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Atomic Fluorescence Determination Traditionally Internal Standard Method for Hydride-Forming Elements

A technology of atomic fluorescence and hydride, applied in the field of internal standard method, can solve the problems of many factors affecting the measurement signal of the instrument, poor correlation of standard curve, large error of measurement results, etc., to eliminate chemical and physical interference, improve Determination of precision and accuracy, the effect of lowering the detection limit

Inactive Publication Date: 2014-10-29
TIANJIN NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0003] The present invention is aimed at chemical vapor generation and sampling—when the non-dispersive atomic fluorescence photometer measures the elements that are easy to form hydrides in the traditional way, there is a lot of interference, and there are many factors that affect the measurement signal of the instrument, resulting in poor correlation of the standard curve, The shortcomings of the measurement results are large errors, and the improved method proposed

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  • Atomic Fluorescence Determination Traditionally Internal Standard Method for Hydride-Forming Elements

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Embodiment 1

[0020] (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 simultaneous determination of two or more elements;

[0021] (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 measured ...

Embodiment 2

[0025] 1. Use strong hollow cathode lamps of gold and arsenic 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 arsenic alternately, and achieve gold and arsenic simultaneous measurement. In terms of solution preparation, 100 ng of gold standard was added to the arsenic-containing standard solution and the sample to be tested at concentrations (0, 2.0, 4.0, 6.0, 8.0 ng / mL) respectively, and all solutions were controlled to have an acidity of hydrochloric acid of 5 %(v / v). Then the experiment used 1.2% (m / V) sodium borohydride solution to react with standard and sample solutions at room temperature for continuous chemical vapor generation (both sodium borohydride flow rate and element solution flow rate were 2.0 ml / min). Simultaneous determination of arsenic and gold is carried out according to the instructions of double-channel atomic ...

Embodiment 3

[0027] Using yttrium hollow cathode lamp and antimony hollow cathode lamp as two light sources, on a dual-channel atomic fluorescence photometer, adopts mechanical light cutting method, so as to obtain the fluorescence signals of yttrium and antimony alternately, and achieve the simultaneous determination of yttrium and antimony. In terms of solution preparation, 100 ng of yttrium was added to the antimony-containing standard solution and the sample to be tested at concentrations (0, 1.0, 2.0, 4.0, 6.0, 8.0 ng / mL), and the acidity of nitric acid was controlled in all solutions. It is 0.20M. Then the experiment uses 1.2% (m / V) sodium borohydride solution and standard solution for continuous chemical vapor reaction at room temperature. Simultaneous determination of yttrium and antimony is carried out. After the measurement, the recorded fluorescence values ​​of the two elements are calculated according to the ratio of the fluorescence intensity of antimony and antimony according...

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Abstract

The invention discloses an internal standard method used in measuring conventional elements easy to form hydrides through atomic fluorescence. The internal standard method comprises the following steps of: (1) setting instruments, wherein an atomizer is alternatively radiated by using an internal standard element triggering light source and a triggering light source of an element to be measured (or in time sequence), so as to alternatively trigger atomic fluorescence signals of the internal standard element and the element to be measured, and achieve the purpose of synchronously measuring the two elements; (2) preparing a solution, wherein a certain quantity of internal standard elements are respectively added into a standard solution and a sample solution; (3) drawing a calibration curve, wherein a fluorescence value ratio I analysis / I internal standard of an analysis element and the internal standard element in the standard solution is measured, and a calibration curve is established for the concentration Ci (i is equal to 1, 2, 3,...) of the analysis element in accordance with the I analysis / I internal standard; and (4) under the same condition, measuring a fluorescence value ratio I analysis / I internal standard of the analysis element and the internal standard element in a test sample, and calculating the content Cx of the element to be tested from the calibration curve. By utilizing the method, the defects that the conventional measurement is large in chemical and physical interference, not good in measurement stability and the like are effectively eliminated, and the measurement precision and the accuracy are improved.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis and measurement, and relates to an internal standard method used when a non-dispersive atomic fluorescence instrument for gaseous sampling is used to measure elements that are traditionally easy to form hydrides. 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. The elements determined for hydride injection are arsenic, antimony, bismuth, selenium, tellurium, germanium, tin, lead, mercury (reduced to elemental species). However, when using the gaseous hydride injection-non-dispersive atomic fluorescence method for the determination of these traditionally volatile elements such as arsenic, antimony, bismuth, selenium, t...

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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