GOST R 56240-2014
GOST R 56240−2014 Copper. Spectral method of measuring impurities
GOST R 56240−2014
NATIONAL STANDARD OF THE RUSSIAN FEDERATION
COPPER
Spectral method of measuring impurities
Copper. Spectral methods of impurity analysis
OKS 77.120.30
Date of introduction 2015−09−01
Preface
1 DEVELOPED by JSC «uralmekhanobr"
2 SUBMITTED by the Technical Committee for standardization TC 368 «Copper"
3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology dated 19 November 2014 N 1675-St
4 INTRODUCED FOR THE FIRST TIME
Application rules of this standard are established in GOST R 1.0−2012 (section 8). Information about the changes to this standard is published in the annual (as of January 1 of the current year) reference index «National standards» and the official text changes and amendments — in monthly information index «National standards». In case of revision (replacement) or cancellation of this standard a notification will be published in a future issue of information index «National standards». Relevant information, notification and lyrics are also posted in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet (gost.ru)
1 Scope
This standard specifies the spectral method of measuring the mass fraction of impurities in the copper in the ranges given in table 1.
General requirements for method of measurement and safety requirements when performing measurements according to GOST 25086, GOST 31382, sampling for measurement — 193 GOST, GOST 546, GOST 4960 and other regulatory documents for specific products.
Table 1
Percentage
Component |
The range of the mass fraction of component |
Tin |
From 0,00010 to 0,150 incl. |
Zinc |
From 0,00010 to 0.100 incl. |
Silver |
From about 0.0006 to 0,150 incl. |
Selenium |
From 0,00010 to 0,0060 incl. |
Tellurium |
From 0,00010 to 0,150 incl. |
Silicon |
From 0.0005 to 0,0070 incl. |
Cobalt |
From 0,00010 to 0,0030 incl. |
Bismuth |
From of 0.00006 to 0.015 incl. |
Nickel |
From 0,00010 to 0.30 incl. |
Sulfur |
From 0.0005 to 0,030 incl. |
Iron |
From 0,00010 to 0,150 incl. |
Cadmium |
From 0,00010 to 0,060 incl. |
Antimony |
From 0,00015 to 0,090 incl. |
Arsenic |
From 0,00010 to 0,030 incl. |
Lead |
From 0,00015 to 0,060 incl. |
Chrome |
From 0,00010 to 0.050 incl. |
Phosphorus |
From 0,00010 to 0,090 incl. |
Manganese |
From 0,00010 to 0,010 incl. |
2 Normative references
This standard uses the regulatory references to the following standards:
GOST 193−79 copper Ingots. Specifications
GOST 546−2001 copper Cathodes. Specifications
GOST 4960−2009 copper Powder electrolytic. Specifications
GOST 18300−87 ethyl rectified technical. Specifications
GOST 25086−2011 non-ferrous metals and their alloys. General requirements for methods of analysis
GOST 31382−2009 Copper. Methods of analysis
GOST R 53228−2008 Scales non-automatic actions. Part 1. Metrological and technical requirements. Test
GOST R ISO 5725−6-2002 Accuracy (correctness and precision) of methods and measurement results. Part 6. The use of precision values in practice
ST SEV 543−77 Number. Record rules and rounding
Note — When using this standard appropriate to test the effect of reference standards in the information system of General use — on the official website of the Federal Agency for technical regulation and Metrology on the Internet or in the annual information index «National standards» published as on January 1 of the current year, and the editions of the monthly information index «National standards» for the current year. If replaced with a reference standard, which was given an undated reference, then it is recommended to use the current version of this standard, taking into account all enabled in this version modifications. If replaced with a reference standard, which is given a dated reference, it is recommended to use the version of this standard referred to above by year of approval (acceptance). If after approval of this standard in the reference standard, which is given a dated reference, a change affecting a provision to which reference, the provision is recommended to be applied without taking into account this change. If the reference standard is cancelled without replacement, the position in which reference is made to him, recommended to be used in part not affecting this link.
3 Characteristics of measurement accuracy
The accuracy of measuring the mass fraction of tin, zinc, silver, selenium, tellurium, silicon, cobalt, bismuth, Nickel, sulfur, iron, cadmium, antimony, arsenic, lead, chromium, phosphorus, manganese corresponds to the characteristics given in table 2 (confidence probability P = 0,95).
Limit values of repeatability and reproducibility of measurements for a confidence probability P = 0.95 is shown in table 2.
