石油产品中水分含量检测方案

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NKVX-01521 KEMApplication Note Petroleum Water Content of Petroleum ProductsVolumetric titration (direct method) byKarl Fischer Moisture Titrator JIS K0113 ASTM E 203 Standard JIS K 0068 ISO 760 JIS K2275 Hydranal manual 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 Products 4)Hydranal manual published by Riedel de Haen 5))ISO 760：1978 Determination of Water-Karl Fischer method (General method) 6))ASTM E 203-96 Standard Test Method for Water Using Volumetric Karl FischerTitration 3.Cautions in measurement 1)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. Http：//www.shxf17. com 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 XF - Blank )/ (Wt1 - Wt2))×0.1 Data 工Titration volume(mL) F Reagent factor Blank Blank level (mg) Wt1 ：Sample + Syringe weight (g) Wt2 Empty syringe (g) 上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 200072 Http：//www.shxf17. com 9.Parameters -Titration parameter MKA-610 MKA-520 Method No. 1 Titrationl Method MKS-500 Titrationl 1 Method Driect Titrationl Titr Mode Normal Titr.Speed 3 Titr.mode Normal Titr Buret No. 1 End Time 30s t(stir) 0s End Time 30 s Final Vol. 0.01 mL t(wait) 10 s Final Vol. 0.01mL Detector Mode Oil t(max) 0 s Titr.Speed 3 t(stir) 0s t(interval) 0s Detector Mode 2 t(max) 0s Max.volume 10mL t(stir) 0s Drift Titr. On Titr.bur.No. 1 t(wait) 10s Max.Volume 10mL Dose mode Off t(max) 0s Drift Titr On Controll Start Manual End time 30 s Max.Volume 10 mL Final vol. 0.01mL Dose mode Off Titr.speed 3 Oven Off Detect.mode 2 Drift titr. On Start mode Manual End level 75mV Samp.time 5s Stir.speed 3 MKA-610 MKA-520 MKS-500 Calculationl 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一 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 refining crude 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 cost performance ●。Low cOSt and highperformance model ·Dispenser easy to deliverand discharge extractingmedium ·User friendly easy tooperate ·Easy key entry by touchpanel on 8-inch large colorLCD ·One touch burette setup ·Two measurements inparallel at a time ·Buretteenozzlee made ofPTFE， standard supplied2 types (regular andanti-diffusion) Both potentiometric andKarl Fischer moisturetitration (coulometricvolumetric) canperformed at a time K-M KYOTO ELECTRONICSMANUFACTURINGCO.，LTD. Overseas Division： Yamawaki Bldg 9F，4-8-21 Kudan-minami，Chiyoda-ku， Tokyo 102-0074 JAPAN Phone：+81-3-3239-7333， Fax： +81-3-3237-0537 Head Office： 56-2 Ninodan-cho，Shinden，Kisshoin，Minami-ku，Kyoto 601-8317 JAPAN Phone：+81-75-691-4122， Fax： +81-75-691-9961 URL： http：//www.kyoto-kem.com 上海旭风科学仪器有限公司 上海市闸北区万荣路388弄17号904室 20007 2 Http：//www.shxf17. com Tel： 021-66581985，63172460 Fax： 021-66581986 周峰13916388882 zhou-feng1027@163.com 上海旭风科学仪器有限公司 上海市闸北区荣路 el： Fax： 周峰 zhou-fengcom