GOST 13047.15-2002
NICKEL. COBALT
METHOD FOR DETERMINATION OF TIN
THE INTER-STATE COUNCIL
FOR STANDARDIZATION, METROLOGY AND CERTIFICATION
Minsk
Preface
1 DEVELOPED by Interstate technical committees for standardization MTK 501 Nickel and MTC 502 «Cobalt», JSC «Gipronikel ' Institute»
INTRODUCED by Gosstandart of Russia
2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol № 21 dated may 30, 2002)
The adoption voted:
| The name of the state | The name of the national authority for standardization |
| The Republic Of Azerbaijan | Azgosstandart |
| The Republic Of Armenia | Armastajad |
| The Republic Of Belarus | Gosstandart Of The Republic Of Belarus |
| Georgia | Gosstandart |
| The Kyrgyz Republic | Kyrgyzstandard |
| The Republic Of Moldova | Moldovastandart |
| Russian Federation | Gosstandart Of Russia |
| The Republic Of Tajikistan | Tajikstandart |
| Turkmenistan | The MDCSU «Turkmenstandartlary» |
| The Republic Of Uzbekistan | Standards |
| Ukraine | Gosstandart Of Ukraine |
3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated 17 September 2002 No. 334-St inter-state standard GOST 13047.15−2002 introduced directly as state standard of the Russian Federation from July 1, 2003
4 REPLACE GOST 13047.12−81, GOST 741.18−80
The CONTENTS
1 Scope 2 Normative references 3 General requirements and safety requirements 4 Atomic absorption method 4.1 Method of analysis 4.2 measuring instruments, auxiliary devices, materials, reagents, solutions 4.3 Preparation for analysis 4.4 analysis 4.5 Processing the analysis results 4.6 accuracy Control analysis Annex A Bibliography |
GOST 13047.15−2002
INTERSTATE STANDARD
NICKEL. COBALT
Method for determination of tin
Nickel. Cobalt.
Method for determination of tin
Date of introduction 2003−07−01
1 Scope
This standard establishes the atomic absorption method for the determination of tin at a mass fraction of from 0.0001% to 0,0020% in primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on.
2 Normative references
The present standard features references to the following standards:
GOST 123−98 Cobalt. Specifications
GOST 849−97 Nickel primary. Specifications
GOST 860−75 Tin. Specifications
GOST 3118−77 hydrochloric Acid. Specifications
GOST 4461−77 nitric Acid. Specifications
GOST 9722−97 Nickel Powder. Specifications
GOST 10157−79 Argon gaseous and liquid. Specifications
GOST 11125−84 nitric Acid of high purity. Specifications
GOST 13047.1−2002 Nickel. Cobalt. General requirements for methods of analysis
GOST 14261−77 hydrochloric Acid of high purity. Specifications
3 General requirements and safety requirements
General requirements for methods of analysis and safety requirements when performing work — according to GOST 13047.1.
4 Atomic absorption method
4.1 Method of analysis
The method is based on measuring absorption at a wavelength of 235,5 nm resonance radiation by atoms of tin, the resulting electrothermal atomization of the sample solution.
4.2 measuring instruments, auxiliary devices, materials, reagents, solutions
Atomic absorption spectrophotometer measurements with electrothermal atomization, the correction non-selective absorption and the automated flow of the solution into the atomizer.
Lamp with hollow cathode for the excitation of spectral lines of tin.
Argon gas according to GOST 10157.
Filters obestochennye [1] or other medium density.
Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1, 1:9 and 1:19.
Hydrochloric acid according to GOST 3118 or, if necessary, according to GOST 14261, diluted 1:1.
Nickel powder according to GOST 9722 or standard sample of Nickel with the prescribed mass fraction of tin is not more than 0.0001%.
Cobalt GOST 123 or standard sample of cobalt with the prescribed mass fraction of tin is not more than 0.0001%.
Tin GOST 860.
The tin solutions of known concentration.
The solution And the mass concentration of tin 0.0001 g/cm3: in a glass with a capacity of 100 cm3 is placed a portion of tin mass 0,1000 g pour 20 — 30cm3 of hydrochloric acid, dissolve while heating on a boiling water bath, cooled, transferred into a measuring flask with volume capacity of 1000 cm3, flow of 50 cm3 of hydrochloric acid and topped up to the mark with water.
Solution B is the mass concentration of tin 0,00001 g/cm3: in a volumetric flask with a capacity of 100 cm3 is taken 10 cm3 of solution A and pour to the mark with nitric acid, diluted 1:19.
Solution of the mass concentration of tin 0,000001 g/cm3: in a volumetric flask with a capacity of 100 cm3 is taken 10 cm3 of a solution and topped up to the mark with nitric acid, diluted 1:19.
