电位滴定法测溴值_AT-510自动电位滴定仪测定环己烯的不饱和度(溴值)含量.pdf
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电位滴定法测定环己烯的不饱和度(溴值)含量
使用日本京都电子公司(KEM)-自动电位滴定仪(AT-510),测定环己烯中溴值的应用资料。
溴值是指在试验条件下与100g试样起反应的溴的克数(gBr/100g)。在石油产品中,溴值通常作为脂肪族不饱和度的一种量度方法。
符合下列标准规范:
ASTM D1159 - 07(2012) Standard Test Method for Bromine Numbers of Petroleum Distillates and Commercial Aliphatic Olefins by Electrometric Titration(电化学滴定法测量石油馏分及商用脂族烯烃的溴值试验方法)。
GB/T 11135 - 1989 石油馏分和工业脂肪族烯烃溴值测定法(电位滴定法)。
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TIZ-12077Kyoto Electronics Manufacturing Co.,Ltd. KEM Application NotePolarization Titration Data No. NX19-12059 Unsaturation of Cyclohexene (titration for bromine number) Summary- As the result of studying the repeatability on the polarization titration by AT-510, a good resultwith 0.9mg/100g of maximum SD was obtained. -Measuring instrument- Main unit : Potentiometric automatic titrator AT-510 Detector: Polarization preamplifier POT-510 Twin platinum electrode M-511 Thermostat water circulator -Reagent- Titrant:0.25mol/L-Potassium bromide/Potassium bromate Addition: Mixed solvent (acetic acid : 1,1,1-trichloroethane : methanol :(1+5)sulfuric acid=714:134:134:18) -Method- Measurement ① Set the applied current at 10pA ② Put 2mL of the sample in 200mL beaker. ③ Add 100mL of the mixed solvent to it. ④ Cool down the above solution to the temperature between 0 and 5°C. ⑤ Titrate with 0.25mol/L potassium bromide/potassium bromate to determine theunsaturation of cyclohexene, i.e. the bromine number. (An end-point is detected from theinflection point on the titration curve.) -Equation- Bromine number(g/100g): (EP1-BLK)×C1(0.03995)×K1(100)/Size EP1: Titer(mL) BLK: Blank volume(mL) C1: Concentration-conversion coefficient (0.25M-KBr/KBrO41mL=0.03995mgBr2 K1: Unit-conversion coefficient -Ambient conditions- -Ambient conditions- Temperature:22.4℃ Relative Humidity: 48% Weather:Cloudy -Reference- -Measurement parameter- Printout data- Data:2012/03/19 14:05 Method No. : 03 Method Name : Method03 Titr.Fom : EP BuretNo. :1 Preampo: POT DetectorNo.: 3 Unit: mV Max. Volume:20.000mL Titr.Wait :30s Direction : Auto [Dose1 Mode :Volume Stop Buret No. : 1 Volume: 9.0mL Cut Off Time: Os Dose Speed : 1s/mL Dose Wait : 0s ***Result *** Sample No. 02-01 Data:2012/03/19 14:17 Sample ID : Method No. :03 Method Name :Method03 Titr.Fom: EP Sample Measurement Conc. 1 Calc.No.: 12 l.Level 772.4mV F.Level 13.6mV F. Volume 10.3500mL D.Volume 9.0000mL Titr.Time 00:07:42 Size 2.0731g Conc-1 18.939mg/100 EP-1 9.8281mL 372.8mV 一 12.EnL] [Control Data:2012/03/19 14:05MethodNo. :03 Method Name:Method03 Titr.Fom : EP End PointNo.: 1 Gain : 1 End Sense : Auto. Cut off Time:15s Unit Volume:0.05mLSpeed::1s/mL Sampling mV: 4.0mV Sampling mL: 0.05mL Calculation] Data:2012/03/1914:05Method No.:03 Method Name: Method03 Sample Measurement Conc.1 End PointNo.: 1 Unit :[mg/100]Coefficient1:.03995K1 : 100 CO1=(E1-B1)*F1*C1*K1/SBlank1 : 0.0mL Factor1: 1.000 -Measurement results- Run Samplesize (mL) Titer(mL) Conc.(g/100g) 12345 2.0731 9.82819.42509.83299.8615 9.7823 18.93918.16318.94919.004 18.851 Statistics MeanSDRSD 18.781g/100g0.3499g/100g1.8631% -Comments- Note that the determination of bromine number should be made at the applicable lowesttemperature because it is associated with the side reaction which is influenced by titrationtemperature. Http://www. shxf17.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-feng com
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