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GOST 13047.14-2014

GOST 13047.14−2014 Nickel. Cobalt. Methods for determination of bismuth


GOST 13047.14−2014

INTERSTATE STANDARD


NICKEL. COBALT

Methods for determination of bismuth

Nickel. Cobalt. Methods for determination of bismuth


ISS 77.120.40

Date of introduction 2016−01−01


Preface

Goals, basic principles and procedure of works on interstate standardization have been established in GOST 1.0−92 «interstate standardization system. Basic provisions» and GOST 1.2−2009 «interstate standardization system. Interstate standards, rules and recommendations on interstate standardization. Rules of development, adoption, application, renewal and cancellation"

Data on standard

1 DEVELOPED by interstate technical committees for standardization MTK 501 Nickel and MTC 502 «Cobalt"

2 as AMENDED by the Federal Agency for technical regulation and Metrology (Rosstandart)

3 ACCEPTED by the Interstate Council for standardization, Metrology and certification (Protocol of October 20, 2014 N 71-N)

The adoption voted:

     
Short name of the country on MK (ISO 3166) 004−97 Country code
MK (ISO 3166) 004−97
Abbreviated name of the national authority for standardization
Azerbaijan
AZ Azstandart
Armenia
AM Ministry Of Economy Of The Republic Of Armenia
Belarus
BY Gosstandart Of The Republic Of Belarus
Georgia
GE Gosstandart
Kazakhstan
KZ Gosstandart Of The Republic Of Kazakhstan
Kyrgyzstan
KG Kyrgyzstandard
Russia
EN Rosstandart
Tajikistan
TJ Tajikstandart
Uzbekistan
UZ Uzstandard

4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St inter-state standard GOST 13047.14−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.14−2002


Information about the changes to this standard is published in the annual reference index «National standards», and the 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 the monthly 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

1 Scope


This standard specifies the spectrophotometric and atomic absorption methods for the determination of bismuth (with bismuth mass fraction of from 0.0001% to 0,010%) in the primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on. As an arbitration method is atomic absorption method.

2 Normative references


This standard uses the regulatory references to the following standards:

GOST 123−2008 Cobalt. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 4232−74 Reagents. The potassium iodide. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5457−75 Acetylene, dissolved and gaseous. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 10928−90 Bismuth. Specifications

OST* 11125−84 nitric Acid of high purity. Specifications
________________
* Probably, the error of the original. Should read: GOST 11125−84. — Note the manufacturer’s database.


GOST 13047.1−2014 Nickel. Cobalt. General requirements for methods of analysis

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 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.

3 General requirements and safety requirements


General requirements for methods of analysis used by the quality of distilled water and laboratory glassware and safety at work — according to GOST 13047.1.

4 a spectrophotometric method (at a mass fraction of bismuth from of 0.0002% to 0.001%)

4.1 Method of analysis


The analysis method is based on measurement of light absorption at a wavelength of 540 nm of a solution of complex compounds of bismuth with selenology orange after pre-extraction of bismuth in the form of godenovo complex compounds with isoamyl acetate.

4.2 measuring instruments, auxiliary devices, materials, reagents and solutions


Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 500 to 560 nm.

pH meter (ion meter) for measurements in the pH range from 1.4 to 1.5.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125 diluted 1:1, molar concentration of solutions 1 mole/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаand 0.03 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

The Stripping solution is prepared as follows: to the nitric acid molar concentration of 0.03 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаadd drop by drop nitric acid molar concentration of 1 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаto establish the pH of the solution in the range from 1.4 to 1.5.

Ascorbic acid of the Pharmacopoeia [1]*, the solution of the mass concentration of 0.05 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.
________________
* See Bibliography. — Note the manufacturer’s database.


Potassium iodide according to GOST 4232, solution mass concentration of 0.02 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

Bismuth GOST 10928.

Selenology orange, solution mass concentration of 0.001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

Isoamyl ether acetic acid (isoamyl acetate) at [2].

Bismuth solutions of known concentration.

The solution And the mass concentration of bismuth of 0.001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis prepared as follows: a sample of bismuth by weight 0,5000 g placed in a beaker with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow from 30 to 40 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, dissolved by heating, boil for 2−3 min, cooled, transferred to a volumetric flask with a capacity of 500 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, 50 cm pourГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаnitric acid, diluted 1:1, adjusted to the mark with distilled water.

Solution B mass concentration of bismuth 0.0001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis prepared as follows: into a measuring flask with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаtransfer 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof solution A, pour 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, adjusted to the mark with distilled water.

