CAJ | 학술논문

建立了合成革原料聚氨酯中单丁基锡、二丁基锡、三丁基锡和三苯基锡的气相色谱-质谱（GC-MS）分析方法。合成革原料聚氨酯经二甲基甲酰胺溶解后用甲醇沉淀高聚物，样液在超声水浴中用四乙基硼化钠进行衍生化，正己烷萃取生成乙基化的有机锡，采用GC-MS总离子流和选择离子进行定性定量测定。对衍生化时间、衍生化pH值、衍生化试剂用量、沉淀试剂用量等样品前处理条件进行了优化，并进行了线性关系、回收率、精密度等考察。结果表明，方法线性范围0．120mg／kg，相关系数R。在0．9938-0．9994之间，加标平均回收率88．3％-102．9％之间，相对标准偏差RSD在3．56％-8．38％之间，方法的检出限在0．5-2．5mg／kg之间。所建立的方法能很好地应用于合成革原料聚氨酯中有机锡化合物的测定。
건립료합성혁원료취안지중단정기석、이정기석、삼정기석화삼분기석적기상색보-질보（GC-MS）분석방법。합성혁원료취안지경이갑기갑선알용해후용갑순침정고취물，양액재초성수욕중용사을기붕화납진행연생화，정기완췌취생성을기화적유궤석，채용GC-MS총리자류화선택리자진행정성정량측정。대연생화시간、연생화pH치、연생화시제용량、침정시제용량등양품전처리조건진행료우화，병진행료선성관계、회수솔、정밀도등고찰。결과표명，방법선성범위0．120mg／kg，상관계수R。재0．9938-0．9994지간，가표평균회수솔88．3％-102．9％지간，상대표준편차RSD재3．56％-8．38％지간，방법적검출한재0．5-2．5mg／kg지간。소건립적방법능흔호지응용우합성혁원료취안지중유궤석화합물적측정。
The paper establishes the gas chromatography mass spectrometry （GC/MS） analysis method for the determination of 40rganotin compounds in the synthetic leather raw material of polyurethane： n-Butyltin-trichloride （MBT）, Dibutyltin dichloride （DBT）, Tributyltin （TBT）, Triphenyltin-chloride （TPhT）. The polyurethane sample is dissolved with N,N-Dimethylformamide and the polymer in the sample is precipitated with methanol, and the target compounds are derivatized with sodium tetraethyl borate and extracted with hexane under ultrasonication, and analysis of the ethyl organotin by GC-MS in scan mode and selective ion mode. It carries out the qualitative and quantitative analysis by GC-MS on the total ion chromatogram and selected ion chromatogram. Meanwhile, it optimizes the derivatization and extraction conditions, such as the derivatization time, derivatization pH value,dosages of derivatization reagent and precipitation reagent and observes the linear ties, recoveries and precisions. The results show that the linearity range is 0.1 - 20mg/kg, the linearity correlation coefficient R2 is 0. 9938 - 0. 9994, the relative standard deviation is 3. 56%-8. 38%, the average recovery rate is 88. 3%-102.9%, and the method detection limit is 0. 5 - 2. 5 mg/kg. The established method can be successfully applied to the determination of organotin compounds in synthetic leather raw material of polyurethane.