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A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography-mass spectrometry

A technology of octamethylcyclotetrasiloxane and GC-MS, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., and can solve the problems of no standard test methods, etc.

Active Publication Date: 2020-09-01
浙江中鼎检测技术有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] At present, there is no standard test method for the detection of octamethylcyclotetrasiloxane content in textiles, and there are no relevant reports in journals and magazines.

Method used

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  • A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography-mass spectrometry
  • A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography-mass spectrometry
  • A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography-mass spectrometry

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Embodiment 1

[0042] A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography, comprising the following steps:

[0043] (1) Take samples from textiles (synthetic textiles) and shred them into small pieces with a diameter not greater than 5mm.

[0044] (2) Weigh 1.0 g of the shredded sample, put it into a 40 mL reaction tube, add 10 mL of methanol of analytical grade or above, and conduct ultrasonic extraction at 50°C for 30 min in an ultrasonic cleaner with a power of 500w and a frequency of 45KHz; Use a 0.45 μm organic filter membrane to filter 1mL of the extract into a sample bottle to obtain a sample solution, and use a gas chromatography-mass spectrometer to analyze the sample solution (see results in figure 2 , image 3 ); the parameters of gas chromatography-mass spectrometry were set as follows.

[0045]

[0046] (3) Quantification by external standard method, the standard curve is composed of 5 concentration points, respectively 0.5, 1, 2, ...

Embodiment 2

[0053] A method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography, comprising the following steps:

[0054] (1) Take samples from textiles (cotton fiber textiles) and shred them into small pieces with a diameter not greater than 5mm.

[0055] (2) Weigh 1.0 g of the shredded sample, and pretreat the sample. The pretreatment process is as follows: put the sample in a polypropylene plastic box, and after airtight, treat it at a microwave power of 200W for 10-15s, and then Treat at 300W for 5-10s, and then at 200W microwave power for 10-15s; then put it into a 40mL reaction tube, add 10mL of methanol of analytical grade or above, and ultrasonically extract in an ultrasonic cleaner at 50°C for 30min, the power of the ultrasonic cleaner It is 500w, and the frequency is 45KHz; use 0.45μm organic filter to filter 1mL extract into the sample bottle to obtain the sample solution, and analyze the sample solution with gas chromatography-mass spectrometry...

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Abstract

The invention discloses a method for detecting otcamethylcyclotetrasiloxane content in a textile by a gas chromatography-mass spectrometer. The method comprises the following steps: 1) taking a samplefrom the textile, and cutting the sample; 2) weighing 1.0 g of the cut sample, placing the sample in a 40 mL reaction tube, adding 10 mL analytically pure methanol, performing ultrasonic extraction in a ultrasonic cleaner at the temperature of 50 DEG C for 30 min, using an organic filter membrane for filtering a 1 mL extract to a sample bottle to obtain a sample solution, using the gas chromatography-mass spectrometer for analysis of the sample solution, and 3) using an external standard method for quantification. The method can rapidly and accurately perform qualitative and quantitative analysis on otcamethylcyclotetrasiloxane in the textile.

Description

technical field [0001] The invention relates to a method for detecting harmful substances in textiles, in particular to a method for detecting octamethylcyclotetrasiloxane content in textiles by gas chromatography. Background technique [0002] Octamethylcyclotetrasiloxane is an important intermediate in organic synthesis, which is used to prepare various important industrial products such as silicone oil, silicone rubber, silicone resin and surfactants. These industrial products are widely used in construction, electronics, Textile, automotive, personal care, food, mechanical processing and other fields. [0003] According to relevant studies, octamethylcyclotetrasiloxane has long-term harmful effects on the aquatic environment and has a potential risk of impairing reproductive ability. In the "Washington State Children's Product Safety Act" announced by Washington State of the United States, octamethylcyclotetrasiloxane was listed as Chemical High Concern to Children (Chi...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/72G01N30/06
Inventor 何晓莹余虎朱露露王淑花
Owner 浙江中鼎检测技术有限公司
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