GOST 23862.2-79
GOST 23862.2−79 Rare-earth metals and their oxides. Direct spectral method of determination of impurities of oxides of rare earth elements (with Amendments No. 1, 2)
GOST 23862.2−79
Group B59
INTERSTATE STANDARD
RARE EARTH METALS AND THEIR OXIDES
Direct spectral method of determination of impurities of oxides of rare earth elements
Rare-earth metals and their oxides. Direct spectral method of determination of impurities in oxides of rare-earth elements
ISS 77.120.99
AXTU 1709
Date of introduction 1981−01−01
The decision of the State Committee USSR on standards on October 19, 1979 N 3988 date of introduction is established 01.01.81
Limitation of actions taken by Protocol No. 7−95 Interstate Council for standardization, Metrology and certification (ICS 11−95)
EDITION with Amendments No. 1, 2 approved in April 1985, may 1990 (IUS 7−85, 8−90).
This standard establishes the direct spectral method of determination of impurities of rare earth elements (Rees) in rare-earth metals (previously translated into oxide) and their oxides.
The method is based on excitation and photographic registration of arc emission spectra of samples and sample comparison.
Mass fraction of rare earth impurities find live streaming chart for the calibration by comparison of relative intensities in the spectra of samples and sample comparison.
The interval defined by the mass fraction of impurities of oxides:
| the oxide of lanthanum: | |
| cerium |
from 1·10 |
| praseodymium |
from 5·10 |
| neodymium |
from 1·10 |
| Samaria |
from 1·10 |
| europium |
from 5·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| dysprosium |
from 5·10 |
| holmium |
from 1·10 |
| erbium |
from 5·10 |
| thulium |
from 1·10 |
| ytterbium |
from 1·10 |
| Lutetia |
from 3·10 |
| yttrium |
from 1·10 |
| the oxides of praseodymium: | |
| Lantana |
from 1·10 |
| cerium |
from 5·10 |
| neodymium |
from 5·10 |
| Samaria |
from 3·10 |
| europium |
from 1·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| dysprosium |
from 3·10 |
| holmium |
from 3·10 |
| erbium |
from 1·10 |
| thulium |
from 5·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 1·10 |
| yttrium |
from 5·10 |
| the oxide of samarium: | |
| terbium |
from 5·10 |
| dysprosium |
from 3·10 |
| holmium |
from 3·10 |
| erbium |
from 5·10 |
| thulium |
from 5·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 1·10 |
| yttrium |
from 1·10 |
| the oxide of gadolinium: | |
| Lantana |
from 5·10 |
| cerium |
from 1·10 |
| praseodymium |
from 3·10 |
| neodymium |
from 1·10 |
| Samaria |
from 3·10 |
| europium |
from 1·10 |
| terbium |
from 5·10 |
| dysprosium |
from 3·10 |
| holmium |
from 3·10 |
| erbium |
from 3·10 |
| thulium |
from 1·10 |
| ytterbium |
from 1·10 |
| Lutetia |
from 5·10 |
| yttrium |
from 3·10 |
| the oxide of neodymium: | |
| europium |
from 5·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| dysprosium |
from 1·10 |
| holmium |
from 3·10 |
| erbium |
from 5·10 |
| thulium |
from 1·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 3·10 |
| yttrium |
from 5·10 |
| in oxide europium: | |
| Lantana |
from 1·10 |
| cerium |
from 1·10 |
| praseodymium |
from 1·10 |
| neodymium |
from 1·10 |
| Samaria |
from 1·10 |
| gadolinium |
from 1·10 |
| terbium |
from 1·10 |
| dysprosium | from 1·10 |
