GOST 16273.0-85

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  ГОСТ 16273.0-85

GOST 16273.0−85 Selenium technical. General requirements for method of spectral analysis (with Change No. 1)

GOST 16273.0−85

Group B59

STATE STANDARD OF THE USSR

SELENIUM TECHNICAL

General requirements for method of spectral analysis

Technical selenium. General requirements for method
of spectral analysis

AXTU 1709

Valid from 01.07.86
to 01.07.91*
_______________________________
* Expiration removed
by the resolution of Gosstandart of Russia from 04.06.91 N 782
(IUS N 9, 1991). -
Note the manufacturer’s database.

DEVELOPED by the Ministry of nonferrous metallurgy of the USSR

PERFORMERS

B. M. Rogov, E. N. Gazalov, Yu.N.Semavin, O. D. Ryabkova, E. B. Makovsky

INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

Member Of The Board Of A. P. Snurnikov

APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from January 30, 1985 N 208

REPLACE GOST 16273.0−71


The Change N 1, approved and promulgated by the Order of Rosstandart from 26.11.2014 No. 1773-St c 01.09.2015

Change No. 1 made by the manufacturer of the database in the text IUS N 3, 2015


This standard specifies the General requirements for method of spectral analysis technical selenium.

1A. NORMATIVE REFERENCES

This standard uses the regulatory references to the following international standards:

GOST 8.010−99* State system for ensuring the uniformity of measurements. The techniques of measurements. The main provisions of the
_______________
* On the territory of the Russian Federation GOST R 8.563−2009 «State system for ensuring the uniformity of measurements. Techniques (methods) of measurements».


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 10298−79 Selenium technical. Specifications

GOST 16273.1−2014 Selenium technical. Methods of spectral analysis

GOST 20996.0−2014 Selenium technical. General requirements for methods of measurements

GOST 25086−2011 non-ferrous metals and their alloys. General requirements for methods of analysis

GOST ISO 5725−6-2002** Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice
_______________
** On the territory of the Russian Federation GOST R ISO 5725−6-2002 «Accuracy (trueness and precision) of methods and measurement results. Part 6. The use of precision values in practice».


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 published annually by the information sign «National standards» published as on January 1 of the current year and related information published monthly indexes published in the current year. If the reference standard is replaced (changed), when using this standard should be guided by replacing (amended) standard. If the reference standard is cancelled without replacement, then the situation in which the given link applies to the extent that does not affect this link.


Section 1A. (Added, Rev. N 1).

1B. METHODS OF TESTING THE ACCEPTABILITY OF RESULTS OBTAINED IN CONDITIONS OF REPEATABILITY AND REPRODUCIBILITY

1B.1. The eligibility check results of parallel measurements obtained in conditions of repeatability, carry out in the preparation of each measurement result of the working samples.

1B.2. Procedure for checking the admissibility of the results of parallel measurements involves comparing the absolute differences between the highest and lowest -the single measurements (assays) , performed in accordance with the method of measurement, limit of repeatability .

If the condition

, (1)

for the result measurements, take the average value of single measurements (1, …, ).

If condition (1) is not satisfied, perform the procedure described in 1B.3.

1B.3. Receive parallel definitions, if the measurement procedure is not expensive, and 1 if the measurement procedure is expensive.

For the outcome measurements take the average value of single measurements under the condition of

, (2)

where is the maximum of single measurements;

 — minimum of single measurements;

 — the critical range for the number of single measurements .

The critical range is calculated by the formula

, (3)

where  — coefficient, which depends on the number of single measurements obtained under conditions of repeatability and confidence . Coefficient values for the acceptance probability of 0.95 is given in table 1;

 — Standard deviation of repeatability calculated by the formula

, (4)

where is the limit of repeatability;

 — coefficient which depends on the accepted probability and the number of parallel measurements .

Values are given in table 1 for the adopted probability of 0.95.

Table 1

1B.4. If the condition (3) is not fulfilled, you must find out the causes resulting in unacceptable measurement results, and take action to correct the final measurement result can be accepted by the median of the single measurements.

1B.5. The discrepancy between the results of measurements obtained in two laboratories, should not exceed the limit of reproducibility. If this condition is acceptable both measurement and as a final can be used their common arithmetic mean value.

If you exceed the limit of reproducibility can be used methods for assessing the acceptability of the results of measurements according to GOST ISO 5725−6.

