Method for rapid determination of content of a plurality of elements in rare earth metal / alloy
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A technology for rapid determination of rare earth metals, applied in measurement devices, preparation and sampling of samples for testing, etc., can solve problems such as low efficiency, large errors, environmental pollution, etc., and achieve the effect of improving efficiency, good linearity, and ensuring precision
Active Publication Date: 2017-11-10
NCS TESTING TECH
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X-ray fluorescence spectrometry can only measure elements with atomic numbers greater than 12, but cannot determine the content of C and N, and for impurity elements with content less than 0.05% and elements with smaller atomic numbers such as Mg, Al, Si, P, S, etc. The repeatability of the measurement results is poor and the error is large
Inductively coupled plasma spectroscopy or mass spectrometry also cannot determine the content of C and N, and the sample pretreatment steps are cumbersome and time-consuming, and a large amount of chemical reagents need to be added for digestion, which not only pollutes the environment, but also may introduce new impurities, and the processing and testing time of a single sample It takes about 1 day
Using these two methods for analysis is inefficient and cannot quickly reflect the relationship between process adjustment and product quality level. Therefore, the rare earth smelting and separation industry urgently needs a rapid analysis technology to guide production process adjustment.
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[0074] The first step, sample pretreatment
[0075] Select a PrNd alloy sample to be tested with a plane with a diameter greater than 5mm, or cut a PrNd alloy to be tested with a plane with a diameter greater than 5mm, and then use abrasive dry grinding or mechanical processing to treat the surface of the sample to be tested to a certain degree of smoothness. To ensure the tightness between the excitation platform and the sample to be tested and the repeatability of the analysis results.
[0076] The second step is to set the excitation conditions of the spark light source
[0077] Preparation of the spark emission spectrometer, start the spectrometer and turn on the constant temperature heating and vacuum pump switch. After the temperature and vacuum degree of the optical chamber are constant to the set range, turn on the excitation protection gas (argon or helium, purity ≥ 99.99%). Excite the waste sample 3 to 5 times, replace the residual air in the air path, and stabilize...
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Abstract
The present invention belongs to the technical field of element determination in a rare earth metal / an alloy, and in particular relates to a method for rapid determination of content of rare earth elements and non rare earth elements in the rare earth metal / the alloy on the basis of full spectrum direct reading spark emission spectrometry. The method includes the following steps: (1) sample pretreatment; (2) setting of excitation conditions of a spark light source; (3) selecting of an analysis line pair; (4) establishing of a working curve; (5) curve correction; and (6) sample analysis. No chemical reagent is used, a solid sample can be directly detected, determination time is shortened to within 2 minutes from a few hours of that of a national standard method, determination results are consistent with those of the national standard method, precision is good, and a blank for rapid element determination of the rare earth metal / the alloy is filled.
Description
technical field [0001] The invention belongs to the technical field of determination of elemental components in rare earth metals / alloys, in particular to a rapid determination of rare earth elements and molybdenum, iron, carbon, phosphorus, sulfur and aluminum in rare earth metals / alloys based on full-spectrum direct reading spark emission spectrometry , silicon, copper, chromium, nickel, calcium, magnesium, tungsten, niobium, tantalum, titanium, manganese, zinc, lead, thorium, zirconium, cadmium, nitrogen, sodium and other non-rare earth elements. Background technique [0002] Rare earth metals / alloys are the products of rare earth smelting and separation. Rare earth metals mainly include scandium, yttrium, lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, etc., rare earth alloys Including praseodymium neodymium alloy, praseodymium neodymium dysprosium alloy, mixed rare earth meta...
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