Method for chemically inducing osmium to be oxidized through static type ultraviolet light and reaction device

A chemically induced and ultraviolet light technology, applied in the field of static ultraviolet photochemically induced osmium oxidation, can solve problems such as high blank, and achieve the effect of reducing the loss of osmium, reducing the process blank, and avoiding contamination.

Inactive Publication Date: 2012-06-27
CHINA UNIV OF GEOSCIENCES (WUHAN)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, a large number of oxidizing reagents are used in the existing methods, which may cause a relatively high blank. Therefore, when the above-mentioned methods are used for the separation and purification of Os, the reagents and utensils used must be repeatedly purified. or cleaning

Method used

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  • Method for chemically inducing osmium to be oxidized through static type ultraviolet light and reaction device
  • Method for chemically inducing osmium to be oxidized through static type ultraviolet light and reaction device
  • Method for chemically inducing osmium to be oxidized through static type ultraviolet light and reaction device

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Prepare the osmium solution of the ore sample after adding the standard and dissolve it with hydrochloric acid, and add inorganic ion S with a concentration of 0.5 μg / mL 2 o 8 2- (S 2 o 8 2- Change to Fe 2+ , Fe 3+ or Cr 6+ ) to form a solution sample to be tested with an osmium concentration of 0.1ng / mL, and the sample is introduced into the above-mentioned ultraviolet light reactor ( figure 1 ) in the Carlos tube type sample reaction quartz tube, the quartz tube is selected as an ordinary quartz tube, the length is selected as 35cm, the outer diameter is 15mm, the wall thickness is 2mm, and the sample volume introduced therein is 45ml. Place 6 high-intensity ultraviolet lamps around the reaction tube. The ultraviolet lamp is a low-pressure mercury lamp. The wavelength used by the ultraviolet lamp is 254nm, and the reaction temperature is 50°C. and UV lamps are installed in a cylindrical reaction chamber. The osmium-containing sample is irradiated by an ultrav...

Embodiment 2

[0025] The osmium in the lake with the osmium isotope diluent added is prepared with nitric acid to form a solution sample to be tested with an osmium concentration of 2 μg / mL, and the sample is introduced into the above-mentioned ultraviolet light reactor ( figure 1) in the Carlos tube type sample reaction quartz tube, the quartz tube is selected synthetic quartz tube, its length is 50cm, the outer diameter is 25mm, the wall thickness is 3mm, and the sample volume imported therein is 70ml. Four high-pressure mercury lamps are placed around the reaction quartz tube. The wavelength of the high-pressure mercury lamp is 185nm, and the reaction temperature is 250°C. The outside of the ultraviolet lamp and the inside of the reactor are protected by aluminum foil. cavity. The sample containing osmium was irradiated by ultraviolet light for 24 hours, and then the osmium solution was purified by distillation. The quartz reagent bottle is heated on an electric heating plate at 115°C, ...

Embodiment 3

[0027] Prepare the osmium in the spiked seawater sample with high-purity water, and add the inorganic ion Fe at a concentration of 100 μg / mL 3+ (Fe can be 3+- Change to Fe 2+ , S 2 o 8 2- or Cr 6+ ) to form a solution sample to be tested with an osmium concentration of 10ng / mL, and the sample is introduced into the above-mentioned ultraviolet light reactor ( figure 1 ) in the Carlos tube type sample reaction quartz tube, the quartz tube is selected as a synthetic quartz tube, the length is selected as 25cm, the outer diameter is 10mm, the wall thickness is 1mm, and the sample volume introduced therein is 30ml. Place 8 high-intensity ultraviolet lamps around the reaction tube. The ultraviolet lamp is a metal halide lamp. The wavelength used by the ultraviolet lamp is 254nm, and the reaction temperature is 150°C. and UV lamps are installed in a cylindrical reaction chamber. The osmium-containing sample is irradiated by a UV lamp for 12 hours in a quartz tube and introduce...

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Abstract

The invention discloses a method for chemically inducing osmium to be oxidized through static type ultraviolet light and a reaction device. The method comprises the following steps of: introducing a to-be-detected solution sample containing osmium into a sample reaction quartz tube, irradiating the sample through ultraviolet light, and inducing osmium in the sample to be oxidized to generate osmium tetroxide, so as to form an osmium tetroxide solution. The osmium tetroxide solution obtained by using the method is measured by directly using ICP-OES (Inductively Coupled Plasma-Optical Emission Spectroscopy) or ICP-MS (Inductively Coupled Plasma-Mass Spectrometry), so that an osmium signal can be obtained; or osmium tetroxide is measured by using the ICP-MS or N-TIMS (Thermal Ionization Mass Spectrometry) after purifying osmium tetroxide in the solution by using an extraction or distillation method, so that the osmium signal can be obtained. The reaction device provided by the invention at least comprises a cylindrical reaction cavity body and the reaction quartz tube positioned in the middle part of the reaction cavity body. 2-8 ultraviolet lamps are arranged on the periphery of the reaction quartz tube in an encircling manner. The method and the reaction device disclosed by the invention have the advantages that: the method is simpler; any oxidization and reduction reagent is not required; loss of osmium in the sample and pollution caused by osmium in a pre-treatment process are reduced; the sensitivity is relatively higher; compared with the traditional atomization sample introduction, the sample can be introduced more effectively; and the detection limit is lower.

Description

Technical field: [0001] The static ultraviolet photochemically induced osmium oxidation method and reaction device provided by the invention belong to the technical field of trace analysis of analytical chemistry and relate to the technical field of separation and purification methods of analytical chemistry. Background technique: [0002] Osmium (Os) is located in the sixth period of the periodic table, subgroup VIII, atomic number 76, atomic weight 190.2, electronic configuration 5d6 6 the s 2 . In nature, osmium has 7 isotopes: 184 Os(0.0177%), 186 Os(1.593%), 187 Os(1.513%), 188 Os (13.29%), 189 Os (16.22%), 190 Os (26.38%) and 192 Os (40.98%). Due to the high sensitivity of osmium isotope tracing and dating, it can provide important information that other isotopes cannot give, and has unique advantages in application in marine environments and lakes. Therefore, the research and development of osmium isotopes in marine environments and lakes The application has...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N1/34G01N21/73G01N27/64
Inventor 朱振利黄春迎胡圣虹郑洪涛
Owner CHINA UNIV OF GEOSCIENCES (WUHAN)
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