气相色谱-负化学离子源质谱法测定聚氯乙烯塑料中的短链氯化石蜡

doi:10.3724/SP.J.1123.2014.10004

色谱 ›› 2015, Vol. 33 ›› Issue (2): 182-187.DOI: 10.3724/SP.J.1123.2014.10004

气相色谱-负化学离子源质谱法测定聚氯乙烯塑料中的短链氯化石蜡

幸苑娜, 林志惠, 冯岸红, 王欣, 龚叶萌, 陈泽勇

深圳市计量质量检测研究院, 广东深圳 518131

收稿日期:2014-10-11 修回日期:2014-11-20 出版日期:2015-02-08 发布日期:2015-01-24
通讯作者: 幸苑娜
基金资助:
广东省质量技术监督局科技项目(2013PZ09).

Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography- negative chemical ion/mass spectrometry

XING Yuanna, LIN Zhihui, FENG Anhong, WANG Xin, GONG Yemeng, CHEN Zeyong

Shenzhen Academy of Metrology and Quality Inspection, Shenzhen 518131, China

Received:2014-10-11 Revised:2014-11-20 Online:2015-02-08 Published:2015-01-24

摘要/Abstract

摘要：

建立了用于聚氯乙烯(PVC)塑料中短链氯化石蜡(SCCPs)含量测定的气相色谱-负化学离子源质谱法。采用超声萃取法对PVC塑料中的SCCPs进行萃取,萃取时间为1.5 h;然后用浓硫酸法对萃取溶液进行净化处理;最后用气相色谱-质谱法在负化学电离模式、离子源温度为160 ℃、甲烷反应气流速为1.5 mL/min等条件下对样品中的SCCPs进行定性定量分析。该方法不受样品中中链氯化石蜡(MCCPs)的干扰,可对样品中的SCCPs进行准确的定量分析。分析的12批次样品均检出SCCPs,含量在0.3×10²~3.5×10⁴mg/kg范围内。依据欧盟对SCCP的限值(1%)要求,4批次样品不符合法规要求,不符合率为33.3%。可见,PVC塑料具有较高的SCCPs污染风险。

关键词: 短链氯化石蜡, 聚氯乙烯塑料, 浓硫酸法, 气相色谱-负化学离子源质谱

Abstract:

A novel method was established to determine short chain chlorinated paraffins (SCCPs) in polyvinyl chloride (PVC) plastics by gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS). Ultrasonic extraction was used to extract SCCPs from PVC plastics. The optimal extraction time was 1.5 h, and concentrated sulfuric acid was adopted to purify the extracted solution. Finally, SCCPs in a sample were detected by GC-NCI/MS at 160 ℃ and with methane reagent gas at 1.5 mL/min. This method was not influenced by medium chain chlorinated paraffins (MCCPs) in the sample, and accurate quantitation was made for SCCPs. Twelve batches of samples were analyzed and SCCPs were detected in each batch with the contents from 0.3×10² mg/kg to 3.5×10⁴ mg/kg. With respect to European limitation of SCCPs (1%), four batches of samples did not comply with the European regulation, and they accounted for 33.3%. Obviously, high SCCPs risk was presented in PVC plastics.

Key words: concentrated sulfuric acid, gas chromatography-negative chemical ion/mass spectrometry (GC-NCI/MS), polyvinyl chloride (PVC) plastics, short chain chlorinated paraffins (SCCPs)

中图分类号:

O658

幸苑娜, 林志惠, 冯岸红, 王欣, 龚叶萌, 陈泽勇. 气相色谱-负化学离子源质谱法测定聚氯乙烯塑料中的短链氯化石蜡[J]. 色谱, 2015, 33(2): 182-187.

XING Yuanna, LIN Zhihui, FENG Anhong, WANG Xin, GONG Yemeng, CHEN Zeyong. Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography- negative chemical ion/mass spectrometry[J]. Chinese Journal of Chromatography, 2015, 33(2): 182-187.

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气相色谱-负化学离子源质谱法测定聚氯乙烯塑料中的短链氯化石蜡

Determination of short chain chlorinated paraffins in polyvinyl chloride plastics by gas chromatography- negative chemical ion/mass spectrometry

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