This standard specifies the determination method of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide in europium oxide. This standard is applicable to the determination of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide in europium oxide. GB/T 8762.8-2000 Chemical analysis method for europium oxide. Inductively coupled plasma atomic emission spectrometry for the determination of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide, lutetium oxide and yttrium oxide in europium oxide. GB/T8762.8-2000 standard download decompression password: www.bzxz.net

GB/T 8762.8--2000
This standard has no corresponding international standard and foreign advanced standard. This standard is formulated to meet the product standard and trade needs of "fluorescent grade oxidized ferrite".
This standard is different from GB/T8762.7--1988 "Chemical spectroscopy and direct spectroscopic method for the determination of the amount of antimony oxide, zirconium oxide, oxide, vanadium oxide and oxide in fluorescent grade europium oxide":
1. The detection method is the advanced and popular plasma spectrometry. 2. The determination of all rare earth impurity elements (14) except adjacent elements is added. 3. It is written in accordance with GB/T1.1--1993 and GB/T1.4--1987 standards. 4. This standard complies with: GB/T1467-1978 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products" This standard is proposed by the Rare Earth Office of the National Development and Planning Commission. This standard is under the jurisdiction of the National Technical Committee for Rare Earth Standardization. This standard was drafted by Shanghai Yuelong Nonferrous Metals Co., Ltd. The main drafter of this standard is Yu Bingyan.
National Standard of the People's Republic of China
Chemical analysis method for europium oxide
Determination of lanthanum oxide,cerium oxide,praseodymium oxide,neodymium oxide, samarium oxide,gadolinium oxide,terbium oxide,dysprosium oxide, holmium oxide,erbium oxide,thulium oxide,ytterbium oxide,lutetium oxide and yttrium oxide contents in europium oxide by inductively coupled plasma atomic emission spectrometric methodGB/T 8762.8- 2000
This standard specifies the determination method of lanthanum oxide, cerium oxide, zirconium oxide, neodymium oxide, vanadium oxide, cobalt oxide, thulium oxide, dysprosium oxide, iron oxide, palladium oxide, tantalum oxide, tantalum oxide, tantalum oxide and yttrium oxide in chalcanthite. This standard is applicable to the determination of lanthanum oxide, cerium oxide, cerium oxide, neodymium oxide, tantalum oxide, yttrium oxide, thulium oxide, dysprosium oxide, iron oxide, palladium oxide, tantalum oxide, tantalum oxide and yttrium oxide in europium oxide. The determination range is shown in Table 1. Table 1
Oxide
Lanthanum oxide
Cerium oxide
Zirconium oxide
Neodymium oxide
Method principle
Determination range, %
0. 001 0~0. 020
0. 001 5~0. 020
0. 001 5~0. 020
0. 001 0-~0. 020
0. 001 0-~ 0. 020
0. 001 0~~0. 020
0. 001 5~0. 020
Oxide
Dysprosium Oxide
Iron Oxide
Zhen Oxide
Iron Oxide
Ytterbium Oxide
Oxide Plating
Yttrium Oxide
Measurement Range, %
0. 001 0~~0. 020
0. 000 5~~0. 020
0, 000 5 ~ 0. 020
0, 000 3-~ 0. 020
0. 000 1-0.020
0. 000 1 -~ 0. 020
0. 000 1~0. 020
The sample is dissolved in hydrochloric acid and excited directly by an argon plasma light source in a dilute hydrochloric acid medium to perform spectrum measurement. 3 Reagents
3.1 Hydrogen peroxide (30%).
Approved by the State Administration of Quality and Technical Supervision on June 5, 2000, implemented on November 1, 2000
3.2 Hydrochloric acid (1+1).
3.3 Nitric acid (1+1).
3.4 ​​Argon (>99.99%).
GB/T 8762. 8--2000
3.5 Sodium oxide standard solution: Weigh 25.0000g of calcined 1h at 900℃ (≥99.999%), place in a 250mL beaker, add 100mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 250mL volumetric flask, dilute to scale with water, and mix. This solution contains 100mg europium oxide in 1mL.
3.6 Lanthanum oxide standard stock solution: Weigh 0.1000g of lanthanum oxide (>99.99%) calcined 1h at 900℃, place in a 100ml beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg of calcined 1mL. Then dilute this solution into 1mL containing 100μg and 1mL containing 10μg of lanthanum oxide standard solution, the acidity of which is 5% hydrochloric acid.
