环己烯中溴检测方案(卡氏水分测定)

KEM Application Note No.KCZ-09184Kyoto ElectronicsNo.LN37-09164 No.KCZ-09184上海市中山西路2366弄1号203室网址： http：//www.kem-china.com Bromine Index Measurement (Coulometry) Bromine index of 0.05%-cyclohexene (90mg/100gBr2) -Abstract- The cyclohexene is a standard substance for bromine index/number. With MKC-520， measurement of cyclohexene to determine bromine index resulted withprecise agreement with theoretical value and repeatability within 1%. -Equipment- Main unit ： Coulometric KF moisture titratorMKC-520 Electrode：Twin Pt electrode M-713Inner cell (#433-0006) -REagent- Anolyte ： mixture of acetic acid 600mL， methanol 260mL，1M-potassium bromide140mL Catholyte ： 0.2M-potassium chloride Catholyte ： 0.2M-potassium chloride -Method- Pretreatment ① AAdded 100mL 0.801g(Wt1) cyclohexene to a flask， and diluted with tolune up Pretreatment ① AAdded 100mL 0.801g(Wt1) cyclohexene to a flask， and diluted with tolune upto the line and weighed at (wt2：86.605g). ② Added 5mL of solution to 100mL flask， and diluted with tolune up to the line.③ Theoretical value of bromine index of the sample was obtained from the eq：Theoretical value=194600xwt1/wt2×100/5=90.0(mg/100g) Preparation ①Added anolyte to titration cell and catholyte to the inner cell. ② After 1mL sample was added， ran Pre-Titration to stabilize drift. Measurement ①)22~3g sample was measured to determine bromine index of the sample/ Measurement ①)22~3g sample was measured to determine bromine index of the sample/ Calculation- Calculation- Bromine index (mg/100g) ： ((Data-Driftxt-Blank)/(Wt1-Wt2))xDx0.1xF Data：measured bromine (ug) Wt1： sample+tare (g) Drift ： drift level at start (ug/s) Wt2 ： weight of tare (g) t： measure time (s) D： dilution ratio (1.0) F=1.00 ： Factor Blank ： Blank((ug) -Ambient condition- Room temperature ： 21.9℃ Humidity： 50% Weather ： fine -Measurement parameter- 一Measurement data· [Titration1 Method 5 t(stir) 0s t(wait) 15 s t(max) 0 s Drift Stop：： Rel 1.00 ug/s Cont. Gain 5.0 Stable 0.5 ug/minStart ： Auto [Calculation1 Calc. No. 7 Unit ： mg/100g Weight ： Fixed Drift Comp：Auto ***Result *** Sample No. 01-01 Date 2009/05/08 10：43 Titr. CellNo. 1 Wt1 74.369g Wt2 71.431 g Net 2.938g D 1.0 Result 2633.6 ug 89.639 mg/100g ***Res ult*** Sample No. 01-02 Date 2009/05/0810：48 Titr. Cell No. 1 Wt1 71.763 g Wt2 69.311 g Net 2.453 g D 1.0 Result 2163.7 ug 88.206 mg/100g 一·Results一 Run Size 2633.6 Statistics (mg/100g) Conc.(mg/100g) 1st2nd3rd4th5th 2163.72263.62583.8 3395.3 MeanSD RSD 0.740.83% 89.6488.2187.9487.80 88.58 一Comment一 Use refined cyclohexene(bp 82.5~83.5℃)with refractive index 1.446~1.447 at20℃. (JAIS No.11Bromine index measurement of benzene)