Method for rapidly measuring trace osmium with inductively coupled plasma-massspectrometry

Abstract

The invention discloses a method for quickly determining trace osmium in nickel alloy by inductively coupled plasma mass spectrometry. By adding a reducing agent ascorbic acid into the solution to be tested, the high-valence osmium (+8) is reduced, and the valence of the osmium standard solution is The state is consistent, so that the atomization efficiency in ICP-MS is consistent, and the standard curve method is used to directly measure the amount of osmium in the nickel alloy test solution on the inductively coupled plasma mass spectrometer. Other coexisting elements in the nickel alloy will not be Restored to solid form and precipitated. The sample does not need to be absorbed by distillation to determine the amount of osmium by ICP-MS; it does not depend on the addition of isotope diluent while processing the sample 190 Os, make it fully mixed with the sample or standard solution, exchange to reach equilibrium, keep the same chemical form of osmium, and then use the ICP-MS method to determine the amount of osmium. The method can accurately and quickly measure the trace osmium in the nickel alloy material rich in platinum group metals by using the method. The method is simple, fast and has high accuracy and meets the analysis requirements of the trace osmium in the nickel alloy.

Description

technical field [0001] The invention belongs to the technical field of testing and analysis of platinum group metals, and relates to a method for analyzing and detecting osmium in a nickel alloy material rich in platinum group metals produced in a nickel smelting process, in particular to an inductively coupled plasma mass spectrometry method for rapid determination of nickel alloys method for trace amounts of osmium. Background technique [0002] Inductively coupled plasma mass spectrometry (ICP-MS for short) method for determining trace osmium usually includes alkali fusion-distillation-reducing agent absorption-inductively coupled plasma mass spectrometry, and isotope diluent 190 In the presence of Os, the samples were separated and enriched by alkali fusion-distillation or fire test, and then determined by ICP-MS. [0003] The ICP-MS method is used to determine trace osmium. According to the introduction of He Hongliong et al. in "Analytical Chemistry" 1994 No. 2, page ...

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Problems solved by technology

However, when applying the isotope dilution method, it is pointed out in He Hongliu’s literature ("Analytical Chemistry" 1994, No. 2, No. 111, 2.3.3) that after the diluent solution is mixed with the standard or sample solution, if the chemical form of osmium is not Sufficient exchange to achieve equilibrium, or differences in the chemical form equilibrium state between the standard and the sample solution, will cause differences in the ICP-MS signal intensity, resulting in erroneous analysis results

The above methods all have the disadvantages of long analysis process and cumbersome operation.

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