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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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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 are very unstable and difficult to reproduce
[0005] In 2003, the inventor also applied for an invention patent titled "Atomic Spectrometer Sample Entry Method", the publication number being CN1527044A, which reported the use of modified polymeric borohydride as a reagent for forming volatiles, but the patent did not point out The specific molecular formula and preparation method of the reagents used are not sufficiently specific theoretical expressions, making it difficult for professional and technical personnel in the same industry to repeat experiments

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
Comparison scheme
Effect test

Embodiment 1

[0054] According to the usual synthesis method, after the dodecaborane disodium salt is synthesized by sodium borohydride, the product dodecaborane disodium salt is formulated into a 1.2% aqueous solution, and then the solution is continuously mixed online with a peristaltic pump and elements containing gold, Silver, copper, platinum, ruthenium, palladium, iridium sample solution (element content is 100ppb, nitric acid acidity 0.6M) the mixed solution is separated in a gas-liquid separator, and the volatile gas hydride generated is sent to When detected by inductively coupled plasma emission spectroscopy, the sensitivity of the measured elements is 80-90 times that of dodecaborane disodium salt in solution under the same conditions.

Embodiment 2

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

Embodiment 3

[0058] Synthesize KB according to the usual synthetic method 3 h 8 (potassium triboron octahydrogenate), this product is formulated into 1.2% aqueous solution, then continuously mixes this solution and the sample solution containing element cobalt, nickel, manganese, vanadium, yttrium, zirconium, scandium with peristaltic pump online (element content Both are 100ppb, and the acidity of nitric acid is 0.2M) the mixed solution is separated in a gas-liquid separator, and the volatile gas hydride generated is sent to the inductively coupled plasma emission spectrum by the carrier gas for detection, and the measured element sensitivity is Under the same conditions, the solution does not contain KB 3 h 8 (Potassium triboroctahydrogenate) 100-120 times.

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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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