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Internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements

An atomic fluorescence, metal element technology, applied in fluorescence/phosphorescence, material excitation analysis, etc., can solve the problems of poor correlation of the standard curve, unstable signal, low fluorescence signal, etc., to improve the low fluorescence intensity and reduce detection. limit and reduce the effect of random errors

Inactive Publication Date: 2015-03-25
TIANJIN NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The present invention aims at the disadvantages of low fluorescence signal, unstable signal and poor correlation of standard curve when measuring non-traditional hydride generating elements, that is, transition and noble metal elements, by using a non-dispersive atomic fluorescence photometer for sample introduction of chemical vapor generation. , the proposed improved method

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  • Internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements

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Experimental program
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Effect test

Embodiment 1

[0022] (1) Instrument settings: During the measurement process, the special hollow cathode lamp made of internal standard elements and the hollow cathode lamp made of elements to be measured alternately irradiate the atomizer, thereby alternately exciting the internal standard elements and the elements to be measured Atomic fluorescence signal to achieve the purpose of simultaneous determination of two elements;

[0023] (2) Solution preparation: Add a certain amount of internal standard elements to the standard solution and the solution to be tested respectively, and measure the fluorescence value ratio of the analytical element and the internal standard element when the standard solution is measured. I 分析 / I 内标 , by I 分析 / I 内标 Concentration of analyzed elements Ci (i=1,2,3,...) Establish a calibration curve; under the same conditions, measure the fluorescence value ratio of the measured element and the internal standard element in the sample I 样品 / I 内标 , the me...

Embodiment 2

[0029] 1. Using rhodium strong hollow cathode lamps and gold hollow cathode lamps as two light sources, on a double-channel atomic fluorescence photometer, use pulse power supply to make the two lamps light up alternately, so as to obtain the fluorescent signals of gold and rhodium alternately, to achieve Simultaneous determination of gold and rhodium. In terms of solution preparation, 40 ng of rhodium was added to the gold-containing standard solution and the sample to be tested at concentrations (0, 10.0, 20.0, 40.0, 60.0, 80.0 ng / mL), and all solutions controlled the concentration of aqua regia. The acidity is 1.0M. Then the experiment adopts 1.2% (m / V) sodium borohydride solution and gold standard solution to carry out continuous chemical vapor generation reaction at room temperature. Carry out the simultaneous measurement of gold and rhodium by the double-channel atomic fluorescence measurement description, after the measurement, the fluorescent values ​​of the two eleme...

Embodiment 3

[0031] Using yttrium hollow cathode lamp and zinc hollow cathode lamp as two light sources, on a double-channel atomic fluorescence photometer, use pulse power supply to make the two lamps light up alternately, so as to obtain the fluorescence signals of yttrium and zinc alternately, and achieve the simultaneous measurement. In terms of solution preparation, 400 ng of yttrium was added to the zinc-containing standard solution and the sample to be tested at concentrations (0, 100.0, 200.0, 400.0, 600.0, 800.0 ng / mL), and the acidity of nitric acid was controlled in all solutions. It is 0.20M. Then the experiment adopts 1.2% (m / V) sodium borohydride solution and gold standard solution to carry out continuous chemical vapor generation reaction at 98 ℃. Carry out the simultaneous determination of yttrium and zinc according to the description of the double-channel atomic fluorescence measurement. After the measurement, the fluorescence values ​​of the two elements recorded will be...

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Abstract

The invention discloses an internal standard method for gas sampling non-dispersive atomic fluorescence detection of transitional and precious metal elements. The internal standard method comprises the steps of: (1) providing an apparatus: irradiating an atomizer by hollow cathode lamps of an internal standard element and a to-be-tested element according to the time order (or alternatively), so as to alternatively stimulate atomic fluorescence signals of the internal standard element and the to-be-tested element and achieve the purpose of detecting the two elements at the same time; (2) preparing solutions: respectively adding a certain amount of internal standard elements to a standard solution and a sample solution; (3) drawing a correction curve: detecting fluorescence value ratio I analysis / I interior label of the analysis element and the internal standard element in the standard solution, and building the correction curve according to the concentration Ci (i=1,2,3,...) of the analysis element by the I analysis / I interior label; and (4) detecting the fluorescence value ratio I sample / I interior label of the analysis element and the interior label element in the sample under the same condition, and determining the content Cx of the to-be-tested element in the sample from the correction curve. By adopting the method, the instability of the apparatus and various interferences in detection can be effectively removed, and the detection precision and accuracy are also improved.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis and measurement, and relates to a method for measuring non-traditional elements by using internal standard element fluorescence. Background technique [0002] The reaction between sodium borohydride and elements to form gaseous hydrides under acidic conditions (CVG) has been used for atomic spectroscopic analysis. Compared with conventional spray injection, gaseous hydride injection has high sample injection efficiency and low detection limit. However, prior to 1996, the elements used for hydride sampling were limited to elements that traditionally form volatiles, such as arsenic, antimony, bismuth, selenium, tellurium, germanium, tin, lead, mercury (reduced as a single substance). In 1996, Sturgeon et al. first discovered that in a self-made reactor, sodium borohydride reduced copper to gaseous volatiles and used it for the determination of copper in samples. Since then, studies ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/64
Inventor 段旭川
Owner TIANJIN NORMAL UNIVERSITY
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