GB/T 15917.2-1995 Chemical analysis of dysprosium metal and dysprosium oxide. Inductively coupled plasma optical emission spectrometry for the determination of copper, molybdenum, nickel and titanium in dysprosium metal. GB/T15917.2-1995 standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Method for chemical analysis of dysprosium metal and its oxide
Inductively coupled plasma atomic emission spectrometry
Determination of copper, molybdenum, nickel and titanium contents in metal picksGB/T 15917.2---1995
Dysprosium and dysprosium oxide-Determination of copper, molybdenum,nickel and titanium contents--Inductively coupled plasmaatomic emission spectroscopic method1Subject content and scope of application
This standard specifies the method for determining the contents of copper, molybdenum, nickel and titanium in dysprosium metal. This standard is applicable to the sequential determination of the contents of copper, molybdenum, nickel and titanium in dysprosium metal. It is also applicable to the sequential determination of the contents of copper oxide and nickelous oxide in dysprosium oxide. Determination range: 0.005% to 0.50%. 2 Reference standards
GB1.4 Guidelines for standardization work Provisions for the preparation of chemical analysis methods GB1467 General principles and general provisions for chemical analysis methods for metallurgical products 3 Principles of the method
The sample is dissolved in nitric acid. In a dilute nitric acid medium, it is directly excited by an argon plasma light source and the spectrum is measured. 4 Reagents
4.1 KS0,, high-grade pure.
4.2 MoO:, spectrally pure.
4.3 CuO, spectrally pure.
4.4 Nio, spectrally pure.
4.5 TiO2, spectrally pure.
4. 6 Dy,0,,≥99. 999%.
4.7 Deionized water, resistance not less than 10°α. 4.8 HNO,(1+1), high-grade pure.
4.9 HCI(1+1), high-grade pure.
4.10H2SO (1+9), high-grade pure.
4.11Ammonia water, high-grade pure.
4.12Fluorine gas,>99.99%.
4.13Standard solution: Weigh 1.1477gDyz) (4.6) calcined at 850℃ for 1h, place in a 100mL beaker, add 20mLHNO, (4.8), heat to dissolve, cool and transfer to a 100mL volumetric flask, dilute to scale with water (4.7), mix well. This solution contains 1ml. Approved by the State Administration of Technical Supervision on December 20, 1995 and implemented on August 1, 1996
10 mg dysprosium.
GB/T15917.2—1995
4.14 Copper standard solution: weigh 0.1252gCu0 (4.3) and place it in a 100mL beaker, add 20mLHNO4.8). Heat to dissolve, cool and transfer to a 100mL volumetric flask, dilute to scale with water (4.7), and mix. This solution contains 1mg copper in 1mL. 4.15 Molybdenum standard solution: weigh 0.1500gMo0 (4.2), place it in a 100L beaker, add 10mL ammonia water (4.11), heat to dissolve, cool and transfer to a 100mL volumetric flask, add 20mLHNO (4.8), dilute to scale with water (4.7), and mix. This solution contains 1mg molybdenum in 1ml.
4.16 Nickel standard solution: Weigh 0.1273g NiO (4.4) into a 100mL beaker, add 20mL HC (4.9), heat to dissolve. After cooling, transfer to a 100ml volumetric flask, dilute to scale with water (4.7), and mix. 1mL of this solution contains 1mg nickel. 4.17 Titanium standard solution: Weigh 0.1668g TiO2 (4.5), place in a 10mL porcelain crucible, add 3.5000g K, S.0), (4.1). Heat on an electric furnace to K, S20, completely melt, then place at 760℃~800℃ to melt for 5min, take out and cool, put into a 100ml beaker, add 60ml H.SO (4.10) to soak the molten block, heat to dissolve, cool, wash the crucible with a small amount of HzSO (4.10). Transfer the solution into a 100ml volumetric flask, dilute to the scale with H, SO (4.10), and mix. This solution contains 1mg titanium in 1mL. 5 Instruments
5.1 Computer-controlled sequential scanning monochromator: The reciprocal line dispersion rate is not greater than 0.26nm/mm. 5.2 Light source: plasma light source, power 2.5kW. 6 Analysis steps
6.1 Preparation of analytical solution
6.1.1 Preparation of metal dysprosium analytical solution
Weigh 0.4000g of metal pot, place it in a 100ml beaker, slowly add 10mL HNO, (4.8), heat for 5min, transfer to a 100ml volumetric flask after cooling, dilute to scale with water (4.7), mix well for testing. 6.1.2 Preparation of dysprosium oxide analytical solution
Weigh 0.4591g Dy2O calcined at 850C for 1h, place it in a 100ml beaker, add 10mL HNO. (1.8), heat to dissolve, transfer to a 100ml volumetric flask after cooling, dilute to scale with water (4.7), mix well for testing. 6.2 Determination
6.2.1 Preparation of standard solution
Transfer the dysprosium standard solution (4.13) and the impurity standard solution (4.14-4.17) into two 100ml. volumetric flasks according to Table 1. Add 10mL HNO. (4.8) to each, dilute to the mark with water (4.7), and mix. Table 1
Standard sample No. 1
Standard sample No. 2
6.2.2 Determination conditions
Content of dysprosium and impurities, ug/ml.
Plasma light source: incident power 1.0kW, reflected power not more than 0.005kW. Argon gas flow rate: cooling gas 12L/min, carrier gas 0.37I/min. Observation height: 15mm above the working coil
Analysis line and determination range are shown in Table 2.
Analysis line, nm
Mo203.844
Cu 224.700
Ni231.604
Ti334.941
GB/T15917.21995
Background position, nm
Measurement range, %
0. 005 ～0. 500
0. 005 ~0. 500
0. 005 ~-0. 500
0.005~~0.500
6.2.3 Perform argon plasma measurement on the analytical solution (6.11 or 6.1.2) and the standard solution (6.2.1) simultaneously. Calculation and expression of analysis results
7.1 Calculation of analysis results of metal pick sample
Input the content of standard solution (6.2.1) into the computer. According to the strength values ​​of standard solution and test solution, the computer outputs the analysis results. 7.2 Calculation of analysis results of dysprosium oxide sample
Multiply the percentage of copper and nickel (7.1) output by the computer by the conversion coefficient in Table 3 to obtain the analysis results. Table 3
Oxide
Conversion coefficient
Allowance
The difference of analysis results between laboratories should not be greater than the allowable relative difference listed in Table 4. Table 4
Cu, Mo, Ni, Ti
Additional notes:
This standard was proposed by the Rare Earth Office of the State Planning Commission. Base content range, %
0. 005 ~0. 010
0.010~0.100
>0. 10～0. 50
This standard was drafted by Beijing Nonferrous Metals Research Institute and Baotou Steel Rare Earth Research Institute. This standard was drafted by Ganzhou Nonferrous Metallurgy Research Institute. The main drafter of this standard is Lv Daorong. Www.bzxZ.net
Allowed relative difference, %
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