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GOST R 56307-2014

GOST R ISO 15353-2014 GOST P 55080-2012 GOST R ISO 16962-2012 GOST R ISO 10153-2011 GOST R ISO 10280-2010 GOST R ISO 4940-2010 GOST R ISO 4943-2010 GOST R ISO 14284-2009 GOST R ISO 9686-2009 GOST R ISO 13899-2-2009 GOST 18895-97 GOST 12361-2002 GOST 12359-99 GOST 12358-2002 GOST 12351-2003 GOST 12345-2001 GOST 12344-88 GOST 12350-78 GOST 12354-81 GOST 12346-78 GOST 12353-78 GOST 12348-78 GOST 12363-79 GOST 12360-82 GOST 17051-82 GOST 12349-83 GOST 12357-84 GOST 12365-84 GOST 12364-84 STATE STANDARD P 51576-2000 GOST 29117-91 GOST 12347-77 GOST 12355-78 GOST 12362-79 GOST 12352-81 GOST P 50424-92 STATE STANDARD P 51056-97 GOST P 51927-2002 GOST P 51928-2002 GOST 12356-81 GOST R ISO 13898-1-2006 GOST R ISO 13898-3-2007 GOST R ISO 13898-4-2007 GOST R ISO 13898-2-2006 STATE STANDARD P 52521-2006 GOST P 52519-2006 GOST R 52520-2006 GOST P 52518-2006 GOST 1429.14-2004 GOST 24903-81 GOST 22662-77 GOST 6012-2011 GOST 25283-93 GOST 18318-94 GOST 29006-91 GOST 16412.4-91 GOST 16412.7-91 GOST 25280-90 GOST 2171-90 GOST 23401-90 GOST 30642-99 GOST 25698-98 GOST 30550-98 GOST 18898-89 GOST 26849-86 GOST 26876-86 GOST 26239.5-84 GOST 26239.7-84 GOST 26239.3-84 GOST 25599.4-83 GOST 12226-80 GOST 23402-78 GOST 1429.9-77 GOST 1429.3-77 GOST 1429.5-77 GOST 19014.3-73 GOST 19014.1-73 GOST 17235-71 GOST 16412.5-91 GOST 29012-91 GOST 26528-98 GOST 18897-98 GOST 26529-85 GOST 26614-85 GOST 26239.2-84 GOST 26239.0-84 GOST 26239.8-84 GOST 25947-83 GOST 25599.3-83 GOST 22864-83 GOST 25599.1-83 GOST 25849-83 GOST 25281-82 GOST 22397-77 GOST 1429.11-77 GOST 1429.1-77 GOST 1429.13-77 GOST 1429.7-77 GOST 1429.0-77 GOST 20018-74 GOST 18317-94 STATE STANDARD P 52950-2008 GOST P 52951-2008 GOST 32597-2013 GOST P 56307-2014 GOST 33731-2016 GOST 3845-2017 STATE STANDARD P ISO 17640-2016 GOST 33368-2015 GOST 10692-2015 GOST P 55934-2013 GOST P 55435-2013 STATE STANDARD P 54907-2012 GOST 3845-75 GOST 11706-78 GOST 12501-67 GOST 8695-75 GOST 17410-78 GOST 19040-81 GOST 27450-87 GOST 28800-90 GOST 3728-78 GOST 30432-96 GOST 8694-75 GOST R ISO 10543-99 GOST R ISO 10124-99 GOST R ISO 10332-99 GOST 10692-80 GOST R ISO 17637-2014 GOST P 56143-2014 GOST R ISO 16918-1-2013 GOST R ISO 14250-2013 GOST P 55724-2013 GOST R ISO 22826-2012 GOST P 55143-2012 GOST P 55142-2012 GOST R ISO 17642-2-2012 GOST R ISO 17641-2-2012 GOST P 54566-2011 GOST 26877-2008 GOST R ISO 17641-1-2011 GOST R ISO 9016-2011 GOST R ISO 17642-1-2011 STATE STANDARD P 54790-2011 GOST P 54569-2011 GOST P 54570-2011 STATE STANDARD P 54153-2010 GOST R ISO 5178-2010 GOST R ISO 15792-2-2010 GOST R ISO 15792-3-2010 GOST P 53845-2010 GOST R ISO 4967-2009 GOST 6032-89 GOST 6032-2003 GOST 7566-94 GOST 27809-95 GOST 22974.9-96 GOST 22974.8-96 GOST 22974.7-96 GOST 22974.6-96 GOST 22974.5-96 GOST 22974.4-96 GOST 22974.3-96 GOST 22974.2-96 GOST 22974.1-96 GOST 22974.13-96 GOST 22974.12-96 GOST 22974.11-96 GOST 22974.10-96 GOST 22974.0-96 GOST 21639.9-93 GOST 21639.8-93 GOST 21639.7-93 GOST 21639.6-93 GOST 21639.5-93 GOST 21639.4-93 GOST 21639.3-93 GOST 21639.2-93 GOST 21639.0-93 GOST 12502-67 GOST 11878-66 GOST 1763-68 GOST 13585-68 GOST 16971-71 GOST 21639.10-76 GOST 2604.1-77 GOST 11930.7-79 GOST 23870-79 GOST 11930.12-79 GOST 24167-80 GOST 25536-82 GOST 22536.2-87 GOST 22536.11-87 GOST 22536.6-88 GOST 22536.10-88 GOST 17745-90 GOST 26877-91 GOST 8233-56 GOST 1778-70 GOST 10243-75 GOST 20487-75 GOST 12503-75 GOST 21548-76 GOST 21639.11-76 GOST 2604.8-77 GOST 23055-78 GOST 23046-78 GOST 11930.11-79 GOST 11930.1-79 GOST 11930.10-79 GOST 24715-81 GOST 5639-82 GOST 25225-82 GOST 2604.11-85 GOST 2604.4-87 GOST 22536.5-87 GOST 22536.7-88 GOST 6130-71 GOST 23240-78 GOST 3242-79 GOST 11930.3-79 GOST 11930.5-79 GOST 11930.9-79 GOST 11930.2-79 GOST 11930.0-79 GOST 23904-79 GOST 11930.6-79 GOST 7565-81 GOST 7122-81 GOST 2604.3-83 GOST 2604.5-84 GOST 26389-84 GOST 2604.7-84 GOST 28830-90 GOST 21639.1-90 GOST 5640-68 GOST 5657-69 GOST 20485-75 GOST 21549-76 GOST 21547-76 GOST 2604.6-77 GOST 22838-77 GOST 2604.10-77 GOST 11930.4-79 GOST 11930.8-79 GOST 2604.9-83 GOST 26388-84 GOST 14782-86 GOST 2604.2-86 GOST 21639.12-87 GOST 22536.8-87 GOST 22536.0-87 GOST 22536.3-88 GOST 22536.12-88 GOST 22536.9-88 GOST 22536.14-88 GOST 22536.4-88 GOST 22974.14-90 GOST 23338-91 GOST 2604.13-82 GOST 2604.14-82 GOST 22536.1-88 GOST 28277-89 GOST 16773-2003 GOST 7512-82 GOST 6996-66 GOST 12635-67 GOST 12637-67 GOST 12636-67 GOST 24648-90