| holmium | from 5·10 |
| erbium | from 1·10 |
| thulium |
from 5·10 |
| ytterbium | from 5·10 |
| Lutetia | from 1·10 |
| yttrium | from 5·10 |
| in oxide of terbium: | |
| Lantana |
from 3·10 |
| cerium |
from 5·10 |
| praseodymium |
from 3·10 |
| neodymium |
from 3·10 |
| Samaria | from 3·10 |
| europium |
from 3·10 |
| gadolinium |
from 1·10 |
| dysprosium |
from 1·10 |
| holmium |
from 3·10 |
| erbium |
from 1·10 |
| thulium |
from 1·10 |
| ytterbium |
from 1·10 |
| Lutetia |
from 3·10 |
| yttrium |
from 1·10 |
| the oxides of dysprosium: | |
| Lantana |
from 1·10 |
| cerium |
from 5·10 |
| praseodymium |
from 5·10 |
| neodymium |
from 5·10 |
| Samaria |
from 3·10 |
| europium |
from 1·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| holmium |
from 1·10 |
| erbium |
from 5·10 |
| thulium |
from 5·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 1·10 |
| yttrium |
from 5·10 |
| the oxide of erbium: | |
| Lantana |
from 5·10 |
| cerium |
from 3·10 |
| praseodymium |
from 3·10 |
| neodymium | from 3·10 |
| Samaria |
from 3·10 |
| europium |
from 3·10 |
| gadolinium |
from 1·10 |
| terbium |
from 3·10 |
| dysprosium |
from 1·10 |
| holmium |
from 1·10 |
| thulium |
from 5·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 5·10 |
| yttrium |
from 5·10 |
| in the oxide of ytterbium: | |
| Lantana |
from 1·10 |
| cerium |
from 3·10 |
| praseodymium |
from 3·10 |
| neodymium | from 1·10 |
| Samaria |
from 5·10 |
| europium |
from 5·10 |
| gadolinium | from 1·10 |
| terbium |
from 3·10 |
| dysprosium | from 1·10 |
| holmium | from 1·10 |
| erbium |
from 5·10 |
| thulium |
from 5·10 |
| Lutetia |
from 5·10 |
| yttrium |
from 5·10 |
| in the oxide of holmium: | |
| Lantana | from 3·10 |
| cerium |
from 3·10 |
| praseodymium |
from 3·10 |
| neodymium |
from 3·10 |
| Samaria |
from 3·10 |
| europium |
from 1·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| dysprosium |
from 1·10 |
| erbium |
from 1·10 |
| thulium |
from 3·10 |
| ytterbium |
from 5·10 |
| Lutetia |
from 3·10 |
| yttrium |
from 1·10 |
| in oxide of thulium: | |
| Lantana |
from 1·10 |
| cerium |
from 3·10 |
| praseodymium |
from 3·10 |
| neodymium |
from 3·10 |
| Samaria |
from 3·10 |
| europium |
from 1·10 |
| gadolinium |
from 1·10 |
| terbium |
from 3·10 |
| dysprosium |
from 1·10 |
| holmium |
from 1·10 |
| erbium |
from 1·10 |
| ytterbium |
from 1·10 |
| Lutetia |
from 1·10 |
| yttrium |
from 1·10 |
| the oxides of lutetium: | |
| Lantana |
from 5·10 |
| cerium |
from 5·10 |
| praseodymium |
from 5·10 |
| neodymium |
from 5·10 |
| Samaria |
from 1·10 |
| europium |
from 5·10 |
| gadolinium |
from 3·10 |
| terbium |
from 5·10 |
| dysprosium |
from 3·10 |
| holmium |
from 1·10 |
| erbium |
from 1·10 |
| thulium |
from 1·10 |
| ytterbium |
from 1·10 |
| yttrium |
from 1·10 |
| the oxides of yttrium: | |
| Lantana |
from 5·10 |
| cerium |
from 1·10 |
| praseodymium |
from 1·10 |
| neodymium |
from 5·10 |
| Samaria |
from 5·10 |
| europium |
from 5·10 |
| gadolinium |
from 5·10 |
| terbium |
from 1·10 |
| dysprosium |
from 5·10 |
| holmium |
from 5·10 |
| erbium |
from 5·10 |
| thulium |
from 5·10 |
| ytterbium |
from 5·10 |
| Lutetia | from 5·10 |
(Changed edition, Rev. N 1, 2).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 23862.0−79.
