石油产品中水分含量检测方案

KMApplication Note NKVX-01521 Petroleum Water Content of Petroleum Products Volumetric titration (direct method) by Karl Fischer Moisture Titrator Standard JIS K0113 ASTM E 203] D1744 JIS K0068 ISO 760 JIS K2275 Hydranal rmanual 1.Abstract Moisture titration using Karl Fischer reagent ispopularly practiced waterdetermination worldwide as the most reliable method. The procedure is adopted inmany official standards as test method specified in ISO，ASTM， DIN， BS and JIS.The test conducted this time is an example of volumetric moisture titration formeasurement of water content in petroleum products. For the extracting medium，we use solvent CM. Moisture titration by this way can measure the followingpetroleum products： Crude oil， Heavy oil， Lubricant and Mineral oil. 2.Reference 1) JIS K 0113-2005： Standard Test Method by Potentiometric， Amperometrtic，Coulometric and Karl Fischer Titration 2)JIS K 0068-2001： Test Method for Water Content in Chemical Products 3))JIS K 2275-1996： Moisture Test Method for Crude Oil and Petroleum Products4Hydranal manual published by Riedel de Haen 5)ISO 760：1978 Determination of Water-Karl Fischer method (General method) 6))ASTM D 1744-13 Standard Test Method for Determination of Water in LiquidPetroleum Products by Karl Fischer Reagent B.Cautions in measurement )In order to refrain from the effect of ambient humidity， the test must beconducted in a well air-conditioned room. 2) Utmost care must be taken in handling a sample with trace amount of water init. 3) Obtain the factor of Karl Fischer reagent using the solvent in advance. 4.Post-measurement care After the reagent in flask is drained out and the electrode is cleaned， keep thetitration flask with solvent in it. 5.Test equipment Main unit： Karl Fischer moisture titration volumetric system Electrode： Twin platinum electrode for KF titration 6.Reagent Reagent Hydranal Composit 5(Riedel de Haen) Solvent ： Extracting medium CM(for oils) (Hayashi Chemicals) 7.Measurement procedure -Pretreatment- 1) Prepare approximately 30mL extracting medium in the titration cell. 2) Dehydrate the measuring cell by performing pretitration in advance. Measurement- 1) Sample 0.1 ~2.5g of test oil in a 5mL syringe. 2) Weigh the syringe on a balance of which resolution is to the nearest 0.1mg. 3) Discharge the sample into titration cell to dissolve in solvent. 4) Press Start key of titrator. 5) Weigh the syringe of above 3). 6) Enter Wt1 with weighed above 2) and Wt2 with 5). 7) The endpoint is automatically detected， from which water content can be obtained. 8.Formula Moisture(%)=((Data × F - Blank )/ (Wt1一Wt2))x0.1 Data Titration volume (mL) F Reagent factor Blank Blank level(mg) Wt1 Sample +Syringe weight (g) Wt2 Empty syringe(g) 上海市中山西路2366弄1号203室 网址： http：//www.kem-china.com 9.Parameters Titration parameter-MKA-610 MKA-520 MKS-500 Method No. 1 Titration Titration Method 1 Method Driect Titrationl Titr Mode Normal Titr.Speed 3 Titr.mode Normal Titr Buret No. 1 End Time 30 s t(stir) Os End Time 30s Final Vol. 0.01 mL t(wait) 10 s Final Vol. 0.01 mL Detector Mode Oil t(max) 0s Titr.Speed 3 t(stir) 0s t(interval) 0s Detector Mode 2 t(max) 0s Max.volume 10 mL t(stir) 0s Drift Titr. On Titr.bur.No. t(wait) 10 s Max.Volume 10 mL Dose mode Off t(max) 0s Drift Titr On Controll Start Manual End time 30 s Max.Volume 10 mL Final vol. 0.01 mL Dose mode Off Titr.speed 3 Oven Off Detect.mode 2 Drift titr. On Start mode Manual End level 75 mV Samp.time 5s Stir.speed 3 MKA-610 MKA-520 MKS-500 lCalculationl Calc.type Sample Blank No. 1 Calc.No. 2 Unit % Decimal 3 Fraction Half adjust Drift comp. Off Evaluation Off Calculation Calc. 2Unit % Weight Variable Calculationlg->% -Measurement resultsS-二 Sample name Sample(g) Extracting medium Water content mg % Crude oil 1.5023 Solvent CM 5.41 0.36 Heavy oil 1.0805 Solvent CM 27.88 2.58 Lubricant 2.419 Solvent CM 12.92 0.534 Mineral oil 0.0694 Solvent CM 40.43 58.26 10.Summary By refiningcrude oil， we obtain not only gasoline， light oil，kerosene but othervarious products including propane， naphtha，jet fuel， heavy oil and asphalt. Theseare called coproducts， which are vital for our daily life. The test sample in this application dissolves in solvent CM， which makes moisturetitration performed with ease. Stable measurement of water content is assured by Karl Fischer moisture titration.Water content of petroleum products can be precisely measured by any of thefollowing models made by Kyoto Electronics Manufacturing Co.，Ltd.(KEM). 【MKA-610】 【MKA-520】 【 MKS-500】 Awarded Product ofSupreme Technology fromKyoto City ·Compact and costperformance ●。Low cost and highperformance model ·User friendly easy tooperate . Easy key entry by touchpanel on 8-inch large colorLCD ·Dispenser easy to deliverand discharge extractingmedium 。One touch burette setup · Two measurements inparallel at a time Burette nozzle made ofPTFE， standard supplied2 types(regularandanti-diffusion) Bothi potentiometric andKarl Fischer moisturetitration (coulometric‘volumetric ) canperformed at a time KEM KYOTO ELECTRONICSMANUFACTURING CO.，LTD. 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