GOST R 56307−2014 Silver. Method of atomic-emission analysis with spark excitation spectrum


GOST R 56307−2014


NATIONAL STANDARD OF THE RUSSIAN FEDERATION

SILVER

Method of atomic-emission analysis with spark excitation spectrum

Silver. Method of spark atomic-emission analysis


OKS 39.060

Date of introduction 2015−07−01


Preface

1 DEVELOPED by the Open joint-stock company «Prioksky factory of nonferrous metals», Open joint stock company «Krasnoyarsk factory of nonferrous metals named after V. N. Gulidova», State scientific center State scientific-research and design Institute of rare metals industry «Giredmet"

2 SUBMITTED by the Technical Committee on standardization TC 304 «Noble metals, alloys, industrial jewelry products, secondary resources containing noble metals"

3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology of December 12, 2014 N 1991-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 applies to silver with a mass fraction of silver is not less than 99.5%.

The standard specifies atomic emission (spark excitation and photoelectric registration of spectrum) method for the determination of impurities, aluminum, bismuth, gallium, indium, Germany, iron, gold, indium, cadmium, cobalt, silicon, magnesium, manganese, copper, arsenic, Nickel, tin, palladium, platinum, rhodium, lead, selenium, sulfur, antimony, tellurium, titanium, chromium, zinc in silver. Requirements to chemical composition set in silver GOST 28595.

