GB/T 8762.7-1988 Determination of the amounts of cerium oxide, praseodymium oxide, samarium oxide, gadolinium oxide and dysprosium oxide in fluorescent grade europium oxide - Chemical spectroscopic and direct spectroscopic methods
Some standard content:
National Standard of the People's Republic of China
Europium oxide of phosphorus grade-.Determination of cerium
oxide, praseodymium oxide , samarium oxide, gadoliniumoxide and dysprosium oxide contents-Spectrochemical method and
direct spectrographic methodUDC 661. 866. 1
GB 8762.7..- 88
This standard is applicable to the simultaneous determination of cerium oxide, praseodymium oxide, samarium oxide, gadoliniumoxide and dysprosium oxide contents in fluorescent europium oxide. The determination range is shown in Table 1.
Oxide
Chemical spectroscopy
Cerium oxide
Zirconium oxide
Yttrium oxide
0.000 08~0.001 5
0. 000 08 ~ 0. 001 5
0. 000 20~0. 001 0
0. 000 20~-0. 001 0
0. 000 20 ~ 0. 001 0
Direct spectroscopy
0. 001 0 ~ 0. 008 0
0. 001 0-~0. 008 0
0. 001 0 -~ 0. 008 0
This standard complies with GB1467--78 "General Principles and General Provisions of Chemical Analysis Methods for Metallurgical Products". 1 Method Summary
Chemical Spectrometry: The sample is dissolved in hydrochloric acid. In a hydrochloric acid medium of pH 2-3, zinc is used to reduce europium (Ion) to europium (Ion), followed by P507 leaching resin to separate it from impurities such as cerium, zirconium, vanadium, and vanadium. After the impurities enriched on the resin are eluted with hydrochloric acid (1+1), stone powder is used as a buffer, and a DC arc is used to excite in an oxygen-argon atmosphere for spectral determination. Direct Spectrometry: The sample is directly excited in an oxygen-argon atmosphere with graphite powder as a buffer, and a DC arc is used to excite in an oxygen-argon atmosphere for spectral determination. 2 Reagents
2.1 Cadmium oxide, the content of each rare earth impurity oxide is less than 2×10-'%. 2.2 Antimony oxide, 99.9%.
2.3 Zirconium oxide, 99.9%.
2.4 Oxidation 99.9%.
2.5 Vanadium oxide, 99.9%.
2.6 Dysprosium oxide, 99.9%.
Zinc powder, 40-80 mesh.
Approved by China National Nonferrous Metals Industry Corporation on February 4, 198826
Implemented on February 1, 1989
GB 8762.7-88
2.8P507 leaching resin: containing P507 (2-ethylhexylphosphonic acid mono-2-ethylhexyl ester) 55%, 100-150 months. 2.9 Graphite powder, spectrally pure.
Ammonia water (μ0.90). bzxz.net
Hydrochloric acid (μ.19).
Hydrochloric acid (1+}).
Hydrochloric acid (5+995).
Hydrochloric acid balanced solution (pH 2.5), prepared with hydrochloric acid (2.12). 2.14
Ammonium chloride-ammonia washing solution: 100 mL of water contains 2 parts of ammonium fluoride and 2 mL of ammonia. 2.15
Europium oxide solution: Weigh 1.2500 g of oxidized platinum (2.1) calcined at 850 for 1 hour, place in a 100 mL beaker, add 2.16
10 mL of hydrochloric acid (2.12), dissolve at low temperature, remove and cool, transfer to a 250 mL volumetric flask, dilute to scale with water, and mix well. This solution contains 5 mg of oxidized platinum in 1 mL.
2.17 Argon, 99%.
2.18 Oxygen, 99%.
3 Instruments, materials and devices
Plane grating spectrometer: reciprocal line dispersion is not less than 0.185nm/mm. Light source: DC arc, voltage 220~380V. 3.2
Microphotometer.
3.4 Graphite electrode. Spectrally pure, @6mm.
Photosensitive plate, UV type 1.
