Journal of Textile Research ›› 2020, Vol. 41 ›› Issue (08): 69-73.doi: 10.13475/j.fzxb.20190904906

• Dyeing and Finishing & Chemicals • Previous Articles     Next Articles

Determination of cyclicsilicates in textile softeners by gas chromatography-mass spectrometry

YU Yan1,2, ZHANG Ruohong2(), ZHONG Yi1, DU Yingying2, MAO Zhiping1, XU Hong1   

  1. 1. Key Laboratory of Science & Technology of Eco-Textile, Ministry of Education, Donghua University,Shanghai 201620, China
    2. Shanghai Institute of Quality Inspection and Technical Research, Shanghai 201114, China
  • Received:2019-09-18 Revised:2020-05-04 Online:2020-08-15 Published:2020-08-21
  • Contact: ZHANG Ruohong E-mail:zhangrh@sqi.org.cn

Abstract:

In order to develop an efficient quantitative analysis method on the content of cyclosiloxane in textile softener, gas chromatography-mass spectrometry (GC-MS) was carried out to establish an analytical method for this purpose. The test sample was extracted by the oscillating extraction method using ethyl acetate as the solvent. The extracted solution was subjected to a derivatization reaction with hexamethyldisilazane, and then was detected using GC-MS. The result shows that within range of solution mass density 1-100 mg/L, the peak areas measured for octamethylcyclotetrasiloxane (D4), decamethylcyclopentasiloxane(D5) and dodecamethylcyclohexasiloxane(D6) demonstrate good linear relationship with solution mass density, with correlation coefficient R2 ≥ 0.995 3. The detection limit of this method is 0.117 0-0.201 0 mg/L, the limit of quantification is 0.390 0-0.670 0 mg/L, the relative standard deviation (RSD) of repeatability and stability are less than 1.0% and 7.4% respectively. The sample recovery rate is 89.8%-114.3%, and the RSD is 1.3%-6.4%, satisfying the testing requirements. This method is easy to operate and capable of determining with accuracy the trace residues of D4, D5 and D6 in textile softeners.

Key words: gas chromatography-mass spectrometry, textile softener, cyclosiloxane determination, octamethylcyclote-trasiloxane, decamethylcyclopentasiloxane, dodecamethylcyclohexasiloxane

CLC Number: 

  • O657.63

Fig.1

Polydimethylsiloxane side reaction"

Fig.2

D4, D5 and D6 standard solution extracted ion chromatogram"

Tab.1

Standard linear equations for D4, D5 and D6"

环硅氧烷 回归方程 R2
D4 Y=9.458×103X+1.676×103 0.998 8
D5 Y=3.601×103X-2.664×103 0.997 3
D6 Y=3.654×103X-4.691×103 0.995 3

Fig.3

Comparison of extraction effects of different extraction solvents"

Fig.4

Comparison of extraction methods of different extraction methods"

Fig.5

Comparison of extraction effects of different extraction times"

Fig.6

Comparison of effects of derivatization reactions"

Tab.2

Detection limit, limit of quantitation, repeatability and stability test results"

环硅
氧烷
检出限/
(mg·L-1)
定量限/
(mg·L-1)
重复性
RSD/%
稳定性
RSD/%
D4 0.117 0 0.390 0 1.0 7.4
D5 0.123 0 0.410 0 0.7 5.4
D6 0.201 0 0.670 0 1.0 4.7

Tab.3

Standardized recovery test results"

环硅氧烷 质量浓度/(mg·L-1) 平均回收率/% RSD值/%
1 109.5 5.2
D4 50 89.8 3.2
100 91.3 1.6
1 114.3 6.4
D5 50 95.2 1.3
100 100.0 2.8
1 97.1 3.9
D6 50 100.1 4.9
100 101.3 6.3

Tab.4

Sample analysis result"

