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Quantitative method of atomic spectrometer

A technology of atomic spectrometer and spectrometer, which is applied in the direction of color/spectral characteristic measurement, instruments, measuring devices, etc., can solve the problems of inability to overcome instrument drift, poor curve correlation, and low analysis efficiency, so as to overcome interference and avoid analysis results Fluctuation, the effect of accurate measurement results

Inactive Publication Date: 2015-06-17
TIANJIN NORMAL UNIVERSITY
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  • Application Information

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Problems solved by technology

The standard addition method can overcome the interference of the matrix, but it cannot overcome the drift of the instrument. When the analysis conditions of the instrument change greatly, the correlation of the obtained curves is often not good, causing relatively large errors in the measurement.
In addition, the standard addition method is cumbersome. In order to determine the concentration of the component to be tested in a sample, multiple samples need to be prepared for measurement, and the analysis efficiency is relatively low.

Method used

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  • Quantitative method of atomic spectrometer

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Effect test

Embodiment 1

[0016] A kind of quantitative method of atomic spectrometer, it is to have used internal standard method to carry out by following steps in standard addition method simultaneously:

[0017] (1) Accurately measure 2-3 samples to be tested, then add an equal amount of internal standard to each sample, and then add unequal amounts of analytes to the second (and third) samples substances, the amount of which is C 1 、C 2 ; Dilute each sample to a certain volume and mix;

[0018] (2) Simultaneously measure the analyte signal Y in each sample on the instrument 0 , Y 1 (and Y 2 ) and internal standard signal Y i 0 , Y i 1 (and Y i2 );

[0019] (3) Calculate the ratio: Y 0 / Y i 0 、 Y 1 / Y i 1 (and Y 2 / Y i2 ), take the first sample with internal standard but no analyte standard as the 0 point of the abscissa of the analysis curve, and take the concentration C1, C2 of the standard analyte added in the second (and third) is the abscissa, Y 0 / Y i 0 、 Y 1 / Y i 1 (an...

Embodiment 2

[0022] When using a certain type of non-dispersive atomic fluorescence to measure arsenic in an industrial wastewater, due to the existence of a large number of interfering elements, the results of the external standard method for hydride generation are quite different from the results of ICP-AES. Now change the quantitative method of the present invention as follows: get 2 parts of waste water (both are 5 milliliters) in two 100 milliliter volumetric flasks, numbered as S0 and S1, after adding 5 milliliters of hydrochloric acid then, add gold respectively in S0 and S1 500ng was used as the internal standard, and finally 100ng of standard arsenic solution was added to the volumetric flask of S1, and the two volumetric flasks were made to volume with distilled water and shaken to obtain the final determination solutions of S0 and S1. Then measure the fluorescence value Y of arsenic and gold in S0 on the atomic fluorescence spectrometer 0 , Y i 0 , the fluorescence values ​​o...

Embodiment 3

[0024] When using a certain type of ICP-AES to measure trace phosphorus in stainless steel standard samples, use 178nm for measurement. Due to the complexity of the sample matrix to be tested, the external standard curve of phosphorus prepared with pure water cannot be accurately determined. And use the standard addition method because the content of phosphorus is too low, the calibration curve correlation of the standard addition method that adds the standard phosphorus of 5 parts of different concentrations in the sample to be tested obtains is not good again, so the standard addition measurement result and standard sample provide The results are also quite different. Now change to the quantitative method of the present invention as follows: get 0.5 gram of stainless steel standard sample to dissolve and settle to volume in 100 milliliter volumetric flasks, then divide and get 3 parts (all 10 milliliters) in 3 50 milliliter volumetric flasks, coded as S0 , S1 and S2, respe...

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Abstract

The invention discloses a quantitative method of an atomic spectrometer. The quantitative method is characterized in that a standard addition method and an internal standard method are integrally combined. According to the quantitative method, in a quantitative test, all needed is to determine two or three data points, very accurate analysis determination results can be obtained. The quantitative method is suitable for determining samples under the conditions that the sample matrix interference is strong, and the determination conditions are unstable, and has the advantages of high speed, accurate results and the like.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis and measurement, and relates to a quantitative method in instrumental analysis. In particular, a quantitative method for atomic spectrometers. Background technique [0002] In the quantitative analysis of atomic spectroscopy instruments, the existing quantitative methods include external standard method, internal standard method and standard addition method. Among them, the external standard method is the most simple and practical. Using the prepared external standard standard curve, the analysis result can be obtained by measuring the sample once. However, when certain conditions of the instrument change during the measurement, and the stability of the instrument is not good enough to cause the analysis signal to drift, it is easy to cause poor correlation of the external standard calibration curve and cause large errors in the analysis results. In this case, it is often used inte...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/25G01N21/64G01N27/62G01N23/223G01N27/626
Inventor 段旭川张静雅
Owner TIANJIN NORMAL UNIVERSITY
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