Pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and analysis method

A technology of emission spectroscopy and pre-enrichment, which is applied in the field of pre-enrichment tandem devices to achieve the effect of improving stability

Active Publication Date: 2015-10-21
INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the use of tungsten wire to pre-enrich zinc to eliminate matrix interference in the analysis of inductively coupled plasma emission spectroscopy

Method used

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  • Pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and analysis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Before the standard solution containing cadmium is injected into the solid sampling device composed of tungsten wire pre-concentration device 10 and electrothermal evaporator 7, the partial pressure of the argon-hydrogen mixed gas source 1 containing 2% hydrogen is set at 0.5Mpa Left and right, the carrier gas mass flowmeter 4 is set at 800mL / min, the auxiliary gas mass flowmeter 6 is set at 300mL / min, zinc is evaporated in the electrothermal evaporator 7, and is captured and released by the tungsten wire pre-concentration device 10 , the aerosol containing atomic zinc enters the confluence tee 11 in the carrier gas path 3, and then mixes with the argon-hydrogen mixed gas flowing out of the auxiliary gas mass flow meter 6 in the confluence tee 11, and the mixed zinc-containing gas The sol enters the torch interface 13 through the combined gas path 12 , and then enters the inductively coupled plasma emission spectrometer 14 . Under the optimal conditions of the solid sam...

Embodiment 2

[0027] Taking 5mg of rice flour (national standard GBW10045) as an example, use argon-hydrogen mixed gas containing 4% hydrogen as the gas source, set the carrier gas mass flowmeter 4 to 700mL / min, use the tungsten wire pre-enrichment device of the present invention and electric heating The evaporator is connected in series with the inductively coupled plasma emission spectrometer, and other conditions are the same as those in the first embodiment. The content of zinc in the three determination samples was 14.9±1.1 mg / kg, within the standard value of 14.4±0.8 mg / kg of the standard substance, and the relative standard deviation of the seven determinations was 6.1%.

Embodiment 3

[0029] Take 2mg of soil powder (national standard GBW07401) as an example, use argon-hydrogen mixed gas containing 4% hydrogen as the gas source, set the carrier gas mass flow meter 4 to 700mL / min, use the tungsten wire pre-enrichment device of the present invention and The electrothermal evaporator is connected in series with the inductively coupled plasma emission spectrometer, and the other conditions are the same as in the first embodiment. The content of zinc in the samples measured three times was 694.5±53.2 mg / kg, within the standard value of 680±25 mg / kg of the standard substance, and the relative standard deviation of the seven times determined was 7.3%.

[0030] The above three examples illustrate that a tungsten wire pre-concentration device and an electrothermal evaporator and an inductively coupled plasma emission spectrometer coupling device provided by the present invention can ensure the stability, sensitivity and accuracy of zinc measurement by inductively coup...

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Abstract

The invention provides a pre-concentration tandem arrangement for measuring zinc by emission spectroscopy and an analysis method, and the pre-concentration tandem arrangement comprises a tungsten pre-concentration device, an electrothermal vaporization device, a torch interface, a carrier gas mass flowmeter, an auxiliary gas mass flowmeter, a diverter three-way, a converging three-way, a carrier gas channel, an auxiliary gas channel and the like. An inductively coupled plasma emission spectrometry for measuring solid sampling of the zinc comprises the steps of dehydrating and ashing a sample to be measured in air to obtain inorganic residues; heating the sample residues at about 1600 DEG C under an argon hydrogen mixture atmosphere, the evaporated aerosol containing zinc atoms contacts with tungsten filament, and the zinc is pre-concentrated by the tungsten filament; heating the temperature of the tungsten filament to be about 1800 DEG C, releasing the zinc atoms, and analyzing the content of the zinc by the inductive coupling plasma emission spectrograph. The pre-concentration tandem arrangement has a simple structure and the problems that a plasma torch is extinguished and a signal is unstable when the tungsten pre-concentration device and the electrothermal vaporization device are in combination with the inductively coupled plasma emission spectrometry are solved. The pre-concentration tandem arrangement has the advantages that the digestion treatment is not needed to be performed on the sample, the trace zinc in the sample can be measured, and the pre-concentration tandem arrangement has the characteristics such as being direct, speediness, high sensitivity and good stability.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a pre-enrichment series device and analysis method for measuring zinc by solid sample introduction inductively coupled plasma emission spectrometry. technical background [0002] Zinc is an essential element for the human body, and it is an indicator of routine detection in the fields of food and hygiene; at the same time, excessive zinc can also cause harm to the human body, especially the discharge of zinc-containing waste residues and wastewater from industrial and mining enterprises will destroy the ecological environment and pass through the biological chain. affect human health. At present, liquid sampling systems are the mainstream technology for the determination of zinc in food instruments and methods. Most of the current national and industry standards for elemental analysis use atomic absorption spectrometry (AAS) and atomic fluorescence spectrometry ( A...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N1/44
Inventor 毛雪飞王敏张英钱永忠高成玲汤晓艳周剑
Owner INST OF QUALITY STANDARD & TESTING TECH FOR AGRO PROD OF CAAS
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