Rare earth single element solution standard substance and its preparation
A technology of standard substances and rare earth solutions, which is applied in the direction of instruments, measuring devices, scientific instruments, etc., can solve the problems of inability to achieve effective deduction of impurity components, lack of traceability, inaccurate measurement of rare earth impurities, etc.
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Embodiment 1
[0055] Embodiment 1 preparation is used for the rare earth solution of purity fixed value
[0056] The high-purity rare earth oxides were burned in a muffle furnace at 900°C, cooled, placed in a vacuum desiccator, and stored in a vacuum. First, accurately weigh a certain amount of oxide in a tall beaker, moisten it with a small amount of water, add a certain amount of 1:1 hydrochloric acid to dissolve it, let it stand and cool to room temperature. Dilute to volume with 10% hydrochloric acid and prepare a solution with a target concentration of 1000 μg mL-1 for purity determination. The hydrochloric acid used was purified by redistillation, and the corresponding rare earth content was lower than 0.001ng g-1 (ICP-MS semi-quantitative results showed No data). The specific sample weighing and dilution results are shown in Table 4.
[0057] Table 4 The sample weight and target content of five kinds of rare earth oxides
[0058]
[0059] Note: The solution matrix is 10% HCl, ...
Embodiment 2
[0060] Embodiment 2 main component of raw material is determined
[0061] Purchased high-purity rare earth oxides (Dy 2 o 3 ,Ho 2 o 3 ,Er 2 o 3 ,Tm 2 o 3 ,Sc 2 o 3 ), the nominal purity is 99.9% to 99.99%. After being mixed with boric acid and pressed into tablets, it was measured by LA-ICP-MS (see Table 1 for the measurement conditions), all of which were found in the characteristic mass-to-nucleus ratios of these elements ( 163 Dy + , 165 Ho + , 166 Er + , 169 T m + and 45 sc + ) is greater than 10 10 The signal intensity of cps is proved to be the raw material corresponding to the main component of rare earth. In addition, an X-ray diffractometer (Panalytical X'PRO) was also used to analyze the main component phase of the raw material samples with reference to the standard "Determination of Mineral Cell Parameters-Powder X-ray Diffraction Method" (EJ / T 553-1991) , which also proves that the sample is the main component of the corresponding rare earth. ...
Embodiment 3E
[0062] Embodiment 3 EDTA complexometric titration metal ion total amount
[0063] The absorption concentration is about 1000μg mL -1 Put 10mL of rare earth standard substance solution in a 250mL Erlenmeyer flask, add 50mL of deionized water, 0.2g of ascorbic acid, shake well, add about 3mL of 1:1 ammonia water dropwise, make the pH value of the solution between 5.0 and 5.5, add 5mL of 1mol L -1 Six times tetramine buffer solution (pH value is about 6.3), 5 drops of 0.3% xylenol orange indicator, the system is blue-purple at this time. Use 0.01mol L -1 Titrate the EDTA standard solution, and add it drop by drop when it reaches 5mL. The color of the solution is from purple red to bright yellow, which is the end point. Each rare earth is titrated 14 times in parallel, which is completed independently by two groups of experimenters. The titration results are shown in Table 5:
[0064] Table 5 Dy, Ho, Er, Tm, Sc standard substance solution titration results (μg g -1 ,n=14)
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