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GOST 6674.1-96

STATE P 57376-2016 GOST 193-2015 GOST 27981.5-2015 GOST 27981.2-2015 GOST 27981.1-2015 GOST 13938.11-2014 GOST P 56240-2014 GOST 859-2014 GOST P 55685-2013 STATE P 54922-2012 STATE STANDARD P 54310-2011 GOST 31382-2009 STATE R 52998-2008 GOST 859-2001 GOST 6674.4-96 GOST 6674.3-96 GOST 6674.2-96 GOST 6674.1-96 GOST 4515-93 GOST 28515-97 GOST 17328-78 GOST 614-97 GOST 15527-70 GOST 13938.13-77 GOST 13938.13-93 GOST 1020-77 GOST 5017-2006 GOST 1652.11-77 GOST 15027.12-77 GOST 15027.11-77 GOST 493-79 GOST 1953.9-79 GOST 23859.2-79 GOST 1953.5-79 GOST 1953.3-79 GOST 1953.12-79 GOST 1953.6-79 GOST 15027.18-86 GOST 27981.2-88 GOST 27981.5-88 GOST 15027.5-77 GOST 1652.12-77 GOST 15027.8-77 GOST 1652.7-77 GOST 15027.6-77 GOST 15027.7-77 GOST 1652.2-77 GOST 1652.4-77 GOST 15027.2-77 GOST 1652.8-77 GOST 1652.3-77 GOST 13938.6-78 GOST 13938.7-78 GOST 13938.1-78 GOST 13938.2-78 GOST 13938.4-78 GOST 13938.8-78 GOST 13938.10-78 GOST 13938.12-78 GOST 23859.8-79 GOST 1953.1-79 GOST 613-79 GOST 9716.2-79 GOST 23912-79 GOST 23859.1-79 GOST 23859.4-79 GOST 1953.2-79 GOST 20068.1-79 GOST 9717.3-82 GOST 9717.1-82 GOST 27981.4-88 GOST 28057-89 GOST 6674.5-96 GOST 23859.11-90 GOST 24978-91 GOST 15027.14-77 GOST 15027.10-77 GOST 15027.4-77 GOST 1652.6-77 GOST 1652.10-77 GOST 15027.9-77 GOST 13938.5-78 GOST 13938.11-78 GOST 18175-78 GOST 13938.3-78 GOST 23859.6-79 GOST 1953.4-79 GOST 1953.8-79 GOST 1953.7-79 GOST 23859.9-79 GOST 1953.11-79 GOST 1953.15-79 GOST 1953.10-79 GOST 1953.16-79 GOST 23859.5-79 GOST 23859.3-79 GOST 9716.3-79 GOST 1953.14-79 GOST 15027.16-86 GOST 15027.17-86 GOST 27981.6-88 GOST 27981.1-88 GOST 15027.20-88 GOST 17711-93 GOST 1652.1-77 GOST 15027.13-77 GOST 1652.5-77 GOST 15027.1-77 GOST 1652.13-77 GOST 1652.9-77 GOST 15027.3-77 GOST 13938.9-78 GOST 23859.10-79 GOST 193-79 GOST 20068.2-79 GOST 1953.13-79 GOST 23859.7-79 GOST 9716.1-79 GOST 20068.3-79 GOST 24048-80 GOST 9717.2-82 GOST 15027.15-83 GOST 15027.19-86 GOST 27981.3-88 GOST 20068.4-88 GOST 27981.0-88 GOST 13938.15-88 GOST 6674.0-96

GOST 6674.1−96 copper phosphorous Alloys. Methods for determination of phosphorus


GOST 6674.1−96

Group B59


INTERSTATE STANDARD

COPPER PHOSPHOROUS ALLOYS

Methods for determination of phosphorus

Copper-phosphorous alloys.
Methods for determination of phosphorus


ISS 77.120.30
AXTU 1709

Date of introduction 2001−07−01


Preface

1 DEVELOPED by the Interstate technical Committee for standardization MTK 107; Donetsk state Institute of non-ferrous metals (Danism)

SUBMITTED to the State Committee of Ukraine for standardization, Metrology and certification

2 ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 10 dated 3 October 1996)

The adoption voted:

   
The name of the state The name of the national authority
standardization
The Republic Of Azerbaijan
Azgosstandart
The Republic Of Armenia
Armastajad
The Republic Of Belarus
Gosstandart Of The Republic Of Belarus
The Republic Of Georgia
Gosstandart
The Republic Of Kazakhstan
Gosstandart Of The Republic Of Kazakhstan
The Republic Of Moldova
Moldovastandart
Russian Federation
Gosstandart Of Russia
The Republic Of Tajikistan
Tajikistandart
Turkmenistan
Glavgosekspertiza «Turkmenstandartlary»
The Republic Of Uzbekistan
Standards
Ukraine
Gosstandart Of Ukraine

3 Resolution of the State Committee of the Russian Federation for standardization and Metrology dated December 19, 2000 N 384-St inter-state standard GOST 6674.1−96 introduced directly as state standard of the Russian Federation from July 1, 2001

4 REPLACE GOST 6674.1−74

1 Scope


This standard specifies the gravimetric and photometric methods for the determination of phosphorus at its content of from 5% to 14% in the copper-phosphorous alloys.

