ガスクロマトグラフ法による無機薬品中の超微量亜硝酸イオンの定量

概要

論文の詳細を見る
A new reagent, l-methylamino-2-amino-4, 6-dibromobenzene (MADB) for the gas chromatographic determination of ultramicro amounts of nitrite ion was synthesized. It reacts with nitrite ion to form 1-methyl-5, 7-dibromobenzotriazole (MDBT) which can be extracted into toluene. The extract is very sensitive to electron capture detection in gas chromatography. Therefore, the conditions for the gas chromatographic determination of ultramicro amounts of nitrite ion were investigated by using MADB. A typical procedure is as follows : Take the sample solution containing less than 60 ng of nitrite ion into a 25 ml of stoppered test tube and dilute to 15ml with distilled water. Add 2 ml of concentrated hydrochloric acid and 0.5 ml of MADB solution(2×10^<-4> mol dm^<-3>), and allow the mixture to stand for 30 min. Extract the MDBT formed into 2 ml of toluene by shaking for 5 min, and wash the toluene extract with 4 ml of 3 mol dm^<-3> hydrochloric acid. Inject 2μl of the toluene extract into gas chromatograph (ECD) and measure the peak height. The calibration curve (peak height) is linear in the range of 2.5 to 10 ng of nitrite ion in 15 ml of solution. The reproducibility at 3.5 ng ml^<-1> was 3%. Trace nitrite ion in commercially available inorganic salts was determined by the proposed procedure.
社団法人日本分析化学会の論文
1985-04-05