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Preparation method of 6N copper sample for GDMS detection and low-S testing method

A sample and volume ratio technology, applied in measuring devices, material analysis by electromagnetic means, instruments, etc., can solve problems such as long stability time of element detection values, influence of soaking time detection results, easy failure of sulfur removal package, etc., to achieve enhanced Test stability, good anti-oxidation effect, and shorten the test time

Pending Publication Date: 2021-09-24
紫金矿业集团黄金冶炼有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The traditional sample treatment method adopts pickling after grinding. The defect is that Si and Al in the sandpaper are easily introduced during the sample grinding process, and the introduced amount is easily higher than the content of the element in the sample itself, resulting in high detection values ​​or element detection values. The stability time is long. In addition, different acids and the length of immersion time also have a certain impact on the test results
[0005] In the GDMS testing industry, the S element background value of the equipment itself has always been a controversial point, because the equipment itself has a certain S element background value, including graphite cones, graphite tubes, and graphite caps of equipment parts, which may have little effect on ordinary sample testing. However, the detection of high-purity samples, especially 6N copper, is particularly important. At present, the desulfurization package is commonly used in the industry for equipment S reduction treatment, but the disadvantage is that the desulfurization package is prone to failure as time goes by.

Method used

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  • Preparation method of 6N copper sample for GDMS detection and low-S testing method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The preparation method of the 6N copper sample that is used for GDMS detection can effectively suppress the oxidation of high-purity copper and does not introduce other impurities, comprising the following steps:

[0035] Step 1: configure nitric acid solution according to the volume ratio of nitric acid: pure water=3:1;

[0036] Step 2: Soak the 6N copper sample to be tested in the nitric acid solution prepared above for 1-2 minutes;

[0037] Step 3: configure citric acid solution by volume ratio citric acid: water=3:1;

[0038] Step 4: Put the 6N copper sample soaked in Step 2 into the citric acid solution prepared in Step 3 and soak for 15 minutes;

[0039] Step 5: Take out the 6N copper sample soaked in step 4, rinse it with pure water, wipe it with a dust-free cloth, and then wipe it with alcohol;

[0040] Step 6: Bake the 6N copper sample treated above in an oven at a temperature of 45° C. for 20 minutes to obtain a 6N copper sample for GDMS detection.

Embodiment 2

[0042] The preparation method of the 6N copper sample that is used for GDMS detection, wherein the nitric acid solution is configured by volume ratio nitric acid: pure water=5:1 in the step 1; In the step 3, the citric acid solution is configured according to the volume ratio citric acid: water=5:1 Configuration; the rest of the steps are the same as in Embodiment 1.

Embodiment 3

[0044] The preparation method of the 6N copper sample that is used for GDMS detection, wherein the nitric acid solution is configured by volume ratio nitric acid: pure water=8:1 in the step one; In the step three, the citric acid solution is configured by volume ratio citric acid: water=8:1 ratio Configuration; the rest of the steps are the same as in Embodiment 1.

[0045] Table 1

[0046]

[0047] It can be seen from Table 1 that the implementation cases are better than the comparison cases of common methods, and the comprehensive quality index of embodiment 2 is the best, and embodiment 2 is the best embodiment.

[0048] Low S test method for 6N copper samples:

[0049] Example 1

[0050] The test method of 6N copper sample: comprise the following steps:

[0051] Step 1: 6N copper sample to be measured is carried out pre-sputtering 5min in GDMS equipment;

[0052] Step 2: After pre-sputtering, take out the graphite cone and cap parts in the GDMS equipment, clean the ...

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Abstract

The invention relates to a preparation method for detecting a 6N copper sample through adoption of GDMS and a low-S testing method, and relates to the technical field of high-purity metal component analys. The preparation method comprises the steps of: putting the 6N copper sample into a nitric acid solution and a citric acid solution to be soaked for 10-20 min; and taking out, washing with pure water, wiping with dust-free cloth, and wiping with alcohol. The low-S test method comprises the following steps: pre-sputtering a 6N copper sample to be tested in GDMS equipment for 5-15 minutes; after pre-sputtering, graphite cone and cap parts in the GDMS equipment are taken out and cleaned up, and then the graphite cone and cap parts are reinstalled on the GDMS equipment for detection; and testing the 6N copper sample according to GDMS normal test steps. According to the preparation method, oxidation of the high-purity copper can be effectively inhibited, other impurities are not introduced, the S element of equipment can be effectively reduced through the low-S testing method, therefore, the testing time of GDMS on the high-purity copper sample is shortened, and accuracy and stability are improved.

Description

technical field [0001] The invention relates to the technical field of high-purity metal component analysis, in particular to a method for preparing a 6N copper sample for GDMS detection and a low S test method. Background technique [0002] Copper is a transition element. The continuous development of science and technology has put forward an urgent requirement for the improvement of material purity. The application of 6N high-purity copper (99.9999%) has been widely valued. High-purity copper has good ductility, good thermal and electrical conductivity, and is widely used in the semiconductor optoelectronic industry. [0003] GDMS is the abbreviation of glow discharge mass spectrometry (glow discharge mass spectrometry). It is an analytical method that uses a glow discharge source as an ion source to connect with a mass spectrometer for mass spectrometry. It is the most effective means for analyzing the composition of high-purity metal materials. It has the characteristic...

Claims

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Application Information

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IPC IPC(8): G01N27/68
CPCG01N27/68
Inventor 钟美娟廖汉祥吴卫煌温才英丁强李茂源廖剑平
Owner 紫金矿业集团黄金冶炼有限公司