This standard is applicable to the simultaneous determination of lanthanum oxide, cerium oxide, praseodymium oxide, neodymium oxide, samarium oxide, europium oxide, gadolinium oxide, terbium oxide, dysprosium oxide, holmium oxide, erbium oxide, thulium oxide, ytterbium oxide and lutetium oxide in fluorescent grade yttrium oxide. GB/T 8762.5-1988 Determination of trace rare earth oxides in fluorescent grade yttrium oxide by chemical spectroscopy and direct spectroscopy GB/T8762.5-1988 Standard download decompression password: www.bzxz.net

National Standard of the People's Republic of China
Determination of tracerare earth oxide contents in fluorescent yttrium oxide
Spectrochemical method and direct spectrographic method UDC 661. 866
GB 8762. 5 -- 88
This standard is applicable to the simultaneous determination of lanthanum oxide, antimony oxide, vanadium oxide, neodymium oxide, vanadium oxide, europium oxide, yttrium oxide, cadmium oxide, ferric oxide, molybdenum oxide, molybdenum oxide, quartz oxide and molybdenum oxide in fluorescent yttrium oxide. The determination range is shown in Table 1. Table 1
Chemical spectroscopy
Direct spectroscopy
Method summary
Oxide
Determination range
0. 000 05-~0. 010 0
0. 000 2 ~ 0. 010 0
0. 000 05 ~ 0. 010 0
0. 000 05 ~0. 010 0
0. 000 05 ~- 0. 005 0
0.000 05-~0.010 0
0. 000 05-~0. 010 0
0. 000 05-~0. 010 0
0. 000 30~0. 010 0
0. 000 30~0. 010 0
0. 000 30 ~ 0. 010 0
0. 000 10 ~ 0. 003 0
0. 001 0 ~~ 0. 010 0
Chemical spectroscopy: The sample is dissolved in hydrochloric acid and separated and enriched with impurity elements such as lanthanum, cerium, zirconium, neodymium, vanadium, platinum, vanadium, dysprosium and part of yttrium by P507 leaching resin column. It is precipitated with oxalic acid and burned into oxides. With graphite powder as buffer, it is excited by DC arc in argon oxygen atmosphere and the spectrum is measured.
Direct spectroscopy: The original sample is excited by a DC arc in an argon oxygen atmosphere with graphite powder as a buffer, and the spectrum is measured. China Nonferrous Metals Industry Corporation approved it on February 4, 1988 and implemented it on February 1, 1989.
2 Reagents
Hydrochloric acid (p1.19) is of high purity.
2.2 Hydrochloric acid (1+1).
GB 8762.588
2.3 Hydrochloric acid (4mol/L.), prepared with hydrochloric acid (2.1), calibrated. 2.4 Hydrochloric acid (1+5).
Hydrochloric acid (1-+9).
2.6 Hydrochloric acid (0.66mol/L), prepared with hydrochloric acid (2.3). 2.7
Hydrochloric acid (0.1mo1/L), prepared with hydrochloric acid (2.3). 2.8
Ammonia water, high purity (p0.90).
Ammonia water (1+7).
1-Phenyl-3-methyl-4-phenylylpyrazolone-［5]benzene solution. PMBP benzene solution (1.5%): 1.5g PMBP is dissolved in 2.10
100mL benzene solution.
Ammonium acetate buffer solution (pH5.7): Weigh 77g ammonium acetate and dissolve it in water, add 8mL glacial acetic acid, and dilute to 500mL with water. Mixed sulfosalicylic acid solution (10%).
Dimethyl yellow indicator benzene solution (0.4%). Cresol red indicator ethanol solution (0.1%). Oxalic acid, high purity.
Pyrite powder, spectrally pure.
Developer and fixer, prepare according to the instructions for the photosensitive plate. Oxidation, 99.999%.
Lanthanum oxide, antimony oxide, zirconium oxide, neodymium oxide, vanadium oxide, europium oxide, vanadium oxide, cerium oxide, dysprosium oxide, sulphur oxide, ytterbium oxide, ytterbium oxide and ytterbium oxide, purity is greater than 99.9%. 3
Instruments, equipment and materials
Spectrograph: reciprocal linear dispersion 0.25nm/mm. Excitation light source: DC arc generator that can provide the required electrical parameters, current greater than 15A. 3.2
3.3 Super thermostat.
Chromatographic column: Φ20×900mm, with a sleeve and a No. 2 glass sand plate at the bottom. 3.41
3.52-Ethylhexylphosphine 2-ethylhexyl ester resin, (P507 resin): P507 content 55%; particle size: 100~150 moles; saturated capacity 0.006 mol/g dry resin; bulk density 0.47 g/mL. 3.6 Microphotometer.
