GOST 23862.8-79
GOST 23862.8−79 Lanthanum, cerium, ytterbium, lutecium, yttrium and their oxides. Chemical-spectral method of determination of impurities of oxides of rare earth elements (with Change No. 1)
GOST 23862.8−79
Group B59
INTERSTATE STANDARD
LANTHANUM, CERIUM, YTTERBIUM, LUTECIUM, YTTRIUM AND THEIR OXIDES
Chemical-spectral method of determination of impurities of oxides of rare earth elements
Lanthanum, cerium, ytterbium, lutecium, yttrium and their oxides. Chemical-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 Change No. 1, approved in April 1985 (IUS 7−85).
This standard specifies the chemical-spectral method of determination of impurities of oxides of rare earth elements lanthanum, the thermodynamic equilibrium, ytterbium, of Lutetia, yttria and their oxides.
The method is based on extraction-chromatographic preconcentration of rare earth impurities. The concentrate is analyzed by the spectral method at evaporation of a thin layer from the end of carbon electrode in an atmosphere of argon, oxygen, excitation and photographic registration of the emission spectrum of the arc with the subsequent determination of mass fractions of impurities in the calibration schedule.
Intervals determined by a mass fraction of impurities of oxides:
in the lanthanum and its oxides: | |
cerium |
2·10% 1·10% |
praseodymium |
2·10% 1·10% |
neodymium |
2·10% to 2·10% |
Samaria |
2·10% 1·10% |
europium |
2·10% 1·10% |
gadolinium |
4·10% to 5·10% |
terbium |
2·10% to 2·10% |
dysprosium |
4·10% to 5·10% |
holmium |
4·10% 1·10% |
erbium |
4·10% to 5·10% |
thulium |
2·10% to 5·10% |
ytterbium |
2·10% 1·10% |
Lutetia |
4·10% to 2·10% |
in the thermodynamic equilibrium and its dioxide: | |
Lantana |
from 1·10to 2%·10% |
praseodymium |
from 1·10% to 5·10% |
neodymium |
from 1·10% to 5·10% |
Samaria |
from 1·10% to 5·10% |
europium |
from 1·10to 2%·10% |
gadolinium |
2·10% to 2·10% |
terbium |
from 1·10% to 5·10% |
dysprosium |
2·10% 1·10% |
holmium |
2·10% to 5·10% |
thulium |
from 1·10% to 5·10% |
ytterbium |
from 1·10to 2%·10% |
Lutetia |
2·10% 1·10% |
in ytterbium and its oxide: | |
Lantana |
4·10% to 5·10% |
cerium |
4·10% to 2·10% |
praseodymium |
4·10% to 2·10% |
neodymium |
4·10% to 5·10% |
Samaria |
4·10% 1·10% |
europium |
4·10% 1·10% |
gadolinium |
from 1·10% to 5·10% |
terbium |
4·10% to 2·10% |
dysprosium |
from 1·10to 2%·10% |
holmium |
from 1·10% 1·10% |
erbium |
from 1·10to 2%·10% |
thulium |
4·10% 1·10% |
in yttria and its oxide: | |
Lantana |
from 1·10% to 5·10% |
cerium |
from 1·10% 1·10% |
praseodymium |
from 1·10% 1·10% |
neodymium |
from 1·10% to 5·10% |
Samaria |
from 1·10% 1·10% |
europium |
from 1·10% 1·10% |
gadolinium |
4·10% to 2·10% |
terbium | 2·10% 1·10% |
dysprosium |
4·10% to 2·10% |
holmium |
4·10% to 2·10% |
erbium |
4·10% to 2·10% |
thulium |
2·10% 1·10% |
ytterbium |
2·10% 1·10% |
Lutetia |
4·10% to 2·10% |
the oxides of lutetium: | |
Lantana |
4·10% to 5·10% |
cerium |
4·10% 1·10% |
praseodymium |
4·10% 1·10% |
neodymium |
4·10% to 5·10% |
Samaria |
4·10% to 2·10% |
europium |
4·10% to 5·10% |
gadolinium |
from 1·10to 2%·10% |
terbium |
4·10% to 5·10% |
dysprosium |
from 1·10to 2%·10% |
holmium |
from 1·10to 2%·10% |
erbium |
from 1·10% 1·10% |
thulium |
4·10% to 2·10% |
ytterbium | 4·10% 1·10% |
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 23862.0−79.
