Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry

ZHANG Yi-dan; YANG Rui-qin; LIAN Zhe

doi:10.12452/j.fxcsxb.23091102

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Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry

Experimental Techniques and Methods | 更新时间：2024-03-13

- Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry
- Journal of Instrumental Analysis Vol. 43, Issue 3, Pages: 464-473(2024)
- 作者机构：
  
  1.中国人民公安大学侦查学院，北京 100038
  2.公安部鉴定中心，北京 100038
- 作者简介：
- 基金信息：
- DOI：10.12452/j.fxcsxb.23091102
  CLC： O657.63;DF794.3
- Published：15 March 2024，
  
  Received：11 September 2023，
  
  Revised：09 November 2023，
- 稿件说明：
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张艺丹,杨瑞琴,廉哲.气相色谱-质谱法检测纸张中的烷基烯酮二聚体施胶剂[J].分析测试学报,2024,43(03):464-473.

ZHANG Yi-dan,YANG Rui-qin,LIAN Zhe.Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(03):464-473.
张艺丹,杨瑞琴,廉哲.气相色谱-质谱法检测纸张中的烷基烯酮二聚体施胶剂[J].分析测试学报,2024,43(03):464-473. DOI： 10.12452/j.fxcsxb.23091102.

ZHANG Yi-dan,YANG Rui-qin,LIAN Zhe.Determination of Alkyl Ketene Dimer Sizing Agent in Paper by Gas Chromatography-Mass Spectrometry[J].Journal of Instrumental Analysis,2024,43(03):464-473. DOI： 10.12452/j.fxcsxb.23091102.

摘要

建立了纸张中烷基烯酮二聚体施胶剂的水解提取结合气相色谱-质谱检测方法。纸张样品以1 mol/L 氢氧化钠溶液在70 ℃恒温水浴条件下水解2 h后，以二氯甲烷静置萃取1 h，提取液经过滤后，待测物采用气相色谱-质谱法测定，以保留时间和特征离子对定性，内标法定量。结果表明：14-二十七酮、16-三十一酮和18-三十五烷酮分别在1.0~50 mg/L、1.0~50 mg/L 和2.5~50 mg/L范围内线性关系良好，相关系数（

）均大于0.98，检出限分别为0.1、0.5、2.0 mg/L，定量下限分别为0.5、1.5、5.0 mg/L。施胶量为1%的杨木纤维手抄纸样品中，基于平均留着率计算得到烷基烯酮二聚体的提取回收率为34.9%~60.9%。利用该方法测定40种不同品牌的静电复印纸，依据特征物质、烷基烯酮二聚体施胶剂原料配比和纸张中总酮含量将40种纸样分为三大类。该方法更简便、温和，适用于法庭科学领域纸张物证的检验与比对区分，可为纸张施胶方式研判、厂家溯源与形成年代推断提供新的参考依据。

Abstract

A hydrolytic extraction method combined with gas chromatography-mass spectrometry（GC-MS） method for the determination of alkyl ketene dimer sizing agent in paper was developed. The paper samples were hydrolyzed with 1 mol/L sodium hydroxide solution in a constant temperature water bath at 70 ℃ for 2 h，and then extracted with methylene chloride for 1 h. After the filtration of the extraction solution，the analytes were measured on GC-MS，characterized by retention time and characteristic ion pairs，and quantified by internal standard method. The results showed that there were good linear relations for the 14-heptacosanone，16-hentriacontanone and 18-pentatriacontanone in the range of 1.0-50 mg/L，1.0-50 mg/L，and 2.5-50 mg/L，respectively，with correlation coefficients（

） more than 0.98. The limits of detection for the analytes were 0.1 mg/L，0.5 mg/L and 2.0 mg/L，and the limits of quantitation were 0.5 mg/L，1.5 mg/L and 5.0 mg/L，respectively. Based on the average retention，the extraction recovery of alkyl ketene dimer from poplar fiber hand-made paper with sizing content of 1% were 34.9%-60.9%. The method was used to detect 40 kinds of different brands of copy paper. According to the characteristic substances，the ratio of raw materials for alkyl ketene dimer，and total ketone content in paper，40 kinds of paper samples were divided into three categories. The method is simpler and milder than existed ones，which is suitable for the examination and comparison of paper material evidence in the field of forensic science. Besides，this method can provide a new reference for the research and judgment of paper sizing method，manufacturer tracing，and formation age inference.

关键词

烷基烯酮二聚体施胶剂气相色谱-质谱法纸张检验法庭科学

Keywords

alkyl ketene dimersizing agentgas chromatography-mass spectrometrypaper examinationforensic science

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