GOST 13047.7-2014

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  ГОСТ 13047.7-81

GOST 13047.7−2014 Nickel. Cobalt. Methods of determining sulphur

GOST 13047.7−2014

INTERSTATE STANDARD

NICKEL. COBALT

Methods of determining sulphur

Nickel. Cobalt. Methods for determination of sulphur

ISS 77.120.40

Date of introduction 2016−01−01

Preface

Goals, basic principles and main 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:

4 by Order of the Federal Agency for technical regulation and Metrology of June 24, 2015 N 816-St inter-state standard GOST 13047.7−2014 introduced as the national standard of the Russian Federation from 1 January 2016.

5 REPLACE GOST 13047.7−2002


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 a spectrophotometric method (at a mass fraction of sulfur from 0,0003% to 0,0050%) and the method of infrared spectrometry (at the mass fraction of sulfur from 0.0001% to 0.050%) for the determination of sulfur in the primary Nickel GOST 849, Nickel powder according to GOST 9722 and GOST cobalt 123 on. As an arbitration method is the method of infrared spectrometry.

2 Normative references

This standard uses the regulatory references to the following standards:

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 123−2008 Cobalt. Specifications

GOST 200−76 Reagents. Sodium posterolaterally 1-water. Specifications

GOST 849−2008 Nickel primary. Specifications

GOST 3118−77 Reagents. Hydrochloric acid. Specifications

GOST 3652−69 Reagents. Citric acid monohydrate and anhydrous. Specifications

GOST 3760−79 Reagents. The aqueous ammonia. Specifications

GOST 4166−76 Reagents. The sodium sulfate. Specifications

GOST 4200−77 Reagents. Acid itestosterone. Specifications

GOST 4233−77 Reagents. Sodium chloride. Specifications

GOST 4236−77 Reagents. Lead (II) nitrate. Specifications

GOST 4461−77 Reagents. Nitric acid. Specifications

GOST 5583−78 (ISO 2046−73) Oxygen gas technical and medical. Specifications

GOST 9147−80 Glassware and equipment lab porcelain. Specifications

GOST 9293−74 (ISO 2435−73) Nitrogen gaseous and liquid. Specifications

GOST 9722−97 Nickel Powder. Specifications

GOST 10157−79 Argon gaseous and liquid. Specifications

GOST 10929−76 Reagents. Hydrogen peroxide. Specifications

GOST 11125−84 nitric Acid of high purity. Specifications

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

GOST 13498−79 platinum and platinum alloys. Brand

GOST 14261−77 hydrochloric Acid of high purity. Specifications

GOST 24147−80 aqueous Ammonia of high purity. 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 400 nm colloidal solution of lead sulfide formed after distillation recovery of hydrogen sulfide from a mixture of sodium and hypophosphite itestosterone acid.

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

Spectrophotometer or photoelectrocolorimeter, which provides measurements in the wavelength range from 390 to 410 nm.

Installation for the distillation of hydrogen sulfide consisting of the reaction flask, glass tubing for nitrogen supply, two receivers, connecting pipes on the ground, outlet tube and mantle.

Nitrogen gas according to GOST 9293 or argon gas according to GOST 10157.

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

Hydrochloric acid according to GOST 3118, if necessary, purified by distillation, or according to GOST 14261, diluted 1:1, 1:9 and 1:10.

Itestosterone acid according to GOST 4200.

Citric acid monohydrate according to GOST 3652, solution mass concentration of 0.02 g/cm.

Ammonia water according to GOST 3760, if necessary, according to GOST 24147, diluted 1:2.

Hydrogen peroxide according to GOST 10929.

Sodium sulfate according to GOST 4166, dried at a temperature of from 95 °C to 105 °C for 3−4 h.

Sodium chloride according to GOST 4233.

Sodium posterolaterally 1-water (hipofosfit sodium) according to GOST 200.

Lead (II) nitrate according to GOST 4236, solution mass concentration of 0.05 g/cmin a solution of citric acid.

The restorative blend is prepared as follows: a portion of hypophosphite sodium weighing 120 g is placed in a three-neck flask with a capacity of 1000 cm, equipped with a reflux condenser, pour 200 cmof hydrochloric acid diluted 1:1, 400 cmitestosterone acid and boil for 5−6 hours, passing through the solution a stream of nitrogen or argon at a speed of 60−80 bubbles per minute. The mixture was stored in a container made of dark glass with a glass stopper.

Platinum according to GOST 13498.

The solution of the mass concentration of platinum 0.001 g/cmis prepared as follows: a sample of platinum weighing 0,100 g were placed in a glass with a capacity of 100 or 150 cm, pour 5 cmof nitric acid, 15 cmof hydrochloric acid, dissolve while heating, evaporate to dryness, dry the residue add 5 cmof hydrochloric acid, 0.1 g of sodium chloride and evaporated to dryness. Treatment 5 cmof hydrochloric acid is repeated four times, the dry residue is dissolved in 20 cmof hydrochloric acid diluted 1:1, transferred to a volumetric flask with a capacity of 100 cmand adjusted to the mark with distilled water.

The solution of the mass concentration of platinum 0,00004 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmstand 4 cmof a solution of mass concentration of platinum 0.001 g/cmand was adjusted to the mark with hydrochloric acid diluted 1:9.

Solutions of known sulfur concentration.