2 Normative references


This standard uses the regulatory references to the following standards:

GOST R 8.563−2009 State system for ensuring the uniformity of measurements. Techniques (methods)of measurements

GOST R ISO 5725−1-2002 Accuracy (trueness and precision) of methods and measurement results. Part 1. General provisions and definitions

GOST R ISO 5725−2-2002 Accuracy (trueness and precision) of methods and measurement results. Part 2. The basic method for the determination of repeatability and reproducibility of a standard measurement method

GOST R ISO 5725−3-2002 Accuracy (trueness and precision) of methods and measurement results. Part 3. Intermediate indicators the precision of a standard measurement method

GOST R ISO 5725−4-2002 Accuracy (trueness and precision) of methods and measurement results. Part 4. The main methods of determining the correctness of a standard measurement method

GOST R ISO 5725−6-2002 Accuracy (correctness and precision) of methods and measurement results. Part 6. The use of precision values in practice

GOST R 52361−2005 Control of the analytical object. Terms and definitions

GOST R 52599−2006 Precious metals and their alloys. General requirements for methods of analysis

GOST R 53228−2008 Scales non-automatic actions. Part 1. Metrological and technical requirements. Test

GOST 5556−81 Wool medical hygroscopic. Specifications

GOST 6709−72 distilled Water. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 18300−87 ethyl rectified technical. Specifications

GOST 28595−90 Silver bullion. Specifications

GOST 29298−2005 cotton and mixed household. General specifications

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 Terms and definitions


This standard applies the terminology according to GOST R ISO 5725−1, GOST R 8.563, GOST R 52361 and recommendations [1].

4 the essence of the method


The method of analysis is based on the evaporation and excitation of the atoms of the sample in the spark discharge, the photoelectric registration of spectrum, measuring the intensity of the analytical lines of the determined elements-impurities and the background, and the subsequent determination of content of impurities in the calibration characteristics. The method allows to determine the mass fraction of impurity elements in the ranges shown in table 1, with indicators of the accuracy of the method of analysis specified in table 2.


Table 1 — Ranges of definition of mass fraction of impurity elements

Percentage

   
The name of the element
The range of definition of mass fraction
Aluminium
From 0,0002 0,0050 to incl.
Bismuth
From of 0.0002 to 0.010 is incl.
Gallium
From 0,0002 0,0050 to incl.
Germanium
From to 0,0002 0,0030 incl.
Iron
From from 0.0002 to 0.020 incl.
Gold
From the 0.0003 to 0.020 incl.
Indium
From 0.0005 to 0,0050 incl.
Cadmium
From 0,0003 0,010 to incl.
Cobalt
From of 0.0002 to 0.010 is incl.
Silicon
From to 0,0002 0,0030 incl.
Magnesium
From of 0.0002 to 0.010 is incl.
Manganese
From of 0.0002 to 0.010 is incl.
Copper
From 0.0001 to 0.020 incl.
Arsenic
From 0.0005 to 0,010 incl.
Nickel
From 0.0001 to 0,010 incl.
Tin
From from 0.0002 to 0.020 incl.
Palladium
From from 0.0002 to 0.020 incl.
Platinum
From the 0.0003 to 0.020 incl.
Rhodium
From to 0,0002 0,0030 incl.
Lead
From 0,0003 0,010 to incl.
Selenium
From 0,0003 0,010 to incl.
Sulfur
From 0.0005 to 0,010 incl.
Antimony
From of 0.0002 to 0.010 is incl.
Tellurium
From 0.0005 to 0,010 incl.
Titan
From to 0,0002 0,0030 incl.
Chrome
From 0.0001 to 0,0050 incl.
Zinc
From the 0.0003 to 0.020 incl.

5 Accuracy (trueness and precision) of the method

5.1 indicators of the accuracy of the method

Indicators of accuracy of the method according to the GOST R ISO 5725−2, GOST R ISO 5725−3: the boundaries of the interval in which with a probability ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраof 0.95 is the absolute error of the results of the analysis (assigned error) ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, standard deviation of repeatability ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраand intermediate precision ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, the values of the critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, intermediate precision ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраand reproducibility limit ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраdepending on the mass fraction of the element-impurities are shown in table 2.


Table 2 — Indicators of accuracy of the method when ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраp = 0.95

Percentage

             
The level of the mass fraction determination
given elements

The boundaries of the interval of absolute error ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

The standard deviation of repeatability ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

The critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

The standard deviation of intermediate precision ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

Limit intermediate pretsizion-
ness ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

Limit to play DVDs. -
clarification ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра

0,00010
Of 0.00006 0,00003 0,00010 0,00003 0,00008 0,00010
0,00030
0,00015 Of 0.00006 0,00024 0,00007 0,00019 0,00026
0,00050
0,00025 0,00010 0,00036 0,00013 0,00037 Is 0 00 045
0,0010
0,0004 0,00011 0,0004 0,00022 About 0.0006 0,0007
0,0030
0,0008 0,0003 0,0011 0,0004 0,0011 0,0013
0,0050
0,0015 About 0.0006 0,0022 0,0007 0,0019 0,0023
0,010
0,002 0,0010 0,004 0,0014 0,004 0,005
0,020
0,005 0.0016 inch 0,006 0,0024 0,007 0,008

5.2 Correctness

To estimate the systematic error of the present method of determining the elements of the impurities in the silver is used as a reference certified value mass fraction of elements in the state standard samples (GSO) composition silver GEO 7817 (set SN) or other GEO, whose set of designated elements-impurities and metrological characteristics.

