GOST R ISO 11400-2016
GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption
GOST R ISO 11400−2016
NATIONAL STANDARD OF THE RUSSIAN FEDERATION
NICKEL, FERRONICKEL AND NICKEL ALLOYS
Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption
Nickel, ferronickel and nickel alloys. Determination of phosphorus content by as phosphovanadomolybdate molecular absorption spectrometric method
OKS 77.100
77.120.40*
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* According to the official website of Rosstandart OKS 71.100.10,
here and further. — Note the manufacturer’s database.
Date of introduction 2016−11−01
Preface
1 PREPARED by the Federal state unitary enterprise «Central research Institute of ferrous metallurgy them.And.P.Bardin," on the basis of their own translations into Russian language the English language version of the standard specified in paragraph 4
2 SUBMITTED by the Technical Committee for standardization TC 145 «monitoring Methods of steel products»
3 APPROVED AND put INTO EFFECT by the Federal Agency for technical regulation and Metrology dated 3 March 2016 N 117th St
4 this standard is identical to international standard ISO 11400:1992* «Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption» (ISO 11400:1992 «Nickel, ferronickel and nickel alloys — Determination of phosphorus content — Phosphovanadomolybdate molecular absorption spectrophotometric method», IDT).
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* Access to international and foreign documents referred to here and hereinafter, can be obtained by clicking on the link to the site shop.cntd.ru. — Note the manufacturer’s database.
The name of this standard changed with respect to names specified international standard for compliance with GOST R 1.5 (subsection 3.5).
In applying this standard it is recommended to use instead of the referenced international standards corresponding national and international standards, details of which are given in Appendix YES
5 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 the upcoming issue of 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 (www.gost.ru)
1 Scope
This standard specifies the spectrophotometric method of molecular absorption for the determination of phosphorus in Nickel, ferronickel and alloys based on Nickel in the range from 0.0005% to 0.06% (mass.).
Arsenic, chromium, hafnium, niobium, silicon, tantalum, titanium and tungsten have a disturbing influence on the determination of phosphorus, but the interferences can be eliminated binding of interfering elements in complex compounds, or delete, for example, Cr. The definition of low phosphorus levels [of 0.0005% (mass.)] can only be achieved in samples with low contents of interfering elements.
2 Normative references
This standard uses the regulatory references to the following international standards*:
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* The table of conformity of national standards international see the link. — Note the manufacturer’s database.
ISO 648:1977ГОСТ R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption oils. Pipettes with one mark (ISO 648:1977, Laboratory glassware — One-mark pipettes)
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GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption Valid ISO 648:2008 «laboratory Glassware glass. Pipette with one mark».
ISO 1042:1983ГОСТ R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption oils. Flasks volumetric with one mark (ISO 1042:1983, Laboratory glassware — One-mark volumetric flasks)
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GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption Valid ISO 1042:1998 «oils. Volumetric flask with one mark».
ISO 5725:1986ГОСТ R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption Precision of test methods. Determination of repeatability and reproducibility of a standard method by interlaboratory tests (ISO 5725:1986, Precision of test methods; Determination of repeatability and reproducibility for a standard test method by inter-laboratory tests)
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GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption Valid ISO 5725−1:1994, ISO 5725−2:1994, ISO 5725−3:1994, ISO 5725−4:1994, ISO 5725−5:1998, ISO 5725−6:1994.
3 the essence of the method
Dissolution of the sample the sample in a mixture of nitric and hydrochloric acids. Heating with perchloric acid solution in a glass of FERPLAST (PFA) or polytetrafluoroethylene (PTFE) to release the Smoking fumes of perchloric acid to remove the chromium in the form of a volatile chloride gromila. Formation of complex fluorides of silicon and heat-resistant elements.
The transfer of phosphorus in rostroventrolateral complex in a solution of perchloric and nitric acids.
Extraction rostroventrolateral complex with methyl isobutyl ketone in the presence of citric acid added to bind arsenic in a compound.
4 Reagents
In the analysis, unless otherwise stated, use only reagents established analytical grade and only distilled water or water of equivalent purity.
