Compounds used for element forming volatile matter

A technology for compounds and volatiles, applied in the field of instrumental analysis, can solve the problems of insufficient theoretical expression, failure to specify the molecular formula and preparation method of reagents, obstacles, etc.

Inactive Publication Date: 2007-12-05
TIANJIN NORMAL UNIVERSITY
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Problems solved by technology

However, the method reported in the above literature has the disadvantages of relatively low efficiency of forming hydrides and relatively serious residual phenomena, which hinders the actual use of the method.
[0004] For another example, Xu chuan Duan et al. reported in JAAS 2002 the monitoring method for online reduction of gold, silver, cobalt, nickel, manganese, zinc, cadmium, copper and other elements into volatiles using sodium borohydride, although the formation efficiency is relatively High, but there are defects that the experimental results ar

Method used

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  • Compounds used for element forming volatile matter
  • Compounds used for element forming volatile matter
  • Compounds used for element forming volatile matter

Examples

Experimental program
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Example Embodiment

[0053] Example one

[0054] According to the usual synthesis method, after synthesizing sodium dodecaborane disodium salt from sodium borohydride, the product dodecaborane disodium salt is formulated into a 1.2% aqueous solution, and then the solution is continuously mixed with elemental gold, Sample solutions of silver, copper, platinum, ruthenium, palladium, and iridium (the element content is 100ppb, and the acidity of nitric acid is 0.6M). The mixed solution is separated in a gas-liquid separator, and the generated volatile gas hydride is sent to the carrier gas Detected in inductively coupled plasma emission spectroscopy, the measured element sensitivity is 80-90 times that of dodecaborane disodium salt under the same conditions.

Example Embodiment

[0055] Example two

[0056] According to the usual synthesis method, after synthesizing undecaborane monosodium salt from sodium borohydride, the product is formulated into a 1.2% aqueous solution, and then the solution is continuously mixed with the elements containing cobalt, nickel, manganese, and vanadium using a peristaltic pump. Sample solutions of yttrium, zirconium, and scandium (the element content is 100ppb, and the acidity of nitric acid is 0.2M). The mixed solution is separated in a gas-liquid separator, and the generated volatile gas hydride is sent to the inductively coupled plasma emission by the carrier gas In the spectrum detection, the measured element sensitivity is 100-150 times that when the solution does not contain undecaborane monosodium salt under the same conditions.

Example Embodiment

[0057] Example three

[0058] Synthesize KB according to the usual synthesis method 3 H 8 (Potassium triboron octahydrogenate), prepare the product into a 1.2% aqueous solution, and then use a peristaltic pump to continuously mix the solution and the sample solution containing the elements cobalt, nickel, manganese, vanadium, yttrium, zirconium, and scandium (element content All are 100ppb, nitric acid acidity is 0.2M) The mixed solution is separated in a gas-liquid separator, and the generated volatile gas hydride is sent to the inductively coupled plasma emission spectroscopy by the carrier gas for detection. The measured element sensitivity is The solution does not contain KB under the same conditions 3 H 8 (Potassium boron octahydrogenate) 100-120 times the time.

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Abstract

The invention relates to the compound used in element formation the volatile matter and this compound molecule composition is HnBmMp and H represents hydrogen n is not less than six and not greater than thirty and B represents boron m is not less than 2 and not greater than 20 and M presents lithium, natrium, kalium, ammonium, chorine, bromine, iodine or organic molecule or organic ion p is not less than 0 and not greater than 3. Adopt one kind or multiple kinds mixture of the compound liquor to react with the water liquor with the measuring element is no only make the arsenic, antimony, bismuth, germanium, tin, lead, selenium, tellurium, hydrargyrum which can easy to form the hydride in tradition formed the volatile matter also makes the other multiple tens elements (gold, silver, colalt, palladium, manganese, calcium and so on) formed the hydride. The compound can apply in the atomic spectrum analysis of the sample inlet so it can enhance the sensitivity of analysis detection and reduces the detection limit also can used in chemistry vapour deposition and the production of inorganic metallic-membrane plating gassy precursor.

Description

technical field [0001] The invention belongs to the technical field of instrumental analysis, and relates to a compound used in the preparation of gaseous precursors for elemental chemical vapor deposition and inorganic coating. As well as compounds capable of converting elements that form less volatiles under normal conditions into volatiles. Background technique [0002] In 1969, Holak combined the classic arsine generation reaction with atomic spectroscopy, and established a combined technique of hydride generation-atomic spectroscopy analysis. This method is to use certain elements to produce nascent hydrogen as a reducing agent or a chemical reaction under certain reaction conditions to reduce the analytical elements in the sample solution to volatile covalent hydrides, and use the carrier gas flow to remove them. Import atomic spectrometry system for quantitative determination. In 1990, Huang Benli and others first reported the flow injection-electrochemical hydride ...

Claims

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Application Information

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IPC IPC(8): G01N1/28C01B35/18G01N21/00
Inventor 段旭川
Owner TIANJIN NORMAL UNIVERSITY
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