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Detection method of annular methylsiloxane in sediment

A technology of methyl siloxane and detection method, which can be used in measurement devices, instruments, scientific instruments, etc., and can solve the problems of long detection time and inability to accurately qualitative and quantitative

Inactive Publication Date: 2016-03-23
HARBIN INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] The purpose of the present invention is to solve the problem that the existing method for detecting methylsiloxane has a long detection time and cannot be accurately qualitative and quantitative when there are impurities, and provides a method for detecting cyclic methylsiloxane in bottom mud. Detection method

Method used

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  • Detection method of annular methylsiloxane in sediment
  • Detection method of annular methylsiloxane in sediment
  • Detection method of annular methylsiloxane in sediment

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specific Embodiment approach 1

[0017] Specific embodiment one: the detection method of cyclomethylsiloxane in a kind of bottom mud of this embodiment is carried out according to the following steps:

[0018] 1. Use the vibration extraction method to pretreat the sample to be tested: ① freeze-dry the sediment sample to obtain the sample to be tested; ② use the extraction liquid to extract the sample to be tested obtained in step ① for the first time, and shake for 25 minutes during extraction ~ 35min, then centrifuged at a centrifugal speed of 2500r / min ~ 3500r / min for 10min ~ 15min, after static layering, the first organic phase and the first residual phase are obtained; the volume of the extract is the same as that of the sample to be tested The ratio of mass is 25mL: (1~2) g; The extract is a mixture of acetone and n-hexane, and the volume of acetone and n-hexane in the extract is equal; Extract the remaining phase, shake it for 25min to 35min during extraction, then centrifuge for 10min to 15min at a cen...

specific Embodiment approach 2

[0022] Specific embodiment two: the difference between this embodiment and specific embodiment one is: Step 1. 1. carry out freeze-drying process to the sediment sample, and the described freeze-drying process is: earlier the sediment sample is pre-frozen in the cold trap for 3 hours until completely frozen, and then vacuum-dry the completely frozen sediment samples at a vacuum degree of 9 Pa, at a temperature of -60°C, and for 20 hours. Other steps and parameters are the same as those in the first embodiment.

specific Embodiment approach 3

[0023] Embodiment 3: This embodiment differs from Embodiment 1 or Embodiment 2 in that: in step 1, a rotary evaporator is used to concentrate the organic phase added with isooctane, and the temperature of the water bath is set at 28°C. Other steps and parameters are the same as those in Embodiment 1 or 2.

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Abstract

The invention relates to a detection method of annular methylsiloxane in sediment, and aims at solving the problems that for an existing method for detecting methylsiloxane, the detection time is long, and accurate qualitativeness and quantification analysis cannot be achieved when impurities exist. The method comprises the steps that 1, a sample to be detected is pretreated through an oscillation extraction method; 2, GC-MS-MS instrument parameters are set; 3, a standard solution is detected; 4, the sample to be detected is detected. The method for detecting the annular methylsiloxane in the sediment has the advantages that the detection time is short, operation is easy, the pretreatment effect is good, interference can be effectively eliminated, and qualitativeness and quantification to the annular methylsiloxane are accurate.

Description

technical field [0001] The invention relates to a method for detecting cyclomethylsiloxane. Background technique [0002] Methylsiloxane is an artificially synthesized compound in which silicon and oxygen atoms are arranged alternately as a skeleton, and silicon atoms are directly connected with methyl groups. The molecular structure is divided into chain and ring. The total output value of cyclic methyl siloxane in my country accounts for about 1 / 2 of the world's total output value, ranking first in the world. Cyclomethicones are ubiquitously present in all silicone substances and in most cosmetic and personal care products. In 2008, the Canadian Ministry of Environment, the Ministry of Health, and the European Union conducted risk assessments on some silicones in 2009, and agreed that volatile methylsiloxanes are priority pollutants in the environment and included in the "substantial elimination" list. Cyclic methyl siloxanes are more harmful than chains, and are reprod...

Claims

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Application Information

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IPC IPC(8): G01N30/88
CPCG01N30/88G01N2030/884
Inventor 任南琪王艺张子峰陈川李一凡徐熙俊张若晨谢鹏
Owner HARBIN INST OF TECH
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