Check by means of the idle experiments (7.6) that the reagents do not contain phosphorus. Party reagents showing high blank values, unusable and should not be used. The result value of the idle experience, designed for 1 g sample must be below 0,0005% (mass.).
4.1 Nitric acid GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption g/smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption, diluted 1:4.
4.2 Hydrofluoric acid (40% wt.), GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption g/smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate spectrophotometrically by the method of molecular absorption.
Note — Hydrofluoric acid has an extremely irritating and corrosive effect on skin and mucous membranes, causing severe skin burns that are slow to heal. In case of acid contact with skin, should rinse thoroughly with water and seek medical help.
4.3 Citric acid solution.
Dissolve 500 g citric acid monohydrate (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption) in water, diluted to 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption and mix.
4.4 methyl isobutyl ketone.
4.5 ammonium Molybdate solution.
Dissolve 15 g of ammonium molybdate tetrahydrate is GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption in water and dilute to 100 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate spectrophotometrically by the method of molecular absorption. This solution was used freshly prepared. If you get a high and unstable blank values, you must replace the batch of the reagent.
4.6 the ammonium Metavanadate solution.
Dissolve 2.5 g of ammonium metavanadate (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption) in water and dilute to 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate spectrophotometrically by the method of molecular absorption.
4.7 sodium Nitrite, solution.
Dissolve 50 g of sodium nitrite (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption) in water and dilute to 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate spectrophotometrically by the method of molecular absorption.
4.8 Fluoro-boric acid, solution
Suspend 75 g of boric acid (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption) of 600 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption in a plastic Cup. Add 50 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption hydrofluoric acid (4.2), dilute to 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption of water and heated until complete dissolution of boric acid. Store the solution in a plastic vessel.
Before use, if boric acid is released in the form of crystals, and the solution gently warmed.
4.9 Phosphorus, the primary standard solution containing 1,000 g/dbhost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption of phosphorus.
Weighed with accuracy to 0.0001 g 4,394 per g of digidrogenfosfat potassium (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption), previously dried to constant weight at 110 °C and cooled in a desiccator. Weighed transferred to a volumetric flask with one mark capacity 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption and dissolve in water. Bring to mark with water and mix.
4.10 Phosphorus, standard solution containing 10 mg/dbhost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption of phosphorus.
Transfer 10.0 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption of the basic solution of phosphorus (4.9) in a volumetric flask with one mark capacity 1000 smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate spectrophotometrically by the method of molecular absorption. Dilute to the mark with water and mix.
5 Instrument
Glass labware should be washed with hot hydrochloric acid (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption g/smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption), opolaskivateli with water and finally rinsed with distilled water.
Use conventional laboratory equipment and the following equipment.
5.1 Spectrophotometer capable of measuring optical density of the solution at a wavelength of 355 nm.
5.2 heat-Resistant plastic cups of polytetrafluoroethylene (PTFE) or preferably from FERPLAST (PFA). Glasses from PFA have a graphite base and a special design allowing operation of evaporation of the acids to a temperature of 280 °C.
The glasses should be thoroughly cleaned before analysis. For this purpose, the glasses you pour hydrochloric acid (GOST R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption g/smost R ISO 11400−2016 Nickel, ferronickel and Nickel alloys. Determination of phosphorus in the form of phosphoromolybdate by spectrophotometry molecular absorption), diluted 1:1, and boil for about 2 minutes, then washed with water and rinsed with distilled water.
5.3 Electric temperature controlled surface.
6 Sampling and sample preparation
6.1 Selection and preparation of the laboratory samples is performed in accordance with the usual procedures agreed upon or in case of disagreement, use the appropriate international standard.
6.2 Laboratory sample usually consists of a milling or drilling chips, and the further sample preparation is not required.
6.3 If it is assumed that the laboratory sample is contaminated with oil or grease in the process of milling or drilling, it must be rinsed with acetone or high-purity and dry air.
6.4 laboratory If the sample contains particles or pieces, which vary greatly in size, the test sample is obtained by selecting uniform particles (or additional grinding).
7 analysis
Note — Fuming perchloric acid is a powerful oxidizing agent and can cause explosions in contact with organic materials. Any evaporation must be performed in a fume hood, adapted for work with perchloric acid.
