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A method for determining hexavalent chromium in leather

A determination method and hexavalent chromium technology, applied in the field of leather analysis, can solve the problems of difficulty in meeting the limit detection requirements, complex and time-consuming sample processing, low resolution, etc., and achieve good economic and social benefits, detection limit and quantification limit. Low, high sensitivity effect

Active Publication Date: 2017-05-31
GUANGZHOU QUALITY SUPERVISION & TESTING INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Spectrophotometry and atomic absorption spectrometry are susceptible to the interference of dyes in leather, and trivalent chromium needs to be removed before the measurement, and the resolution is low, so it is difficult to meet the limited detection requirements; liquid chromatography requires derivatization treatment, and the operation is cumbersome; ion chromatography The method only relies on retention time for qualitative analysis and is susceptible to the interference of coexisting ions; the inductively coupled plasma mass spectrometry needs to digest the sample, and the sample pretreatment is complicated and time-consuming

Method used

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  • A method for determining hexavalent chromium in leather
  • A method for determining hexavalent chromium in leather
  • A method for determining hexavalent chromium in leather

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0046] The establishment of hexavalent chromium reference substance chromatogram comprises the following steps:

[0047] (1) Preparation of standard working solution of hexavalent chromium:

[0048] The potassium dichromate reference substance was dried at 102°C for 16 hours, weighed 2.829g (accurate to 0.0001g) of the dried potassium dichromate reference substance, dissolved in ultrapure water, transferred to a 1000mL volumetric flask, and added ultrapure water Constant volume, prepared into 1mg / mL (calculated as Cr) hexavalent chromium standard stock solution;

[0049] Dilute the hexavalent chromium standard stock solution step by step with ultrapure water into hexavalent chromium standard working solutions with concentrations of 0, 0.02, 0.05, 0.1, 0.5, and 1.0 mg / L.

[0050] (2) Ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry:

[0051] Perform ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry on the standard...

Embodiment 2

[0078] This embodiment is an example of the extraction and determination of hexavalent chromium in the bovine leather control sample, comprising the following steps:

[0079] (1) Preparation of test solution:

[0080] Chop the cow leather control sample to a size of 3mm×3mm, weigh 2.0g (accurate to 0.01g) of the chopped cow leather control sample in a 250mL Erlenmeyer flask with a stopper, blow in nitrogen for 5min, and add ultrapure water (Ammonia water to adjust the pH to 8.0) 100mL, continue to pass through nitrogen for 5min, cover the ground bottle stopper, shake and extract for 3h at 25°C, and shake at a frequency of 100min -1 , take the supernatant and adjust the pH to 8.0 with formic acid or ammonia water, and pass through a 0.22 μm polytetrafluoroethylene filter membrane to obtain a test solution for testing.

[0081] (2) Ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry conditions

[0082] With embodiment 1.

[0083] (3) Determination...

Embodiment 3

[0086] This embodiment is an example of the extraction and determination of hexavalent chromium in a bovine leather sample with an added concentration of hexavalent chromium of 0.25mg / L, including the following steps

[0087] (1) Preparation of test solution

[0088] Accurately weigh 2.0 g of the negative bovine leather control sample processed in Example 2 in a 250 mL conical flask with a stopper, add 25 μL of a hexavalent chromium standard stock solution with a concentration of 1.0 mg / mL to the sample, Then the added concentration of hexavalent chromium is 0.25mg / L. Subsequent treatment was the same as in Example 2 to obtain a test solution.

[0089] (2) Ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry conditions

[0090] With embodiment 1.

[0091] (3) Determination of recovery rate:

[0092] Carry out ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry to the test solution according to the conditions of step ...

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Abstract

The invention relates to a method for measuring hexavalent chromium in leather. The method is characterized in that the hexavalent chromium in the leather is subjected to oscillation extraction through ultrapure water, and ultra-high performance liquid chromatography-mass spectrometry / mass spectrometry measurement is performed in a multiple reaction monitoring (MRM) mode. The sample pretreatment method is simple, has high recovery rate, low substrate interference, low detection limit, high accuracy and good economic and social benefits, the blank of the conventional liquid chromatography-mass spectrometry / mass spectrometry measurement of the hexavalent chromium in the leather is filled, the defects in the conventional method for measuring the hexavalent chromium in the leather are overcome, and important technical support is provided for safe detection of leather quality.

Description

technical field [0001] The invention relates to the field of leather analysis, in particular to a method for determining hexavalent chromium in leather. Background technique [0002] The processing of leather requires the use of chromium salt as a tanning agent. Although the chromium in chromium salt is trivalent chromium, it is easily converted into hexavalent chromium in a strong oxidizing environment. Trivalent chromium is an essential trace element for the human body, and hexavalent chromium is easily absorbed by the human body through the cell membrane, interfering with the normal physiological process in the human body, and is an inducing factor for carcinogenesis and mutagenesis, and will lead to death when the concentration is high. Domestic QB / T2880-2007 "Children's Leather Shoes" has a limit of 10mg / kg for hexavalent chromium, and EU REACH regulations require that the content of hexavalent chromium in leather products or parts that come into contact with the skin s...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88G01N30/06
CPCG01N30/06G01N30/88
Inventor 罗海英孙世彧吴楚森韩婉清吴玉銮郭新东侯向昶
Owner GUANGZHOU QUALITY SUPERVISION & TESTING INST
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