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Mobile detection method and detection device for chemically inducing osmium to be oxidized by using ultraviolet light

A detection method and chemical oxidation technology, applied in the field of trace analysis of analytical chemistry, can solve problems such as high blank, reduce the loss of osmium, avoid separation and enrichment steps, and save analysis and testing time.

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

AI Technical Summary

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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  • Mobile detection method and detection device for chemically inducing osmium to be oxidized by using ultraviolet light
  • Mobile detection method and detection device for chemically inducing osmium to be oxidized by using ultraviolet light
  • Mobile detection method and detection device for chemically inducing osmium to be oxidized by using ultraviolet light

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] The concentration of the osmium sample in the spiked river water is 0.1ng / mL of the solution sample containing osmium, and the solution sample containing osmium placed in the reagent bottle 1 is pumped into the flow injector through a peristaltic pump, and the sample solution is introduced into the reaction The flow rate of the quartz tube is 1.5ml / min, and then the reaction quartz tube (such as figure 1In the shown), the wavelength used by the low-pressure mercury lamp is 254nm, and the reaction quartz tube is an ordinary quartz tube. In this embodiment, the low-pressure mercury lamp is a customized ultraviolet lamp, and the reaction quartz tube passes through the interior of the ultraviolet lamp. The length of the reaction quartz tube is 20cm. The UV lamp was continuously irradiated for 30 s during the whole reaction process. The sample containing osmium enters the gas-liquid separator after being irradiated by a UV lamp. The heating temperature of the gas-liquid sep...

Embodiment 2

[0027] Add standard osmium samples in seawater, the osmium solution was prepared by hydrochloric acid solution and added 2 μg / mL inorganic ion Fe 3+ (can also be Fe 2+ , S 2 o 8 - or Cr 6+ ) to form the solution sample to be tested containing osmium with an osmium concentration of 100ng / mL, the solution sample to be tested containing osmium placed in the reagent bottle 1 is pumped into the flow injector by the peristaltic pump, and then the high-pressure mercury is introduced by the flow injector The reaction quartz tube irradiated by the lamp, the flow rate of the sample solution into the reaction quartz tube is 1ml / min, the wavelength used by the high-pressure mercury lamp is 254nm, and the reaction quartz tube is selected as a synthetic quartz tube, wherein the reaction quartz tube is outside the ultraviolet lamp, and its length is 25cm. The ultraviolet lamp was continuously irradiated for 2 minutes during the whole reaction process. After being irradiated by the ultra...

Embodiment 3

[0029] The osmium solution of the dissolved ore sample was prepared by nitric acid solution, and 100 μg / mL of inorganic ion Fe was added 2+ (can also be Fe 3+ , S 2 o 8 - or Cr 6+ ) to form a solution sample containing osmium with an osmium concentration of 2 μg / ml, the solution sample to be tested containing osmium placed in the reagent bottle 1 is pumped into the flow injector by a peristaltic pump, and then the metal halide is introduced into the flow injector The reaction quartz tube irradiated by the lamp, the flow rate of the sample solution into the reaction quartz tube is 0.5ml / min, the wavelength used by the metal halide lamp is 185nm, and the reaction quartz tube is selected as a synthetic quartz tube, wherein the reaction quartz tube is outside the ultraviolet lamp, and its length It is 30cm. The ultraviolet lamp continued to irradiate for 15 minutes during the whole reaction process. After being irradiated by the ultraviolet lamp, the sample containing osmium ...

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Abstract

The invention discloses a mobile detection method and a detection device for chemically inducing osmium to be oxidized by using ultraviolet light. The detection method comprises the following steps that: an osmium-containing solution sample to be detected is introduced into a sample reaction quartz tube, and is irradiated by the ultraviolet light to induce osmium in the sample to be oxidized into an osmium tetroxide solution; and the osmium tetroxide solution is introduced into a gas-liquid separator for gas-liquid separation to produce osmium tetroxide steam, and the osmium tetroxide steam is measured by ICP-OES or ICP-MS to obtain osmium signals. The detection device at least comprises the reaction quartz tube and an ultraviolet lamp, wherein the quartz tube is positioned inside or outside the ultraviolet lamp, and is communicated with the gas-liquid separator by a pipeline, and a gas carrier inlet is positioned in the middle of the reaction quartz tube and the gas-liquid separator through a three-way pipe; an upper section of the gas-liquid separator is a straight condenser pipe, and a lower section of the gas-liquid separator is provided with a coolant inlet; and the coolant inlet is wrapped with a metal wire or heating tape. The method provided by the invention is relatively simple, does not need any redox reagent, and reduces the loss of osmium in the sample and the pollution brought in the pretreatment process; and the sensitivity is higher, the sample can be introduced more effectively than the traditional nebulization sampling method, and the detection limit is lower.

Description

Technical field: [0001] The flow type ultraviolet photochemically induced osmium oxidation detection method and detection 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 5d 6 6s 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 appli...

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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