3.7 Antimony oxide standard storage solution: weigh 0.1000g of antimony oxide (>99.99%) that has been calcined at 900℃ for 1h, place it in a 100mL beaker, add 10mL nitric acid (3.3), add 10mL hydrogen peroxide (3.1), dissolve at low temperature, remove and cool, transfer to a 100ml volumetric flask, dilute with water to the scale, and mix well. This solution contains 1mg antimony oxide in 1ml. Then dilute this solution into 1ml containing 100g and 1ml containing 10pg of cerium oxide standard solution, the acidity of which is 5% nitric acid. 3.8 Zirconia standard stock solution: Weigh 0.1000g of zirconium oxide (>99.99%) calcined at 900℃ for 1h, place in a 100mL beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg of zirconium oxide in 1mL. This solution is then diluted into 1mL containing 100μg and 1mL containing 10μg of zirconium oxide standard solutions, and the acidity is 5% hydrochloric acid. bzxZ.net
3.9 Neodymium oxide standard stock solution: Weigh 0.1000g of neodymium oxide (99.99%) calcined at 900℃ for 1h, place in a 100mL beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg of neodymium oxide in 1ml. Then dilute this solution into 1mL containing 100μg and 1mL containing 10μg of neodymium oxide standard solution, the acidity of which is 5% hydrochloric acid.
3.10 Oxidation standard storage solution: weigh 0.1000g of oxidation (99.99%) that has been burned at 900℃ for 1h, place it in a 100mL beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute with water to the scale, and mix well. This solution contains 1mg oxidation in 1mL. Then dilute this solution into 1mL containing 100ug and 1mL containing 10ug of oxidation standard solution, the acidity of which is 5% hydrochloric acid.
3.11 Standard stock solution of oxide: Weigh 0.1000g of oxide (>99.99%) that has been burned at 900℃ for 1h, place it in a 100ml beaker, add 10ml of hydrochloric acid (3.2), dissolve it at low temperature, remove it and cool it, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and mix it. 1ml of this solution contains 1mg of oxide. This solution is then diluted into 1ml containing 100μg and 1ml containing 10μg of standard solution, and the acidity is 5% hydrochloric acid.
3.12 Standard stock solution of thorium oxide: Weigh 0.1000g of thorium oxide (99.99%) that has been burned at 900℃ for 1h, place it in a 100ml beaker, add 10ml of hydrochloric acid (3.2), dissolve it at low temperature, remove it and cool it, transfer it to a 100ml volumetric flask, dilute it to the mark with water, and mix it. 1 mL of this solution contains 1 mg of dysprosium oxide. Then dilute this solution into 1 ml containing 100 μg and 1 ml containing 10 μg of standard solution, both of which contain 5% hydrochloric acid.
3.13 Dysprosium oxide standard storage solution: weigh 0.1000 g of dysprosium oxide (>99.99%), placed in a 100mL beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg dysprosium oxide in 1mL. This solution is further diluted into 1mL containing 100μg and 1mL containing 10μg dysprosium oxide standard solutions, both of which contain 5% hydrochloric acid.
3.14 Standard storage solution of tin oxide: weigh 0.1000g of iron oxide (≥99.99%) that has been calcined at 900℃ for 1h, place in a 100ml beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to scale with water, and mix. This solution contains 1mg iron oxide in 1mL. This solution is further diluted into 1mL containing 100g and 1mL containing 10μg tin oxide standard solutions, both of which contain 5% hydrochloric acid.
3.15 Standard storage solution of oxidized bait: weigh 0.1000g of oxidized bait (99.99%) calcined at 900℃ for 1h, place in a 100ml calcination cup, add 10mL of hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100ml volumetric flask, dilute to scale with water, and mix well. 1mL of this solution contains 1mg of oxidized bait. Then dilute this solution into 1mL containing 100μg and 1ml containing 10μg of oxidized bait, the acidity of which is 5% hydrochloric acid.
3.16 Standard stock solution of manganese oxide: weigh 0.1000g of manganese oxide (>99.99%) that has been burned at 900℃ for 1h, place it in a 100ml beaker, add 10ml of hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100ml volumetric flask, dilute to scale with water, and mix. 1ml of this solution contains 1mg of manganese oxide. This solution is then diluted into 1mL containing 100ug and 1mL containing 10μg of manganese oxide. The acidity is 5% hydrochloric acid.
3.17 Standard stock solution of ytterbium oxide: weigh 0.1000g of manganese oxide (99.99%) that has been burned at 900C for 1h, place it in a 100ml beaker, add 10ml of hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100ml volumetric flask, dilute to scale with water, and mix well. 1mL of this solution contains 1mg of ytterbium oxide. This solution is then diluted into 1mL containing 100μg and 1mL containing 10μg of ytterbium oxide standard solutions, both of which contain 5% hydrochloric acid.
