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Method for detecting organophosphate flame retardant

A technology of organic phosphate ester and flame retardant, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effect of accurate method, high sensitivity, and simple sensitivity

Inactive Publication Date: 2014-03-05
PEOPLES REPUBLIC OF CHINA BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] At present, the analysis of organophosphorus flame retardants mainly focuses on the research on textiles, plastic products and environmental samples (environmental water samples, atmospheric air and soil and sediments), while at the same time, tris(2-chloroethyl) phosphate in children's toys There is no report on the detection of various chlorine-based organophosphorus flame retardants such as ester, tris(2-chloro-1-methylethyl) phosphate and tris(1,3-dichloroisopropyl) phosphate.

Method used

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  • Method for detecting organophosphate flame retardant
  • Method for detecting organophosphate flame retardant
  • Method for detecting organophosphate flame retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1: Determination of the contents of three chlorine-based organic flame retardants in toy samples

[0037]1. Sample treatment: Accurately weigh 1.0g sample, put it in a microwave extraction tank, add 15mL acetone, vortex for 2min, microwave extraction at 75°C for 20min, collect the extract into a chicken heart bottle; use 15mL acetone for the second For the second extraction, microwave extraction at 75°C for 20 minutes, combine the two extracts, rotary evaporate to 1mL, and then blow dry with a nitrogen blower; use 1mL acetone to make up volume, and filter with a 0.20μm microporous membrane to obtain a sample solution;

[0038] 2. Prepare standard working solution: Weigh 25mg (accurate to 0.1mg) tris(2-chloroethyl)phosphate, tris(2-chloro-1-methylethyl)phosphate and tris(1,3 - dichloroisopropyl) ester standard substance, is mixed with acetone respectively to the standard working solution that concentration is 0.1, 0.5, 1.0, 10, 20, 50mg / L;

[0039] 3. Determinat...

Embodiment 2

[0050] Embodiment 2. Extraction condition optimization experiment

[0051] 1. Optimization of extraction solvent

[0052] Considering the chemical properties, price and toxicity of various solvents, the effects of six organic solvents of different polarities on methanol, ethanol, acetone, acetonitrile, n-hexane and ethyl acetate on the resistance of three chlorine-based organophosphorus in the sample were investigated. The extraction effect of fuel. Sample processing was carried out according to the method in Example 1. The experimental results are shown in Table 4. As can be seen from Table 4, the comprehensive extraction efficiency of acetone to the target analyte in children's toys is higher than methanol, ethanol, acetonitrile, n-hexane and ethyl acetate, therefore, the present invention selects acetone as the most preferred extraction solvent.

[0053] Table 4: Extraction recoveries of target analytes by extraction solvent type

[0054]

[0055] 2. Optimization of ...

Embodiment 3

[0059] Embodiment 3: precision and recovery rate experiment

[0060] Using the method of Example 1, the standard addition recovery experiment was carried out on the blank sample of children's toys not containing chlorine-based organophosphate flame retardants. The recovery rate and precision results of 6 parallel determinations are shown in Table 5, and the precision data table is shown in Table 6.

[0061] Table 5: Recovery and precision (n=6)

[0062]

[0063] Table 6: Precision data table (1mg / L TCEP, TCPP and TDCP)

[0064]

[0065] The recovery rate of standard addition of this method is between 82.0% and 94.2%, and the relative standard deviation is 4.63% to 7.96%. The method is accurate, fast, simple and sensitive, and can be used for the actual detection of chlorine-based organophosphate flame retardants in children's toys.

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Abstract

The invention discloses a method for detecting an organophosphate flame retardant, belonging to the field of inspection and detection. The method for detecting the organophosphate flame retardant comprises the steps of (1) treating a sample; (2) preparing a standard working solution; (3) determining the standard working solution and a sample solution by using a gas chromatography-mass spectrometry; (4) acquiring an equation of linear regression and a standard curve of the organophosphate flame retardant by using detection data of the standard working solution, and acquiring the content of the organophosphate flame retardant in the sample by using detection data of the sample solution through the equation of linear regression or the standard curve. The method disclosed by the invention has the advantages of accuracy, fastness, simplicity, convenience and high sensitivity.

Description

technical field [0001] The invention relates to a method for detecting an organic phosphate flame retardant, belonging to the technical field of inspection and detection. Background technique [0002] Phosphate ester flame retardants have the characteristics of long-lasting flame retardant effect, good compatibility with polymer substrates, water resistance, weather resistance, heat resistance and migration resistance, and are a class of flame retardants with great potential. Studies have found that halogen-containing phosphate flame retardants have better flame retardant effects due to the synergistic effect of phosphorus-halogen. The halogen atoms in such flame retardant molecules are generally Cl and Br. Chlorine-based organic phosphate flame retardants are mainly tris(2-chloroethyl)phosphate (tris(2-chloroethyl)phosphate, TCEP), tris(2-chloro-1-methylethyl)phosphate (tris( 2-chloro-1-methylethyl)phosphate, TCPP), and tris (1,3-dichloroisopropyl) phosphate (tris[2-chloro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06
Inventor 高欣杨晓兵郑如兰李少青刘咏梅
Owner PEOPLES REPUBLIC OF CHINA BEIJING ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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