GOST 13047.9−2014

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  ГОСТ 13047.9-81

GOST 13047.9−2014 Nickel. Cobalt. Method of determination of phosphorus

GOST 13047.9−2014

INTERSTATE STANDARD

NICKEL. COBALT

Method of determination of phosphorus

Nickel. Cobalt. Method for determination of phosphorus

ISS 77.120.40

Date of introduction 2016−01−01

Preface

Goals, basic principles and main procedure of works on interstate standardization established 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:

4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St interstate standard GOST 13047.9−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 INSTEAD of GOST 13047.9−2002


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 method for the determination of phosphorus (at a mass fraction of phosphorus from of 0.0002% to 0.005%) in the primary in Nickel GOST 849 and in cobalt GOST 123.

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 2603−79 Reagents. Acetone. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 3765−78 Reagents. Ammonium molybdate. Specifications

GOST 4198−75 Reagents. Potassium phosphate odnosemjannyj. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 6006−78 Reagents. Butanol-1. Specifications

GOST 6016−77 Reagents. Alcohol isobutyl. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

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

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 18300−87 ethyl rectified technical. Specifications

GOST 20015−88 Chloroform. Specifications

GOST 20490−75 Reagents. Potassium permanganate. 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 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

4.1 Method of analysis

The method is based on measuring light absorption at a wavelength of from 610 to 720 nm of the solution integrated the molybdophosphoric compounds, tin dichloride restored, after a preliminary extraction of isobutyl alcohol or a mixture of butyl alcohol and chloroform of the rate environment.

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

Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 590 to 630 nm or from 700 nm to 740 nm.

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

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation or GOST 14261, diluted 1:1 or 1:9.

Acid chloride in [1], diluted 1:9.

Filters obestochennye [2]* or other thick filters.
________________
* See Bibliography. — Note the manufacturer’s database.


Ammonium molybdate according to GOST 3765 recrystallized and solution mass concentration of 0.1 g/cm.

The recrystallized ammonium molybdate is prepared as follows: a sample of ammonium molybdate with a mass of 70.0 g were placed in a glass with a capacity of 600 or 1000 cm, pour 400 cmof distilled water, dissolved by heating from 70 °C to 80 °C, filtered through a filter (white or blue ribbon), heated and filtered again. To the hot solution was poured 250 cmof ethyl alcohol, cooled, kept for at least 1 h and filtered off the crystalline precipitate in the porcelain filtering funnel. The precipitate is washed two or three times with ethanol at 20−30 cmand dried in air.

Potassium permanganate according to GOST 20490, solution mass concentration of 0.003 g/cm.

Potassium phosphate according to GOST 4198, dried at a temperature of from 100 °C to 110 °C.

Tin dichloride [3].

Solution 1 mass of tin dichloride concentration 0.02 g/cmin hydrochloric acid, diluted 1:1.

A solution of 2 mass concentration of tin dichloride 0.002 g/cmin hydrochloric acid, diluted 1:9.

The technical rectified ethyl alcohol according to GOST 18300.

The 1-butanol (butyl alcohol) according GOST 6006.

Isobutyl alcohol according to GOST 6016.

Acetone according to GOST 2603.

The chloroform GOST 20015 or Pharmacopoeia [4].

The mixture for the extraction is prepared as follows: mix three volumes of chloroform and two volume of butyl alcohol.

Solutions of known phosphorus concentration.

Solution, And the mass of the phosphorus concentration 0.0001 g/cmis prepared as follows: a suspension of potassium phosphate mass 0,4394 g were placed in a glass with a capacity of 250 cm, is dissolved in a volume of 80 to 100 cmof distilled water, transferred to a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass concentration of phosphorus 0,00001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof the solution, and adjusted to the mark with distilled water.

Solution of mass concentration of phosphorus 0,000002 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cm andstand 20 cmof solution B and adjusted to the mark with distilled water.