The solution And the mass concentration of sulfur 0,001 g/cmis prepared as follows: a sample of sodium sulfate with a mass 4,4304 g were placed in a glass with a capacity of 250 cm, flow 50 to 60 cmof distilled water, dissolved by heating, cooled, transferred into a measuring flask with volume capacity of 1000 cmand adjusted to the mark with distilled water.

Solution B mass concentration of sulphur 0.0001 g/cmis prepared as follows: into a measuring flask with a capacity of 100 cmtransfer 10 cmof solution A and bring to the mark with distilled water.

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

4.3 Preparation for analysis

4.3.1 Prior analysis of the installation for the distillation of hydrogen sulfide clean. To this reaction flask is poured 7−8 cmof hydrochloric acid diluted 1:1, 30 cmrestoration of the mixture, attach the flask to the receiver, in which pre-entered: the first — from 7 to 10 cmof hydrochloric acid, diluted 1:10, the second 15 cmof ammonia, diluted 1:2. The second receiver is placed in a container filled with crushed ice. Set the flow of nitrogen or argon at a speed of 60−80 bubbles / min. Heat the solution in the reaction flask to boiling and boil for 30−35 minutes solutions from the receivers are cast.

4.3.2 For the construction of calibration curve in the reaction flask sequentially poured 0,5; 1,0; 2,0; 3,0; 4,0 and 5,0 cmof a solution of sulphur In, 6−8 cmof hydrochloric acid diluted 1:1, 30 cmrestoration of the mixture and carried out the Stripping in accordance with 4.4.

When constructing a calibration curve allowed to hold no more than four processes of distillation without adding the recovery of the mixture. To this reaction flask is poured 20 cmof hydrochloric acid diluted 1:1, 80 cmrecovery mixture, pour the solution In the sulfur and Stripping carried out in accordance with 4.4.

The mass of sulfur in the calibration solutions is 0,000005; 0,000010; 0,000020; 0,000030; 0,000040 and 0,000050 G.

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

4.4 analysis

A portion of the sample with a mass of 2,000 g (at a mass fraction of sulfur no more than 0,002%) and a weight of 1,000 g (with mass fraction of sulfur, more than 0,002%) were placed in a glass with a capacity of 250 cm, 25 cm pour thehydrochloric acid, diluted 1:1, 1 cmof a solution of mass concentration of platinum 0,00004 g/cm, dissolved by heating, added 7−10 times hydrogen peroxide 0.5−1.0 cm, avoiding violent boiling. The solution is evaporated to a volume of 5−10 cm, cooled, transferred to the reaction flask, then rinsed a glass in which to conduct the dissolution, poured 15 cmrecovery mixture, 15 cmof distilled water and 15 cmof restorative mixture.

The reaction flask is attached to two receivers, which are previously poured in the first — from 7 to 10 cmof hydrochloric acid, diluted 1:9 in the second 15 cmof ammonia, diluted 1:2. The second receiver is placed in a container filled with crushed ice. Set the flow of nitrogen or argon at a speed of 60−80 bubbles / min. the Solution was heated to boiling and boiled for 30−35 min.

A solution of the second receiver is transferred to a volumetric flask with a capacity of 50 cm, pour 2 cmof a solution of nitrate of lead, adjusted to the mark with ammonia diluted 1:2 and stirred. Light absorption of the solution measured after 5−10 min on the spectrophotometer at a wavelength of 400 nm or photoelectrocolorimeter at a wavelength range from 390 to 420 nm.

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

4.5 Processing the analysis results

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

, (1)

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

Mis the mass of sulfur 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 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

5 the Method of infrared spectrometry

5.1 Method of analysis

The method is based on measuring the absorption of infrared radiation by molecules of sulphur oxide (IV) after selecting it from the metal by combustion in induction high-frequency furnace in oxygen flow in the presence of flux.

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

Sulfur analyzer based on the principle of infrared spectrometry with an induction high-frequency furnace, and weights to account for the mass of sample sample.

Refractory ceramic crucible, calcined at a temperature of from 1100 °C to 1200 °C for 3−4 h.

Marshes: marshes provided by the manufacturer, complete with a sulfur analyzer, tungsten [1]* the iron carbonyl in [2] and other substances that provide combustion, and the results of the reference experiment in accordance with 5.3.
________________
* See Bibliography. — Note the manufacturer’s database.


Technical oxygen gas according to GOST 5583.

Standard samples according to GOST 8.315 composition of Nickel, for example [3], cobalt, for example, [4], or alloys based on Nickel, cobalt or iron with a certified mass fraction of sulfur.

5.3 Preparation for assay

Preparing the analyzer to work and his grading is carried out in accordance with the manual. To build a calibration curve using standard samples of composition of Nickel, cobalt, or alloys based on Nickel, cobalt or iron.

A portion of the beach that mass, which is used in the analysis of samples placed to carry out control experience in the crucible and analyze in accordance with 5.4.

Allowed for the introduction of flux to use metering devices.

The result of the reference experiment is considered satisfactory if the reading of the mass fraction of sulfur on the digital display of the analyzer does not exceed the value of the indicator control accuracy (expanded uncertainty) of the method of analysis specified in 5.6 to define the mass fraction of sulfur.

5.4 analysis

A portion of sample weighing 0.200 to 1,000 g was placed in a crucible, add the flux, the weight of which must be the same when conducting the reference experiment, the calibration and analysis, and conduct analysis in accordance with the manual of the analyzer.

5.5 Processing of analysis results

The result of measuring the mass fraction of sulfur in the percentage values of the reference experiment is shown on the display or printer of the analyzer.

5.6 Control of accuracy of 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 2.


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