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Kit for detecting trace hexavalent chromium in sample by LC-ICPMS (liquid chromatograph-inductively coupled plasma-mass spectrometer), and detection method of hexavalent chromium

A technology for detecting samples and hexavalent chromium, applied in measuring devices, instruments, scientific instruments, etc., can solve problems such as interference, insufficient sensitivity, lack of detection technology, etc., and achieve low detection limit, strong anti-interference ability, and pretreatment. simple effect

Active Publication Date: 2014-11-05
广州谱临晟科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Sensitivity is not high enough: the detection limit cannot meet the needs of some samples. 10μg / L samples cannot be accurately quantified;
[0005](2) There are interference factors: if the sample itself is colored, it will also absorb light at 540nm, which will cause serious interference. In addition, if there are other Oxidants (such as ferric iron, pentavalent vanadium, etc.) can also oxidize diphenylcarbohydrazide and form colored complexes, so they can also cause serious interference;
[0006](3) Long time-consuming: the experiment process needs to mix and react the sample and the color reagent (diphenylcarbohydrazide) for 15 minutes, and the color development process Factors such as temperature and pH value will affect the experimental results.
[0007] At present, trace amounts of hexavalent chromium (less than 10μg / L) may be contained in samples such as water, toys, and food, and the hexavalent chromium in these samples is usually Extract with water, organic solvent, acid or salt solution, etc., filter or centrifuge to obtain the extract, which contains trace amounts of hexavalent chromium, and some samples (such as toys, food) also have a large amount of matrix interference. There is still a lack of effective detection technology for the detection of chromium

Method used

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  • Kit for detecting trace hexavalent chromium in sample by LC-ICPMS (liquid chromatograph-inductively coupled plasma-mass spectrometer), and detection method of hexavalent chromium
  • Kit for detecting trace hexavalent chromium in sample by LC-ICPMS (liquid chromatograph-inductively coupled plasma-mass spectrometer), and detection method of hexavalent chromium
  • Kit for detecting trace hexavalent chromium in sample by LC-ICPMS (liquid chromatograph-inductively coupled plasma-mass spectrometer), and detection method of hexavalent chromium

Examples

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Embodiment 1

[0037] Taking the trace amount of hexavalent chromium in the detection standard as an example, the kit provided in this embodiment contains the following reagents:

[0038] (1) pH regulator ammonia for adjusting the pH value of the sample solution to be tested greater than 6.8;

[0039] (2) Oxygenate ammonium nitrate for LC mobile phase;

[0040] (3) Alkanol-containing quaternary amine resins used to fill anion-exchange chromatographic columns;

[0041] (4) Purifying agent aluminum nitrate used to purify the sample solution to be tested.

[0042] The method for detecting trace amounts of hexavalent chromium in the standard substance provided by the HPLC-ICPMS method provided by the present embodiment comprises the following steps:

[0043] (1) Take 100ppm hexavalent chromium standard solution and dilute to 0.025ppb;

[0044] (2) Take 2mL of the above solution, add 0.1mL of the purification agent aluminum nitrate in the above kit, and then add 0.2mL of the pH regulator ammonia...

Embodiment 2

[0055] Taking the detection of trace amounts of hexavalent chromium in toys as an example, the kit provided in this embodiment contains the following reagents:

[0056] (1) pH regulator ammonia for adjusting the pH value of the sample solution to be tested greater than 6.8;

[0057] (2) Oxygenate ammonium sulfate used in LC mobile phase;

[0058] (3) Alkyl-containing quaternary ammonium resins used to fill anion-exchange chromatographic columns;

[0059] (4) Purifying agent aluminum sulfate for purifying the sample solution to be tested;

[0060] (5) Matrix matching agent The matrix matching agent is ammonium chloride.

[0061] The method for detecting trace amounts of hexavalent chromium in a sample by LC-ICPMS method provided in this embodiment includes the following steps:

[0062] (1) Take the toy sample, first carry out extraction treatment, the extract is 70mM hydrochloric acid, take 0.1g sample and extract with 5mL70mM hydrochloric acid for 2 hours, then filter to o...

Embodiment 3

[0076] Taking the detection of trace amounts of hexavalent chromium in water samples as an example, the kit provided in this embodiment contains the following reagents:

[0077] (1) pH regulator sodium hydroxide and acetic acid for adjusting the pH value of the sample solution to be tested greater than 6.8;

[0078] (2) Oxyacid ammonium bicarbonate used in LC mobile phase;

[0079] (3) Alkyl-containing quaternary ammonium resins used to fill anion-exchange chromatographic columns;

[0080] (4) Purifying agent bismuth nitrate for purifying the sample solution to be tested;

[0081] The method for detecting trace amounts of hexavalent chromium in a sample by LC-ICPMS method provided in this embodiment includes the following steps:

[0082] (1) Take water samples, filter and wait for treatment;

[0083] (2) Take 2mL water sample, add 0.1mL purifying agent bismuth nitrate in the kit, then add 0.2mL pH regulator sodium hydroxide and acetic acid in the above kit to adjust the pH ...

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Abstract

The invention discloses a kit for detecting trace hexavalent chromium in a sample by an LC-ICPMS (liquid chromatograph-inductively coupled plasma-mass spectrometer). The kit contains the following reagents: (1) a pH value regulator for regulating the pH value of a sample solution to be detected to be greater than 6.8; (2) an oxysalt for an LC mobile phase; and (3) a quaternary alkanol amine or alkyl quaternary amine containing resin for filling an anion exchange column. The invention also discloses a method for detecting the trace hexavalent chromium in the sample by using the kit. The kit has the advantages of low detection limit, strong anti-interference ability, quickness and the like by combining with the detection method.

Description

technical field [0001] The invention belongs to the technical field of detection methods for hexavalent chromium, and in particular relates to a kit for detecting trace amounts of hexavalent chromium in samples by LC-ICPMS and a detection method for hexavalent chromium. Background technique [0002] Existing methods for detecting hexavalent chromium mainly use spectrophotometry (for example, the national standard "GBT 17593.3-2006 Textiles - Determination of heavy metals - Part 3: Hexavalent chromium - Spectrophotometry"). The detection principle of the spectrophotometric method is to use hexavalent chromium to have strong oxidizing properties. It can oxidize diphenylcarbohydrazide in an acidic environment and form a colored complex. Measure its light absorption at 540nm, thereby Quantitative analysis by Lambert-Beer's law. [0003] But this method has the following disadvantages: [0004] (1) The sensitivity is not high enough: the detection limit cannot meet the needs of...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/14G01N30/26
Inventor 林建贤
Owner 广州谱临晟科技有限公司