GOST 23862.26-79
GOST 23862.26−79 Rare-earth metals and their oxides. Methods for determination of Nickel (with Change No. 1)
GOST 23862.26−79
Group B59
INTERSTATE STANDARD
RARE EARTH METALS AND THEIR OXIDES
Methods for determination of Nickel
Rare-earth metals and their oxides. Methods of determination of nickel
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 3989 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 sets the photometric method for the determination of Nickel in yttria and its oxide (with a mass fraction of Nickel from 1·10to 2%·10
% 1·10
% to 5·10
%), in Lantana, yttria and their oxides (at a mass fraction of Nickel from 5·10
% to 3·10
%) and visual colorimetric method for the determination of Nickel in rare-earth metals and their oxides except cerium dioxide and cerium (with a mass fraction of Nickel from 5·10
% to 3·10
%).
(Changed edition, Rev. N 1).
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 23862.0−79.
2. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF NICKEL IN YTTRIA AND ITS OXIDE
The method is based on the reaction of Nickel with dimethylglyoxime. Optical density of the solution is measured on a photoelectrocolorimeter. Mass fraction of Nickel found by the calibration schedule.
2.1. Apparatus, reagents and solutions
Photoelectrocolorimeter FEK-56, or equivalent device.
Bath water.
Tile electric.
Volumetric flasks with a capacity of 25, 100 and 1000 cm.
Glasses with a capacity of 50 cm.
Cup porcelain.
The litmus paper.
Paper universal indicator.
Hydrochloric acid of high purity according to GOST 14261−77 diluted 1:1.
Nitric acid of high purity according to GOST 11125−84, diluted 3:2 and 0.01 mol/DMsolution.
Potassium hydroxide, H. C., solutions with a concentration of 50 and 100 g/DM.
Ammonia water according to GOST 3760−79, H. h., diluted 1:1.
Citric acid according to GOST 3652−69, H. h
Ammonium citrate according to NTD, h. e. a., a solution with a concentration of 500 g/DMin terms of citric acid: 50 g citric acid is dissolved at 65−70 cm
of ammonia solution, set pH 9 by universal indicator paper, adjusted in a volumetric flask with a capacity of 100 cm
the volume of the solution to the mark with water and mix.
Ammonium neccersarily according to GOST 20478−75, h. e. a., a solution with a concentration of 200 g/DM; prepared on the day of use.
Dimethylglyoxime according to GOST 5828−77, h. e. a., a solution with a concentration of 10 g/DMsolution of potassium hydroxide (50 g/DM
).
Nickel GOST 849−97*.
_______________
* On the territory of the Russian Federation from
A standard solution of Nickel (spare) containing 1 mg/cmNickel: 1 g of Nickel is placed in a porcelain Cup, pour the 35 cm
of nitric acid (3:2) and dissolved by heating in a water bath, evaporated to a volume of 3−5 cm
, is dissolved in 30−40 cm
of water. The solution is transferred into a measuring flask with volume capacity of 1000 cm
, adjusted to the mark with water and mix.
A solution of Nickel containing 2 mg/cmof Nickel, prepared on the day of use by dilution of a standard solution 500 times 0.01 mol/DM
solution of nitric acid.
(Amended,
Izm. N 1).
2.2. Analysis
2.2.1. A portion of the sample of an oxide of yttrium ground 1−0,1 g or the corresponding amount of metal, depending on the Nickel content is placed in a beaker with a capacity of 50 cm, moistened with water, dissolved by heating in 10 cm
of hydrochloric acid diluted 1:1. After complete digestion the sample solution is evaporated to a volume of 2−3 cm
, pour 5 cm
of a solution of ammonium citrate, 0.5 cm
of the solution naternicola ammonium is neutralized with solution of potassium hydroxide until the blue color of litmus-paper. Then pour 2 cm
of dimethylglyoxime solution, stirred for 10 minutes transferred to a volumetric flask with a capacity of 25 cm
, adjusted to the mark with water and mix. Optical density of the solution is measured on photoelectrocolorimeter at 403 nm in a cuvette with the thickness of the light absorbing layer was 50 mm.
