癸烯中溴检测方案(卡氏水分测定)

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KEM Application Note No.KCZ-09189Kyoto ElectronicsNo.LN37-09169 No.KCZ-09189 Bromine number Measurement (Coulometry) Bromine number of decene -Abstract一 With MKC-520， measurement of bromine number of decene resulted with goodrepeatability， and it is considered to be practical to use MKC-520. -Equipment- Main unit ： Coulometric KF moisture titratorMKC-520Electrode ： Twin Pt electrode M-713 Inner cell (#433-0006) -Reagent- Anolyte ： mixture of acetic acid 600mL， methanol 260mL，1M-potassium bromide140mL Catholyte ： 0.2M-potassium chloride -Method- Pretreatment ① Added 7.007g(Wt1) decene to 100mL flask， and diluted with toluene up to theline and weighed at (wt2：86.605g). ② Added 1mL of solution to 100mL flask and diluted with toluene to the line. ③Dilution ratio was obtained from eq： Dilution ratio=Wt2/Wt1×100=1211 Preparation Added anolyte to titration cell and catholyte to the inner cell. ② Added 1mL sample and performed Pre-Titration to stabilize drift level. Measurement ① Approx. 1.7g sample was measured to determine bromine number of sample. 一Calculation- Bromine index (g/100g)：((Data-Driftxt-Blank)/(Wt1-Wt2))xDx0.0001xF 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 (1211) F=1.00 ： factor Blank ： blank level (ug) -Ambient condition- Room temperature： 21.9℃ Humidity：50% Weather： fine -Measurement parameter一 一Measurement data- [Titration] Method 5 t(stir) 0s t(wait) 15 s t(max) 0s Drift Stop：： Rel 1.00 ug/s Cont. Gain 5.0 Stable 0.5 ug/minStart ： Auto [Calculation] Calc. No. 7 Unit ：g/100g Weight ： Fixed Drift Comp：Auto ***Result *** Sample No. 01-01 Date 2009/05/09 13：48 Titr. Cell No.. 1 Wt1 69.631 g Wt2 67.881 g Net 1.750 g D 1211 Result 1828.9 ug 126.56 g/100g ***Result *** Sample No. 01-02 Date 2009/05/09 14：17 Titr. Cell No. 1 Wt1 68.721g Wt2 66.724g Net 1.997g D 1211 Result 2084.2 ug 126.39 mg/100g 一·Results-一 Run Size Bromine(ug) Conc.(g/100g) Statistics (mg/100g) 1st2nd3rd 1.750 1.997 1.666 1828.92084.2 1726.7 126.56126.39 125.51 Mean SD RSD 126.15 0.56 0.45% -Comment一 Measurement of bromine number by coulometric method requires dilution ofsample. For solvent use toluene which is easy to handle and stable.