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Method for enhancing atomic spectrum gaseous sampling efficiency

A kind of atomic spectroscopy and gaseous technology, applied in the direction of material analysis, measuring devices, instruments, etc. through electromagnetic means, can solve problems such as difficult stability

Inactive Publication Date: 2012-08-15
TIANJIN NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, this patent uses an online heating device, which makes it difficult to stabilize the actual operation

Method used

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  • Method for enhancing atomic spectrum gaseous sampling efficiency

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] Dissolve 1.2000 g of sodium borohydride, 10 ml of ethylene glycol butyl ether (Lewis base), and dilute to 100 ml with water. Then use a peristaltic pump to continuously mix the solution and the sample solution containing elemental gold and silver (the element content is 100ppb, the acidity of hydrochloric acid is 0.80M), the flow rate of the two solutions is 2mL / min, and the mixed solution is separated in a gas-liquid manner The volatile gas hydride is separated by the carrier gas and sent to inductively coupled plasma emission spectroscopy for detection. The measured element signal intensity is the same as that under the same conditions without adding ethylene glycol butyl ether but only sodium borohydride (this The optimal dosage of sodium borohydride is 1.2% (m / V). Compared with the signal intensity, the signal intensity increases by 10-22 times. See the process figure 1 .

Embodiment 2

[0056] Dissolve 0.6000 g of sodium borohydride and 5 ml of dimethyl sulfide (Lewis base) and dilute to 100 ml of water. Then use a peristaltic pump to continuously mix the solution and the sample solution containing arsenic, antimony, and bismuth (the element content is 100ppb, and the acidity of nitric acid is 0.20M). The flow rate of the two solutions is 2mL / min, and the mixed solution is in one gas The volatile gas hydride is separated by the 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 signal intensity is the same as that when no dimethyl sulfide is added under the same conditions and only sodium borohydride ( At this time, the optimal amount of sodium borohydride is 1.2% (m / V)) The signal intensity is equivalent, that is to say, the amount of sodium borohydride is reduced, but the intensity does not change. See the process figure 1

Embodiment 3

[0058] Dissolve 1.8000 grams of potassium borohydride in 100 ml of diethylene glycol dimethyl ether solution to make a 1.8% (m / V) diethylene glycol dimethyl ether solution, and then use a peristaltic pump to continuously mix the solution with the containing The sample solution of the elements (the content of zinc, nickel, manganese, and cobalt are all 100ppb, and the acidity of nitric acid is 0.2M), and the flow rate of the two solutions is 2mL / min. The mixed solution is separated in a gas-liquid separator to generate volatiles The gas hydride is sent to the inductively coupled plasma emission spectroscopy by the carrier gas for detection. The signal intensity of the obtained element is compared with the signal intensity obtained when only 1.8% (m / V) potassium borohydride aqueous solution is used, and the efficiency is increased. 3-6 times.

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Abstract

The invention relates to a method for enhancing atomic spectrum gaseous sampling efficiency. According to the method, when element solution to be measured and boron hydride reducer solution of a certain concentration are mixed to perform chemical vapor generation reaction, lewis base containing lone-pair electrons is used as a chemical vapor generation reaction catalyst, so that the efficiency of a generated element volatile is enhanced, the sensitivity for an instrument to measure the element is improved, and the detection limit is reduced, wherein the reducer is hydroboron or borane; the lewis base is ether, amine, a sulfur-containing organic matter with lone-pair electrons, a heterocyclic organic matter, phosphine or phosphite (hypophosphite) and an iodine complex; and the contained element to be measured is gold, silver, copper, palladium, platinum, rhodium, ruthenium, osmium, iridium, zinc, cadmium, cobalt, nickel, manganese, iron, chromium, calcium, vanadium, yttrium, zirconium and scandium elements and the like.

Description

Technical field [0001] The invention relates to a method for using a Lewis base (catalyst) to promote the formation of high-efficiency elemental gaseous volatiles between a boron-containing reducing agent and an element, and the method can be used for the entry of atomic spectroscopy samples. Background technique [0002] In 1969, Holak combined the classic arsine reaction with atomic spectroscopy, and established a combined technology of hydride generation and atomic spectroscopy. This method uses certain elements to produce nascent hydrogen as a reducing agent or chemical reaction under certain reaction conditions to reduce the analytical elements in the sample solution to volatile covalent hydrides, and use carrier gas to reduce them. Import the atomic spectrum analysis system for quantitative determination. In 1990, Huang Benli et al. first reported the flow injection-electrochemical hydride generation technology, which extended the elements generated by electrochemical hydr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N21/73G01N27/626
Inventor 段旭川季慧苹
Owner TIANJIN NORMAL UNIVERSITY