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ICP-MS measuring method of trace metal impurities in high purity lead

An ICP-MS, trace metal technology, applied in the field of analysis and testing, can solve the problems affecting the measurement accuracy, high detection limit of atomic absorption method, signal suppression, etc., to reduce the memory effect, eliminate the matrix effect, and improve the test accuracy.

Inactive Publication Date: 2009-10-07
NO 53 RES INST OF CHINA NORTH IND GRP
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Problems solved by technology

This method is simple to operate, but the matrix effect is serious. Since the detection limit of the atomic absorption method is relatively high, sample concentration is necessary, and other impurities are easily brought into the concentration process, thereby affecting the measurement accuracy.
[0004] The ICP-MS method has been widely used in the detection of trace and trace elements, but the high total dissolved solids (TDS) will cause the gradual clogging of the sampling cone, which will seriously suppress the signal and cause serious memory effects
Huang Donggen et al. introduced an ICP method using sulfuric acid precipitation to process samples in the article "ICP-MS Determination of Trace and Impurity Components in Lead Grids" ("Physical and Chemical Detection-Chemical Volume" 2006, 42 (1) 31-34). -MS metal impurity detection method, using the sulfuric acid precipitation method to remove a large amount of lead, and then use the ICP-MS method to detect the metal impurities, due to the complexity of the sulfuric acid matrix spectrum, it is easy to produce polyatomic ion interference, thus affecting the measurement accuracy

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Embodiment Construction

[0014] The technical solution involved in the invention will be further described below in conjunction with specific embodiments, but not as a limitation to the content of the invention.

[0015] Taking the test of Fe, Zn, Sn, Cu, Al, Bi, Mg, Sb, As and Ag elements in high-purity lead as an example, the technical solution involved in the invention is described in detail.

[0016] a. Sample treatment: Weigh 1 to 2 g of high-purity lead (accurate to 0.0002 g), and add 40 mL of 1:10 (nitric acid: water) high-purity nitric acid to a 400 mL clean quartz beaker. Prepared by sub-boiling distillation), heated below 50°C until completely dissolved, and added 200mL of sub-boiling distilled water.

[0017] Move the quartz beaker containing the sample to the electrolyzer, add the cleaned stirring magnet to stir, insert the clean platinum mesh electrode, electrolyze for 5 hours under the electrolytic current of 1.2A, and take it out quickly without cutting off the power supply. Electrode,...

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Abstract

The invention relates to an ICP-MS measuring method of trace metal impurities in high purity lead, which adopts a high-purity nitric acid dissolving sample and uses the electrolytic method to remove lead in the high purity nitric acid dissolving sample, and utilizes inductive coupled plasma mass spectrometer and adopts peak jumping mode to scan and test blank, work-curve standard solution and sample elements to be detected so as to obtain the content of the elements to be detected. The ICP-MS measuring method of trace metal impurities in high purity lead is convenient in operation and can effectively eliminate matrix effect caused by excessively high total solid content and avoid pollution during the preparation process of samples, thus greatly reducing memory effect and obviously increasing measuring accuracy. The ICP-MS measuring method of trace metal impurities in high-purity lead is applicable to the analysis and testing of the content of a plurality of trace metal impurities.

Description

[0001] 1. Field [0002] The invention belongs to the technical field of analysis and testing, and relates to the processing and testing technology of trace impurities in high-purity metals, in particular to an ICP-MS method for trace impurities in high-purity metals. 2. Background technology [0003] Usually, the determination method of trace metal impurities in high-purity lead adopts atomic absorption method, and electrolytic method or precipitation method is used for sample treatment to remove a large amount of lead in the sample, and after concentration, atomic absorption method is used for determination of impurity components. This method is simple to operate, but the matrix effect is serious. Since the detection limit of the atomic absorption method is relatively high, sample concentration is necessary, and other impurities are easily brought into the concentration process, thereby affecting the measurement accuracy. [0004] The ICP-MS method has been widely used in th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N27/68
Inventor 李本涛冯典英赵华黄辉
Owner NO 53 RES INST OF CHINA NORTH IND GRP
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