2 Normative references


The present standard features references to the following standards:

The Copper GOST 859−78. Stamps*
_______________
* On the territory of the Russian Federation GOST 859−2001, here and hereafter. — Note the manufacturer’s database.


GOST 1277−75 Silver nitrate. Specifications

GOST 3118−77 hydrochloric Acid. Specifications

GOST 3652−69 citric Acid monohydrate and anhydrous. Specifications

GOST 3760−79 Ammonia water. Specifications

GOST 3765−78 Ammonium molybdate. Specifications

GOST 3773−72 Ammonium chloride. Specifications

GOST 4198−75 Potassium phosphate odnosemjannyj. Specifications

GOST 4209−77 Magnesium chloride 6-water. Specifications

GOST 4461−77 nitric Acid. Specifications

GOST 5712−78 Ammonium oxalate 1-aqueous. Specifications

GOST 6344−73 Thiourea. Specifications

GOST 6674.0−96 copper phosphorous Alloys. General requirements for methods of analysis

GOST 18300−87 ethyl rectified technical. Specifications

GOST 20490−75 Potassium permanganate. Specifications

3 General requirements


General requirements — according to GOST 6674.0.

4 Gravimetric method

4.1 the essence of the method


The method is based on measuring the mass of precipitate of magnesium pyrophosphate after its calcination to constant weight.

4.2 Reagents and solutions


Nitric acid according to GOST 4461 and diluted 1:1.

Hydrochloric acid according to GOST 3118 and diluted 1:1 and 1:99.

Citric acid according to GOST 3652, a solution of 500 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

Ammonium chloride (ammonium chloride) according to GOST 3773, solution 100 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

Magnesium chloride (magnesium chloride) according to GOST 4209.

A mixture of magnesia: a solution of 55 g of crystalline magnesium chloride and 105 g of ammonium chloride in 1 DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof water.

Ammonia water according to GOST 3760, diluted 1:1 and 1:9.

Silver nitrate (silver nitrate) GOST 1277, a solution of 10 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

4.3 analysis

4.3.1 the sample of alloy weighing 0.5 g of bring in a glass with a capacity of 300 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, is dissolved in 20 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof nitric acid solution, transferred to a porcelain Cup, add 10 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof hydrochloric acid and evaporated on a boiling water bath to dryness. To the dry residue add 5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof hydrochloric acid and evaporated under the same conditions. The residue is dried at a temperature of (130±5) °C. To the dried residue add 5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof nitric acid, 5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof hydrochloric acid and 50 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof hot water. The solution was transferred to a beaker with a capacity of 300 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора. If upon dissolution of the remainder is allocated silicic acid, the beaker content was filtered through filter «blue ribbon». In this case the precipitate is washed with hot dilute hydrochloric acid (1:99) to the disappearance of the reaction of copper (control is carried out with dilute ammonia (1:1) by the reaction of formation of the ammonia complex of copper, a solution which has a deep blue color).

To the obtained solution was added 10 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof the citric acid solution, 20 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof ammonium chloride solution and 25 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof magnesia with

MESI.

4.3.2 the solution was added gradually with stirring ammonia, diluted 1:1, before the formation of the ammonia complex of copper blue. The solution is thoroughly stirred with a glass rod touching the walls of the glass prior to the discharge of sediment. Then pour the excess diluted ammonia (1:1) in number, constituting ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораa part of the volume content of the glass, and left overnight.

4.3.3 solution and the precipitate was filtered through filter «blue ribbon» by washing the precipitate with diluted ammonia (1:9). The filter cake is dissolved in 10 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораhot dilute hydrochloric acid (1:1) and washed the filter 3−5 times with hot dilute hydrochloric acid (1:99), collecting the filtrate and washings in a beaker, which held an initial deposition of phosphorus.

To the obtained hydrochloric acid solution was added 10 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof a solution of ammonium chloride, 5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof magnesia mixture, diluted to 100 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораwith water and then do as specified in 4.3.2.