Solution of the mass concentration of bismuth 0,000005 g/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis prepared as follows: into a measuring flask with a capacity of 100 cm andГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаstand 5 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof solution B and bring to the mark with nitric acid molar concentration of 1 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

4.3 Preparation for analysis


To build a calibration curve in a separating funnel with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаstand 0,5; 1,0; 2,0; 4,0 and 6,0 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаsolution, poured to a volume of 40 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid molar concentration of 1 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, 1.0 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof potassium iodide solution and further carried out the analysis in accordance with 4.4.

The mass of bismuth in the calibration solutions is 0,0000025; 0,0000050; 0,0000100; 0,0000200 and 0,0000300 G.

The light absorption values of the calibration solutions and corresponding masses of bismuth build the calibration graph, given the values of absorption of the calibration solution, is prepared without introducing a solution containing bismuth.

4.4 analysis


A portion of the sample with a mass of 3,000 g were placed in a glass with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow from 30 to 40 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, is dissolved when heated, is evaporated to a volume of 5 to 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow 15 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof distilled water and transfer the solution into a separating funnel with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута. Pour distilled water to a volume of 40 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, 1.0 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof potassium iodide solution, 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof isoamyl acetate and extracted with 1 min. the Aqueous lower phase is transferred into a clean separatory funnel with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, pour 5 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof isoamyl acetate and repeating the extraction 1 min. the Aqueous phase is discarded and the organic phases combined.

To the combined organic phase poured 20 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid molar concentration of 1 mol/DMГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, 0.5 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof a solution of ascorbic acid, 0.5 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof potassium iodide solution and gently turning funnel five or six times, washed the organic phase. The aqueous phase is discarded, wash the organic phase again. To the washed organic phase poured 15 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof the solution for Stripping, 0.2 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаkylinalove orange funnel and shake for 1 min. the Aqueous phase is transferred to a volumetric flask with a capacity of 25 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, filtering it through a funnel with a cotton swab, pre-washed with a solution for Stripping. After filtration, the swab is washed with a solution for Stripping and bring to mark with a solution for Stripping.

Light absorption of solutions of the sample and the reference experiment is measured after 20 minutes on the spectrophotometer at a wavelength of 540 nm or photoelectrocolorimeter in the wavelength range from 500 to 560 nm. As a comparison, using a solution of distilled water and the cell thickness of the absorbing layer of 5 cm.

The value of the light absorption of the sample solution find the mass of bismuth on the calibration schedule.

4.5 Processing the analysis results


Mass fraction of bismuth in the sample X, %, is calculated by the formula

ГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, (1)


where M ГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута — the mass of bismuth in the sample solution, g;

MГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis the mass of bismuth in the solution in the reference experiment, g;

M — weight of sample, g.

4.6 Control of accuracy of analysis results


Control of accuracy of analysis results is carried out according to GOST 13047.1.

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are shown in table 1.


Table 1 — Requirements of control precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis at a confidence probability P=0,95

Percentage

         
Mass fraction of bismuth The limit of repeatability (two results of parallel measurements), r The limit of repeatability (for three results of parallel measurements), r
The limit of reproducibility (for two results of the analysis), R The expanded uncertainty U (k=2)
0,00020 Of 0.00006 0,00007 0,00012
0,00008
0,00030 0,00008
0,00010 0,00015 0,00010
0,00050
0,00010 0,00012 0,00020 0,00015
0,00100
0,00020 0,00024 0,00040 0,00030

5 Atomic absorption method with electrothermal atomization (at a mass fraction of bismuth from 0.0001% to 0.001%)

5.1 Method of analysis


The analysis method is based on measurement of absorption at a wavelength of 223,1 nm resonance radiation by atoms of bismuth resulting from the electrothermal atomization of the sample solution.

5.2 measurement Means, auxiliary devices, materials, reagents and solutions


Atomic absorption spectrometer for 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 bismuth.

Argon gas according to GOST 10157.

Filters obestochennye in [3] or other filter medium density.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1, 1:9.

Nickel powder according to GOST 9722 or standard sample of Nickel pre-installed (certified) mass fraction of bismuth is not more than 0.0001%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of bismuth is not more than 0.0001%.

Bismuth GOST 10928.

Bismuth solutions of known concentration.

The solution And the mass concentration of bismuth of 0.001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаat 4.2.

Solution B mass concentration of bismuth 0.0001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаat 4.2.

