
热裂解气相色谱法快速筛查高分子材料中4种邻苯二甲酸酯类增塑剂
熊松松, 简佩玲, 孙秀敏, 郭范娟, 苏健梅, 丑天姝
热裂解气相色谱法快速筛查高分子材料中4种邻苯二甲酸酯类增塑剂
Rapid Screening of Four Phthalate Ester Plasticizers in Polymeric Materials Using Pyrolyzer Gas Chromatography
采用热裂解气相色谱法(Py-GC)建立了快速筛查高分子材料中4种邻苯二甲酸酯类化合物(PAEs)的分析方法。将样品粉碎研磨后,直接称取一定量样品,进样于热裂解邻苯检测仪进行分析,采用外标法定量分析,考察了取样量、温度等因素对回收率的影响,确定最佳前处理条件。结果表明:分析物在100~4 000 mg/kg浓度范围内线性关系良好(r 2>0.996 0),检出限为12.1~33.4 mg/kg。采用不同浓度的阳性物质分析方法的准确度和精密度,分析物的回收率为77.4%~125.5%,相对标准偏差为1.7%~12.8%。采用此方法对26个实际样品进行检测分析,在12个样品中检测出PAEs,检出率高达46%。该方法不使用化学试剂,直接对样品进行测试,能够满足企业对PAEs的快速筛查要求,为企业内部管控PAEs提供方法支持。
A rapid screening method for the analysis of four phthalate esters (PAEs) in polymeric materials was established using pyrolysis gas chromatography (Py-GC). After grinding the samples into powder, a certain amount of the sample was directly weighed and injected into the pyrolysis phthalate detector for analysis. External standard method was used for quantitative analysis. Factors such as sample amount and temperature that affect the recovery rate were investigated, and the optimal pre-treatment conditions were determined. The results show that the analytes exhibited good linearity within the concentration range of 100~4 000 mg/kg (r²>0.996 0), with detection limits ranging from 12.1 to 33.4 mg/kg. The accuracy and precision of the method were evaluated using positive substances at different concentrations. The recovery rates of the analytes were between 77.4% and 125.5%, with relative standard deviations ranging from 1.7% to 12.8%. This method was applied to analyze 26 actual samples, and PAEs were detected in 12 of them, with a high detection rate of 46%. The method does not use chemical reagents and allows direct testing of samples, which can meet the requirements of enterprises for rapid screening of PAEs and provides a methodological support for internal control of PAEs within enterprises.
Phthalate ester / Polymeric materials / Pyrolyzer / Rapid screening
O657.71
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