A kind of hydride generation sampling method of selenite ion

Abstract

The invention discloses a hydride generation and sample introduction method of seleninic acid radical ions. The method comprises the following steps: inorganically digesting a to-be-detected sample, and reducing selenate radical ions into seleninic acid radical ions to obtain a digested solution; adding solid acid and soluble salt containing chloride ions or iodide ions into the digested solution, and fixing the volume with pure water to obtain a to-be-detected sample solution; respectively extracting the to-be-detected sample solution and an alkaline potassium borohydride solution by virtue of a sampling pump, and mixing; reacting the seleninic acid radical ions in the to-be-detected sample solution with potassium borohydride under an acidic condition to generate hydrogen selenide and hydrogen after the to-be-detected sample solution and the alkaline potassium borohydride solution are mixed; separating liquid-state components of the generated hydrogen selenide and hydrogen in a gas-liquid separator, and feeding into an atomizer of atomic fluorescence so as to complete the hydride generation and sample introduction processes of atomic fluorescence detection. Compared with the method only using sulfamic acid, the method has the advantages that 90 percent of reagent consumption is reduced, and the problem that detection is influenced by easily crystallized high-concentration sulfamic acid is solved. The method has excellent popularization and application values.

Description

technical field [0001] The invention relates to the field of atomic spectroscopic analysis, in particular to a hydride generation sampling method for selenite ions. Background technique [0002] In the field of atomic spectrometry analysis, hydride generation / vapour generation sampling technology has been used as one of the sampling methods for atomic spectrometers because of its higher sampling efficiency compared with conventional atomization sampling, in order to obtain higher High analytical sensitivity, while greatly reducing matrix interference. [0003] Hydride generation sampling technology of selenite ion is currently widely used in atomic spectroscopy analytical instruments, such as atomic absorption spectrophotometer, atomic fluorescence spectrometer, inductively coupled plasma-emission spectrometer and inductively coupled plasma-mass spectrometer, etc. [0004] The application number is 201210238016.7, and the patent titled "Portable On-site Atomic Fluorescence ...

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Problems solved by technology

[0004] The application number is 201210238016.7, and the patent titled "Portable On-site Atomic Fluorescence Rapid Detection Solid Acid Press Tablet and Its Preparation Method and Application" discloses a method of using sulfamic acid as a solid acid instead of concentrated acid, which solves the problem of rapid on-site atomic fluorescence detection. When concentrated acid is difficult to carry, the potential danger is great, and the field environment is changeable, it is difficult to quantitatively pipette

But above-mentioned patent is when being applied to the hydride generation sampling technique of selenite ion, if only need the mass concentration of sulfamic acid to exceed 20% just can reach the sensitivity close to 20% hydrochloric acid, so the consumption of sulfamic acid Very large, high analysis cost, and high concentration of sulfamic acid is easy to precipitate and crystallize, which affects the determination of selenite ion

Also do not have relevant patent or document to propose the method for solving the above-mentioned problem at present

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