Quartz cyclone gas chamber, shape and size see Figure 1. 3.6
Figure 丨 Quartz cyclone gas chamber diagram
3.7 Peristaltic pump.
GB8762.7—88
3.8 Reduction column and separation column: both are Φ22×110mm, with 3# glass sand plate at the bottom. 3.9
Reduction-separation device (Figure 2).
Figure 2 Schematic diagram of reduction-separation
1--sample beaker; 2--sampling tube; 3 reduction column, 4 separation column, 5-equilibrium liquid reservoir; 6-elution liquid reservoir, 7-dynamic pump; 8-elution liquid outlet; 9-effluent liquid outlet, 10-waste liquid outlet; 11, 12, 13-four-way active cold 4 Analysis steps
4.1 Determination quantity
4.1.1 Chemical spectroscopy: weigh 3 samples for determination and take the average value. 4.1.2 Direct spectroscopy: weigh 1 sample. 4.2 Sample quantity
4.2.1 Chemical spectroscopy: weigh 1.6008 sample for each sample. 4.2.2 Direct spectroscopy: weigh 0.100g sample for each sample. 4.3 Separation and enrichment
4.3.1 Preparation of reduction column and separation column
4.3.1.1 Weigh 15g zinc powder (2.7), place in a 50mL beaker, add 5mL hydrochloric acid (2.12), stir for 30s, wash with water until nearly neutral, transfer to the reduction column, remove the bubbles at the bottom of the reduction column and set aside. 4.3.1.2 Weigh 10g P507 leaching resin (2.8), place in a 100mL beaker, mix with hydrochloric acid (2.13) to make a slurry, transfer to the separation column, cover the resin surface with foam plastic, wash the separation column with 300mL hydrochloric acid (2.12) at a flow rate of 2mL/min, and then wash the separation column with 300mL hydrochloric acid equilibrium solution (2.14) and set aside. 4.3.1.3 Connect the prepared reduction column and separation column according to Figure 2, and turn pistons 11, 12, and 13 to discharge the bubbles in the entire flow path. 4.3.2 Enrichment of impurities
4.3.2.1 Place the sample (4.2.1) calcined at 850℃ for 1h in a 200mL beaker 1, add 10mL hydrochloric acid (2.12), heat at low temperature on an electric furnace to dissolve, and evaporate until almost dry. Remove and cool, dissolve the salts with 5mL hydrochloric acid (2.13), add 150mL water, and mix well (the sample solution should have a pH of 2 to 3 at this time).
GB 8762.7-—88
4.3.2.2 Insert the sampling tube 2 into the sample beaker 1, turn pistons 11 and 12, connect the reduction column 3 with the separation column 1 and the flow discharge port 9, start the peristaltic pump 7, and control the flow rate to be 2.5mL/min for injection. After the sample solution has finished flowing, wash the beaker twice with 20 mL of water. Then wash the wall of the reduction column four times with 20 mL of water. 4.3.2.3 Turn the pistons 11, 12, and 13 to connect the eluent reservoir 6 with the separation column 4 and the eluent outlet 8, and use 100 mL of hydrochloric acid (2.12) to desorb the impurities enriched on the separation column. The eluent is placed in the outlet 8 with the original beaker 1 to receive it. After the eluent has finished flowing, turn the piston 12 to close the flow path and remove the beaker 1.
Note: () Regeneration of the reduction column: Turn the piston 11 to connect the reduction column 3 with the waste liquid outlet 10, wash the reduction column with 20 ml of hydrochloric acid (2.13), and then wash it with 50 ml of water until the pH is 3~4, and set aside.
