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A rapid detection method for svoc in cloth wool samples based on total volatile headspace

A detection method and headspace technology, applied in the field of inspection and quarantine, can solve problems such as difficult detection, and achieve the effects of improving detection efficiency, simple operation, and high detection sensitivity

Active Publication Date: 2019-07-09
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this limits the detection of semivolatiles with higher boiling points (SVOC, boiling point between 250°C and 400°C), because under low temperature equilibrium conditions, the volatilization of semivolatiles is negligible and difficult to detect

Method used

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  • A rapid detection method for svoc in cloth wool samples based on total volatile headspace
  • A rapid detection method for svoc in cloth wool samples based on total volatile headspace
  • A rapid detection method for svoc in cloth wool samples based on total volatile headspace

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] A method for rapid detection of SVOC in velvet samples based on full-volatility headspace, comprising the steps of: pulverizing the velvet sample to a particle size of less than 2 mm, mixing, and accurately weighing 20 mg of the sample, accurate to 0.1 mg, placing it in Add 20 μL of acetone solvent to a 20mL headspace bottle, quickly seal the headspace bottle, and place it in a 44-position headspace autosampler. A gas-solid equilibrium is formed. At this time, the partial pressure of the SVOC to be measured in the headspace gas is proportional to its content in the sample, and all of it is transferred to the gas phase or part of it remains in the sample. 1mL of the gas in the quantitative loop is introduced into the gas chromatograph-mass spectrometer for detection. The chromatographic retention time and characteristic ions of each substance are qualitative, and the standard curve method of blank matrix is ​​used for quantification.

[0071] Gas chromatography-mass spe...

Embodiment 2

[0096] A method for rapid detection of SVOC in velvet samples based on full-volatility headspace, comprising the steps of: pulverizing the velvet sample to a particle size of less than 2 mm, mixing, and accurately weighing 20 mg of the sample, accurate to 0.1 mg, placing it in Add 20 μL of acetone solvent to a 20mL headspace bottle, quickly seal the headspace bottle, and place it in a 44-position headspace autosampler. A gas-solid equilibrium is formed. At this time, the partial pressure of the SVOC to be measured in the headspace gas is proportional to its content in the sample, and all of it is transferred to the gas phase or part of it remains in the sample. 1mL of the gas in the quantitative loop is introduced into the gas chromatograph-mass spectrometer for detection. The chromatographic retention time and characteristic ions of each substance are qualitative, and the standard curve method of blank matrix is ​​used for quantification.

[0097] Gas chromatography-mass spe...

Embodiment 3

[0122] The difference from Example 1 is that in the headspace condition of the headspace sampler:

[0123] Equilibrium temperature: 180°C;

[0124] Quantitative loop temperature: 190°C;

[0125] Transmission line temperature: 200°C;

[0126] Others are with embodiment 1.

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Abstract

The present invention discloses a method for rapidly detecting semi-volatile organic matters (SVOC) in a flannel sample based on full volatilization headspace. The method comprises: crushing a flannel sample, uniformly mixing, placing into a headspace bottle, adding an acetone solvent, rapidly sealing the headspace bottle, placing into a 44-bit headspace autosampler, volatilizing SVOC to be detected from the sample under a set headspace condition, and rapidly forming gas-solid balance in the bottle, wherein the partial pressure of the SVOC to be detected in the headspace gas is proportional to the content of the SVOC to be detected in the sample; and completely transferring into a gas phase or partially remaining in the sample, introducing the gas in a quantitation ring into a gas chromatography-mass spectrometer to detect, carrying out qualitation through the chromatographic retention times of various substances and characteristic ions, and carrying out quantitation by using a blank matrix standard addition standard curve method. According to the present invention, the method has advantages of simple operation, time saving, and environment protection.

Description

technical field [0001] The invention relates to the field of inspection and quarantine, in particular to a rapid detection method for semi-volatile organic compounds (SVOC) in cloth samples based on fully volatile headspace. Background technique [0002] The detection of organic chemical substances in velvet samples usually requires pretreatment of the samples. On the one hand, the analytes in the samples are extracted, and on the other hand, impurities are removed as much as possible, so that the analytes exist in a cleaner extraction solution. middle. Among the commonly used pretreatment techniques, ultrasonic extraction and solid-phase extraction are more complicated, which are easy to introduce errors and impurities, and consume a large amount of organic solvents; solid-phase microextraction has high sensitivity and is relatively environmentally friendly, but its reproducibility is relatively poor. Headspace extraction technology is simple to operate, highly automated, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/02G01N30/88
CPCG01N30/02G01N30/88G01N2030/884
Inventor 王志娟吕庆张庆李海玉白桦
Owner CHINESE ACAD OF INSPECTION & QUARANTINE