3.7 Counter electrode: upper electrode ±6 mm conical electrode, top cross-sectional diameter Φ1 mm; lower electrode Φ3×3×0.5 mm, see Figure 1. 3.8 Stepped photosensitive plate.
3.9 Photosensitive plate: UV type IⅡ.
3.10 Graphite electrode cutting lathe.
3.11 Quartz cyclone chamber, see Figure 2.
3.12 Argon, (99%).
3.13 Oxygen (99%).
4 Analysis steps
4.1 Determination quantity
GB8762.5-88
Electrode diagram
Figure 2 Quartz cyclone chamber diagram
4.1.1 Chemical spectroscopy: Weigh 2 samples for measurement and take the average value. 4.1.2 Direct spectroscopy: Weigh 1 sample. 3
4.2 Sample quantity
GB8762.5—88
4.2.1 Chemical spectroscopy: Weigh 1.000g sample for each sample. 4.2.2 Direct spectroscopy: Weigh 0.100g sample for each sample. 4.3 Sample preparation
4.3.1 Chemical spectroscopy sample preparation
4.3.1.1 Preparation of chromatographic column
Weigh 130g P507 resin (3.5) and mix it into a slurry with hydrochloric acid (2.2). First add a certain amount of hydrochloric acid (2.2) to the chromatographic column, then pour the slurry resin into the column while releasing the hydrochloric acid solution in the chromatographic column. After the resin settles, cover it with foam plastic. Elute the resin with hydrochloric acid (2.?) until there is no trivalent iron ion in the effluent (check with ammonium thiocyanate). Then wash with water until the effluent is pH 1: Use 200)mL hydrochloric acid (2.7) to balance the chromatographic column and set aside. 4.3.1.2 Separation of impurity elements
Place the sample (4.2.1) burned at 850℃ for 1h in a 50mL beaker, add 10mL hydrochloric acid (2.2), cover with cover III, heat on a low temperature electric furnace to completely dissolve the sample, and evaporate to near dryness. Dissolve with 10mL water, the acidity of the solution should be pH2.5-3.0, add 40mL water, and stir with a stirring rod.
Connect the super thermostat (3.3) to make the water temperature in the chromatographic column jacket 50±1C. Put the solution in the chromatographic column until the two resins are flat, moisten with the sample solution, control the flow rate to 0.25mL/cmmin, and collect the effluent with a 250mL volumetric flask. Wash the beaker with a small amount of hydrochloric acid (2.6) and transfer the solution into the column. When the solution in the column flows to the resin surface, connect the hydrochloric acid (2.6) storage bottle for elution, set the flow rate to 1mLcm-min, and collect the impurity elements from lanthanum to part of 100 million in a 1400mL beaker. Note: The regeneration of the chromatographic column is to elute with 200mL of hydrochloric acid (2.2) and other heavy rare earth impurities. After washing, balance with 200ml of hydrochloric acid (2.7), and the chromatographic village can be used next time.
4.3.1.3 Enrichment of impurity elements
Take 500mL of the collected solution (4.3.1.2) in turn, add 2ml of sulfosalicylic acid solution (2.12) and 1 drop of dibasic yellow indicator benzene solution (2.13), adjust with ammonia water (2.8) or (2.9) until the solution just turns yellow, then add 1 drop of hydrochloric acid (2.4) to make the solution star red, add 50mL of ammonium acetate buffer solution (2.11), transfer to a 1L separatory funnel, extract with 100mL of PMBP benzene solution (2.10), oscillate for 3 to 5min, discard the aqueous phase after stratification, and keep the organic phase for the second extraction. The total collected solution (4.3.1.2) was extracted with benzene three times, the organic phase was washed with 20-30 mL of water, and then back-extracted with 50 mL of hydrochloric acid (2.5) twice, each time shaking for 2-3 min. The back-extracted solution was connected to a 250 mL beaker, 4 drops of cresol red indicator ethanol solution (2.14) were added, and the color was adjusted to orange with ammonia water (2.8) or (2.9), the solution was heated to near boiling, and 10 g of oxalic acid (2.15) Precipitate rare earth, place for 4 hours, filter, ash, burn at 850°C for 1 hour, and weigh after cooling. 4.3.1.4 Mix the enriched sample (4.3.1.3) with an equal amount of graphite powder (2.16), grind it in an agate mortar, and then load it into the electrode for spectrum recording.