2. APPARATUS, MATERIALS AND REAGENTS
Column chromatography of molybdenum glass with a height of 600−800 mm of two types: column water jacket for columns without a water jacket (see the devil.1) 23862.7 GOST-79.
Quartz column inner diameter 15 mm, height 35 mm.
Evaporators made of molybdenum glass (see the devil.2, GOST 23862.7−79).
The thermostat TS-16 or similar, which provides hot water to (40±2) °C.
Potentiometer LPU-01, or similar, for measuring pH in the range from 1 to 11.
Ball mill metal with a diameter of 210 mm, height 200 mm, weight 4 kg.
Metal balls with a diameter of 30 mm, 25 PCs.
Sieves of metal.
Drying oven with thermostat providing temperatures up to 200 °C.
Muffle furnace with thermostatic control, providing temperature up to 1000 °C.
Motor sewing DSS-2.
The diffraction spectrograph DFS-13 with a grating 1200 lines/mm operating in the first order reflection and single-lens lighting system or similar.
The arc generator type DG-2 with optional rheostat or similar, suitable for ignition of the arc DC high-frequency discharge.
Rectifier 250−300, 30−50 A.
Microphotometer geregistreerde type MF-2 or similar.
Spectromancer PS-18 or similar.
Analytical scale.
Libra torsion type VT-500 or similar.
The machine tool for sharpening of electrodes.
Tile electric.
Water jet pump laboratory glass according to GOST 25336−82.
Camera of quartz, consisting of a cylinder with a height of 42 mm, 50 mm in diameter, made of optical quartz and two round plates with a diameter of 70 mm made of technical quartz, which are enshrined in the tripod of the instrument. Quartz cylinder lies freely on the bottom plate, the upper plate is lowered onto the cylinder. In each of the plates has an outlet pipe for gas supply and the opening for the electrodes.
The flowmeters type RS-3.
Reducers oxygen.
Pressure gauges according to GOST 2405−88 1−4 kgf/cm.
Coals spectral high purity-7−3, with a diameter of 6 mm.
The electrodes are machined from high purity coals spectral-7−3, 6 mm in diameter, sharpened to a truncated cone with an apex angle of 15° and a platform with a diameter of 1.5 mm.
The electrodes are machined from high purity coals spectral-7−3, 6 mm in diameter with a side height of 1 mm.
The graphite powder of high purity according to GOST 23463−79.
Photographic plate for spectrographic type I, size 9х24 or equivalent, providing normal blackening of analytical lines in the spectrum.
Beakers, glass.
Separating funnel with a capacity of 1000, 2000 cm.
A Buchner funnel with a diameter of 132 mm.
Bunsen flask with a capacity of 200, 500, 1000 cm.
Pipette.
Micropipettes 0.1 cmhydrophobized: dried in drying oven at 120−150 °C pipette is cooled, washed inner surface of each pipette with dimethyldichlorosilane and dried in a drying Cabinet at 120 °C.
Burette 25 cm.
Glass cylinders with a capacity of 1,000 cmwith a glass stopper.
Flasks glass conical.
A glass bulb with a capacity of 1,000 cmwith a reflux condenser.
Volumetric flasks.
Glass propeller stirrer.
The quartz crucibles with a capacity of 10−15 cmhydrophobized: the inner wall of the crucible is washed with dimethyldichlorosilane and dried at 120 °C.
A device for distillation flask furca, with a capacity of 500−1000 cm.
Tube rubber.
The polyethylene film.
Paper universal indicator pH 1−10.
Silica gel brand KSK N 2 or N 2.5.
Ftoroplast-4 (Teflon), powder with grain size ~0.1 mm.
The wool is Teflon.
Oxides of rare earth elements: lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium and yttrium, clean-defined impurities.
Copper sulfate 5-water according to GOST 4165−78, 0.5 mol/DMsolution.
