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Detection method for directly determining trace halogen

A detection method and micro-quantity technology, applied in the detection system field, can solve problems such as low sample volume, harsh test solution requirements, and low atomization efficiency, and achieve the effect of improving measurement sensitivity, improving analysis sensitivity, and broad application value

Active Publication Date: 2020-05-29
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

A conventional sampling system includes a spray chamber, a nebulizer, a peristaltic pump and a pump tube. The concentric nebulizer is the core component of the sampling system. It has the advantages of simple structure and convenient operation. (Generally only about 3% of the aerosol enters the ICP, and most of the solution flows away as waste liquid), easy to block, and harsh requirements for the test solution (high-salt solution is easy to deposit at the nozzle), etc.
[0005]Liquid sampling is the most common and mature method of ICP-OES at present. When using conventional liquid sampling, the atomization efficiency is only about 1-5%, and most of the solution is The waste liquid flows away, and the atomization efficiency is also very low, less than 1%, which makes the detection performance of ICP-OES often fail to meet the test requirements when analyzing elements with low sensitivity (such as halogens), and the sampling system becomes the weak link of the instrument
The above-mentioned aspects make ICP-OES unable to be used for the determination of trace amounts of halogens in samples

Method used

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  • Detection method for directly determining trace halogen
  • Detection method for directly determining trace halogen
  • Detection method for directly determining trace halogen

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0078] This example is based on figure 1 The detection system shown uses the aforementioned detection method provided in this manual to detect bromine and iodine in the sample. The detection device wherein adopts the ICP-OES of Platinum Elmer Company, and the working condition of this detection device is as comparative example 1, and the oxidizing agent in the reaction reagent that the present embodiment adopts is 20mM KMnO 4 Solution, and the kind and concentration of acid used can refer to Table 2, and, in the adopted standard sample, bromine concentration is 10mg / L, and iodine concentration is 1mg / L. As can be seen from Table 2, the test results show that compared with the direct determination of bromine and iodine by the conventional sampling system, the emission intensity of bromine and iodine in this embodiment has been significantly improved, that is, its determination sensitivity has been significantly improved.

[0079] Table 2 to the determination result of bromine ...

Embodiment 2

[0082] This embodiment is basically the same as Embodiment 1. The difference is that the concentration of nitric acid in the reaction reagent used is 4M, and the concentration of the oxidizing agent used can refer to Table 3. And, the bromine concentration in the standard sample adopted is all 1mg / L, and the iodine concentration is all 0.5mg / L. It can be seen from Table 3 that the oxidant KMnO 4 When the concentration is 1-50mM. Referring to Table 3, the test results show that compared with the direct measurement method using a conventional sampling system, the determination sensitivity of bromine and iodine in this embodiment is significantly improved.

[0083] Table 3 is the impact result of the concentration of oxidant on assay effect

[0084]

[0085]

Embodiment 3

[0087] This embodiment is basically the same as Example 1, the difference is that the reaction reagent used in this embodiment is KMnO with a concentration of 2mM 4 solution and a concentration of 4M HNO 3 , Table 4 is the measurement result of bromine and iodine using the present embodiment. It can be seen from Table 4 that the linearity of the bromine and iodine standard solution series at each analysis line is good (R>0.999), which meets the requirements of the ICP-OES quantitative test. In addition, from Table 1 and Table 4, it can be calculated that the sensitivity of the analytical method of the present invention to measure bromine and iodine has improved at least 20 times, and the detection limit of the detection device also obviously reduces (wherein the detection limit of bromine has reduced 26 times, and the detection limit of iodine The limit of detection was reduced by a factor of 14).

[0088] The determination result of table 4 bromine and iodine

[0089]

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Abstract

The invention discloses a detection method for directly determining trace halogen. The detection method comprises stepsof mixing reaction reagent with to-be-detected solution to oxidize halogen ions in the to-be-detected solution to form volatile halogen elementary substances, and introducing the halogen elementary substances into a detection device for detection so as to realize detection of trace halogen. The detection method is advantaged in that analysis sensitivity of a detection device (such as an inductively coupled plasma atomic emission spectrometer) to halogen is greatly improved, moreover, interference of a coexisting matrix to halogen to be detected is reduced. The detection method can be successfully applied to detection of trace halogen in a water sample and has very wide application value in the test industry.

Description

technical field [0001] The invention relates to a sampling device, in particular to a detection method for directly measuring trace halogens, and belongs to the technical field of detection systems. Background technique [0002] At present, the analysis methods used for the determination of trace halogens mainly include photometry, ion chromatography and ICP-MS, among which photometry is cumbersome to operate, the analysis speed is low, and the linear range of the elements to be measured is narrow; ion chromatography requires at least one sample. In more than ten minutes, trace amounts of chlorine, bromine and iodine with higher concentration can be measured simultaneously, but for trace amounts of iodine, an electrochemical detector (such as an amperometric detector) and a corresponding chromatographic column should be used for separate determination, thus further reducing the analysis efficiency . However, ICP-MS interferes with the mass spectrum of polyatomic ions in the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73
CPCG01N21/73
Inventor 柴小丽董亚萍李海军
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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