4.3.2 Preparation of the first contact spectrum sample
Mix the sample (4.2.2) burned at 850°C for 1 hour with an equal amount of graphite powder (2.16), grind it evenly, and load it into the electrode for spectrum recording. 4.4 Preparation of standard series
Put the oxide matrix (2.18) and lanthanum oxide, cerium oxide, zirconium oxide, neodymium oxide, vanadium oxide, europium oxide, yttrium oxide, uranium oxide, dysprosium oxide, vanadium oxide, ytterbium oxide and oxide (2.19) with a purity greater than 99.9% in a muffle furnace and burn at 850C for 1 hour, take out, cool, and prepare a 0.1% main standard sample according to the calculated amount, and grind it in an agate mortar for 2 hours. Then dilute them one by one with yttrium oxide matrix (2.18) to prepare a series of standard samples of 0.03%, 0.01%, 0.003%, 0.001%, 0.0003% and 0.0001%. 4.5 See Table 2 for the spectral measurement conditions. The analysis line and internal standard line are shown in Table 3. 4.6 The enriched sample (4.3.1.4) and the original sample (4.3.2) are photographed on the same plate using the standard sample method. 4.7 The darkroom treatment of the photosensitive plate is carried out according to the instructions of the photosensitive plate. 4.8 Measure the blackness of the step photosensitive plate and draw the emulsion characteristic curve. 4.9 Use a microphotometer to measure the blackness S of the analysis line, background and internal standard line in turn, and calculate the IgR value of the analysis line pair. Draw the working curve with 1g?~gc.
Analysis
Determination of impurities
Spectrograph slit
Central wavelength
Ventilation device
Vapor flow ratio
Pre-combustion time
Sunrise time
Material and shape of counter electrode
Photosensitive plate model
GB8762.5--88
La,O,、CeO,、Pr.On.、Nd,O,、Sm.O,、Eu,O,、Gd,O,Tb,O,Dy,O.,Ho,OFr,O,,TmO.,Yb,O..Lu.o.0.0150.020
Direct current
15～18
Quartz cyclone gas chamber
Arto, A : 1
Graphite electrode, (3.7)
Ultraviolet type 1
Igt ~-IgeWww.bzxZ.net
5 Calculation of analysis results
5.1 Direct spectrum calculation
GB 8762.5--88
Analysis line
According to the 1gR average value of the sample, the percentage content of the analyzed element is found on the working curve. 5.2 Calculation of chemical spectrum
5.2.1 Calculation of enrichment multiple
Where: mo-
Sample amount, 8;
Amount of oxide after precipitation enrichment, g.
5.2.2 Calculation of enrichment element analysis results
z (%)
Wherein m2 -------
6 Allowable difference
Impurity mass found on the white working curve, (percentage content); enrichment multiple.
The difference in analysis results between laboratories shall not exceed the allowable difference listed in Table 4. 20 | | tt | 10 -3 ~1× 10-
2 × 10-*~ 1. 5 × 10 -3
>1. 5 × 10- ~3 × 10-#
>3×10-3～1×10-2
5×105~5×10,
>5×10- ~3×10-3
>3×10-1~1×10-1
5× 10-~5× 10-
≥ 5× 10-4~5× 10-1
>5×10-~1×10
5 × 10 -s ~ 3 × 10 -
>3×10-4 ~3× 10 -3
> 3 × 10-1 ~1 × 10-1
5 10-
5×10-- ~3 ×10-*
≥ 3 × 10 -4 ~3 × 10-3
>3×10:1～1×10 2
5×10~5×10
>5×10-1~3×10-
>3×10- ~1 ×10-2
5×10-~3×10-
>3×10-1~3×10-
>3×10-1~~1×10-2
3×10 -+~~3×10-1
>3×10-1～1×10-2
3×10-~3×10-
>3×10-~1×10-
3 × 10-- ~3 × 10 -
>3×10-3~1× 10-
1 ×10-+ ~1 × 10-3
>/ × 10-3 ～~3× 10-
1 ×10-～1×10-2
This standard was drafted by Beijing General Research Institute of Nonferrous Metals and Shanghai Yuelong Chemical Plant. This standard was drafted by Shanghai Yuelong Chemical Plant. The main drafters of this standard are Lü Aizhu and Hu Renkun. Allowable difference
6×10-
2 ×10-
5×10 +
2.5×10-4
3 × 10-.
5×10-
6 × 10-
2×10--4
5×10-
1. 5 × 10 *
3 × 10-.
1×10-4
6×10-
2. 5 × 10
4×10-
5×10-
2 ×10-
5×104
2×10-
2×10-4
5×10~
2 × 10-
4×10*
5 × 10--9 Use a microphotometer to measure the blackness S of the analytical line, background and internal standard line in turn, and calculate the IgR value of the analytical line pair. Draw a working curve with 1g?~gc.
