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Method for determining content of residual methylsiloxane in organosilicon softener by using HS-GC external standard method

A technology of silicone softener and methyl siloxane, applied in the field of analytical chemistry, can solve problems such as damage, complicated operation process, carcinogenicity, etc., and achieve the effect of shortening analysis time, simple and safe method, and high precision

Pending Publication Date: 2020-11-13
ZIBO LURUI FINE CHEM CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, after research, it was found that hexamethylcyclotrisiloxane (hereinafter referred to as D3), octamethylcyclotetrasiloxane (hereinafter referred to as D4), decamethylcyclopentasiloxane (hereinafter referred to as D5) and dodecamethyl Cyclohexasiloxane (hereinafter referred to as D6) has long-term harmful effects on the aquatic environment and has a potential risk of impairing reproductive capacity
It has been reported in the literature that methylsiloxane is also toxic to the nervous, immune and reproductive systems of the human body, and is carcinogenic and mutagenic
Moreover, methyl siloxanes such as D3, D4, D5, and D6 also have high volatility and high diffusion coefficient, which can easily diffuse out of silicone products, thereby entering the human body and causing damage to the environment.
[0003] However, at present, there is little analysis of the residues of D3, D4, D5, and D6 in silicone softeners. Among the few existing analysis methods, a large amount of organic solvents are needed for extraction, the operation process is complicated, and the error is large. Analyzing the experimenter's body is harmful to a certain extent

Method used

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  • Method for determining content of residual methylsiloxane in organosilicon softener by using HS-GC external standard method
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  • Method for determining content of residual methylsiloxane in organosilicon softener by using HS-GC external standard method

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Embodiment 1

[0036] 1. Instrument preparation:

[0037] Adopt Agilent 7890B gas chromatograph, 7697A headspace sampler for headspace injection, equilibrate at 130°C for 30min; the chromatographic column is DB-1701 (or a chromatographic column with equivalent polarity), the column length is 30m, and the inner diameter of the column is 320μm. The initial column temperature is 100°C, keep it for 2min, then increase the temperature to 260°C at a rate of 10°C / min, keep it for 10min, the carrier gas flow rate is 3mL / min; 251, the injection volume is 20μL; the hydrogen flame detector detects its temperature at 260°C, the hydrogen flow rate is 30mL / min, and the air flow rate is 300mL / min.

[0038] 2. Drawing of standard curve

[0039] Prepare standard solutions: Accurately weigh 50 mg of D3, D4, D5, and D6 standard products in beakers, dilute with n-hexane, transfer to a 500mL volumetric flask, adjust the volume of n-hexane to the mark, and prepare 100 mg / L for storage Liquid VI; then accurately...

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Abstract

The invention belongs to the technical field of analytical chemistry, and particularly relates to a method for determining the content of residual methylsiloxane in an organosilicon softener by usingan HS-GC external standard method. A headspace gas chromatograph is used for detection, and an external standard method is used for quantitative analysis. The gas chromatograph is an Agilent gas chromatograph 7890B, the gas chromatographic analysis conditions are as follows: a chromatographic column is DB-1701 or a chromatographic column with equivalent polarity, the column length is 30m, the column inner diameter is 320 microns, the initial column temperature is 100 DEG C, the temperature is kept for 2 minutes, then the temperature is increased to 260 DEG C at the rate of 10 DEG C / min, the temperature is kept for 10 minutes, and the carrier gas flow rate is 3mL / min. The method has the advantages of high precision, good reproducibility, no need of any solvent extraction pretreatment operation on the sample, reduction of the use amount of the organic solvent, shortening of the analysis time, and simplicity and safety.

Description

technical field [0001] The invention belongs to the technical field of analytical chemistry, and in particular relates to a method for determining the content of residual methylsiloxane in silicone softeners by using an HS-GC external standard method. Background technique [0002] Due to the advantages of lubricity, softness, and good hydrophobicity of silicone, silicone softeners are widely used in textile finishing, and they are a type of softener with outstanding performance and effect. The main raw materials for synthesizing silicone softeners are octamethylcyclotetrasiloxane, decamethylcyclopentasiloxane, etc. However, after research, it was found that hexamethylcyclotrisiloxane (hereinafter referred to as D3), octamethylcyclotetrasiloxane (hereinafter referred to as D4), decamethylcyclopentasiloxane (hereinafter referred to as D5) and dodecamethyl Cyclohexasiloxane (hereinafter referred to as D6) has long-term harmful effects on the aquatic environment and has a poten...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02G01N30/06G01N30/16G01N30/86
CPCG01N30/02G01N30/06G01N30/16G01N30/8634G01N2030/047
Inventor 谢瑞丽王艾德刘露露
Owner ZIBO LURUI FINE CHEM CO LTD
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