样品编号 质量浓度/(mg·L-1)
D4 D5 D6
1 5.82 6.87 7.02
2 52.97 14.34 15.09
3 27.00 22.66 9.72
4 6.52 23.74 16.47
5 45.22 23.36 8.32
[1] 周勇. 三元嵌段有机硅柔软剂的制备及其在纺织品上的应用[D]. 广州:华南理工大学, 2017: 1-51.
ZHOU Yong. Preparation of ternary block silicone softener and its application in textiles[D]. Guangzhou: South China University of Technology, 2017: 1-51.
[2] 许伟俊, 覃一峰, 李哲瀚. 有机硅柔软剂在织物整理方面的应用现状和发展[J]. 化工设计通讯, 2018,44(2):77.
XU Weijun, QIN Yifeng, LI Zhehan. Application status and development of silicone softener in fabric fini-shing[J]. Chemical Engineering Design Communications, 2018,44(2):77.
[3] 田丽. 纺织品柔软剂的应用现状及趋势[J]. 轻纺工业与技术, 2011,40(1):69-73.
TIAN Li. Application status and trend of textile soften-ers[J]. Textile Industry and Technology, 2011,40(1):69-73.
[4] 陈杰. 有机硅类纺织助剂[J]. 广州化工, 2015,43(13):41-42, 84.
CHEN Jie. Organicsilicon textile auxiliaries[J]. Guangzhou Chemical Industry, 2015,43(13):41-42, 84.
[5] 魏元博, 安秋凤, 赵洁. 有机硅柔软剂在织物整理方面的应用现状及发展[J]. 有机硅材料, 2014,28(6):479-483.
WEI Yuanbo, AN Qiufeng, ZHAO Jie. Application status and development of silicone softeners in fabric finishing[J]. Silicone Material, 2014,28(6):479-483.
[6] 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.
FU Qiang, QIAN Zhiyang. Determination of D4 by gas chromatography[J]. Modern Scientific Instruments, 2000(5):46-47.
[7] 李了, 黄健. 溶剂解吸-气相色谱-质谱法测定沼气中两种硅氧烷[J]. 江苏科技信息, 2018,35(18):40-42.
LI Le, HUANG Jian. Determination of two silicones in biogas by solvent desorption-gas chromatography-mass spectrometry[J]. Jiangsu Science & Technology Information, 2018,35(18):40-42.
[8] LUCIANA C R, LORENA V, ANTONIO C. Determination of siloxanes in water samples employing graphene oxide/Fe3O4 nanocomposite as sorbent for magnetic solid-phase extraction prior to GC-MS[J]. Journal of Separation Science, 2018,41(22):4177-4184.
doi: 10.1002/jssc.201800577 pmid: 30239125
[9] 吴嘉碧, 黎军, 陈纪文, 等. GC-MS测定涂料原料二甲基环体硅氧烷[J]. 化学工程与装备, 2009(8):151-153.
WU Jiabi, LI Jun, CHEN Jiwen, et al. GC-MS determination of coating material dimethylcyclosilo-xane[J]. Chemical Engineering & Equipment, 2009(8):151-153.
[10] 许嘉祥, 陈奕伊, 陈萌萌, 等. 硅油中微量二甲基硅氧烷环体的定量分析研究[J]. 杭州师范大学学报(自然科学版), 2018,17(5):462-467.
XU Jiaxiang, CHEN Yiyi, CHEN Mengmeng, et al. Quantitative analysis of trace dimethylsiloxane rings in silicone oil[J]. Journal of Hangzhou Normal Univer-sity (Natural Science Edition), 2018,17(5):462-467.
[11] BROTHERS H M, BOVENS E, BRUNI A, et al. A practical gas chromatography flame ionization detection method for the determination of octamethyl-cyclotetrasiloxane, decamethylcyclopentasiloxane, and dodecamethylcyclohexasiloxane in silicone emulsions[J]. Journal of Chromatography A, 2016,1441:116-125.
doi: 10.1016/j.chroma.2016.02.069 pmid: 26968230
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