A solution of comparison used water. Simultaneously with the analysis of the sample through all stages of the carried out control experience in chemicals. The obtained value of optical density is subtracted from the value of optical density of test solution. The value of the optical density of the solution in the reference experiment shall not exceed 0,07. The weight of the Nickel find at the calibration schedule
.
2.2.2. Construction of calibration curve
In a volumetric flask with a capacity of 25 cmis introduced: 0,50; 1,0; 3,0; 5,0; 10 cm
solution (containing 2 mg/cm
Nickel), pour 5 cm
of a solution of ammonium citrate, 0.5 cm
of the solution naternicola ammonium neutralized dropwise with a solution of potassium hydroxide until the color of litmus paper from red to blue, pour 2 cm
of the solution dimethylglyoxime, adjusted to the mark with water, mix.
After 10 minutes measure optical density of solutions on the photoelectrocolorimeter at 403 nm in a cuvette with the thickness of the light absorbing layer 50 mm as solution, comparison, use water. In one of the glasses introduce all reagents except the solution of Nickel (zero solution). The optical density of the zero solution should not exceed 0.05, otherwise change the reagents. The value of optical density of the zero solution is subtracted from the values of optical density of solutions of the scale.
Found an average of five values of the optical densities and their corresponding masses of Nickel to build a calibration curve in the coordinates, and the mass of Nickel — optical density of the solutions, individual points chart check at least once per month.
2.3. Processing of the results
2.3.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in sample found on the schedule, mcg;
— the weight of the portion of the sample,
2.3.2. Discrepancies in the results of two parallel determinations or the results of the two tests should not exceed values of allowable differences specified in table.1.
Table 1
| Mass fraction of Nickel, % |
Allowable difference, % |
1·10 |
5·10 |
1·10 |
5·10 |
2·10 |
5·10 |
3. A VISUAL COLORIMETRIC METHOD FOR THE DETERMINATION OF NICKEL IN RARE-EARTH METALS AND THEIR OXIDES EXCEPT CERIUM DIOXIDE AND CERIUM
The method is based on the extraction concentration of Nickel impurities in the form of its connection with furildioxime in chloroform and subsequent fotomaterialy coloured compounds in the organic phase.
3.1. Apparatus, reagents and solutions
The chemical glasses with a capacity of 50 cm.
Volumetric flasks with a capacity of 250 cm.
Watch-glasses.
Tile electric.
Separating funnel with a capacity of 50 cm, with a drain pipe with a length of 10 mm.
Set of cylinders for colorimetrically of colorless glass with ground stoppers with a height of 200 mm and 8 mm in diameter; use dry.
Nitric acid of high purity according to GOST 11125−84, concentrated.
The oxide of rare earth metals (among analyzed) containing not more than 1·10% Nickel.
The water is deionized.
Hydrogen peroxide according to GOST 10929−76, high purity, concentrated.
Ammonium acetate according to GOST 3117−78, OS.CH., an aqueous solution with a concentration of 500 g/DM.
-furildioxime, alcohol solution with a concentration of 5 g/DM
.
Nitroso-R-salt NTD, a solution with a concentration of 1 g/DM, store in a dark bottle no longer than a week.
Chloroform technical according to GOST 20015−88; before use, vigorously shaken with thiosulphate solution for 2 min at phase ratio aqueous: organic=1:3.
Nickel sulfate according to GOST 4465−74.
Sulfuric acid according to GOST 4201−79; 0.005 mol/DMsolution.
A standard solution of Nickel (spare) containing 0.1 mg/cmof Nickel: 0.12 g of Nickel sulfate dissolved in 0.005 mol/DM
sulfuric acid and the volume was adjusted solution to the mark in a volumetric flask with a capacity of 250 cm
0.005 mol/DM
sulfuric acid.
A solution of Nickel containing 1 µg/cmof Nickel prepared on the day of use by dilution of a standard solution of 0.005 mol/DM
sulfuric acid in 100 times.
(Amended,
Izm. N 1).