1B.6. When checking the admissibility of the two measurement results obtained by one method of measurement with different values of precision (if the interval representation), limit of repeatability , intermediate precision and reproducibility is calculated according to the formulas:

, (5)

where and  — the limits of repeatability corresponding to the values determined by the component in the sample;

, (6)

where and  — the limits of intermediate precision;

, (7)

where and indicators of reproducibility.

Section 1B. (Added, Rev. N 1).

1B. ACCURACY CONTROL OF MEASUREMENT RESULTS IN THE LABORATORY

1B.1. Accuracy control of measurement results within a laboratory exercise for measurement procedures with established indices of accuracy (correctness and precision) and approved for use in the prescribed manner in accordance with GOST 8.010.

1B.2. During the implementation of the measurement methods in the laboratory provide operational control of the measurement procedure and control of stability of measurement results.

Algorithm for operational control procedures measurement result in the internal documents of the laboratory.

Control procedures stability measurements reglamentary in the documents of the laboratory.

1B.3. As a means of control can be used:

— samples for control (s): standard samples (SS) according to GOST 8.315 or certified mixture (AC) [3];

— working samples with known additive detectable component;

— working samples of a stable composition;

— work samples, diluted in a specific ratio;

— other methods of measurement with the established indices of accuracy (control of measurement).

1B.4. Control of measurement procedures with the use of OK is to compare the result of the control determining the certified properties of the specimen to control with the certified value in [2]. At the same time OK must be adequate to the analyzed samples (possible differences in the compositions of the analyzed samples should not contribute to the measurement results statistically significant error). The error of the certified value of CR should be not more than one-third of the accuracy specifications of the measurement results.

If during the inspection, apply the OK, which are not used for establishing the measure of the accuracy of measurement results in case of exceeding the error of the OK one third of the error of measurement allowed the ratio control is calculated by the formula

, (8)

where  — error certified value is OK;

 — the indicator of the accuracy of measurement results corresponding to the certified value approx.

The calibration feature recognize stable under the condition:

, (9)

where is the certified value of the mass concentration of the component in the calibration sample;

 — was found in the calibration chart value of the mass concentration of the component in the calibration sample;

the value of the standard stability control calibration curve established in the laboratory by construction of calibration curve.

1B.5. Operational control procedures measurement using the method supplements test method of measurement method or sample dilution implemented in accordance with the algorithms given in [2]. Allowed to use other methods of operational control of the measurement procedure.

1B.6. To check the stability of the measurement results within the lab using the control procedure according to GOST ISO 5725−6 [2].

Section 1B. (Added, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements — according to GOST 20996.0, GOST 25086 with additions.

(Changed edition, Rev. N 1).

1.1.1. The selection and preparation of samples for analysis — according to GOST 10298−79.

1.1.2. With the aim of selective feature definition requires the choice of analytical spectral lines free of blending lines of the matrix chemical composition of the sample.

1.1.3. In the definition by the method of atomic emission (flame photometry) wavelength, the composition of the gas flame, a reducing or oxidizing action of the flame, turn the burner and other measurement conditions are chosen to achieve optimal measurement sensitivity and accuracy for the relevant component and device.

1.1.4. When using measurement techniques (GOST 16273.1) subject to the achievement of the metrological characteristics specified in the measurement technique allowed:

— to use when measuring different resonance spectral lines;

— use automated build system calibration charts, measurements in automated mode with the results of the measurements on paper or electronic media;

— consistently determine multiple components in one test portion of the sample after decomposition and appropriate dilution of the sample solution so that the mass concentration (mass) detectable component therein was in the range of mass concentrations (mass) calibration curve.

1.1.2−1.1.4 (Revised edition, Edit. N 1).

1.1.5. Mass fraction of impurities determined in batches equal to the parallel definitions, the number of which is specified in a particular method of measurement, but at least two. Simultaneously with the measurements in the same conditions conduct control experience for making the appropriate corrections in the measurement result. In the determination of impurities the number of parallel definitions in a control experiment it should correspond to the number of parallel measurements specified in method of measurement.

(Added, Rev. N 1).

2. SAFETY REQUIREMENTS

Safety requirements — according to GOST and GOST 25086 20996.0.

Section 2. (Changed edition, Rev. N 1).

Bibliography

Bibliography (added, Rev. N 1).