Hydride generation and sample introduction method of germanium

Abstract

The invention discloses a hydride generation and sample introduction method of germanium. The method comprises the following steps: inorganically digesting a to-be-detected sample to obtain a digested solution; adding solid acid and soluble salt containing phosphate anions 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 germanium in the to-be-detected sample solution with potassium borohydride under an acidic condition to generate hydrogen germanide 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 germanide 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. 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 of germanium element. 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] The hydride generation sampling technology of germanium 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 solid acid tablet for rapid on-sit...

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Problems solved by technology

[0004] The application number is 201210238016.7, and the patent titled solid acid tablet for rapid on-site atomic fluorescence detection 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 concentrated acid during rapid on-site atomic fluorescence detection. The acid is difficult to carry, the potential danger is large, and the field environment is changeable, so it is difficult to quantitatively pipette

However, when the above-mentioned patent is applied to the hydride generation sampling technology of germanium element, under optimized conditions, when the mass concentration of sulfamic acid is 20%, its sensitivity is only 1 / 5 of the traditional 20% phosphoric acid method

Therefore, there are great difficulties in dealing with the ultra-trace analysis of germanium

In addition, the consumption of sulfamic acid is huge, the analysis cost is high, and the high concentration of sulfamic acid is easy to precipitate and crystallize, which affects the determination of germanium.

[0005] Also do not have relevant patent or document to propose the method for solving the above-mentioned problem at present

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