Standard solutions of lanthanum, cerium, praseodymium, neodymium, samarium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium containing 10 mg/cmof one of REE in the calculation of the oxide. Each solution is prepared separately:
1 g of the respective oxides of REE (svezhepriobretennoy) were placed in a glass with a capacity of 100 cm, add 10 cmof hydrochloric acid diluted 1:1, and heated to complete dissolution of the oxide; the solution was then cooled, transferred to a volumetric flask with a capacity of 100 cmand the volume was adjusted to the mark with water.
Solutions internal standard containing 1 mg/cmcerium or 1 mg/cmerbium, based on the oxide, is prepared by diluting 10 cmof a standard solution containing 10 mg/cmof erbium or cerium based on the oxide.
A solution of 1 containing 0.1 mg/cmof lanthanum, cerium, praseodymium, neodymium, samarium, europium, calculated on oxide: 1 cmof each standard solution (10 mg/cm) of lanthanum, cerium, praseodymium, neodymium, samarium, europium, based on the oxide is placed in a volumetric flask with a capacity of 100 cmand the volume was adjusted up to the mark of 1 mol/DMhydrochloric acid solution.
Solution 2 containing 0.1 mg/cmof gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium, based on the oxide: 1 cmof each standard solution (10 mg/cm) of gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium and lutetium in the calculation of the oxide is placed in a volumetric flask with a capacity of 100 cmand the volume was adjusted up to the mark of 1 mol/DMhydrochloric acid solution.
Sodium acetate according to GOST 199−78, H. h, a saturated solution.
Sodium carbonate crystal according to GOST 84−76, H. h, solution with a concentration of 50 g/DM.
Sodium chloride according to GOST 4233−77, solutions with a concentration of 100 g/land 20 g/DM.
Sodium hydroxide according to GOST 4328−77, H. h
Potassium branovitsky according to GOST 4457−74, H. C.: 0.1 mole/DMsolution (16.8 mg dissolved in 1000 cmof water); 0.1 mol/DMsolution of 3.5 mol/DMnitric acid solution; 0.1 mol/DMsolution of 7 mol/DMnitric acid solution. Prepared on the day of use.
Ammonium radamisty 0.3 mol/l, 0.8 mol/DMsolutions with a pH of 4.7.
Distilled water, distilled twice in a quartz distillation unit.
Hydrochloric acid by the GOST 3118−77, H. h, concentrated and titrated solutions: 0,01; 0,1; 0,3; 0,4; 0,5; 0,8; 1; 1,1; 1,2; 1,5; 2; 2,2; 2,4; 2,5; 3; 4; 5; 7 mol/DM.
Hydrochloric acid, double-distilled, a 1.5 mol/DMsolution.
Oxalic acid according to GOST 22180−76 H. h, a saturated solution.
Nitric acid GOST 4461−77, H. h, concentrated, 3,5; 7 mol/DMsolutions.
Hydrofluoric acid according to GOST 10484−78, H. h, concentrated, 1 mole/DMsolution.
Ammonia water according to GOST 3760−79, H. h, concentrated solution with a concentration of 50 g/DM.
Hydrogen peroxide according to GOST 10929−76.
Acetone according to GOST 2603−79.
Arsenazo III solution with a concentration of 0.2 g/DM.
For NTD phenolphthalein, alcohol solution with a concentration of 10 g/DM.
Di (2-ethylhexyl) phosphoric acid (D2EHPA), technical (50−70%) and improved (at least 95%).
D2EHPA 100% get technical D2EHPA or D2EHPA improved, the purification according to GOST 23862.7−79 (PP.3.1 and 3.2).
The tributyl phosphate (TBP) purified according to GOST 23862.7−79, p.3.3.
The ethyl ether.
The technical rectified ethyl alcohol GOST 18300−87.
The dimethyldichlorosilane.
Carbon tetrachloride according to GOST 20288−74.
The dimethyldichlorosilane solution in carbon tetrachloride (1:4).
The ethylene glycol according to GOST 10164−75.
Ascorbic acid, a solution with a concentration of 5 g/lin 1 mol/DMhydrochloric acid; prepared on the day of use.
Benzene according to GOST 5955−75.
Polystyrene.
A solution of polystyrene in benzene with a concentration of 20 g/DM; prepared on the day of use.
Argon gas GOST 10157−79.
Oxygen gas GOST 5583−78.
The gaseous nitrogen according to GOST 9293−74.
Sec. 2. (Changed edition, Rev. N 1).