Analysis
Determination of impurities
Spectrograph slit
Central wavelength
Ventilation device
Vapor flow ratio
Pre-combustion time
Sunrise time
Material and shape of counter electrode
Photosensitive plate model
GB8762.5--88
La,O,、CeO,、Pr.On.、Nd,O,、Sm.O,、Eu,O,、Gd,O,Tb,O,Dy,O.,Ho,OFr,O,,TmO.,Yb,O..Lu.o.0.0150.020
Direct current
15～18
Quartz cyclone gas chamber
Arto, A : 1
Graphite electrode, (3.7)
Ultraviolet type 1
Igt ~-Ige
5 Calculation of analysis results
5.1 Direct spectrum calculation
GB 8762.5--88
Analysis line
According to the 1gR average value of the sample, the percentage content of the analyzed element is found on the working curve. 5.2 Calculation of chemical spectrum
5.2.1 Calculation of enrichment multiple
Where: mo-
Sample amount, 8;
Amount of oxide after precipitation enrichment, g.
5.2.2 Calculation of enrichment element analysis results
z (%)
Wherein m2 -------
6 Allowable difference
The amount of impurities found on the white working curve, (percentage content); enrichment multiple.
The difference in analysis results between laboratories shall not be greater than the allowable difference listed in Table 4. 20 | | tt | 10 -3 ~1× 10-
2 × 10-*~ 1. 5 × 10 -3
>1. 5 × 10- ~3 × 10-#
>3×10-3～1×10-2
5×105~5×10,
>5×10- ~3×10-3
>3×10-1~1×10-1
5× 10-~5× 10-
≥ 5× 10-4~5× 10-1
>5×10-~1×10
5 × 10 -s ~ 3 × 10 -
>3×10-4 ~3× 10 -3
> 3 × 10-1 ~1 × 10-1
5 10-
5×10-- ~3 ×10-*
≥ 3 × 10 -4 ~3 × 10-3
>3×10:1～1×10 2
5×10~5×10
>5×10-1~3×10-
>3×10- ~1 ×10-2
5×10-~3×10-
>3×10-1~3×10-
>3×10-1~~1×10-2
3×10 -+~~3×10-1
>3×10-1～1×10-2
3×10-~3×10-
>3×10-~1×10-
3 × 10-- ~3 × 10 -
>3×10-3~1× 10-
1 ×10-+ ~1 × 10-3
>/ × 10-3 ～~3× 10-
1 ×10-～1×10-2
This standard was drafted by Beijing General Research Institute of Nonferrous Metals and Shanghai Yuelong Chemical Plant. This standard was drafted by Shanghai Yuelong Chemical Plant. The main drafters of this standard are Lü Aizhu and Hu Renkun. Allowable difference
6×10-
2 ×10-
5×10 +
2.5×10-4
3 × 10-.
5×10-
6 × 10-
2×10--4
5×10-
1. 5 × 10 *
3 × 10-.
1×10-4
6×10-
2. 5 × 10
4×10-
5×10-
2 ×10-
5×104
2×10-
2×10-4
5×10~
2 × 10-
4×10*
5 × 10--9 Use a microphotometer to measure the blackness S of the analytical line, background and internal standard line in turn, and calculate the IgR value of the analytical line pair. Draw a working curve with 1g?~gc.
Analysis
Determination of impurities
Spectrograph slit
Central wavelength
Ventilation device
Vapor flow ratio
Pre-combustion time
Sunrise time
Material and shape of counter electrode
Photosensitive plate model
GB8762.5--88
La,O,、CeO,、Pr.On.、Nd,O,、Sm.O,、Eu,O,、Gd,O,Tb,O,Dy,O.,Ho,OFr,O,,TmO.,Yb,O..Lu.o.0.0150.020
Direct current
15～18
Quartz cyclone gas chamber
Arto, A : 1
Graphite electrode, (3.7)
Ultraviolet type 1
Igt ~-Ige
5 Calculation of analysis results
5.1 Direct spectrum calculation
GB 8762.5--88
Analysis line
According to the 1gR average value of the sample, the percentage content of the analyzed element is found on the working curve. 5.2 Calculation of chemical spectrum
5.2.1 Calculation of enrichment multiple
Where: mo-
Sample amount, 8;
Amount of oxide after precipitation enrichment, g.
5.2.2 Calculation of enrichment element analysis results
z (%)
Wherein m2 -------
6 Allowable difference
The amount of impurities found on the white working curve, (percentage content); enrichment multiple.