2. APPARATUS, MATERIALS AND REAGENTS
The diffraction spectrograph DFS-13 with a grating 1200 gr/mm or 2400 lines/mm, operating in first order of reflection from being a lighting system or similar.
The arc generator type DG-2 with optional rheostat or similar, adapted to ignite the arc AC or DC high-frequency discharge.
Rectifier 250−300, 30−50 A.
Microphotometer geregistreerde type MF-2 or similar.
Spectromancer of PS-18 or similar.
Analytical scale type ADV-200 or similar.
Libra torsion type VT-500 or similar.
Box of organic glass.
The mortar and pestle of jade.
Muffle furnace with thermostatic control, providing the temperature to 950 °C.
The machine tool for sharpening of electrodes.
Coals spectral high purity-7−3, with a diameter of 6 mm.
The electrodes are machined from high purity coals spectral-7−3 with a diameter of 6 mm the following types:
electrodes with a crater depth of 1.5 mm and a diameter of 2.4 mm, a wall thickness of 1 mm (I); with a crater depth of 3 mm, 4 mm in diameter (II);
electrodes of the type «glass» with a wall thickness of 1 mm, a height of the outer wall is 4 mm, the height of the «legs» 2 mm thick «legs» of 2 mm, diameter 4 mm:
a crater depth of 2 mm (III);
a crater depth of 3 mm (IV);
electrodes with the height of the sharpened part 10 mm and the crater: a depth of 2 mm, diameter 2 mm, wall thickness 1 mm (V); depth 3 mm, diameter 2 mm, wall thickness 1 mm (VI); depth 3 mm, diameter 2 mm, wall thickness 0.7−0.8 mm (VII); depth 4 mm, diameter 1.5 mm, wall thickness 0.7−0.8 mm (VIII); depth 4 mm, diameter 2 mm (IX);
electrodes, sharpened to a truncated cone with ground diameter of 1 mm (X).
Graphite powder of high purity according to GOST 23463−79.
Crucibles porcelain.
The chemical glasses with a capacity of 1000 cm.
Pipettes with a capacity of 1, 2, 5, 10 cm.
Volumetric flasks with a capacity of 100 cm.
Spectrographic plates type S, type I, type II, or similar, size 9x12 or 9х24 for normal blackening of analytical lines in the spectrum.
Oxides of rare earth elements: lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium — clean-defined impurities and a purity of at least 99.9% for the preparation of standard solutions.
The technical rectified ethyl alcohol GOST 18300−87.
Tracing paper according to GOST 982−80.
Medical compress according to NTD or hygroscopic GOST 5556−81.
Oxalic acid according to GOST 22180−76, H. C., and saturated solution with a concentration of 1 g/DM.
Hydrochloric acid by the GOST 3118−77, H. h., diluted 1:1 and 1% solutions.
Nitric acid GOST 4461−77, H. h., diluted 1:1 and 1% solutions.
Hydrogen peroxide according to GOST 10929−76.
Ammonia water according to GOST 3760−79.
The cesium chloride.
Sodium chloride OS.h. 6−4 GOST 4233−77.
Buffer a mixture of 1 — graphite powder containing 6% sodium chloride: 6 g sodium chloride was mixed with 94 g of powder graphite in a mortar made of organic glass, was stirred for 3 h. alcohol is added, maintaining the mass in a pasty condition. The mixture is dried in a drying Cabinet at a temperature of 100−105 °C for 4 h.
Buffer a mixture of powdered graphite containing 5% cesium chloride: 5 g of cesium chloride was mixed with 95 g of graphite powder in a mortar made of organic glass, was stirred for 3 h. alcohol is added, maintaining the mass in a pasty condition. The mixture is dried in a drying Cabinet at a temperature of 100−105 °C for 4 h.
