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Overlimit control method and device for high-concentration sample electrothermal evaporation sampling

A technology of electrothermal evaporation and over-limit control, applied in the preparation of test samples, etc., can solve the problems of time-consuming and labor-intensive, low analysis results, high analysis results, etc., and achieve the effects of simple operation, simple steps and simple structure.

Active Publication Date: 2014-10-22
BEIJING JITIAN INSTR CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Commonly used digestion methods such as electric heating plate digestion, microwave digestion, etc. are not only time-consuming and labor-intensive, but also in trace analysis, the contamination of reagents and instruments used in digestion will lead to high analysis results. When determining volatile elements, Volatile loss during sample digestion will lead to lower analysis results

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  • Overlimit control method and device for high-concentration sample electrothermal evaporation sampling
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  • Overlimit control method and device for high-concentration sample electrothermal evaporation sampling

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Experimental program
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Effect test

Embodiment 1

[0029] The atomic fluorescence spectrometer determines that the element is cadmium (Cd), and the sample is a Cd standard aqueous solution with a concentration of 100 μg / kg. The low-condition process of heating and evaporating cadmium is carried out according to the conditions listed in Table 1. In order to determine the part of the Cd standard aqueous solution after the low-condition process The percentage of the evaporated Cd to the total Cd, within the range not exceeding the measuring range, each injection is evaporated once through a low-condition process and all the remaining Cd is evaporated. The specific injection conditions, evaporation conditions and the obtained results are shown in Table 2 .

[0030] As shown in Table 2: the partially evaporated Cd after the low-condition process accounts for 1-2.5% of the total Cd, so the peak area of ​​the partially evaporated analyte is calculated by (40~100) to obtain the estimated peak value of the total analyte The peak area, ...

Embodiment 2

[0041] The element determined by atomic fluorescence spectrometer is cadmium (Cd), the sample is GSS-2 soil standard material (the reference value of Cd content is 71±14μg / kg), and the low-condition process of heating and evaporating cadmium is carried out according to the conditions listed in Table 4. After the low-condition process, the percentage of Cd partially evaporated from the GSS-2 soil standard substance to the total Cd, within the range not exceeding the range, each injection is evaporated once in the low-condition state and all the remaining Cd is evaporated, The specific injection conditions, evaporation conditions and the obtained results are shown in Table 5.

[0042] As shown in Table 5, the partially evaporated Cd after the low-condition process accounts for 1-2% of the Cd, so the peak area of ​​the partially evaporated analyte x (50~100) is obtained to obtain the estimated peak of the total analyte The area, which is close to the actual peak area value of the...

Embodiment 3

[0052] The element measured by atomic fluorescence spectrometer is mercury (Hg), and the sample is GBW10010 rice standard substance (the reference value of Hg content is 5.3±0.5μg / kg). The percentage of Hg partially evaporated from the GBW10010 rice standard material to the total Hg after low conditions. Within the range not exceeding the measurement range, each sample is evaporated once through the process of low conditions and all the remaining Hg is evaporated. The specific injection conditions , evaporation conditions and the obtained results are shown in Table 8,

[0053] As shown in Table 8, the partially evaporated Hg after the low-condition process accounts for 1-2% of the Hg, so the peak area of ​​the partially evaporated analyte x (50~100) is used to obtain the estimated peak of the total analyte The area, which is close to the actual peak area value of the total analyte, is used to calculate the peak height to determine whether the peak height exceeds the range. Ac...

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Abstract

The invention relates to an ultra-limit control method for high-concentration sample electric heating evaporation sample introduction and a device using the method. The ultra-limit control method is simple in step and can be used for preventing high-concentration matter to be measured from polluting a pipeline. The device is simple in structure, and simple and convenient for operation. The method provided by the invention comprises the following steps of: 1) controlling an electric heating evaporator to heat and evaporate a sample in a low-condition process, and sending the partial evaporated sample into a sample detection instrument for detection; 2) by using the peak area*(40-100) of the partial evaporated matter to be detected as the peak area of the total estimation peak of the matter to be detected, calculating the principle peak height of the total estimation peak of the matter to be detected according to the peak area of the total estimation peak of the matter to be detected; and 3) comparing the principle peak height of the total estimation peak of the matter to be detected with a peak height range of a sample detection instrument. The device provided by the invention comprises the electric heating evaporator and the sample detection instrument, and further comprises a data processing device and an electric heating controller for controlling heating power and heating time of the electric heating evaporator.

Description

technical field [0001] The invention relates to a signal overrun control method and a device thereof, in particular to a signal overrun control method and a device for high-concentration sample electrothermal evaporation sampling injection. Background technique [0002] Before analyzing the sample, it is generally necessary to digest the sample to remove the organic matter in the sample and convert the cadmium element in the sample into a uniform form. Commonly used digestion methods such as electric heating plate digestion, microwave digestion, etc. are not only time-consuming and labor-intensive, but also in trace analysis, the contamination of reagents and instruments used in digestion will lead to high analysis results. When determining volatile elements, Volatile loss during sample digestion will lead to lower analysis results. [0003] Compared with the solution analysis technique, the electrothermal evaporation sample injection analysis has the advantages of simplify...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N1/44
Inventor 刘霁欣周齐冯礼郑逢喜路东
Owner BEIJING JITIAN INSTR CO LTD