Table 2 — Values of the measure of the accuracy, limits of repeatability and reproducibility of measurements of the mass fraction of the component at a confidence probability P = 0,95 | ||||
Percentage | ||||
Component | Measurement range of mass fraction of component | The accuracy rate of |
Limits (absolute values) | |
repeatability r (n=2) |
of rehabilitation of conductivity R | |||
Tin | From 0,00010 to 0,00030 incl. | Of 0.00006 |
0,00005 | 0,00007 |
SV. 0,00030 «0,00100 « | 0,00014 |
0,00014 | 0,00020 | |
«0,0010» 0,0030 « | 0,0005 |
0,0004 | About 0.0006 | |
«0,0030» 0,0090 « | 0,0013 |
0,0013 | 0,0019 | |
«0,009» 0,030 « | 0,004 |
0,003 | 0,005 | |
«0,030» 0,090 « | 0,010 |
0,009 | 0,015 | |
«0,090» 0,150 « | 0,020 |
0,020 | 0,028 | |
Zinc | From 0,00010 0,00020 to incl. | 0,00009 |
0,00010 | 0,00012 |
SV. 0,00020 «0,00060 « | 0,00015 |
0,00009 | 0,00020 | |
«About 0.0006» 0,0020 « | 0,0002 |
0,0002 | 0,0004 | |
«0,0020» 0,0060 « | 0,0005 |
0,0004 | 0,0005 | |
«0,0060» 0,0100 « | 0,0013 |
0,0013 | 0,0018 | |
«0,010» 0,030 « | 0,003 |
0,003 | 0,004 | |
«0,030» 0,100 « | 0,015 |
0,015 | 0,021 | |
Silver | From about 0.0006 to 0,0020 incl. | 0,0002 |
0,0002 | 0,0003 |
SV. 0,0020 «0,0060 « | 0,0004 |
0,0003 | 0,0004 | |
«0,0060» 0,0100 « | 0,0013 |
0,0013 | 0,0018 | |
«0,010» 0,030 « | 0,003 |
0,003 | 0,004 | |
«0,030» 0,090 « | 0,010 |
0,010 | 0,015 | |
«0,090» 0,150 « | 0,015 |
0,015 | 0,021 | |
Selenium | From 0,00010 to 0,00030 incl. | 0,00007 |
0,00005 | 0,00009 |
SV. 0,00030 «0,00100 « | 0,00018 |
0,00019 | 0,00027 | |
«0,0010» 0,0030 « | About 0.0006 |
About 0.0006 | 0,0008 | |
«0,0030» 0,0060 « | 0,0013 |
0,0013 | 0,0018 | |
Tellurium | From 0,00010 to 0,00030 incl. | Of 0.00006 |
0,00005 | 0,00008 |
SV. 0,00030 «0,00100 « | 0,00017 |
0,00017 | 0,00024 | |
«0,0010» 0,0030 « | About 0.0006 |
About 0.0006 | 0,0008 | |
«0,0030» 0,0060 « | 0,0013 |
0,0013 | 0,0018 | |
«0,006» 0,010 « | 0,002 |
0,002 | 0,003 | |
«0,010» 0,150 « | 0,003 |
0,003 | 0,004 | |
Silicon | To from 0,0005 0,0010 incl. | 0,0004 |
0,0004 | 0,0005 |
SV. 0,0010 «0,0030 « | 0,0007 |
0,0007 | 0,0010 | |
«0,0030» 0,0070 « | 0,0014 |
0,0015 | 0,0020 | |
Cobalt | From 0,00010 0,00020 to incl. | 0,00005 |
0,00004 | 0,00007 |
SV. Of 0.0002 «to about 0.0006 « | 0,0001 |
0,0001 | 0,0002 | |
«About 0.0006» 0,0010 « | 0,0004 |
0,0003 | 0,0005 | |
«0,0010» 0,0030 « | 0,0008 |
0,0007 | 0,0008 | |
Bismuth | From of 0.00006 to 0,00030 incl. | Of 0.00006 |
0,00005 | 0,00008 |
SV. 0,00030 «0,00050 « | 0,00017 |
0,00017 | 0,00023 | |
«To 0.0005» 0,0015 « | 0,0004 |
0,0003 | About 0.0006 | |
«0,0015» 0,0050 « | 0,0009 |
0,0009 | 0,0013 | |
«Of 0.005» to 0.015 « | 0,002 |
0,002 | 0,003 | |
Nickel | From 0,00010 to 0,00030 incl. | Of 0.00006 |
Of 0.00006 | 0,00008 |
SV. 0,00030 «0,00100 « | 0,00018 |
0,00019 | 0,00025 | |
«0,0010» 0,0030 « | About 0.0006 |
About 0.0006 | 0,0008 | |
«0,003» 0,010 « | 0,002 |
0,002 | 0,003 | |
«0,010» 0,030 « | 0,004 |
0,004 | 0,006 | |
«0,030» 0,100 « | 0,014 |
0,010 | 0,024 | |
«To 0.10» to 0.30 « | 0,04 |
0,03 | 0,06 | |
Sulfur | Between 0.0005 and 0.0015 incl. | 0,0002 |
0,0002 | 0,0003 |
