基于固体分散剂制样的裂解/气相色谱-质谱联用定量测定PC/ABS共混物比例  

Quantitative Analysis of Blend Ratio of Polycarbonate to Acrylonitrile-Butadiene-Styrene Copolymer by Pyrolysis Gas Chromatography-Mass Spectrometry Using Solid Dispersant for Sample Preparation

作　　者：袁丽凤 罗川 徐善浩 张樱 丁明政 林振兴 YUAN Li-feng;LUO Chuan;XU Shan-hao;ZHANG Ying;DING Ming-zheng;LIN Zhen-xing(Technology Center of Ningbo Customs,Ningbo 315103,China;Ningbo Institute of Inspection and Quarantine Science and Technology,Ningbo 315103,China)

机构地区：[1]宁波海关技术中心,浙江宁波315103 [2]宁波检验检疫科学技术研究院,浙江宁波315103

出　　处：《分析测试学报》2020年第6期769-773,共5页Journal of Instrumental Analysis

基　　金：宁波市公益类科技计划(2019C50031);海关总署科研计划(2019HK016);浙江省基础公益研究计划(LGC20B040001)。

摘　　要：建立了以二氧化硅为分散剂制样的裂解/气相色谱-质谱联用测定聚碳酸酯(PC)/丙烯腈-丁二烯-苯乙烯共聚物(ABS)共混物比例的分析方法。将样品冷冻破碎成粉末后,以二氧化硅为固体分散剂与样品混合后进样,在600℃裂解温度下裂解得到相应的裂解色谱图,选择PC/ABS共混物裂解色谱图上ABS的特征裂解产物——苯乙烯为定量峰,计算PC/ABS共混物中ABS的质量分数,再进一步推算PC的质量分数。以二氧化硅为固体分散剂制备系列已知含量的PC/ABS分散体,以ABS含量为横坐标,对应的苯乙烯峰面积为纵坐标绘制校准曲线,ABS在分散体中含量在0.06~20 g/kg(对应PC∶ABS=99.7∶0.30~0∶100)范围内的线性良好,相关系数(r2)为0.994,以5倍信噪比(S/N=5)计算得到ABS的检出限为0.06 g/kg(对应的PC∶ABS比例为99.7∶0.30)。采用该方法对已知混合比例的PC/ABS样品进行测定,所得结果的回收率为95.3%~103%,相对标准偏差(RSDs,n=3)为1.1%~3.8%。该方法简便、准确度高,适用于PC/ABS共混物全范围比例的定量分析。A pyrolysis gas chromatography-mass spectrometry with silica as dispersant for sample preparatio was developed for the quantitative analysis of blend ratio of polycarbonate(PC) to acrylonitrile-butadiene-styrene copolymer(ABS).The samples were dispersed with silica after freeze-fracturing,then weighed carefully and injected.The pyrograms of the samples were obtained at a pyrolysis temperature of 600 ℃.The characteristic peak of styrene in thermally decomposed polyester was selected as the quantitative peak for determination of the blending ration of PC and ABS in PC/ABS blend.A series of content-known PC/ABS blend standards were prepared using silica as dispersant.Results showed that there were good linear relationships between styrene peak area and ABS concentration in the range of 0.06-20 g/kg(corresponding to PC ∶ABS ratio of 99.7 ∶0.3-0 ∶100),with their correlation coefficient(r2) of 0.994.The detection limit(S/N=5) of the method for ABS was 0.06 g/kg(corresponding a PC to ABS ratio of 99.7 ∶0.30).The method was applied to the PC/ABS blend samples with known bending ratios.The recoveries ranged from 95.3% to 103% with relative standard deviations(RSDs,n=3) of 1.1%-3.8%.The method is simple,convenient and accurate,ant it is suitable for the analysis of PC/ABS blending ratio in the full range.

关 键 词：裂解/气相色谱-质谱联用 PC/ABS共混物比例 固体分散剂 定量测定 

分 类 号：O657.71[理学—分析化学]