4.3 Preparation for analysis

To build a calibration curve in a separating funnel with a capacity of 100 cmtransfer 1,0; 2,0; 4,0; 6,0 and 8,0 cmof a solution of phosphorus In, the volume was adjusted to 50 cmof perchloric acid, diluted 1:9, pour 3 cmof a solution of ammonium molybdate and then perform the analysis in accordance with 4.4.2, if as an extractant, a mixture of extraction or in accordance with 4.4.3, if the extractant used isobutyl alcohol.

The mass of phosphorus in the calibration solutions is 0,000002; 0,000004; 0,000008; 0,000012 and 0,000016 G.

The light absorption values of the calibration solutions and corresponding mass of phosphorus build a calibration curve taking into account the light absorption values of the calibration solution, is prepared without introducing a solution containing phosphorus.

4.4 analysis

4.4.1 Sample the sample weight in accordance with table 1 were placed in a glass made of quartz glass or Teflon, with a capacity of 250 cm.

Table 1 Conditions of preparation of sample solution

To the weighed samples poured from 15 to 30 cmof nitric acid, diluted 1:1, add five or six drops of solution of potassium permanganate and dissolved by heating to a temperature of from 60 °C to 70 °C. the Solution is evaporated to a volume of 10 to 15 cm, pour 5 cmof perchloric acid, heated for 10 min and cooled. Poured 30 cmof perchloric acid, diluted 1:9, heated to dissolve the salts, and cooled. The solution was transferred to a separatory funnel with a capacity of 100 cm, bring the solution volume up to 50 cmof perchloric acid, diluted 1:9, and then, depending on the chosen extractant is carried out the analysis on 4.4.2 or 4.4.3.

4.4.2 the solution in a separating funnel pour 3 cmof a solution of molybdate of ammonium, a 20 cmmixture for extraction, shake the funnel for 1 min. After separation of phases the organic phase is decanted into a dry volumetric flask with a capacity of 50 cm, the water phase flow 5 cmmixture for extraction and washed it for 30 s. After separation of phases the organic phase is decanted into a volumetric flask with the organic phase, the aqueous phase is discarded. To the organic phase poured 5 cm.of butyl alcohol, add three to four drops of solution of tin dichloride 1, adjusted to the mark butyl alcohol, and measure the light absorption of the solution in accordance with 4.4.4.

4.4.3 To the solution in separating funnel pour 3 cmof molybdate ammonium solution, stirred for 10 minutes pour 10 cmof isobutyl alcohol and shake for 1 min. the Organic phase was drained into another separatory funnel with a capacity of 100 cm, and the aqueous phase poured 10 cmisobutyl alcohol and repeat the extraction. The aqueous phase is discarded. To the combined organic phase poured 15 cmdichloride solution of 2 tin funnel and shake for 1 min. the Aqueous phase is discarded and the organic phase is decanted into a dry volumetric flask with a capacity of 50 cm. Separating funnel is washed with 5 to 10 cmof acetone, adding it to the solution in a volumetric flask, adjusted to the mark with acetone and measure the absorption in accordance with 4.4.4.

4.4.4 light Absorption of the sample solution is measured after 15 minutes on the spectrophotometer at a wavelength of 610 nm or 720 or photoelectrocolorimeter in the wavelength range from 590 to 640 or 700 to 740 nm in cuvettes with the thickness of the absorbing layer of 3 cm

The analysis on 4.4.2 as a solution of comparison, a mixture of 15 cmof chloroform and 35 cmbutyl alcohol, in the analysis for 4.4.3 is a blend of 20 cmisobutyl alcohol and 30 cmof acetone.

The value of the light absorption of the sample solution find the mass of phosphorus for the calibration schedule.

4.5 Processing the analysis results

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

, (1)

where Mis the mass of phosphorus in the sample solution, g;

Mis the mass of phosphorus in solution in the reference experiment, g;

K — dilution factor of sample solution;

M — weight of sample, g.

4.6 accuracy Control analysis

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 2 — 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

Bibliography