Systematic error of the method at a significance level of ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра5% according to GOST R ISO 5725−4на all defined levels of mass fraction of impurity elements in silver insignificant.

5.3 Precision

5.3.1 Range (ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра) four results of determinations obtained for the same sample by one operator using the same equipment within the shortest possible time intervals that may exceed the specified in table 2, the critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраfor ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра4 on average not more than once in 20 cases.

5.3.2 within one laboratory two results of the analysis of the same sample obtained in accordance with sections 7−10 of this standard, different operators using the same equipment on different days, can vary with the excess specified in table 2 of the limit of intermediate precision ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраon the average not more than once in 20 cases.

5.3.3 Results of the analysis of the same samples, obtained in two laboratories, in accordance with sections 7−10 of this standard may vary in excess of the limit of reproducibility ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраindicated in table 2, on average not more than once in 20 cases.

For intermediate values of mass fraction of impurity elements the values of precision find using linear interpolation according to the following formula

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, (1)


where ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — the indicator of the accuracy of the analysis resultГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра;

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраthe values of precision, corresponding to the lower and upper level mass fraction of detectable elements, between which is the result of the analysis;

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — the result of the analysis;

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраvalues of the lower and upper levels of the mass fraction of elements, between which there is the result.

6 Requirements

6.1 General requirements and safety requirements

General requirements for method of analysis, the requirements for security of works — according to GOST R 52599.

6.2 qualifications of performers

The analysis allowed persons over the age of 18, trained in the prescribed manner and allowed to work independently on used equipment.

7 measuring instruments, auxiliary equipment, materials and reagents


Optical emission spectrometer with spark excitation source spectrum and the working wavelength range 120−700 nm, equipped with a computer and appropriate software.

Laboratory scales in accordance with GOST R 53228 with a limit of permissible absolute error of less than ±0.01 g.

Press and mold with a diameter of 40 mm.

Milling machine.

Medical absorbent cotton wool GOST 5556.

Distilled water according to GOST 6709.

Hydrochloric acid according to GOST 14261.

Argon gaseous and liquid GOST 10157.

Cotton fabric according to GOST 29298.

Rectified ethyl alcohol according to GOST 18300.

Standard samples of composition silver GEO 7817 (set SN) or the other WITH equal composition of impurity elements and precision.

Allowed the use of other measurement means, auxiliary devices, materials and reagents, subject to obtaining accuracy rate that rivals those in table 2.

8 Selection and preparation of samples

8.1 Sampling for analysis is carried out in accordance with the requirements of GOST 28595. Requirements for the size and mass of the samples are determined depending on the used spectrometer.

8.2 Samples of silver could enter the analysis in the form of ingots, rods, plates, strips, shavings, sponge, powder.

8.3 Samples in the form of strips, plates, shavings boiled in a solution of hydrochloric acid diluted 1:1 for 3−5 min to remove surface contamination. The resulting solution was decanted, the sample was washed 4−5 times with distilled water by decantation and dried in air.

Samples of the powder and sponge not treated with acid.

8.4 the surface of the rods and plates should be flat, and processed by cutting or grinding, the tape surface should be smooth and without delamination. Samples in the form of a monolithic specimen having not less than one flat surface treated with a milling machine. On the treated surface should be free of holes, scratches, cracks, and slag inclusions.

Directly before analysis allowed samples and standard samples wipe clean with a cloth moistened with alcohol.

8.5 From the sample in the form of chips or powder taken weighed 20−30 g and pressed with a force equal to 600 kN per tablet.

9 Preparation of equipment for measurement


Spectrometer ready to work according to the operating documents of the device.

The recommended mode of operation of the spectrometer:

the discharge frequency of 300 Hz;

— capacity — (2−5) UF

— inductance — µh 130;

— purging with argon — 3.

The wavelengths of the analytical lines, background, and line of internal standard is recommended to perform the analysis shown in table 3.


