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A method for enhanced efficiency when elements form volatiles

A technology of volatiles and elements, applied in the field of instrument analysis, can solve the problems of the influence of the detection sensitivity of elemental analysis, the efficiency of forming volatiles is different, and the efficiency is low.

Inactive Publication Date: 2020-06-02
TIANJIN NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
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Problems solved by technology

[0005] Although the above-mentioned method of chelating reagents and elements to form volatiles has many advantages, it still has the following disadvantages: (1) currently, the chelating reagents that can be used to form volatiles are limited, mainly ethylenediamine disulfide Substituted carbamic acid (sodium or potassium, etc.) and sodium diethyldithiophosphate (or potassium, etc.), while the formation efficiency of other chelating reagents is indeed very low, and has no practical value; (2) even ethylenediamine dithiophosphate Thiocarbamic acid (sodium or potassium, etc.) and sodium diethyldithiophosphate (or potassium, etc.) are two reagents, although they are found to form volatiles with many elements, the efficiency of forming volatiles is not the same for different elements. different
Therefore, the detection sensitivity of some elemental analysis is still affected

Method used

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  • A method for enhanced efficiency when elements form volatiles
  • A method for enhanced efficiency when elements form volatiles

Examples

Experimental program
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Effect test

Embodiment 1

[0036] (1) Prepare a sample solution containing elemental gold (gold content is 50ppb, nitric acid acidity 0.1 M) and 0.4% sodium diethyldithiocarbamate (copper reagent, DDTC) solution (the solution contains 2% volume concentration of ethanol), and then use a peristaltic pump to extract the above two solutions at a flow rate of 2 ml / min, so that the two solutions are combined in a three-way pipe and then react.

[0037] (2) The reaction liquid flowing out of the three-way outlet pipe immediately flows into a gas-liquid separator, where the element volatiles (DDTC and element complexes) are separated by bubbling or spraying, and the The waste liquid after the reaction is removed in time. The generated gold volatiles are introduced into the atomization or ionizer of the atomic spectrometer for spectrum or mass spectrometry. The measured element sensitivity is twice that of the solution without ethanol under the same conditions. It can be seen that the sensitivity of the determ...

Embodiment 2

[0039] (1) The sample solution containing elemental nickel (nickel content is 40ppb, the acidity of nitric acid is 0.15M, the amount of methanol added is 2% volume concentration) and 0.5% sodium diethyldithiophosphate (DDTP) solution are mixed online, Then, a peristaltic pump was used to extract the above two solutions at a flow rate of 1.8 ml / min, so that the two solutions were combined in a three-way pipe to react.

[0040] (2) The reaction liquid flowing out of the three-way outlet pipe immediately flows into a gas-liquid separator, where the element volatiles (DDTC and element complexes) are separated by bubbling or spraying, and the The waste liquid after the reaction is removed in time. The generated gold volatiles are introduced into the atomization or ionizer of the atomic spectrometer for spectrum or mass spectrometry. The sensitivity of the measured nickel element is 2.5 times that of the solution without methanol under the same conditions. It can be seen that the ...

Embodiment 3

[0042] (1) Prepare a sample solution containing elemental cobalt (the cobalt content is 50ppb, and the acidity of nitric acid is 0.1 M) and 0.5% sodium dimethyldithiocarbamate (Sodium Fubax) solution (the solution contains 2% volume concentration of acetonitrile ), and then use a peristaltic pump to draw the above two solutions at a flow rate of 2 ml / min, so that the two solutions are combined in a three-way pipe and then react.

[0043] (2) The reaction liquid flowing out of the three-way outlet pipe immediately flows into a gas-liquid separator, where the element volatiles (DDTC and element complexes) are separated by bubbling or spraying, and the The waste liquid after the reaction is removed in time. The generated cobalt volatiles are introduced into an atomic spectrometer atomization or ionizer for spectrum or mass spectrometry. The measured elemental sensitivity is three times that of the solution without acetonitrile under the same conditions. It can be seen that the ...

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Abstract

The invention discloses a method used for increasing efficiency in conversion of elements into volatile matters. According to the method, water soluble small molecular organic compounds are added intoa reaction system used for conversion of elements into volatile matters, the volume concentration of the added water soluble small molecular organic compounds is controlled to be 0.25 to 4% of that of the reaction system; the reaction system is a mixed solution of a chelating agent and an element-containing sample solution at a volume ratio of 0.1:1-1:0.25; the water soluble small molecular organic compounds are water soluble alcohols and heterocyclic compounds. The method can be used for element sample introduction in instrumental analysis to increase element analysis sensitivity and improvedetection limit, and can be used for preparation of gaseous state precursors in chemical vapor deposition and inorganic film plating.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis, and relates to a sample injection method for an atomic spectrometer. More broadly, the invention is also used for the preparation of gaseous precursors for chemical vapor deposition and inorganic coatings, especially for the enhanced efficiency of an element when forming volatiles Methods. Background technique [0002] At present, most of the hydride generation sampling systems used in atomic spectrometers use sodium borohydride (potassium) as the reducing reagent for hydride generation, and the elements in the sample solution are reduced by the hydrogen in sodium borohydride (potassium) After forming gaseous hydrides, the elements are determined in an atomic spectrometer. Because the hydride sampling efficiency is higher than that of conventional pneumatic atomization in atomic spectroscopy (conventional pneumatic atomization sampling is only 3-5%, the determination sensitivity is...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N21/31G01N21/73G01N27/62
CPCG01N21/3103G01N21/73G01N27/62
Inventor 段旭川马国朋孙睿
Owner TIANJIN NORMAL UNIVERSITY
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