Standard solutions of lanthanum, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium containing 10 mg/cmof one of REE in the calculation of the oxide.
Each solution is prepared separately, 1 g of the appropriate oxide of re is placed in a beaker with a capacity of 100 cm, add 10 cm
of hydrochloric acid diluted 1:1, was heated until complete dissolution of oxides: solution was cooled, transferred to a volumetric flask with a capacity of 100 cm
and the volume was adjusted to the mark with water.
A standard solution of cerium containing 10 mg/cm, based on the cerium dioxide, 1 g of cerium dioxide is placed in a beaker with a capacity of 100 cm
, add 10 cm
of nitric acid, diluted 1:1, 10 cm
of hydrogen peroxide and heated to complete dissolution of the oxide; the solution was then cooled, transferred to a volumetric flask with a capacity of 100 cm
and the volume was adjusted to the mark with water.
Working solutions for the preparation of the samples for each of the REE oxides are prepared by successive dilution of the corresponding mixtures of standard solutions determined by the REE.
Working solutions containing 1 mg/cmof each of the identified elements in the calculation of its oxide: in a volumetric flask with a capacity of 100 cm
placed at 10 cm
standard solutions of the respective rare earth elements shown in table.1, and the volume was adjusted to the mark with 1% solution of hydrochloric acid.
Working solutions B containing 0.1 mg/cmof each of the identified elements in the calculation of its oxide, is prepared by appropriate dilution of the solution to 10 times: 10 cm
solution And placed in a volumetric flask with a capacity of 100 cm
and the volume was adjusted to the mark with 1% solution of hydrochloric acid. The compositions of the working solutions are given in table.1.
Table 1
| The composition of the working solution | ||
| The number of working solution | Name |
Mass concentration of each element in the calculation of its oxide, mg/cm |
| 1A | Cerium, praseodymium, neodymium, samarium, europium | 1 |
| 1B |
0,1 | |
| 2A |
Gadolinium, terbium, dysprosium |
1 |
| 2B |
0,1 | |
| 3A |
Lanthanum, praseodymium, neodymium |
1 |
| 3B |
0,1 | |
| 4A |
Samarium, europium, gadolinium, terbium, dysprosium | 1 |
| 4B |
0,1 | |
| 5A |
Holmium, erbium, thulium, ytterbium, lutetium, yttrium | 1 |
| 5B |
0,1 | |
| 6A | Samarium, terbium, dysprosium, holmium, erbium | 1 |
| 6B |
0,1 | |
| 7A | Europium, gadolinium, thulium, ytterbium, lutetium, yttrium | 1 |
| 7B |
0,1 | |
| 8A |
Europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium | 1 |
| 8B |
0,1 | |
| 9A | Terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium | 1 |
| 9B |
0,1 | |
| 10A | Lanthanum, cerium, praseodymium, terbium |
1 |
| 10B |
0,1 | |
| 11A | Neodymium, samarium, gadolinium | 1 |
| 11B |
0,1 | |
| 12A | Dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium | 1 |
| 12B |
0,1 | |
| 13A | Lanthanum, cerium, praseodymium, neodymium, europium | 1 |
| 13B |
0,1 | |
| 14A |
Samarium, terbium, yttrium | 1 |
| 14B | 0,1 | |
| 15A | Samarium, terbium, dysprosium, yttrium |
1 |
| 15B | 0,1 | |
| 16A |
Dysprosium, holmium, erbium, thulium, ytterbium, lutetium | 1 |
