GOST 13047.6-2002
NICKEL. COBALT
METHODS FOR DETERMINATION OF CARBON
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 13047.6−2002 introduced directly as state standard of the Russian Federation from July 1, 2003
4 REPLACE GOST 13047.2−81, GOST 741.3−80
The CONTENTS
1 Scope 2 Normative references 3 General requirements and safety requirements 4 Coulometric 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 5 the Method of infrared spectrometry 5.1 Method of analysis 5.2 measurement Means, auxiliary devices, materials, reagents, solutions 5.3 Preparation for assay 5.4 analysis 5.5 Processing of analysis results 5.6 Control of accuracy of analysis Appendix A. Bibliography |
GOST 13047.6−2002
INTERSTATE STANDARD
NICKEL. COBALT
Methods for determination of carbon
Nickel. Cobalt.
Methods for determination of carbon
Date of introduction 2003−07−01
1 Scope
This standard specifies the coulometric method and the method of infrared spectrometry to determine the carbon mass fraction from 0.003% to 0.50% in the primary Nickel GOST 849, Nickel powder according to GOST 9722, GOST cobalt 123 and cobalt powder to GOST 9721.
2 Normative references
The present standard features references to the following standards:
GOST 8.315−97 State system for ensuring the uniformity of measurements. Standard samples of composition and properties of substances and materials. The main provisions of the
GOST 123−98 Cobalt. Specifications
GOST 849−97 Nickel primary. Specifications
GOST 859−2001 Copper. Brand
GOST 860−75 Tin. Specifications
GOST 2603−79 Acetone. Specifications
GOST 5583−78 (ISO 2046−73) Oxygen gas technical and medical. Specifications
GOST 9147−80 Glassware and equipment lab porcelain. Specifications
GOST 9721−79 cobalt Powder. Specifications
GOST 9722−97 Nickel Powder. Specifications
GOST 13047.1−2002 Nickel. Cobalt. General requirements for methods of analysis
GOST 16539−79 Copper (II) oxide. 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 Coulometric method
4.1 Method of analysis
The method is based on measuring the amount of electricity required to achieve a given initial pH of the absorption solution, through which oxide of carbon (IV) combustion of the sample in flowing oxygen at a temperature of 1300 — 1400 °C.
4.2 measuring instruments, auxiliary devices, materials, reagents, solutions
Express-analyzer of carbon based on the method of coulometric titration, complete with all accessories, including automatic scales (correction mass).
Boat porcelain with GOST 9147, calcined at a temperature of 1000 — 1100 °C and optionally calcined in flowing oxygen at the operating temperature of not less than 1.5 min.
Mullite refractory tube of length 65 — 80 cm internal diameter 1.8 — 2.2 cm.
The hook is made of heat-resistant low-carbon steel with a diameter of 0.3 — 0.5 cm in length 50 — 60 cm.
Oxygen gas according to GOST 5583.
Acetone according to GOST 2603.
The solutions and absorption of the subsidiary is prepared in accordance with the type of the used analyzer according to the instructions supplied with the analyzer.
Marshes: copper GOST 859 in the form of chips or wire; copper oxide (II) according to GOST 16539, preheated for 3 to 4 hours at a temperature of 800 — 850 °C; tin GOST 860 and other materials for combustion control and the value of the experience specified in 4.3.
Standard samples according to GOST 8.315 composition of Nickel, cobalt, or alloys on their basis and on the basis of iron with the certified mass fraction of carbon.
4.3 Preparation for analysis
Preparing the analyzer to work and his grading is carried out in accordance with the operation manual. For calibration using standard samples of composition of Nickel, cobalt, or alloys on their basis and on the basis of iron.
To carry out control experience in the boat placed a portion of the beach that mass, which is used in the analysis of the sample, and analyze as specified in 4.4.
Allowed for the introduction of flux to use metering devices.
Supervisory experience is considered satisfactory, if the measured mass fraction of carbon on the digital display of the analyzer does not exceed the error of the method of analysis specified in 4.6 to define the mass fraction of carbon.
The negative results in the reference experiment, it is recommended to calcine pumps as specified in 4.2, and the flux in the form of metal washed with acetone and dried at a temperature of 20 — 30 °C. it is allowed to use other volatile organic solvents, providing the required values in the reference experiment.
