Method for detecting lead content in submicron silver powder prepared through PVD method by using ICP

A sub-micron level, lead content technology, applied in the field of ion emission spectrometer (Ion Emission Spectrometer) detection, can solve the problems of unfavorable factory production detection, difficulty in finding spectral lines, high detection cost, etc., and achieve the effect of reducing detection input cost, reducing cost, and simple operation

Active Publication Date: 2012-02-08
JIANGSU BOQIAN NEW MATERIALS
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  • Application Information

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Problems solved by technology

However, at present, when ICP detects the lead content in nickel powder, the internal standard method is mostly used. This detection method has the following disadvantages: it is difficult to find spectral lines, and the detection cost is too high, which is not conducive to the actual production detection of the factory.

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  • Method for detecting lead content in submicron silver powder prepared through PVD method by using ICP
  • Method for detecting lead content in submicron silver powder prepared through PVD method by using ICP
  • Method for detecting lead content in submicron silver powder prepared through PVD method by using ICP

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Embodiment Construction

[0048] Standard sterling silver: use national standard reagents, manufacturer: Tianjin Guangfu Fine Chemical Research Institute, purity 99.99%;

[0049] 2. Using PVD method (conventional method) to make sub-micron silver powder;

[0050] 3 Draw a calibration curve for calibration lead;

[0051] Use the standard solution, under specified working conditions, measure under four kinds of spectral lines respectively, the integral spectral line of lead is drawn automatically by computer, see Figure 1~4 .

[0052] 4 Comparative analysis and screening of calibration curve results

[0053] The results are shown in Table 1.

[0054] Table 1 Parameters for drawing standard curve

[0055]

[0056] Result analysis, can compare and draw from the SNR S data: the SNR under this spectral line of 220.353nm is 10.065, and this SNR S is the strongest, namely in the present invention detects silver in silver by ICP-AES The spectral line 220.353nm is the best in the content of lead.

[00...

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Abstract

The invention discloses a method for detecting a lead content in submicron silver powder prepared through a PVD method by using ICP. The method comprises the following steps: (1) preparing submicron silver powder; respectively adding standard sterling silver or the silver powder sample to nitric acid according to a certain ratio, then carrying out mixing and heating to completely dissolve the silver, wherein 1 g of the standard sterling silver or the silver powder is added to 10-30 mL of the nitric acid; (2) cooling the two resulting solutions and respectively carrying out metered volume; (3) drawing standard curves of different lead spectrum lines in the silver solution, wherein the standard curve is drawn through the following steps that: a lead standard solution with a concentration of 0.00 mug / mL and a lead standard solution with a concentration of 10.00 mug / mL are adopted, the spectrum line intensity of the lead is determined under working conditions set through an inductively coupled plasma spectrometer, the lead concentration is adopted as the abscissa, the spectrum line intensity is adopted as the ordinate; (4) selecting the optimal spectrum line; (5) determining the spectrum line intensity in the silver powder solution, and the corresponding lead content, then calculating the lead content in the silver powder. The method provided by the present invention has the following advantages that: the spectrum line is easy to find; the detection cost is low; the method is applicable for the practical detection in the factory.

Description

technical field [0001] The invention relates to the field of ICP-AES (inductively coupled plasma emission spectrometer) detection methods, in particular to a method for detecting lead content in submicron (particle size diameter 100nm-1.0μm) silver powder manufactured by PVD (Physical Vapor Deposition) method by ICP . Background technique [0002] With the increasing maturity of nanotechnology, in order to fully ensure the use effect of the product, the requirements for the impurity content in nano-scale pure metals are becoming more and more stringent, and the accuracy of detection is getting higher and higher, especially for sub- For micron-sized silver powder, the amount of impurity lead in it is an important factor that directly affects the use effect of the product. However, in order to improve the comprehensive value of products while requiring the accuracy of test results, enterprises require the advantages of high efficiency and low cost in testing. But at present,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/28G01N1/38
Inventor 冯冬梅彭家斌刘猛王琴
Owner JIANGSU BOQIAN NEW MATERIALS
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