② Regeneration of separation column: Turn pistons 11.12 and 13 to connect the balance liquid reservoir 5 with the separation column 4 and the eluent outlet 8, and wash the separation column with 200 nL of hydrochloric acid balance liquid (2.14) for use. 4.4 Preparation of spectral samples
4.4.7 Preparation of chemical spectral samples
Concentrate the solution in beaker 1 (4.3.2.3) to about 10 mL at low temperature on an electric furnace, and dilute it with water to about 30 mL. Heat to near boiling, add 25 mL of ammonia water (2.10) and 4 mL of europium oxide solution (2.16), continue to boil, remove and cool slightly. Filter with slow quantitative filter paper while hot, wash the beaker 5 times with hot ammonium chloride-nitrogen water washing solution (2.15), and wash the precipitate 7 to 8 times. Put the precipitate and the filter paper in a porcelain flask, dry at low temperature, and ash. Burn at 850℃ for 1h. Take out, place in a desiccator, cool to room temperature, weigh, and obtain an enriched sample. When the weight is less than 40 mg, add 2.1% sodium oxide to 40 mg. Mix it with graphite powder (2.9) Mix equal amounts, grind in an agate mortar and load the electrode for spectrum recording. 4.4.2 Preparation of direct spectrum sample
Mix the sample (4.2.2) calcined at 850℃ for 1h with an equal amount of graphite powder (2.9), grind and load the electrode for spectrum recording. 4.5 Spectral measurement
4.5.1 Preparation of standard sample
Calcinate the oxidized sodium (2.1) and each impurity oxide (2.2~2.6) at 850℃ for 1h. According to the calculated amount, each impurity oxide is added to the oxidized sodium hydroxide to prepare a 1% main standard sample, which is then diluted one by one with europium oxide and mixed with an equal amount of graphite powder to prepare a set of standard samples. The content is shown in Table 2. 4.5.2 Spectral measurement conditions
Spectrometer: band range 400.0~~440.0nm, three-lens illumination system, slit width 14μm, center light bar height 5.0mmTable 2
Impurities Chloride content
Gross standard sample
Standard sample No.
Standard sample No.
Standard sample No. 4
Standard sample No. 5
Standard sample No. 6
Light source: voltage 220V, current 14A, DC arc anode excitation. Sm,o
Electrode: Lower electrode Φ3×3×0.5mm, cup-shaped, see Figure 3; upper electrode is flat cone, cross section Φ2mm. Dy.o,
Oxygen-argon ratio: 1:4, total flow 5L/min. Exposure time: 80s.
GB 8762.7-88
Figure 3 Cup-shaped electrode
Darkroom treatment: Developer A+B formula, diluted with equal amount of water, developed at 20±1℃ for 2.5min, fixed, washed and dried. Blackness measurement: S scale, slit width 200um. Analysis line pairs and linear range are shown in Table 3.
Analysis line
Ce 408.323
Pr422.298
Sm 428. 078
Gd409.891
Dy 418.681
5 Calculation of analysis results
5.1 Direct spectroscopy method
Internal standard line
Eu 409.682
Eu 422.729
Eu 427.764
Eu 409.682
Eu 418.319
Draw the working curve according to igR～1gC and calculate the analysis results. 5.2 Chemical spectroscopy method
Calculate the percentage of each impurity oxide according to the following formula: a(%)
Wherein: mi -
the percentage of each impurity oxide found from the working curve; m. Enrichment sample volume,;
Sample volume, name.
Allowable difference
The difference in analysis results between laboratories should not be greater than the allowable difference listed in Table 4. 30
Linear range
Ce0, 0. 003 0~~0. 120 0
Pr,0.: 0. 003 0~~0. 120 0
Sm,0.0.001 0~0.060 0
Gd,0, 0. 001 0~ 0. 060 0
Dy,0, 0. 001 0~0. 060 0
Oxide
Additional remarks:
GB8762.7--88
Measurement range
0. 000 08 ~ 0. 000 15
>0.00015~0.000 30
>0.00030~0.00080
>0. 000 8 ~ 0. 001 5
0.0002~0.0010
>0. 001 0 ~ 0. 003 0
>0. 003 0 ~ 0. 005 0
>0.005 0~0.008 0
This standard was drafted by Beijing General Research Institute of Nonferrous Metals and Shanghai Yuelong Chemical Plant. This standard was drafted by Beijing General Research Institute of Nonferrous Metals. The main drafters of this standard are Wang Zhenying, Wang Changqing, Wu Xing and Mu Zongxu. Allowable difference
0. 000 10
Tip: This standard content only shows part of the intercepted content of the complete standard. If you need the complete standard, please go to the top to download the complete standard document for free.