4.4 analysis
In a porcelain boat is placed a portion of the sample weighing 0,200 — 1,000 g and adds the smoother, the weight of which must be the same when control experience, calibration and analysis. With a hook introduce the boat into the furnace at a temperature of 1300 — 1400 °C in the most heated portion of the refractory tube and carry out the combustion in a current of oxygen for 1.5 and 3.0 min.
When poor convergence results of parallel measurements allowed the sample selected in the form of chips, before the test, rinse acetone, as described in section 4.3 for the beach.
4.5 Processing the analysis results
Mass fraction of carbon in the sample is X %, is calculated by the formula
(1)
where Mo is the weight of the portion of the standard sample used in the calibration of the analyzer, g;
Andx — reading digital display of the analyzer obtained during the analysis of samples, %;
Andit is the arithmetic mean value of indications of the analyzer when conducting the reference experiment, %;
M — the weight of the portion of the sample,
When using the analyzer corrector mass mass fraction of carbon in the sample is X %, is calculated by the formula
X = Ax — Ato(2)
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 1.
Table 1 — Standards for monitoring and error analysis method
Percentage
| Mass fraction of carbon | 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 |
| 0,0030 | 0,0008 | 0,0010 | 0,0012 | 0,0010 |
| 0,0050 | 0,0014 | 0,0017 | 0,0021 | 0,0015 |
| 0,010 | 0,003 | 0,004 | 0,005 | 0,003 |
| 0,030 | 0,005 | 0,006 | 0,008 | 0,006 |
| 0,050 | 0,008 | 0,010 | 0,012 | 0,008 |
| 0,100 | 0,015 | 0,018 | 0,023 | 0,016 |
| 0,300 | 0,020 | 0,024 | 0,030 | 0,021 |
| 0,50 | 0,03 | 0,04 | 0,05 | 0,04 |
5 the Method of infrared spectrometry
5.1 Method of analysis
The method is based on measuring the absorption of gaseous carbon oxide (IV) in the infrared region of the spectrum after selecting it from the metal combustion in high-frequency induction furnace in flowing oxygen.
5.2 measurement Means, auxiliary devices, materials, reagents, solutions
Automated analyzer based on the principle of infrared spectrometry, with high frequency induction furnace, and weights to account for the mass of sample.
Crucibles refractory ceramic provided with the analyzer, or similar type, if necessary, calcined at a temperature of 1100 — 1200 °C for 3 to 4 hours
Marshes: marshes, provided with the analyzer by the manufacturer; copper GOST 859 in the form of chips or wire; tungsten [1]; carbonyl iron [2] and other materials for combustion control and the value of the experience specified in 5.3.
Oxygen gas according to GOST 5583.
Standard samples according to GOST 8.315 composition of Nickel, cobalt, or alloys on their basis and on the basis of iron with the certified mass fraction of carbon.
5.3 Preparation for assay
Preparing the analyzer to work and his grading is carried out in accordance with the operation manual. For calibration using standard samples of composition of Nickel, cobalt, or alloys on their basis and on the basis of iron.
To check the value of the reference experiment in the crucible is placed a portion of the beach that mass, which is used in the analysis of samples and conduct analysis as indicated in 5.4.
Allowed for the introduction of flux to use metering devices.
Supervisory experience is considered satisfactory, if the measured mass fraction of carbon on the digital display of the analyzer does not exceed the error of the method of analysis specified in section 4.6 to define the mass fraction of carbon.
When an unsatisfactory result, the control experience is recommended to be heated crucibles, as specified in 5.2, and the flux in the form of metal washed with acetone and dried at a temperature of 20 — 30 °C. it is allowed to use other volatile organic solvents, providing the required values in the reference experiment.
5.4 analysis
The crucible is placed in a portion of the sample weighing 0,200 — 1,000 g, add the flux, the weight of which must be the same when conducting the reference experiment, the calibration and analysis, and conduct analysis as indicated in the instructions supplied with the analyzer. When poor convergence results of parallel measurements allowed the sample selected in the form of chips, before the test, rinse acetone as specified in 5.3 for the beach.
5.5 Processing of analysis results
Mass fraction of carbon in percent with automatic registration of values in the reference experiment is read from the display or printer of the analyzer.
5.6 Control of accuracy of 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 1.