SV. 0,0015 «0,0030 « |
0,0004 | 0,0004 | About 0.0006 | |
«0,0030» 0,0100 « |
0,0010 | 0,0008 | 0,0012 | |
«0,010» 0,030 « |
0,003 | 0,003 | 0,004 | |
Iron | From 0,00010 to 0,00040 incl. |
0,00009 | 0,00008 | 0,00011 |
SV. 0,0004 «0,0020 « |
0,0003 | 0,0003 | 0,0004 | |
«0,0020» 0,0060 « |
0,0009 | 0,0007 | 0,0011 | |
«0,006» 0,030 « |
0,004 | 0,003 | 0,005 | |
«0,030» 0,080 « |
0,014 | 0,014 | 0,010 | |
«0,080» 0,150 « |
0,020 | 0,020 | 0,028 | |
Cadmium | From 0,00010 to 0,00060 incl. |
0,00007 | 0,00007 | 0,00009 |
SV. About 0.0006 «0,0020 « |
0,0002 | 0,0002 | 0,0004 | |
«0,0020» 0,0060 « |
0,0005 | 0,0004 | About 0.0006 | |
«0,0060» 0,0100 « |
0,0013 | 0,0013 | 0,0018 | |
«0,010» 0,030 « |
0,003 | 0,003 | 0,004 | |
«0,030» to 0,060 « |
0,012 | 0,012 | 0,018 | |
Antimony | From 0,00015 to 0,00060 incl. |
0,00009 | 0,00009 | 0,00015 |
SV. About 0.0006 «0,0020 « |
0,0004 | 0,0004 | About 0.0006 | |
«0,0020» 0,0100 « |
0,0015 | 0,0012 | 0,0020 | |
«0,010» 0,030 « |
0,005 | 0,004 | 0,008 | |
«0,030» 0,090 « |
0,012 | 0,012 | 0,018 | |
Arsenic | From 0,00010 0,00020 to incl. |
0,00004 | 0,00004 | Of 0.00006 |
SV. Of 0.0002 «to about 0.0006 « |
0,0001 | 0,0001 | 0,0002 | |
«About 0.0006» 0,0010 « |
0,0004 | 0,0003 | 0,0005 | |
«0,0010» 0,0030 « |
0,0008 | 0,0007 | 0,0008 | |
«0,003» 0,010 « |
0,002 | 0,002 | 0,003 | |
«0,010» 0,030 « |
0,004 | 0,004 | 0,007 | |
Lead | From 0,00015 to 0,00060 incl. |
0,00010 | 0,00010 | 0,00015 |
SV. About 0.0006 «0,0020 « |
0,0004 | 0,0004 | 0,0005 | |
«0,0020» 0,0060 « |
0,0013 | 0,0013 | 0,0019 | |
«0,006» 0,010 « |
0,003 | 0,003 | 0,004 | |
«0,010» 0,030 « |
0,007 | 0,007 | 0,009 | |
«0,030» to 0,060 « |
0,011 | 0,011 | 0,016 | |
Chrome | From 0,00010 to 0,00060 incl. |
0,00007 | 0,00007 | 0,00009 |
SV. About 0.0006 «0,0020 « |
0,0002 | 0,0002 | 0,0004 | |
«0,0020» 0,0060 « |
0,0005 | 0,0004 | About 0.0006 | |
«0,0060» 0,0100 « |
0,0013 | 0,0013 | 0,0018 | |
«0,010» 0,030 « |
0,003 | 0,003 | 0,004 | |
«0,030» 0,050 « |
0,01 | 0,01 | 0,014 | |
Phosphorus | From 0,00010 to 0,00060 incl. |
0,00010 | 0,00009 | 0,00012 |
SV. About 0.0006 «0,0010 « |
0,0004 | 0,0003 | 0,0005 | |
«0,0010» 0,0030 « |
0,0008 | 0,0007 | 0,0010 | |
«0,0030» 0,0100 « |
0,0014 | 0,0010 | 0,0020 | |
«0,010» 0,030 « |
0,004 | 0,003 | 0,006 | |
«0,030» 0,090 « |
0,011 | 0,011 | 0,015 | |
Manganese | From 0,00010 0,00020 to incl. |
0,00005 | 0,00004 | 0,00008 |
SV. Of 0.0002 «0,0010 « |
0,0001 | 0,0001 | 0,0002 | |
«0,0010» 0,0030 « |
0,0007 | About 0.0006 | 0,0010 | |
«0,003» 0,010 « |
0,002 | 0,002 | 0,003 |
4 measurement Means, auxiliary devices, materials
When performing measurements using the following measuring instruments and auxiliary devices:
spectrometer atomic emission;
— scale special accuracy class according to GOST R 53228 with the largest weighing limit of 200 g and a readability of 0.0001 g;
— milling machine or cutting machine;
— pressure gauge with measuring range from 0 to 10 MPa;
— induction furnace or resistance furnace for melting the samples at a temperature of from 1180 °C to 1200 °C;
— graphite crucible;
the graphite mold;
— the state standard samples of composition of copper.
