyle acetateMethyl cellosolveEthylene glycolAcetonitrileN,N-Dimethyl formamide91.829946.72914.216897.8948371.270.794.554.031.51.137.471.850.0593.431049.730.714517296.395.18510.950.261.552.680.461.493.163.590.32Instrument: CA-200 Moisture Meter with single solution type electrode (Mitsubishi Chemical Analytech) Sample size: 0.5-2.0gReagent: AQUAMICRON ® AXI or FLS 100mL Average value for n=3 Unit: ppm unless noted as %Sample Name AQUAMICRON ® AXI AQUAMICRON ® FLS(KF-oven method) Measured Moisture RSD, % Measured Moisture RSD, %Polyethylene terephthalatePolystyreneNylon6,60.46%2452.35%0.221.180.270.46%2382.42%2.62.51.01Instrument: CA-200 with single solution type electrode + VA-200 (Mitsubishi Chemical Analytech)Sample size: 0.05-0.2g at KF-oven methodReagent: AQUAMICRON AXI or FLS 150mL Average value for n=3 Unit: ppm unless noted as %4

Volumetric ReagentsThe items required for volumetric titration are a Karl Fischer titrant and methanol or a dehydrated solvent (usedto dissolve or disperse the sample).AQUAMICRON ® offers a wide range of products suitable for measuring the moisture content of various samplesat every levels. Users can select a solvent that is suitable for the samples based on the following tables.SS-Z Series (pyridine-free and chloroform-free type)AQUAMICRON ®Product name Code No. Specification PackageTitrant SS-ZSolvent GEXSolvent OLXSolvent OLIISolvent KTXSolvent SUSSZ10MSSZ30MSSZ50M*SSZ50LGEXOLXOL2KTXSSUTiter0.7-1.2mgH2O/mLTiter2.5-3.5mgH2O/mLTiter4.5-5.5mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.5mgH2O/mLMoisturemaximum 0.3mgH2O/mLMoisturemaximum 0.5mgH2O/mLMoisturemaximum 0.2mgH2O/mL500mLglass bottle500mLglass bottle500mL, *1Lglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottleMain solventDiethyleneglycolemonoethyletherDiethyleneglycolemonoethyletherDiethyleneglycolemonoethyletherMethanolHexanol,EthanolChloroform,MethanolPropylenecarbonate,DiethyleneglycolemonoethyletherFormamide,MethanolFor General-useLow moisture content SamplesFor General-useFor General-useHigh moisture content SamplesFor General-useOrganic solvents, Inorganic chemicals, Agriculturalchemicals, Pharmaceuticals, Fertilizers,Detergents, Foodstuffs, etc.For OilsNaphtha, Gasolone, Diesel oil, Electrical insulationoil, etc.For Oils and FatsNaphtha, Gasolone, Diesel oil, Heavy oil, Electricalinsulation oil, Oils and Fats(Hardened oil,Margarine, etc.),etc.For KetonesKetones, Silicone oils, Acetic and other lowercarboxylic acids, aldehydes(exceptacetaldehydes),etc.For SugarsSugars, Proteins, Gelatine, Additives, Animal feeds,etc.When using a moisture vaporization method, mix Solvent GEX with propylene glycol(PG) in a 3:1 ratio (e.g. 90mL of GEX + 30mL of PG).When using Solvent KTX, it will be needed to make proper adjustments to the parameters. Please contact a manufacturer of the instruments.An addition of 3g of salicylic acid enables the time for dehydration to get shorter at the first measurment in combined use of 50mL of Solvent SU.UseSS Series (pyridine type)AQUAMICRON ®Product name Code No. Specification PackageTitrant SSSolvent MLSolvent MSSolvent CMSolvent CPSolvent PPSolvent PESolvent FMSolvent MEGKS10MGKS30MGKS100MGMLGMSGCMGCPGPPGPEGFMGMETiter0.7-1.2mgH2O/mLTiter2.5-3.5mgH2O/mLTiter8-12mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.3mgH2O/mLMoisturemaximum 0.5mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.2mgH2O/mLMoisturemaximum 0.2mgH2O/mL500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottle500mLglass bottleMain solventChloroform,PyridineChloroform,PyridineChloroform,PyridineMethanolMethanol, PyridineChloroform,MethanolChloroform,PropylenecarbonatePyridine,Propylene glycolePyridine,Ethylene glycoleFormamide,MethanolMethanol,Ethylene glycoleFor General-useLow moisture content SamplesFor General-useFor General-useHigh moisture content SamplesFor General-useOrganic solvents, Inorganic chemicals, Agriculturalchemicals, Pharmaceuticals, Fertilizers,Detergents, Foodstuffs, etc.For General-useOrganic solvents, Inorganic chemicals, Agriculturalchemicals, Pharmaceuticals, Fertilizers,Detergents, Foodstuffs, etc.For OilsNaphtha, Gasolone, Diesel oil, Heavy oil, Electricalinsulation oil, Oils and Fats(Hardened oil,Margarine, etc.),etc.For KetonesKetones, Silicone oils, Acetic and other lowercarboxylic acids, aldehydes(exceptacetaldehydes),Anilines, etc.For AldehydesAcetaldehydes, propionaldehydes, Butyraldehydes,etc.For KetonesKetones, Silicone oils, Acetic and other lowercarboxylic acids, aldehydes(exceptacetaldehydes),Anilines, etc.For SugarsSugars, Proteins, Gelatine, Additives, Animal feeds,etc.For VaporizerGaseous samples, Nitrogen, etc.When using a moisture vaporization method, mix Solvent MS with propylene glycol(PG) in a 3:1 ratio (e.g. 90mL of MS + 30mL of PG).An addition of 3g of salicylic acid enables the time for dehydration to get shorter at the first measurment in combined use of 50mL of Solvent FM.Use5