Solution of the mass concentration of bismuth 0,00001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis prepared as follows: into a measuring flask with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаtransfer 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof a solution, pour 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, adjusted to the mark with distilled water.

The solution G of the mass concentration of bismuth 0,000001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis prepared as follows: into a measuring flask with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаtransfer 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof the solution, pour 10 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, adjusted to the mark with distilled water.

5.3 Preparation for assay


To build a calibration chart, a portion of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 0,500 g was placed in a beaker or flask with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута. The number of batches must match the number of points of calibration curve, including Supervisory experience.

The suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in 15−20 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1. When using the Nickel powder in the slurries was filtered through a filter (red or white ribbon), washed two or three times with nitric acid, diluted 1:9. The filters are washed two or three times with hot distilled water. The solutions were evaporated to a volume of 10 to 15 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow from 40 to 50 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof distilled water, heated to boiling, cooled and transferred to volumetric flasks with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

Flasks poured 0,5; 1,0; 2,0; 3,0; 4,0 and 5,0 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof the solution In the flask with the solution in the reference experiment, the solution containing the bismuth, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 5.4.

The mass of bismuth in the calibration solutions is 0,0000005; 0,0000010; 0,0000020; 0,0000030; 0,0000040 and 0,0000050 G.

5.4 analysis

A portion of sample weighing 0,500 g was placed in a beaker or flask with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow 15 to 20 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, is dissolved when heated, is evaporated to a volume of 5 to 7 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, transferred to a volumetric flask with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, cooled and adjusted to the mark with distilled water.

The absorbance of the sample solution and the calibration solutions at a wavelength of 223,1 nm, slit width less than 0.5 nm with the correction non-selective absorption in the current of argon is measured at least two times, sequentially spraying them in an atomizer. Depending on the type of spectrometer to select the optimal amount of solution injected into the atomizer, from 0.010 to 0.050 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаor optimal time of the aerosol spraying of the solution from 5 to 50 C. Washed the spray system with distilled 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 in accordance with 5.3.

Selection of optimal temperature regimes for the atomizer is carried out individually for the used spectrometer for the calibration solutions.

Recommended operating conditions of the atomizer are shown in table 2.


Table 2 — operating conditions of the atomizer

                 
The name of the stage
Temperature, °C Time
Drying
120 to 150 incl. 2 to 20 incl.
Ashing
«700 « 900 « «10 « 20 «
Atomization «2000 « 2400 « «4 « 5
«


The values of absorption of the calibration solutions and corresponding masses of bismuth build the calibration graph.

The value of absorbance of sample solution find the mass of bismuth on the calibration schedule.

5.5 Processing of analysis results


Mass fraction of bismuth in the sample X, %, is calculated by the formula

ГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, (2)


where MГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаis the mass of bismuth in the sample solution, g;

M — weight of sample, g.

5.6 Control of accuracy of analysis results


Control of accuracy of analysis results is carried out according to GOST 13047.1.

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are shown in table 3.


Table 3 — Requirements of control precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis at a confidence probability P=0,95

Percentage

         
Mass fraction of bismuth The limit of repeatability (for two results of parallel measurements), r
The limit of repeatability (for three results of parallel measurements), r
The limit of reproducibility (for two results of the analysis), R The expanded uncertainty U (k=2)
0,00010
0,00003 0,00004 Of 0.00006 0,00004
0,00020
0,00004 0,00005 0,00008 0,00008
0,00030
0,00005 Of 0.00006 0,00010 0,00007
0,00040
Of 0.00006 0,00007 0,00012 0,00008
0,00050
0,00007 0,00009 0,00014 0,00010
0,00060
0,00008 0,00010 0,00017 0,00012
0,00100
0,00015 0,00020 0,00030 0,00020

6 Atomic absorption method with flame atomization (at a mass fraction of bismuth from 0.002% to 0,010%)

6.1 Method of analysis


The method is based on measuring absorption at a wavelength of 223,1 nm resonance radiation by atoms of bismuth resulting from the fiery atomization when spraying a solution of the sample in the flame acetylene-air.

6.2 measurement Means, auxiliary devices, materials, reagents and solutions


Atomic absorption spectrometer for measurements in the flame acetylene-air.

Lamp with hollow cathode for the excitation of spectral lines of bismuth.

Acetylene gas according to GOST 5457.

Filters obestochennye in [3] or other filter medium density.

Nitric acid according to GOST 4461, if necessary, purified by distillation, or according to GOST 11125, diluted 1:1, 1:9.