3.2. Analysis
3.2.1. A portion of the sample weighing 1 g is placed in a beaker with a capacity of 50 cm, moistened with 2−3 cm
of water, pour 2 cm
of nitric acid, 2−3 drops of hydrogen peroxide, cover the beaker watch glass and dissolve with a moderate heat. At the completion of the dissolution, remove the watch glass, the solution is evaporated to dryness, slightly Prokaeva the rest on the hot tiles.
The dry residue is dissolved in 15 cmof a solution of acetate of ammonium (if the balance is poorly soluble, then the contents of the Cup slightly heat and stir a few times), pour five drops of thiosulphate solution, five drops of solution, nitroso-R-salt, 1 cm
of solution
-furildioxime, stirring the solution after each addition of the reagent, and allowed to stand for 3 min. the Solution was transferred to a separatory funnel, pour 2 cm
of chloroform and vigorously shaken for 2 min. After separation of the phases merge one drop of chloroform extract, wipe dry the nozzle of the funnel with filter paper and poured the extract in the dry cylinder for colorimetrically. The color intensity of the extract is compared to a white background with a color intensity scale comparison, watching the painting from the top down
.
3.2.2. Preparation of the scale comparison
In glasses with a capacity of 50 cmpour 2−3 cm
of water, 2 cm
of nitric acid, 2−3 drops of hydrogen peroxide, introduce the tip of the spatula 20 mg oxide REE corresponding to the analyzed basis, and containing not more than 1·10
% of Nickel, introduced 0; 0,05; 0,10; 0,20; 0,30; 0,50; 0,80; 1,0 cm
of a solution of Nickel (containing 1 µg/cm
Ni), and the solution is evaporated to dryness. The dry residue is dissolved in 15 cm
of a solution of ammonium acetate, poured five drops of thiosulphate solution, five drops of solution, nitroso-R-salt, 1 cm
of solution
-furildioxime, stirring the solution after each addition of the reagent, and leave the contents of the beaker to stand 3 min. the solution was Then transferred to a separatory funnel, pour 2 cm
of chloroform and vigorously shaken for 2 min. After separation of the phases merge one drop of chloroform extract, wipe dry the nozzle of the funnel with filter paper and poured the extract in the dry cylinder for colorimetria
niya.
3.3. Processing of the results
3.3.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in sample, µg;
— the weight of the portion of the sample,
The result of the analysis take the average of results of two parallel measurements.
3.3.2. Discrepancies in the results of two parallel determinations or the results of the two tests should not exceed values of allowable differences specified in table.2.
Table 2
| Mass fraction of Nickel, % |
Allowable difference, % |
5·10 |
5·10 |
3·10 |
2·10 |
5·10 |
3·10 |
1·10 |
5·10 |
4. THE PHOTOMETRIC METHOD FOR THE DETERMINATION OF NICKEL IN LANTHANUM, YTTRIA AND THEIR OXIDES
The method is based on the reaction of the Nickel -furildioxime. The absorption spectra of the solutions recorded on the spectrophotometer SF-18. The Nickel content is found by the calibration schedule.
4.1. Apparatus, reagents and solutions
Registered spectrophotometer type SF-18 or similar device.
Analytical scale.
The chemical glasses with a capacity of 100 cm.
Volumetric flasks with a capacity of 25, 100 and 250 cm.
Glass pipettes with volume capacity of 1, 5 and 10 cm.
Distilled water GOST 6709−72.
Hydrochloric acid of high purity according to GOST 14261−77 diluted 1:1 and 1:10.
Ammonia water according to GOST 3760−79, h. e. a., diluted 1:10.
Sodium hydroxide according to GOST 4328−77, h. e. a., a solution with a concentration of 100 g/DM.
-furildioxime, a solution with a concentration of 5 g/l
, prepared by dissolving
-furildioxime in acetone, then dilute the resulting solution with distilled water in the ratio 1:9.
Sulfuric acid GOST 4204−77, h. e. a., 0.005 mol/DMsolution.
Nickel sulfate according to GOST 4465−74, h.d. a.
A standard solution of Nickel (spare) containing 100 µg/cmof Nickel: 0,120 g of Nickel sulfate dissolved in 0.005 mol/DM
sulfuric acid. The solution was transferred to a volumetric flask with a capacity of 250 cm
, and topped up to the mark and 0.005 mol/l
sulfuric acid solution.