Examples of sample measurement.Apparatus:Volumetric Moisture Meter KF-100 (Mitsubishi Chemical Corporation)General samplesSample NameMethanolEthanolIsopropanolEthylene glycolPropylene glycolSampleAmount(g)4.03.84.05.55.0SS-Z 5mgSolvent GEX627ppm524ppm227ppm237ppm167ppmSS 3mgSolvent MS622ppm521ppm228ppm236ppm164ppmComposite 5mgSolvent GEX630ppm530ppm226ppm242ppm164ppmAminesSample NameDiethanolamineMonoethanolamineDi-n-buthylamineSampleAmount(g)3.01.80.8SS-Z 5mg(GEX+Salicylic acid)0.126%0.291%0.221%SS 3mg(MS+Salicylic acid)0.128%0.301%0.218%Composite 5mg(GEX+Salicylic acid)0.128%0.302%0.224%OilsSample NameSalad oilOlive oilSampleAmount(g)9.510SS-Z 5mgSolvent OLX362ppm409ppmSS 3mgSolvent CM359ppm396ppmComposite 5mgSolvent for Oil356ppm401ppmSugarsSample NameInstant coffeeHoneyCream powderSampleAmount(g)0.10.020.1SS-Z 5mgSolvent SU2.23%17.3%2.94%SS 3mgSolvent FM2.12%17.2%2.94%Composite 5mgSolvent SU2.23%17.7%2.94%KetonesSample NameAcetoneMethyl ethyl ketoneAcetylacetoneCyclohexanoneSampleAmount(g)3.92.24.70.8SS-Z 5mgSolvent KTX0.162%610ppm461ppm755ppmSS 3mgSolvent CP0.167%619ppm465ppm730ppmComposite 5mgSolvent for Ketone0.173%678ppm525ppm890ppmGeneral samplesSample NameTolueneXyleneChloroformSampleAmount(g)4.64.115SS-Z 1mgSolvent GEX139ppm168ppm44ppmComposite 1mgSolvent GEX139ppm170ppm44ppmOilsSample NameTurbine oilInsulating electric oilSampleAmount(g)8.68.9SS-Z 1mgSolvent OLX41ppm39ppmComposite 1mgSolvent for Oil38ppm38ppmSS-Z seriesSS series6

Water StandardsReliable reference materials are necessary to standardize reagents, and to check the titrator according tothe requirements of ISO, ASTM, JIS guidelines.AQUAMICRON ® offers a series of excellent standards that have advantages: low toxicity, easy to use andto manage. To ensure the high quality, all of our Water Standards are manufactured under stricted controland accurately measured using validated procedures traceable to the international prototype at the BIPMin France.Also AQUAMICRON ® Liquid Water Standard (AWS01,02,10,100) is directry traceable to NIST SRM 2890.Liquid Water Standard (with Test Certification)Product name Code No. Specification Package Main solvent UseAQUAMICRON ®Water Standard 0.1AWS01Titer0.1±0.01mgH2O/g5mL ampule×10/casePropylenecarbonateFor checking the accuracy of thecoulometric moisture meterAQUAMICRON ®Water Standard 0.2AWS02Titer0.2±0.01mgH2O/g5mL ampule×10/casePropylenecarbonateFor checking the accuracy of thecoulometric moisture meterAQUAMICRON ®Water Standard 1AWS10Titer1±0.05mgH2O/g5mL ampule×10/casePropylenecarbonateFor checking the accuracy of thecoulometric moisture meterAQUAMICRON ®Water Standard 10AWS100Titer10±0.5mgH2O/g8mL ampule×10/casePropylenecarbonateFor determination of Karl Fischerreagent titerSolid Water Standard (with Test Certification)Product name Code No. Specification Package Main solvent UseAQUAMICRON ®Solid Water StandardSWSMoisture3.83±0.1%10gglass bottlePotassium tertaratehemihydrateFor evaluation a moisture meter witha water vaporizerCheck SolutionProduct name Code No. Specification Package Main solvent UseAQUAMICRON ®Check Solution PGCHPMoisture4.0±0.2mgH2O/mL100mLglass bottlewith septum capPropylenecarbonateThe end-point adjustment solution can beused with both AX and AXK. It can alsobe used for day-to-day management ofcoulometric moisture mesurementsystems.Liquid Standard for assess titerProduct name Code No. Specification Package Main solvent UseAQUAMICRON ®Standard Water/MethanolGMW202.0±0.04mgH2O/mL250mLglass bottleMethanolUsed to assess titer of Karl Fischerreagents (3-10mgH2O/mL). Also can beused to reverse titration.Tokyo Head Office2-3-4, Nihonbashi, Chuo-ku, Tokyo 103-0027, JapanTelephone: 81-3-5205-0632 Facsimile: 81-3-5205-0641Email: mcckf@cc.m-kagaku.co.jpAn affiliate ofMay.2013