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Sample preparation method for GDMS detection, and sample

A sample preparation and ultrasonic cleaning technology, which is applied in the sample preparation field of GDMS detection, can solve the problems of low cleanliness, extended detection time, and reduced detection accuracy, so as to improve detection accuracy, ensure cleanliness, improve accuracy and stability sexual effect

Pending Publication Date: 2020-08-14
宁波锦越新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The present invention designs a sample preparation method and sample for GDMS detection, which solves the technical problem that the sample contains residual or embedded inclusions on the surface of the sample or attached trace foreign elements due to mechanical processing, grinding and polishing, and external contact , the low cleanliness of the sample will lead to the extension of the detection time and the reduction of the detection accuracy

Method used

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Examples

Experimental program
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Effect test

preparation example Construction

[0029] A sample preparation method for GDMS detection, comprising the following steps:

[0030] Step 1, using an oil cleaning solution to ultrasonically clean the sample to remove organic matter on the surface of the sample;

[0031] Step 2, using a rinsing solution to rinse the sample after ultrasonic cleaning in step 1 to remove organic residues;

[0032] Step 3, using pickling liquid to ultrasonically pickle the sample washed in step 2;

[0033] Step 4, cleaning the sample after ultrasonic pickling in step 3 with an impurity cleaning solution to remove the pickling solution and impurities remaining on the surface of the sample;

[0034] Step five, drying the sample cleaned in step four.

[0035] In step 1, the oil stain cleaning liquid is acetone or ethanol, preferably acetone, the cleaning temperature of ultrasonic cleaning is 25-30° C., the cleaning time is 4-6 minutes, and the organic matter on the surface is mainly oil stains.

[0036] In step 2, the rinsing liquid i...

Embodiment 1

[0042] A method for preparing an ultra-high-purity aluminum sample for GDMS detection, comprising the following steps:

[0043] Step 1: Use acetone to ultrasonically clean the machined sample to remove organic matter on the surface of the sample. The cleaning temperature of the ultrasonic cleaning is 25° C., and the cleaning time is 4 minutes.

[0044] Step 2, use ultrapure water to rinse the sample after ultrasonic cleaning in step 1 to remove organic residues, the number of rinses is 2 to 4 times, and the resistivity of ultrapure water is ≥ 18.2 MΩ.cm.

[0045] Step 3: Ultrasonic pickling is performed on the sample washed in step 2 with pickling solution. The pickling solution is mixed with nitric acid, hydrochloric acid, and ultrapure water in a volume ratio of 1:3:6. The washing temperature is 25°C, and the ultrasonic pickling time is 1 min.

[0046] Step 4, use ultrapure water to rinse the sample after step 3, the number of rinses is 2 times, and the resistivity is ≥ 18....

Embodiment 2

[0050] Step 1: Use acetone to ultrasonically clean the machined sample to remove organic matter on the surface of the sample. The cleaning temperature of the ultrasonic cleaning is 30° C., and the cleaning time is 6 minutes.

[0051] Step 2: Use ultra-pure water to rinse the sample after ultrasonic cleaning in Step 1 to remove organic residues. The number of rinses is 2 to 4 times, and the resistivity is ≥ 18.2 MΩ.cm.

[0052]Step 3: Ultrasonic pickling is performed on the sample washed in step 2 with pickling solution. The pickling solution is mixed with nitric acid, hydrochloric acid and ultrapure water in a volume ratio of 1:5:7. The washing temperature is 25°C, and the ultrasonic pickling time is 1 min.

[0053] Step 4, use ultrapure water to rinse the sample after step 3, the number of rinses is 4 times, and the resistivity is ≥ 18.2MΩ.cm.

[0054] Step 5: Use absolute ethanol to ultrasonically clean the sample washed in step 4 to further remove the pickling solution and...

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Abstract

The invention relates to a sample preparation method for GDMS detection, and a sample. The method comprises the following steps: 1, carrying out the ultrasonic cleaning on the sample through employingan oil stain cleaning solution to remove organic matters on the surface of the sample; 2, flushing the sample subjected to ultrasonic cleaning in step 1 by using a flushing liquid to remove organic matter residues; 3, carrying out ultrasonic acid washing on the sample washed in step 2 by using an acid washing solution; 4, cleaning the sample subjected to ultrasonic acid washing in step 3 by usingan impurity cleaning solution to remove residual pickling solution and impurities on the surface of the sample; and 5, drying the sample cleaned in step 4. Ultrasonic cleaning and ultrapure water flushing are matched, gas protection is adopted in the drying link, trace impurity elements in an external medium are well relieved, and the accuracy and stability in the detection process are improved.

Description

technical field [0001] The invention relates to the technical field of ultra-high-purity aluminum sample preparation, in particular to a sample preparation method and a sample for GDMS detection. Background technique [0002] GDMS is an abbreviation for glow discharge mass spectrometry. It is an analytical method that uses glow discharge source as an ion source to connect with a mass spectrometer for mass spectrometry. GDMS has gained important applications in many disciplines. In the field of materials science, GDMS has emerged as a tool for the control and characterization of reactive and non-reactive plasma deposition processes. GDMS has become a powerful method for the analysis of impurity components in inorganic solid materials, especially high-purity materials. [0003] The test sample in GDMS is an ultra-pure aluminum test sample. Due to mechanical processing, grinding and polishing, and external contact, the sample contains residual or embedded inclusions or attac...

Claims

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Application Information

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IPC IPC(8): G01N1/34G01N1/44
CPCG01N1/34G01N1/44
Inventor 张瑾叶翔周建波李春生张飞
Owner 宁波锦越新材料有限公司