Table 3 — wavelengths of the analytical lines

In nanometers

   
The name of the element
Wavelength of analytical line
Aluminium
396,153
Bismuth
306,772
Gallium
417,206
Germanium
199,88
Iron
259,940; 372,0
Gold
267,595
Indium
410,177
Cadmium
228,802
Cobalt
345,351
Silicon
288,160
Magnesium
285,213
Manganese
403,499
Copper
324,754
Arsenic
234,984; 189,0
Nickel
361,939
Tin
175,790
Palladium
340,46
Platinum
531,890
Rhodium
343,489
Lead
405,782; 283,307
Selenium
196,1
Sulfur
180,731
Antimony
206,838
Tellurium
214,275; 185,7
Titan
498,173
Chrome
425,435
Zinc
334,502; 213,9
Background
200,860; 310,500
Silver, internal standard
338,289


Note — the use of other modes and the analytical lines subject to receipt of the accuracy rate that rivals those in table 2.

10 measurements


To obtain the calibration dependencies consistently reinforce the cell spark discharge standard samples of composition of silver and laid in the spectrometer’s program, perform measurements of the intensity of the analytical lines of the determined elements, background, and lines the internal standard. For graduation choose three or more standard samples of composition of the silver so that the value of the content of each analyzed element-impurities in the sample was within the range between the highest and lowest values of the mass fraction of this element in the standard samples. For each standard sample perform measurement in four different points of the surface.

The calibration relationships are obtained in the coordinates: the average value of the intensity of the analytical lines of the determined elements (including the background or comparison lines) of the four points of the sample surface — the mass fraction of the element in the standard sample.

Measured intensity of analytical lines of the determined elements, background, and lines the internal standard in four points on the surface of the sample. Embedded in the spectrometer program using a calibration dependencies get four results of parallel measurements in the sample.

11 Evaluation of the acceptability of the results of parallel measurements and obtaining the final result of the analysis


The acceptability of the results of parallel measurements was evaluated in accordance with GOST R ISO 5725−6 by matching range, results (ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра) with the critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, the values of which are given in table 2 or calculated by the formula (1).

If the range of the four results of the parallel definition (aГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра) does not exceed the critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, all the results and recognise acceptable for the final result of the analysis taking the arithmetic mean of the four results of parallel measurements.

If the range of the four results of parallel measurements exceeds ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, spend four parallel determinations.

The critical range is ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраcalculated by the following formula

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, (2)


where ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраis the number of parallel definitions;

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — coefficient depending on the number ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраof individual analysis results, obtained in conditions of repeatability and confidence probability ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраof 0.95. For eight parallel measurements ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраof 4.29;

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — standard deviation of repeatability are given in table 2.

If the received eight results of parallel measurements, the value (ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра) does not exceed the critical range ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, as a final result of the analysis taking the arithmetic mean value of the eight results of parallel measurements. Otherwise, as a final result of the analysis taking the median of the eight results of parallel measurements. The lower bits of the numerical result and the numeric values of the accuracy metrics should be the same.

12 Control of accuracy of analysis results

12.1 Control of intermediate precision and reproducibility

When monitoring intermediate precision (taking into account the influencing factors of time, operator) absolute difference of the two results of the analysis of the same sample obtained by different operators using the same equipment on different days, should not exceed the limit of intermediate precision ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраspecified in table 2 or calculated by the formula (1).

Under the control of the reproducibility of the absolute disparity of the two results of the analysis of the same samples, obtained in two laboratories, in accordance with the requirements of this standard must not exceed the limit of reproducibility ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраshown in table 2 or calculated by the formula (1).

12.2 verification of correct

The checking is carried out by analysis of standard samples (CO) composition silver. The samples used for control of correctness should not be used to obtain the calibration dependencies.

When checking the difference between the analysis result and the accepted reference (certified) value of the content of element impurities in the standard sample should not exceed a critical value ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра.

Critical value ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектраcalculated by the following formula

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра, (3)


where ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — the error of setting the reference (certified) value of mass fraction of element-impurities in.

ГОСТ Р 56307-2014 Серебро. Метод атомно-эмиссионного анализа с искровым возбуждением спектра — the indicator of the accuracy of the analysis result, the corresponding certified value.

Bibliography

     
[1] Recommendations on the interstate
standardization
RMG 61−2003
State system for ensuring the uniformity of measurements. Indicators of accuracy, trueness, precision methods of quantitative chemical analysis



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UDC 669.231:543.06:006.354 OKS 39.060

Keywords: silver, silver bullion, methods of analysis, impurities, atomic emission method of analysis spark excitation spectrum, spark, standard samples of composition, correctness of the method of analysis, precision analysis method, the absolute error, limit of repeatability, limit of intermediate precision, limit of reproducibility, control of accuracy of analysis results