| 16B | 0,1 | |
| 17A |
Lanthanum, cerium, praseodymium, neodymium, samarium, europium, dysprosium | 1 |
| 17B |
0,1 | |
| 18A |
Gadolinium, holmium, erbium, thulium, ytterbium, lutetium, yttrium | 1 |
| 18B |
0,1 | |
| 19A | Lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium | 1 |
| 19B |
0,1 | |
| 20A |
Lanthanum, cerium, praseodymium, neodymium, samarium, europium | 1 |
| 20B |
0,1 | |
| 21A |
Gadolinium, terbium, thulium, ytterbium, lutetium |
1 |
| 21B |
0,1 | |
| 22A |
Dysprosium, erbium, yttrium | 1 |
| 22B |
0,1 | |
| 22V |
0,01 | |
| 23A |
Gadolinium, terbium, dysprosium, holmium, thulium, ytterbium, lutetium, yttrium | 1 |
| 23B | 0,1 | |
| 24A | Gadolinium, terbium, dysprosium, holmium, erbium, ytterbium, lutetium, yttrium | 1 |
| 24B |
0,1 | |
| 25A | Gadolinium, terbium, dysprosium, holmium, erbium, thulium, lutetium, yttrium | 1 |
| 25B |
0,1 | |
| 26A | Gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium | 1 |
| 26B |
0,1 | |
| 27A |
Gadolinium, terbium, dysprosium, holmium, erbium, ytterbium, thulium, yttrium | 1 |
| 27B | 0,1 | |
| 28A |
Lantan |
1 |
| 28B |
Cerium and neodymium |
0,1 |
(Changed edition, Rev. N 1, 2).
3. PREPARATION FOR ASSAY
3.1. Sample preparation comparison
The reference sample (OS) prepared before photographing spectra with mixing samples for REE oxide powder graphite in a ratio of 1:1.
In the determination of the oxides of lanthanum, cerium and neodymium in an oxide of praseodymium OS is prepared by mixing samples of praseodymium oxide powder with graphite in the ratio 2:1.
(Changed edition, Rev. N 1).
3.2. Preparation of samples on the oxides of the REE
10 g of an oxide of re, clean at the designated impurities was placed in a beaker with a capacity of 1000 cm, add 100 cm
of hydrochloric acid diluted 1:1, and heated to complete dissolution.
A sample of cerium dioxide, pure at the designated impurities, weighing 10 g were placed in a glass with a capacity of 1000 cm, moisten with water, add 60−70 cm
of nitric acid, diluted 1:1, 20 cm
of hydrogen peroxide and heated to complete dissolution.
The solutions are evaporated to wet salts, dissolved in 100 cmof distilled water in each of the resulting solutions enter working solutions A or B in amounts given in table.2−33.
After mixing the solutions, add water to a volume of 500−600 cmand the ammonia to pH 1.5−2. The solutions were heated to boiling, add 150 cm
of hot saturated solution of oxalic acid. Solution and the precipitate was kept for 24 h. the Precipitate was filtered through a filter with a blue ribbon, washed with 20 cm
of a 0.1% strength solution of oxalic acid, placed in a porcelain crucible, dried on a hotplate and calcined in a muffle furnace at 900 °C to constant weight. Calcined oxide is stored in a desiccator in packages of tracing paper.
Composition, mass fraction and number of added working solutions determined REE are given in table.2−33.
Allowed preparation of samples comparison by mixing the oxides defined by the REE with the corresponding base (oxide REE) or according to GOST 23862.1−79, while maintaining the values of the mass fractions of the determined elements are listed in the table.2−33.