4.3 Preparation for analysis
4.3.1 For calibration chart 1 in determining the mass fraction of tin is not more than 0,0010% in beakers or flasks with a capacity of 250 cm3 place hitch weight 1,000 g sample of Nickel powder or cobalt, or a standard sample of Nickel or cobalt with the prescribed mass fraction of tin. The number of batches must match the number of points of calibration curve, including Supervisory experience.
The sample flow 15 — 20 cm3 of nitric acid, diluted 1:1 and dissolved by heating. When using the Nickel powder in the solutions were filtered through filters (red or white ribbon), washed 2 — 3 times with nitric acid, diluted 1:9, the filters are washed 2 — 3 times with hot water. The solutions were evaporated to a volume of 10 — 15 cm3, flow 40 — 50 cm3 of water, heated to boiling, cooled, transferred to volumetric flasks with a capacity of 100 cm3.
In the flask is taken 1,0; 2,0; 4,0; 6,0; 8,0; 10,0 cm3 of the solution in the flask with the solution in the reference experiment the solution of tin is not administered, made up to the mark with water and then measure the absorbance as indicated in 4.4.
The mass of tin in solutions for the calibration is 0,000001; 0,000002; 0,000004; 0,000006; 0,000008; 0,000010 G.
4.3.2 For calibration curve 2, when determining the mass fraction of tin over 0,0010% in volumetric flasks with a capacity of 100 cm3 is taken in 20 cm3 of a solution in the reference experiment, prepared as specified in 4.3.1, enter 1,0; 2,0; 4,0; 6,0; 8,0; 10,0 cm3 of a solution In one of the flasks with a solution of the reference experiment a solution of tin do not enter, made up to the mark with nitric acid, diluted 1:19, and measure the absorbance as indicated in 4.4.
The mass of tin in solutions for the calibration specified
4.4 analysis
In a glass or flask with a capacity of 250 cm3 place the weighed sample mass of 1,000 g, pour 15 — 20 cm3 of nitric acid, diluted 1:1, evaporated to a volume of 5 — 7 cm3, was transferred to a volumetric flask with a capacity of 100 cm3, cooled and topped to the mark with water.
When the mass fraction of tin over 0,0010% in a volumetric flask with a capacity of 100 cm3 is taken aliquot part of the solution a volume of 20 cm3 and topped to the mark with nitric acid, diluted 1:19.
Measure the absorbance of the sample solution and solutions for calibration at a wavelength of 35.5 nm, slit width of not more than 0.7 nm with a correction non-selective absorption in the current of argon at least two times, sequentially inserting them into the atomizer. Depending on the type of spectrophotometer select the optimal volume of the solution from 0.005 to 0.050 cm3 or the optimal time of an aerosol spray from 5 to 50 C. wash the system with water, check the zero point and the stability of the calibration curve. To check the zero point solution is used, the appropriate control experience, prepared as described in section 4.3.
Selection of optimal temperature is carried out individually for the used spectrophotometer on solutions for calibration. Recommended operating conditions of the atomizer shown in table 1.
Table 1 — operating conditions of the atomizer
| The name of the stage | Temperature, °C | Time |
| Drying | 120 — 150 | 2 — 30 |
| Ashing | 700 — 1000 | 10 — 30 |
| Atomization | 2200 — 2400 | 4 — 5 |
The values of absorption solutions for the calibration and their corresponding masses tin build the calibration graphs.
The value of absorbance of sample solution find the mass of the tin on the appropriate calibration schedule.
4.5 Processing the analysis results
Mass fraction of tin in the sample of X %, is calculated by the formula
where Mx is the mass of tin in the sample solution, g;
K — dilution factor of sample solution;
M — the weight of the portion of the sample,
4.6 accuracy Control analysis
Control of metrological characteristics of the results of the analysis carried out according to GOST 13047.1.
Standards monitoring and error analysis method are given in table 2.
Table 2 — Standards for monitoring and error analysis method
Percentage
| Mass fraction of tin | The permissible discrepancy between two parallel definitions d2 |
Permissible discrepancies in the results of three parallel measurements d3 | The allowable discrepancy of the two results of analysis D | The error analysis method D |
| 0,00010 | 0,00003 | 0,00004 | Of 0.00006 | 0,00004 |
| 0,00030 | 0,00005 | Of 0.00006 | 0,00010 | 0,00007 |
| 0,00050 | 0,00007 | 0,00008 | 0,00014 | 0,00010 |
| 0,00100 | 0,00012 | 0,00014 | 0,00020 | 0,00015 |
| 0,0020 | 0,0002 | 0,0003 | 0,0004 | 0,0003 |