3.18 Oxidation standard storage solution: Weigh 0.1000g of oxide (99.99%) that has been burned at 900℃ for 1h, cover it in a 100ml beaker, add 10ml of hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to the scale with water, mix well, and this solution contains 1mg of oxide. This solution is then diluted into 1mL containing 100ug and 1mL containing 10μg of oxide standard solutions, both of which contain 5% hydrochloric acid.
3.19 Oxidation standard stock solution: Weigh 0.1000g of yttrium oxide (>99.99%) that has been burned at 900℃ for 1h, cover it in a 100ml beaker, add 10mL of hydrochloric acid (3.2), dissolve at low temperature, remove and cool, transfer to a 100mL volumetric flask, dilute to the mark with water, and add water. This solution contains 1mg yttrium oxide in 1mL. This solution is then diluted into 1mL containing 100μg and 1mL containing 10pg of yttrium oxide standard solution, and the acidity is 5% hydrochloric acid.
4 Instruments
4.1 Computer-controlled sequential scanning monochromator: The reciprocal line dispersion is not greater than 0.25nm/mm (-level spectrum). 4.2 Light source: Argon plasma light source, the power used is not less than 1.2kW. 5 Sample
Burn the sample at 900℃ for 1h, place it in a desiccator, cool to room temperature, and weigh it immediately. 6 Analysis steps
6.1 Preparation of analytical solution
Weigh 1.0000g of sample (5), place in a 100mL beaker, add 10mL hydrochloric acid (3.2), dissolve at low temperature, cool to room temperature, transfer to a 100mL volumetric flask, dilute to scale with water, mix well and set aside. 6.2 Preparation of standard solution
Transfer the standard solution of platinum oxide (3.5) and the standard solutions of each rare earth oxide (3.6~3.19) into 6 100mL volumetric flasks according to Table 2, add 10mL hydrochloric acid (3.2), dilute to scale with water, mix well, and prepare 6 standard solutions. Table 2
Standard solution number
Platinum oxide
10 000
Lanthanum oxide
Concentration of each rare earth (in terms of oxide), ug/ml. Cerium oxide
Zirconium oxide
Neodymium oxide
Standard liquid number
6.3 Determination
6.3.1 Determination conditions:
Alpha oxide
Dysprosium oxide
GB/T 8762.8—2000
Table 2 (complete)
Concentration of each rare earth (in vapor form) ug/mlOxide
Ammonium oxide
Plasma light source: incident power 1.0kW, reflected power less than 0.005kW. Chlorine gas flow rate: cooling gas flow rate 12L/min, carrier gas flow rate 0.42L/min. Observation height: 12mm above the coil.
6.3.2 Analysis line and linear range are shown in Table 3. Table 3
analysis line, nm
linear range, %
0. 001 0~~0, 020
0. 001 5~0. 020
0. 001 5~0. 020
0. 001 0~~0. 020
0. 001 0~0. 020
0. 001 0-~0. 020
0. 001 0~-0. 020
0. 001 0~~0. 020
0. 001 5~-0. 020
0. 001 5~~0. 020
1) According to different instruments, the two analysis lines can be selected.
Oxidation mirror
Analysis line, nm
6.3.3 The analysis solution (6.1) and the standard solution (6.2) are simultaneously subjected to argon plasma spectrometry. The analysis results are calculated.
Linear range, %
0. 001 0~ 0. 020
0. 000 5 ~0. 020
0. 000 5-- 0. 020
0. 000 5 ~~0. 020
0. 000 3~0. 020
0. 000 1--0. 020
0. 000 1-~0. 020
0. 000 1~0. 020
Directly input the content of the standard solution into the computer, and the computer will calculate and output the analysis results based on the strength values ​​of the standard solution and the analytical solution.
8 Allowable difference
The difference between the analysis results of laboratories should not be greater than the allowable relative difference listed in Table 4. Table 4
Oxides
Cerium oxide
Terium oxide
Cerium oxide
Content range, %
0. 001 5~0. 005 0
>0. 005 0~ 0- 020 0
Allow relative difference, %
Oxides
Lanthanum oxide
Neodymium oxide
Yttrium oxide
Gallium oxide
Titanium oxide
Ytterbium oxide
Yttrium oxide
GB/T 8762. 8--2000
Table 4 (End)
Content range, %
0. 001 0~~ 0. 005 0
>0. 005 0~0. 020 0
0. 000 5~ 0. 002 0
>0. 002 0~~0. 020 0
0. 000 3~0. 000 5
≥0. 000 5 ~0. 002 0
>0. 002 0~0. 020 0
0. 000 1 ~0. 000 3
>0. 000 3~0. 000 5
>0. 000 5 ~ 0. 002 0
>0. 002 0~0. 020 0
Relative difference allowed, %020 0
Relative difference allowed, %
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