检测样品 原油
检测项目 理化分析
方案详情文
智能文字提取功能测试中
APAT-0239en京都電子工業株式会社KYOTO ELECTRONICSMANUFACTURING CO.,LTD. APAT-0239er Application Note Bromine numbers of petroleum distillates andaliphatic olefins by potentiometric titration IndustryChemicalsInstrumentAutomatic potentiometric titratorMeasurement methodPotentiometric titrationStandardsASTMD1159-07 1. Scope Caution This measurement is performed using organic solvents and strong acids. When youfollow this application note, wear masks, gloves, protective equipments, etc. Theautomatic potentiometric titrator should be installed and used in fume hoods wherelocal exhaust ventilation is possible. The bromine number is the number of grams of bromine added to carbon-carbon unsaturatedbonds in 100 g of petroleum fraction, expressed as gBr2/100 g, and is measured as a valueindicating the number of unsaturated components contained in petroleum products. Thisapplication shows an example of bromine number measurement based on ASTM D1159-07(Note1). The measurement sample was prepared by dissolving cyclohexene in dichloromethane to aknown concentration (approximately 30 gBr2/100 g) (reaction formula (1)). 2.Precautions 1) To suppress side reactions during titration, cool the solution to 5 ℃ or less duringmeasurement. 2) Before starting measurements each day, purge the titrant several times between the reagentbottle and the burette to equalize the titrant concentration, then discharge about 10 mL of thetitrant between the burette and the titration nozzle. 3. Apparatus Main unit Automatic potentiometric titrator (Preamplifier POT)Electrode Blank test and measurement Twin platinum electrode (M-511)Temperature compensation electrode (T-171) 4.Reagents Titrant 0.25 mol/L Bromide-bromate standard solution (potassium bromide andpotassium bromate) Dissolve 51.0 g of potassium bromide (KBr) and 13.92 g of potassiumbromate (KBrO3) each dried at 105 ℃ for 30 min, in pure water and dilute to1L. Titration solvent A solution consisting of a mixture of 714 mL of acetic acid, 134 mL ofdichloromethane, 134 mL of methanol, and 18 mL of sulfuric acid (1+5). 5. Procedure -Preparation of sample solution- 1) Add 10 mL of dichloromethane into a 50 mL volumetric flask. 2) Add around 4-5 g of cyclohexene into the flask and measure the mass of it (approximately30 gBr2/100 g). 3) Add dichloromethane to the mark of the flask and mix it. -Setting of the constant current value- 1) Cool the solution to 0-5 ℃, then press [Calibration] button. 2) Set Channel/Unit to“Ch3/Pol”. 3) Press [Details] button and set as follows.Calibration Mode CurrentPolar Current 10.00 uA 4) Immerse the twin platinum electrode in titration solvent and perform calibration. -Blank test- 1) Collect 5 mL of dichloromethane and mix with 110 mL of the titration solvent. 2) Cool the solution to 0-5C, then titrate with 0.25 mol/L Bromide-bromate standard solution -Measurement- 1) Collect 5 mL of the sample solution* and mix with 110 mL of titration solvent. .2) Cool the solution to 0-5℃, then titrate with 0.25 mol/L Bromide-bromate standard solution . *1 To avoid phase separation, adjust the sample collection volume so that the titration volumeis less than 20 mL. 6. Calculation Bromine number (gBr2/100 g)=(EP1-BL1)×TF×C1×K1×R/S EP1 Titration amount (mL) BL1 Titration amount (mL) of blank test=0.0377(mL) Factor of titrant = 1.005 Concentration conversion coefficient=39.95 Unit conversion factor =0.1 0c Sample size=4.6716 (g) R Dilution coefficient (10) 7.Example 一Parameter —
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