A solution of Nickel containing 1 µg/cmof Nickel, prepared on the day of use by dilution of a standard solution 100 times 0.005 mol/DM
solution of sulfuric
acid.
4.2. Construction of calibration curve
In a volumetric flask with a capacity of 25 cmis introduced: 0; 0,1; 0,2; 0,3; 0,5; 1,0; 5 cm
of a solution containing 1 µg/cm
of Nickel, is poured 10 cm
of distilled water and set pH to 7.5−9 with ammonia solution diluted 1:10 (control by universal indicator paper).
Then in the flask poured 1 cmof solution
-furildioxime, leave the contents of the flasks for 30 min, and then set a pH of 1−2 with hydrochloric acid, diluted 1:10 (control by universal indicator paper) and bring the volume of the solutions to the mark with distilled water.
The solutions are alternately transferred to the cuvette of the spectrophotometer with the thickness of the light absorbing layer 50 mm, and record the absorption spectrum of each solution in the spectrophotometer SF-18 is in the range of wavelengths from 530 to 450 nm. As a solution used for the first comparison of these solutions. The results of absorption spectra to build calibration curve in the coordinates ,
(where
is the mass of Nickel in the solution in µg,
the height of the peak in the spectrum of the absorption at
486 nm). Individual points of the graph are checked at least once in m
esac.
4.3. Analysis
A portion of the oxides of lanthanum mass of 2 g of yttrium oxide content of 1 g or the corresponding amount of metal placed in chemical glass with a capacity of 100 cm, moistened with 2−3 cm
of distilled water, dissolved by heating to 5−7 cm
of hydrochloric acid diluted 1:1, the solution is evaporated to wet salts and the residue is dissolved in 5−10 cm
of distilled water. The solution was cooled to room temperature and then to it with vigorous stirring poured dropwise ammonia solution (for analysis of lanthanum oxide) or sodium hydroxide (for analysis of oxides of yttrium) prior to the turbidity of the solution (pH ~6−7) and 1 cm
of solution
-furildioxime. The contents of the glass leave it for 30 min. Then pour the ammonia solution or sodium hydroxide until reaching pH ~7,5−9, not paying attention to the precipitate of hydroxide of the lanthanide (control the pH value of the solution by universal indicator paper), then the contents of the Cup and leave for 15 minutes, Then at intensive stirring and poured hydrochloric acid solution, diluted 1:10 (for analysis of oxides of lanthanum) or 1:1 (in the analysis of yttrium oxide) to dissolve the precipitate hydroxide (pH ~1−4). The resulting solution was transferred to a volumetric flask with a capacity of 25 cm
and the volume was adjusted solution to the mark with distilled water. Then record the absorption spectrum of the solution as described under construction of calibration curve in step 4.2. The mass of Nickel in the solution found by the calibration schedule. Simultaneously with the analysis of samples carried out control experience in the chemicals through all stages of the analysis and introduce an amendment
.
4.4. Processing of the results
4.4.1. Mass fraction of Nickel () in percent is calculated by the formula
where is the mass of Nickel in sample found on the schedule, mcg;
— the mass of Nickel in a control experiment, µg;
— the weight of the portion of the sample,
The result of the analysis taking the arithmetic mean of two parallel definitions, drawn from separate batches.
4.4.2. Discrepancies in the results of two parallel determinations or the results of the two tests should not exceed values of allowable differences specified in table.3.
Table 3
| Analyzed basis |
Mass fraction of Nickel, % |
Allowable difference, % |
| Oxide of lanthanum |
5·10 |
4·10 |
1·10 |
0,7·10 | |
5·10 |
2,5·10 | |
1·10 |
0,4·10 | |
3·10 |
1,2·10 | |
| Oxide of yttrium |
1·10 |
0,8·10 |
5·10 |
3·10 | |
1·10 |
0,5·10 | |
3·10 |
1,4·10 | |
5·10 |
2·10 |
Sec. 4. (Added, Rev. N 1).
