Method of measuring micro-amount niobium in steelmaking blast furnace slag
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A technology of blast furnace slag and micro-quantity, which is applied in the direction of measuring devices, material analysis by electromagnetic means, instruments, etc., can solve problems such as unsuitable analysis of micro-quantity niobium, unsatisfactory measurement, interference in measurement, etc., to achieve good application effect and eliminate matrix effect, the effect of easy operation
Inactive Publication Date: 2015-07-08
INNER MONGOLIA BAOTOU STEEL UNION
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[0002] At present, in the national standard analysis methods and the literature found, the methods for determining niobium include chlorosulfonol-C spectrophotometry, nitrosulfonol-M spectrophotometry and antipyridine azo spectrophotometry. These three methods Low sensitivity Molybdenum, vanadium, tungsten, etc. interfere with the determination, and are not suitable for the analysis of trace niobium; Xue Yulan et al. studied "IPC-AES Determination of Niobium in Slag". Solvent melting treatment residue, long process and large amount of flux added, easy to introduce elements to be measured, the detection limit of the method is 0.1%, which cannot meet the determination of trace niobium in slag
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Embodiment 1
[0053] Blast furnace slag samples were weighed and determined by acid-soluble-chlorosulfonol C spectrophotometry and the above method, respectively, and the results are shown in Table 1.
[0054] Table 1 Sample determination results
[0055]
Embodiment 2
[0056] Embodiment 2: standard addition recovery
[0057]Weigh the niobium-free blast furnace slag standard sample YSBC28851-98, and add niobium standard to the blast furnace slag YSBC28852-98, so that the niobium content is 0.0050%, 0.0100%, 0.020%, and 0.050%, respectively, and measure it according to the above method, and the results are shown in the table 2.
[0058] Table 2 Standard sample spiked recovery determination results
[0059]
[0060] From the data in the above table, it can be calculated that the recovery rate of the addition of niobium is 96%-106%, and the measurement results are accurate, meeting the requirements for the determination of trace amounts of niobium in blast furnace slag.
Embodiment 3
[0062] Select slag standard sample R-712 (Nb 2 o 5 The certified value is 0.066%, and this standard sample exceeds the upper limit of the analytical method by weighing 0.0500g sample), R-715 (Nb 2 o 5 Certified value is 0.042%), measured by the above-mentioned method, the results are shown in Table 3.
[0063] Table 3 Determination results of standard samples
[0064]
[0065] Therefore, the present invention adopts the low-temperature acid dissolution-ICP-MS mass spectrometry method to simultaneously rapidly and accurately measure the content of trace niobium in steelmaking blast furnace slag. The recovery rate and accuracy of this method all meet the detection and analysis requirements, and the linear correlation coefficients of the elements are all between 0.9991 and 0.9999, which has high practicability and wide promotion value.
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Abstract
The invention discloses a method of measuring micro-amount niobium in steelmaking blast furnace slag. The method includes steps: (1) preparing standard work solutions of niobium in different concentrations; (2) introducing an inductively coupled plasma source mass spectrometer to measure the signal intensity of to-be-test ions and draying calibration curves of the standard work solutions of niobium; (3) weighing a blast furnace slag sample and successively adding nitric acid, hydrochloric acid and hydrofluoric acid to dissolve the sample; (4) preparing a blank sample added with the nitric acid, the hydrochloric acid and the hydrofluoric acid without addition of the blast furnace slag sample, adding perchloric acid to generate smoke for expelling residual hydrofluoric acid, and cooling the blank sample to room temperature; (5) adding a water solution of tartaric acid and hydrochloric acid to an electric heating plate for heating and dissolving salts, cooling the solution to room temperature and moving the solution to a volumetric flask; (6) adding a cesium standard solution and performing a constant volume operation with high-purity water; (7) introducing the blast furnace slag sample solution and the blank sample solution into the inductively coupled plasma source mass spectrometer and measuring the signal intensity of the to-be-test ions; and (8) calculating the content of niobium in the sample solution according to the 93Nb standard work solution calibration curve being known in concentration.
Description
technical field [0001] The invention relates to the technical field of iron and steel metallurgical analysis, in particular to a method for measuring trace amounts of niobium in steelmaking blast furnace slag. Background technique [0002] At present, in the national standard analysis methods and the literature found, the methods for determining niobium include chlorosulfonol-C spectrophotometry, nitrosulfonol-M spectrophotometry and antipyridine azo spectrophotometry. These three methods Low sensitivity Molybdenum, vanadium, tungsten, etc. interfere with the determination, and are not suitable for the analysis of trace amounts of niobium; Xue Yulan et al. studied "IPC-AES Determination of Niobium in Slag". Solvent melting treatment residue, long process and large amount of flux added, easy to introduce elements to be measured, the lower detection limit of the method is 0.1%, which cannot meet the determination of trace niobium in slag. Contents of the invention [0003] ...
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