The difference in analysis results between laboratories shall not be greater than the allowable difference listed in Table 4. 20 | | tt | 10 -3 ~1× 10-
2 × 10-*~ 1. 5 × 10 -3
>1. 5 × 10- ~3 × 10-#
>3×10-3～1×10-2
5×105~5×10,
>5×10- ~3×10-3
>3×10-1~1×10-1
5× 10-~5× 10-
≥ 5× 10-4~5× 10-1
>5×10-~1×10
5 × 10 -s ~ 3 × 10 -
>3×10-4 ~3× 10 -3
> 3 × 10-1 ~1 × 10-1
5 10-
5×10-- ~3 ×10-*
≥ 3 × 10 -4 ~3 × 10-3
>3×10:1～1×10 2
5×10~5×10
>5×10-1~3×10-
>3×10- ~1 ×10-2
5×10-~3×10-
>3×10-1~3×10-
>3×10-1~~1×10-2
3×10 -+~~3×10-1
>3×10-1～1×10-2
3×10-~3×10-
>3×10-~1×10-
3 × 10-- ~3 × 10 -
>3×10-3~1× 10-
1 ×10-+ ~1 × 10-3
>/ × 10-3 ～~3× 10-
1 ×10-～1×10-2
This standard was drafted by Beijing General Research Institute of Nonferrous Metals and Shanghai Yuelong Chemical Plant. This standard was drafted by Shanghai Yuelong Chemical Plant. The main drafters of this standard are Lü Aizhu and Hu Renkun. Allowable difference
6×10-
2 ×10-
5×10 +
2.5×10-4
3 × 10-.
5×10-
6 × 10-
2×10--4
5×10-
1. 5 × 10 *
3 × 10-.
1×10-4
6×10-
2. 5 × 10
4×10-
5×10-
2 ×10-
5×104
2×10-
2×10-4
5×10~
2 × 10-
4×10*
5 × 10--5× 10- ~5× 10-
5×10-- ~3 ×10-*
≥ 3 × 10 -4 ~3 × 10-3
>3× 10:1～1×10 2
5×10~5×10
>5×10-1~3×10-
>3×10- ~1 ×10-2
5×10-~3×10-
>3×10-1~3×10-
>3×10-1～~1×10 -2
3×10 -+~~3×10-1
>3×10-1～1×10-2
3×10-~3×10-
>3×10- ~1×10-
3 × 10-- ~3 × 10 -
>3×10-3~1× 10-
1 ×10-+ ~1 × 10-3
>/ × 10 -3~~3× 10-
1 ×10-～1×10-2
This standard was drafted by Beijing Nonferrous Metals Research Institute and Shanghai Yuelong Chemical Plant. This standard was drafted by Shanghai Yuelong Chemical Plant. The main drafters of this standard are Lü Aizhu and Hu Renkun . Allowable difference
6×10-
2 ×10-
5×10 +
2.5×10-4
3 × 10-.
5×10-
6 × 10-
2×10--4
5×10-
1. 5 × 10 *
3 × 10-.
1× 10-4
6×10-
2. 5 × 10
4×10-
5×10-
2 ×10-
5×104
2×10-
2×10-4
5×10~
2 × 10-|| tt||4×10*
5 × 10--5× 10- ~5× 10-
5×10-- ~3 ×10-*
≥ 3 × 10 -4 ~3 × 10-3
>3× 10:1～1×10 2
5×10~5×10
>5×10-1~3×10-
>3×10- ~1 ×10-2
5×10-~3×10-
>3×10-1~3×10-
>3×10-1～~1×10 -2
3×10 -+~~3×10-1
>3×10-1～1×10-2
3×10-~3×10-
>3×10- ~1×10-
3 × 10-- ~3 × 10 -
>3×10-3~1× 10-
1 ×10-+ ~1 × 10-3
>/ × 10 -3~~3× 10-
1 ×10-～1×10-2
This standard was drafted by Beijing Nonferrous Metals Research Institute and Shanghai Yuelong Chemical Plant. This standard was drafted by Shanghai Yuelong Chemical Plant. The main drafters of this standard are Lü Aizhu and Hu Renkun . Allowable difference
6×10-
2 ×10-
5×10 +
2.5×10-4
3 × 10-.
5×10-
6 × 10-
2×10--4
5×10-
1. 5 × 10 *
3 × 10-.
1× 10-4
6×10-
2. 5 × 10
4×10-
5×10-
2 ×10-
5×104
2×10-
2×10-4
5×10~
2 × 10-|| tt||4×10*
5 × 10--
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