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A method for the determination of trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry

A technology of emission spectroscopy and plasma, which is applied in the field of determination of trace elements in high-purity magnesium-based oxides, can solve the problems of lack of measurement, unseen, and unreachable detection limits, etc., to ease detection pressure, eliminate mutual interference, good stability effect

Active Publication Date: 2022-07-15
WESTERN MINING CO LTD +2
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Problems solved by technology

Unfortunately, both standards lack the determination of other elements except calcium, iron, and manganese (excluding magnesium oxide), and calcium adopts a higher content (minimum 10 -1 Order of magnitude) EDTA titration method, the detection limit cannot reach 10 -4 At the same time, these two methods lack the reproducibility and reproducibility indicators required by quality control, and the laboratory lacks the basis for judging the reliability of its own test results
At present, there has been no report on the determination of impurity elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry. In one of the few similar studies, Tao Meijuan used the interference coefficient method to study cadmium, lead, nickel, aluminum in magnesium and magnesium alloys , silicon, zirconium, manganese, beryllium, copper, iron, titanium, lead, silver, calcium, yttrium, lanthanum, cerium and neodymium and other 17 kinds of element content determination, Meitan uses the matrix matching method to determine the silicon content in magnesium and magnesium alloys Carry out mensuration, the mass percent composition that contains heteroelement in both determination samples is in 10 -2 Order of magnitude, not suitable for mass percentage content is usually 10 -4 Determination of impurity elements in order-order high-purity magnesium-based oxides

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  • A method for the determination of trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry
  • A method for the determination of trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry
  • A method for the determination of trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry

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Embodiment Construction

[0036] Further description is given below in conjunction with specific implementations:

[0037] In this embodiment,

[0038] 1. Main instruments and working conditions:

[0039] Inductively coupled plasma atomic emission spectrometer: iCAP 7000SERIES, Thermo Fisher Scientific Co., Ltd.;

[0040] Electronic balance: ME204E type, with a sense of 0.0001g, Switzerland METTLER TOLEDO Measurement Technology Co., Ltd.;

[0041] Thermo7400, RF frequency is 27.12MHz, high-efficiency concentric nebulizer, plasma observation method: vertical (diameter term), wavelength range 166-847nm, optical resolution (FHW)≤0.007nm, at 200nm; 0.014nm, at 400nm; 0.021nm, 600nm; semiconductor refrigeration CID detector, detection unit> 290000.

[0042] Thermoelectric ICP7400, power 950W, cooling gas 12L / min, auxiliary gas 0.5L / min, carrier gas 0.5L / min, observation height 12mm; integration time: long wave 5S, short wave 15S; pump speed: flushing 50rpm, analysis pump speed 50rpm.

[0043] Analytical...

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Abstract

The invention discloses a method for determining trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry. The sample is pretreated first, and then aluminum, calcium, potassium, sodium, boron, iron, manganese, cadmium, The multi-element standard mixed solution of lead and sulfur or the standard solution of single-element silicon is added with hydrochloric acid, diluted, and finally the series of standard solutions are measured by inductively coupled plasma atomic emission spectrometer. Using the general laws of emission spectra of aluminum, calcium, potassium, sodium, boron, iron, manganese, cadmium, lead, sulfur, and silicon elements in inductively coupled plasma to simulate high-purity series of magnesium-based oxide substrates, coexisting elements and background emission Spectral research, measurement medium, analytical spectral line screening, mutual interference elimination test between matrix and impurity-containing element spectral lines, and condition optimization to establish the best sample measurement conditions; using standard addition method as a technical means to achieve high-purity series magnesium Determination of trace impurity elements in base oxide samples.

Description

technical field [0001] The invention relates to the technical field of analysis and detection in the salt lake chemical industry, in particular to a method for determining trace elements in high-purity magnesium-based oxides by inductively coupled plasma emission spectrometry. Background technique [0002] Salt lake resources are the advantages and characteristic resources of Qinghai region of my country. In-depth development and utilization of salt lake resources, breakthroughs in the key technology of magnesium extraction from salt lakes, and the output and quality of western magnesium products have reached "five world firsts". The comprehensive development and utilization of salt lake water chlorite waste resources provides another new way, "magnesium damage" has become "magnesium treasure". In order to solve the problem of "magnesium damage" in the development and utilization of salt lake resources, the industry has successively developed a series of high-purity magnesium...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/73G01N1/28
CPCG01N21/73G01N1/28
Inventor 王景凤黎永娟胡燕秀李颜君岳萍罗仙平吴敏王春英梁金凤
Owner WESTERN MINING CO LTD
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