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Method for determining mercury content in textile auxiliary through microwave digestion-atomic fluorescence spectrophotometry

A technology of textile auxiliaries and atomic fluorescence, which is applied in the field of microwave digestion-atomic fluorescence spectrophotometry (AFS) to determine the mercury content in textile auxiliaries, can solve the problems of low sensitivity detection limit and achieve high sensitivity, low detection limit, Analyzing fast results

Active Publication Date: 2015-02-25
THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In order to solve the problem of the detection method of mercury content in textile auxiliaries, the object of the present invention is to provide a method for measuring mercury content in textile auxiliaries by microwave digestion-atomic fluorescence spectrophotometry (AFS), which has high sensitivity, detection Low limit and accurate, fast and simple features

Method used

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  • Method for determining mercury content in textile auxiliary through microwave digestion-atomic fluorescence spectrophotometry

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Sample: water-based flame retardant adhesive TF-681, suspension, industrial product, produced by Zhejiang Transfar Co., Ltd.

[0048] 1. Sample pretreatment method

[0049]1. Preparation of test solution

[0050] Weigh 0.2502g sample of water-based flame retardant adhesive TF-681, place it in a microwave digestion tube, add 3 mL nitric acid (mass concentration 65-68%), 2 mL hydrogen peroxide (mass concentration 30%), 2 mL fluoroboric acid (mass concentration 49.5~50.5%), after covering the safety valve, put the digestion tube into the microwave digestion instrument, and keep it at 195°C for 15 minutes. After the solution was cooled to room temperature after digestion, the solution was transferred to a 25 mL volumetric flask, made up to volume with deionized water, and filtered through a water membrane before use.

[0051] Take 5.00 ml of digestion solution, dilute to 10.00 ml with water, shake well and let it stand for 1 hour, the test solution is to be tested.

[00...

Embodiment 2

[0095] Sample: salt-resistant high-temperature leveling agent TF-212B, brown solution, industrial product, produced by Zhejiang Transfar Co., Ltd.

[0096] 1. Sample pretreatment method

[0097] 1. Preparation of test solution

[0098] Weigh 0.2003g sample of salt-resistant high-temperature leveling agent TF-212B, place it in a microwave digestion tube, add 3 mL nitric acid (mass concentration 65~68%), 2 mL hydrogen peroxide (30%), 2 mL fluoroboric acid (mass concentration 49.5~50.5%), after covering the safety valve, put the digestion tube into the microwave digestion instrument, and keep it at 190°C for 20 minutes. After the solution was cooled to room temperature after digestion, the solution was transferred to a 25 mL volumetric flask, made up to volume with deionized water, and filtered through a water membrane before use.

[0099] Take 5.00 ml of digestion solution, dilute to 10.00 ml with water, shake well and let it stand for 1 hour, the test solution is to be tested...

Embodiment 3

[0131] Sample: fluorescent whitening agent TF-351, yellow-green suspension, industrial product, produced by Zhejiang Transfar Co., Ltd.

[0132] 1. Sample pretreatment method

[0133] 1. Preparation of test solution

[0134] Weigh 0.3000g fluorescent whitening agent TF-351 sample, put it in a microwave digestion tube, add 3 mL nitric acid (mass concentration 65~68%)), 2 mL hydrogen peroxide (mass concentration 30%), 2 mL fluorine Boric acid (mass concentration 49.5~50.5%), after covering the safety valve, put the digestion tube into the microwave digestion apparatus, and keep it at 200°C for 10 minutes. After the solution was cooled to room temperature after digestion, the solution was transferred to a 25 mL volumetric flask, made up to volume with deionized water, and filtered through a water membrane before use.

[0135] Take 5.00 ml of digestion solution, dilute to 10.00 ml with water, shake well and let it stand for 1 hour, the test solution is to be tested.

[0136] 2....

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Abstract

The invention discloses a method for determining the mercury content in a textile auxiliary through a microwave digestion-atomic fluorescence spectrophotometer. The method consists of: subjecting a textile auxiliary sample to microwave digestion by nitric acid, hydrogen peroxide as well as fluoroboric acid and filtration, then adding sodium borohydride to reduce ionic mercury to atomic mercury, and by means of a set atomic fluorescence spectrophotometer and under a fluorescence wavelength of 253.7nm, determining the mercury content by comparing a standard curve. The method provided in the invention can determine the content of mercury in the textile auxiliary on the atomic fluorescence spectrophotometer only by simple pretreatments, and the method has the advantages of fast analysis speed, good stability, high sensitivity, low detection limit to 0.005mg / kg, and recovery rate of 87.8%-105.3%. The invention is sufficient to satisfy the requirements for textile auxiliary detection, and is suitable for detection of the heavy metal item mercury in a textile auxiliary.

Description

technical field [0001] The invention relates to a method for measuring mercury content in textile auxiliaries, in particular to a microwave digestion-atomic fluorescence spectrophotometry (AFS) method for measuring mercury content in textile auxiliaries. Background technique [0002] Mercury is harmful to the human body and is cumulative in the human body. Once absorbed by the human body, it will accumulate in the liver, bones, kidneys, heart and brain of the human body. When it reaches a certain level, it will cause irreversible damage to human health, especially for children. very. Therefore, in domestic and foreign laws and regulations, mercury content is an indicator that is required to be tested frequently. GB / T 18885 "Technical Requirements for Ecological Textiles" and Oeko-Tex Standard 100 General and special conditions strictly stipulate that different target textiles include mercury The limit value of heavy metals including mercury, FZ / T 81014 "clothes for infants ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
Inventor 谢维斌刘婷吴俭俭赵珊红
Owner THE INSPECTION & QUARANTINE TECH CENT ZHEJIANG ENTRY EXIT INSPECTION & QUARANTINE BUREAU
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