Nickel powder according to GOST 9722 or standard sample of Nickel pre-installed (certified) mass fraction of bismuth is not more than 0,002%.

Cobalt GOST 123 or standard sample of cobalt pre-installed (certified) mass fraction of bismuth is not more than 0,002%.

Bismuth GOST 10928.

Bismuth solutions of known concentration.

The solution And the mass concentration of bismuth of 0.001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаat 4.2.

Solution B mass concentration of bismuth 0.0001 g/cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаat 4.2.

6.3 Preparation for analysis


To build a calibration chart, a portion of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt with a mass of 3,000 g were placed in a glass or flask with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута. The number of batches must match the number of points of calibration curve, including Supervisory experience.

The suspension of Nickel powder or cobalt or of a standard sample of composition of Nickel or cobalt is dissolved by heating in 25−30 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1. When using the Nickel powder in the solution was filtered through a filter (red or white ribbon), washed two or three times with nitric acid, diluted 1:9. The filters are washed two or three times with hot distilled water. The solutions were evaporated to a volume of 10 to 15 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow from 40 to 50 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof distilled water, heated to boiling, cooled and transferred to volumetric flasks with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута.

Flasks poured 0,5; 1,0; 2,0; 3,0 and 4,0 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof solution B. the flask with the solution in the reference experiment, the solution containing the bismuth, not poured, adjusted to the mark with distilled water and measure the absorbance in accordance with 6.4.

The mass of bismuth in the calibration solutions is 0,00005; 0,00010; 0,00020; and 0,00040 0,00030 g.

6.4 analysis


A portion of the sample with a mass of 3,000 g were placed in a glass or flask with a capacity of 250 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, was dissolved with heating in 25−30 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof nitric acid, diluted 1:1, boiled for 2−3 min, evaporated to a volume of 10 to 15 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмута, flow from 40 to 50 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаof distilled water, heated to boiling and cooled. The solution is transferred to volumetric flasks with a capacity of 100 cmГОСТ 13047.14-2014 Никель. Кобальт. Методы определения висмутаand adjusted to the mark with distilled water.

The absorbance of the sample solution and the calibration solutions at a wavelength of 223,1 nm, slit width of 0.3 nm measured at least two times, sequentially spraying them in the flame acetylene-air, spray rinsed the system with distilled water, check the zero point and the stability of the calibration curve. To check the zero point of the solution is used in the reference experiment, prepared in accordance with 6.3.

According to the obtained values of absorbance of the calibration solutions and corresponding masses of bismuth build the calibration graph.

The value of absorbance of sample solution find the mass of bismuth on the calibration schedule.

6.5 Processing of analysis results


Mass fraction of bismuth in the sample X, %, is calculated by the formula (2).

6.6 Control of accuracy of analysis results


Control of accuracy of analysis results is carried out according to GOST 13047.1.

The regulations control the precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis are given in table 4.


Table 4 — Specifications of control precision (limits of repeatability and reproducibility) and the rate control accuracy (expanded uncertainty) of the results of the analysis at a confidence probability P=0,95

Percentage

         
Mass fraction of bismuth The limit of repeatability (for two results of parallel measurements),r
The limit of repeatability (for three results of parallel measurements), r
The limit of reproducibility (for two results of the analysis), R The expanded uncertainty U (k=2)
0,0020 0,0002
0,0003 0,0004 0,0003
0,0030 0,0004
0,0005 0,0007 0,0005
0,0050 About 0.0006
0,0007 0,0012 0,0008
0,0100 0,0010
0,0012 0,0020 0,0015

Bibliography

     
[1] FS 42−2662 (8)-89 (95)*
(Register of medicines in Russia. M., 1993, Informiam)
Ascorbic acid USP
______________
* The document is not given. For additional information, please refer to the link. — Note the manufacturer’s database.
[2] THAT 6−09−06−1229−85** Isoamyl ether acetic acid (isoamyl acetate), H. h
________________
** The one referred to here and hereinafter, not shown. For additional information, please refer to the link. — Note the manufacturer’s database.
[3] THAT 6−09−1678−95*** Obestochennye filters (white, red, blue tape)

________________
*** Valid on the territory of the Russian Federation.

     
UDC 669.24/.25:543.06:006.354
ISS 77.120.40  
Key words: Nickel, cobalt, bismuth, chemical analysis, mass fraction, measuring tools, solution, reagent, sample, calibration curve, the result of the analysis, the calculation of the control