Allowed to use other means of measurements with metrological characteristics and equipment with technical characteristics as listed above.
When performing measurements using the following materials:
— ethyl alcohol according to GOST 18300.
5 Method of measurement
The method is based on measuring the intensity of spectral lines is determined by the components in the analyzed sample monolithic form, rolled copper samples and comparison with the use of atomic emission spectrometry with arc and spark excitation source and the photoelectric registration of spectrum.
6 Preparation for measurements
6.1 Preparation of the spectrometer
Preparing the spectrometer to the measurements carried out in accordance with the requirements of the user’s manual.
Graduate spectrometer using standard samples of composition of copper and build the dependence of the intensity of the analytical line from the mass fraction for each component you define. In future work adjust calibration parameters in accordance with the manual of the spectrometer.
6.2 to the sample Requirements
Samples for measurement must come in the form of a monolithic specimen having at least one flat surface with a diameter of 20 mm and a height of not less than 4 mm.
Sample electrolytic copper powder must be fused in template with a diameter of 20 mm and a height of not less than 10 mm For this sample powder is melted in a graphite crucible (form) with a tight-fitting lid in an induction furnace or a resistance furnace at a temperature of from 1180 °C to 1200 °C. the Molten metal in the crucible is kept under a lid for 5 to 10 min and cast in a graphite ingot mold two test ingot with a diameter of 20 mm and a height of not less than 10 mm. the Ingot is kept in the graphite mold into the air not more than 1 min, then cooled the mold with the ingot in cold water.
If measurements of core samples using a special adapter.
When measuring samples of rolled copper use a special adapter. Samples should have a thickness of at least 0.2 mm, sample thickness less than 0.2 mm must be pre-folded several times.
6.3 Preparation of samples for measurement
The surface of the sample directly before the measurement process on a milling machine or any other metal cutting machines without the use of lubricating fluids. Treatment is carried out in accordance with the manual of the machine. After machining the surface should be free of holes, scratches, cracks, inclusions and burrs.
The surface of the samples rolled copper is treated with ethyl alcohol. Alcohol consumption in one measurement is at least 10 cm.
7 performance measurement
The measurements are carried out in accordance with the manual of the spectrometer. The number of samples for measurements determined in accordance with the normative documents on products or internal documents of the company. For each sample perform at least two parallel definitions.
8, the Processing of the measurement results
8.1 Processing of results of measurements carried out using the computer of the spectrometer automatically for a given program and present them in the form of values of the mass fraction of the designated component.
8.2 the result of measurement taking the arithmetic mean of two parallel definitions, provided that the absolute difference between them in terms of repeatability does not exceed the value (at confidence probability P = 0,95) repeatability limit rgiven in table 2.
If the difference between the highest and lowest results of parallel measurements exceeds the limit value of the frequency of occurrence, perform the procedure described in GOST R ISO 5725−6-2002 (paragraph
8.3 discrepancy between the results of measurements obtained in two laboratories, should not exceed the limit of reproducibility shown in table 2. In this case, the final result may be decided to their arithmetic mean value. At default of this condition can be used the procedure described in GOST R ISO 5725−6.
8.4 Rounding of measurements carried out in accordance with the requirements of ST CMEA 543.
UDC 669.3:546.56.06:006.354 | OKS 77.120.30 |
Key words: copper, component, method of measurement, a standard sample of the measurement range, the accuracy rate of |