Tungsten filament pre-enrichment device for determining zinc and using method

A pre-enrichment, tungsten wire technology, applied in the field of chemical analysis and detection, can solve problems such as matrix interference, and achieve the effects of convenient operation, accurate zinc content and good repeatability

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

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Problems solved by technology

At present, there is no report on the use of tungsten wire to pre-enrich zinc to eliminate matrix interference

Method used

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  • Tungsten filament pre-enrichment device for determining zinc and using method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Before the standard solution containing zinc is injected into the tungsten wire capture electrothermal evaporation solid sampling device, the partial pressure of the argon-hydrogen mixed gas source 1 containing 10% hydrogen is set at about 0.5Mpa, and the carrier gas mass flowmeter 2 is set to Set at 600mL / min, zinc is evaporated in the electrothermal evaporation device 4, and is captured and released by the tungsten wire 8, and the aerosol containing atomic zinc enters the atomic fluorescence spectrometer 11 through the release gas path 10. Under optimal conditions, the linear range of zinc detection is 0-2.5 μg, the regression coefficient of the standard curve is above 0.995, the detection limit of zinc can reach 0.1 pg, and the relative standard deviation of multiple determinations is within 5%.

Embodiment 2

[0026] Taking 5mg of rice flour (national standard GBW10045) as an example, use argon-hydrogen mixed gas containing 10% hydrogen as the gas source, set the carrier gas mass flow meter 2 at 700mL / min, and use the zinc pre-enrichment device of the present invention in conjunction with electrothermal evaporation The solid sampling device is connected in series with the atomic fluorescence spectrometer, and other conditions are the same as those in Example 1. The value of zinc in the determination sample was 13.9±0.3 mg / kg, within the standard value of 14.4±0.8 mg / kg of the standard substance, the relative standard deviation of 7 determinations was 7.1%.

Embodiment 3

[0028] Taking 2mg of soil powder (national standard GBW07401) as an example, use argon-hydrogen mixed gas containing 10% hydrogen as the gas source, set the carrier gas mass flow meter 2 at 700mL / min, use the zinc pre-enrichment device of the present invention in conjunction with electric heating The evaporative solid sampling device is connected in series with the atomic fluorescence spectrometer, and other conditions are the same as in Example 1. The determination of zinc in the sample was 703.5 ± 33.2 mg / kg, within the standard value of 680 ± 25 mg / kg of the standard substance, and the relative standard deviation of 7 times of determination was 8.3%.

[0029] The above three examples illustrate that the present invention provides a tungsten wire pre-enrichment device and method for the determination of zinc by electrothermal evaporation atomic fluorescence spectrometry for solid sampling, which can effectively eliminate matrix interference when measuring zinc and ensure the ...

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Abstract

The invention provides a tungsten filament pre-enrichment device for determining zinc and a using method. The device comprises a boat-shaped sample injector, an electric heating evaporation device, a pre-enrichment device, a carrier gas path, a carrier gas mass flowmeter, a release gas path, an atomic fluorescence spectrometer and the like. A solid sample injection atomic fluorescence spectrometry for determining zinc comprises dehydrating and ashing a sample to be determined in air to obtain inorganic residues; increasing the temperature of the sample residues to about 1600DEG C in an argon and hydrogen mixed gas atmosphere, wherein aerosol containing zinc atoms is in contact with a tungsten filament and zinc is pre-enriched by the tungsten filament; increasing the temperature of the tungsten filament to about 1800DEG C to release zinc atoms, and analyzing the content of zinc by using the atomic fluorescence spectrometer. The device solves the problem of matrix interference during zinc determination by using the solid sample injection electric heating evaporation atomic fluorescence spectrometry, and has the advantage that the content of zinc can be accurately and stably analyzed without digesting the sample.

Description

technical field [0001] The invention relates to the field of chemical analysis and detection, in particular to a tungsten wire pre-enrichment device and a use method for determining zinc. 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 ( AFS), Inductively Coupled Plasma Emission Spectrometry (ICP-AES), Inducti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/40G01N21/64
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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