Samples for oxides of lanthanum (OOL)
Table 2
| Marking sample |
Mass fraction of oxides of cerium, praseodymium, neodymium, samarium, europium in OOL, % | The number of added working solutions, see | |
| 1A |
1B | ||
| OOL 1 |
1·10 |
10 |
- |
| OOL 2 |
5·10 |
5 |
- |
| OOL 3 |
3·10 |
3 |
- |
| OOL 4 |
1·10 |
- |
10 |
| OOL 5 |
5·10 |
- |
5 |
| OOL 6 |
2·10 |
- |
2 |
| OOL 7 |
1·10 |
- |
1 |
Table 3
| Marking sample |
Mass fraction of oxides of gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium in OOL, % | The number of added working solutions, see | ||||
| 2A |
2B |
5A |
5B |
22V | ||
| OOL 8 |
1·10 |
10 |
- |
10 |
- |
- |
| OOL 9 |
5·10 |
5 |
- | 5 |
- |
- |
| OOL 10 |
3·10 |
3 |
- |
3 |
- |
- |
| OOL 11 |
1·10 |
- |
10 | - |
10 |
- |
| OOL 12 |
5·10 |
- |
5 |
- |
5 |
- |
| OOL 13 |
3·10 |
- |
3 |
- |
3 |
- |
| OOL 14 |
1·10 |
- |
1 |
- |
1 |
- |
| OOL 15 |
5·10 |
- |
- | - |
- |
5 |
Samples of cerium dioxide (OOC)
Table 4
| Marking sample | Mass fraction of oxides of lanthanum, praseodymium, neodymium in oots, % | The number of added working solutions, see | |
| 3A |
3B | ||
| OOC 1 |
1·10 |
10 |
- |
| OOC 2 |
5·10 |
5 |
- |
| OOC 3 |
3·10 |
3 |
- |
| Oots 4 |
1·10 |
- |
10 |
| OOC 5 |
5·10 |
- |
5 |
Table 5
| Marking sample |
Mass fraction of oxides of samarium, europium, gadolinium, dysprosium, terbium, holmium, erbium, thulium, ytterbium, lutetium, yttrium in oots, % | The number of added working solutions, see | |||
| 4A |
4B |
5A |
5B | ||
| Oots 6 |
1·10 |
10 |
- |
10 |
- |
| Oots 7 |
5·10 |
5 |
- |
5 |
- |
| Oots 8 |
3·10 |
3 |
- |
3 |
- |
| Oots 9 |
1·10 |
- |
10 |
- |
10 |
| The oots 10 |
5·10 |
- |
5 |
- |
5 |
Samples of oxides of praseodymium (OOP)
Table 6
| Refer to the value of the sample |
Mass fraction of oxides of samarium, terbium, dysprosium, holmium, erbium in OOP, % | The number of added working solutions, see | |
| 6A |
6B | ||
| OOP 1 |
2·10 |
20 |
- |
| PLO 2 |
1·10 |
10 |
- |
| PLO 3 |
5·10 |
5 |
- |
| PLO 4 |
3·10 |
3 |
- |
| PLO 5 |
1·10 |
- |
10 |
Table 6A
| Marking sample | Mass fraction of oxides of lanthanum, cerium, neodymium CPS % | The number of added working solutions, see | |
| 28A |
28B | ||
| The PLO 1A |
2·10 |
20 |
- |
| PLO 2A |
1·10 |
10 |
- |
| PLO 3A |
5·10 |
5 |
- |
| PLO 4A | 3·10 |
3 |
- |
| PLO 5A |
1·10 |
- |
10 |
Table 7
| Marking sample |
Mass fraction of oxides of europium, gadolinium, thulium, ytterbium, lutetium, yttrium CPS % | The number of added working solutions, see | |
| 7A |
7B | ||
| PLO 6 |
1·10 |
10 |
- |
| PLO 7 |
5·10 |
5 |
- |
| PLO 8 |
3·10 |
3 |
- |
| PLO 9 |
1·10 |
- |
10 |
| PLO 10 |
5·10 |
- |
5 |
Samples of the oxides of neodymium (UN)
Table 8
| Marking sample |
Mass fraction of oxides of europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, yttrium in UN, % | The number of added working solutions, see | |
| 8A |
8B | ||
| UN 1 |
2·10 |
20 |
- |
| UN 2 |
1·10 |
10 | - |
| UN 3 |
5·10 |
5 |
- |
| UN 4 |
3·10 |
3 |
- |
| UN 5 |
1·10 |
- |
10 |
| UN 6 |
5·10 |
- |
5 |
Samples of samarium oxide (OOS)
