TD-GCMS测定密封胶中二甲基环硅氧烷含量
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摘要
采用热脱附-气相色谱/质谱联用仪(TD-GCMS)测定了密封胶中二甲基环硅氧烷(D_3～D_(10))的含量。通过谱库对照和特征离子分析,确认了各组分在谱图中对应的峰;并以十甲基环五硅氧烷(D_5)为标准曲线,建立了用于测定环硅氧烷含量的半定量法;考察了脱附管解析时间、解析温度和解析流量对吹扫捕集的影响;最后测试了在80、100和120℃时2种密封胶中D_3～D_(10)的含量。该方法具有操作简单、分析周期短、经济适用、覆盖环硅氧烷范围广等优点。
The content of dimethylcyclosiloxane( D3～ D10) in the sealant was determined by thermal desorption-gas chromatography/mass spectrometry( TD-GCMS). The corresponding peaks of each components in the spectrum were confirmed by the comparison with spectral library and analysis of characteristic ion. The decamethylcyclopentasiloxane( D5) was used as the standard curve to prove the semi-quantitative method. The effects of the desorption time,temperature and flow rate on purging and trapping were investigated. Finally,the contents of each components of D3～ D10 at 80℃,100℃ and 120 ℃ were tested. The method is easy,timesaving,economic and can be used be test other cyclosiloxanes.
The content of dimethylcyclosiloxane( D3～ D10) in the sealant was determined by thermal desorption-gas chromatography/mass spectrometry( TD-GCMS). The corresponding peaks of each components in the spectrum were confirmed by the comparison with spectral library and analysis of characteristic ion. The decamethylcyclopentasiloxane( D5) was used as the standard curve to prove the semi-quantitative method. The effects of the desorption time,temperature and flow rate on purging and trapping were investigated. Finally,the contents of each components of D3～ D10 at 80℃,100℃ and 120 ℃ were tested. The method is easy,timesaving,economic and can be used be test other cyclosiloxanes.
引文
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[4] KALA S V,LYKISSA E D,NEELY M W,et al. Low molecular weight silicones are widely distributed after a single subcutaneous injection in mice[J]. Am J Clin Pathol,1998,152(3):645-649.
[5]郝玉红,吴建军.气相色谱-质谱法测定硅凝胶中两种硅氧烷[J].理化检验(化学分册),2015,51(6):818-820.
[6]吴建军,薛民杰,朱力敏.顶空-气相色谱-质谱法测定整形用有机硅制品中两种硅氧烷[J].上海计量测试,2017,44(3):17-19.
[7]傅强,钱之杨.气相色谱法测定八甲基环四硅氧烷[J].现代科学仪器,2000(5):46-47.
[8]吴惠勤,林晓珊,朱志鑫.食品中聚二甲基硅氧烷检测方法研究[J].分析测试学报,2010,29(12):1143-1146.