4.3.4 the beaker Content was filtered through filter «blue ribbon», the precipitate washed with dilute ammonia (1:9), disappearance of reaction on chloride ions (the control is carried out using silver nitrate). Dried at 105 °C in a desiccator, the precipitate together with the filter placed in preheated and weighed crucible, the filter is incinerated, and then calcined to constant weight at a temperature of (1100±20) °C.

At the same time spend control experience.

4.4 Processing of results

4.4.1 the Content of phosphorus ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, %, is calculated by the formula

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, (1)


where ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораis the mass of the calcined precipitate of magnesium pyrophosphate from a sample of the alloy, g;


ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — weight of the calcined precipitate of magnesium pyrophosphate in a control experiment, g;

0,2783 — the ratio of pyrophosphate of magnesium on the phosphorus;

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — the weight of the portion of alloy,

4.4.2 Discrepancy between the results of two parallel determinations should not exceed permissible value (at p = 0.95), equal to 0.10%.

4.4.3 the Discrepancy of the two results of the analysis of the same sample obtained at different times by different performers, shall not exceed the permissible value (at p = 0.95), 0.20%.

5 Photometric method

5.1 the essence of the method


The method is based on measurement at a wavelength of 570 nm optical density of the solution formed in the presence of thiourea phosphorus-molybdenum complex (molybdenum blue).

5.2 the Instrument, reagents and solutions


Photoelectrocolorimeter or spectrophotometer.

Nitric acid according to GOST 4461, diluted 1:1.

Potassium permanganate (potassium permanganate) according to GOST 20490, solution 20 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

Ammonium oxalate (ammonium oxalate) according to GOST 5712, a solution of 25 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

Hydrochloric acid according to GOST 3118, diluted 1:2.

Rectified ethyl alcohol (ethanol) according to GOST 18300 and diluted 5:8.

Ammonium molybdate (ammonium molybdate) according to GOST 3765, recrystallized from alcoholic solution, a freshly prepared solution 50 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора. The recrystallization of ammonium molybdate is carried out as follows: 70 g of drug is dissolved in 400 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof water when heated to 70−80 °C and filtered twice with a hot solution through the same filter of «blue ribbon». To the solution add 250 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof ethanol. The solution was cooled and allowed to settle for 1 h. the Precipitated crystals filtered off using a suction, sucking the solution and repeat the recrystallization. After filtration the crystals are washed 2−3 times with ethanol, diluted 5:8, portions of 20 to 30 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора. After this they are dried in the air.

Thiourea according to GOST 6344, solution 100 g/DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора.

Potassium phosphate odnosemjannyj (monokaliy) according to GOST 4198.

Preparation of a standard solution of phosphorus: 8,7874 g monokaliy (previously dried at 105 °C to constant weight) was placed in a volumetric flask with a capacity of 1 DMГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, is dissolved in water, made up to the mark with water and mix.

1 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораstandard solution contains 0.002 g of phosphorus.

Copper according to the GOST 859.

5.3 analysis

5.3.1 a sample of alloy weighing 0.1 g was placed in a conical flask with a capacity of 250 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, dissolved in 20 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof a solution of nitric acid and boil to remove oxides of nitrogen.

5.3.2 Add 5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof potassium permanganate solution and kept warm on the stove until the complete coagulation of manganese oxide (IV). Add dropwise a solution of ammonium oxalate until the precipitate has fully dissolved. In order to avoid an excess of ammonium oxalate after adding each drop of its solution is thoroughly mixed.

The solution was cooled, transferred to a volumetric flask with a capacity of 200 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, adjusted to the mark with water and mix thoroughly.

5 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof solution is placed in a volumetric flask with a capacity of 100 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, 12 cm is addedГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораdiluted hydrochloric acid (1:2), 10 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof solutions of thiourea and ammonium molybdate. All the reagents poured slowly with constant stirring. Bring to mark with water and mix again. The sample is ready for analysis.

5.3.3 For construction of calibration curve six conical flasks with a capacity of 250 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораis placed 0.1 g of copper, add 2,0; 3,0; 4,0; 5,0; 6,0 and 7,0 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораstandard solution phosphorus and dissolved by adding to each flask at 20 cmГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораof a solution of nitric acid, boil to remove oxides of nitrogen and then act as specified in 5.3.2.

5.3.4 after 15 min after preparation, measure the optical density of the sample solution and solutions for constructing the calibration curve on photoelectrocolorimeter at a wavelength of 570 nm in a cuvette with a layer thickness of 20 mm.

Solution comparison is water.

According to the obtained results build a calibration curve in coordinates «optical density of the solution is the mass of phosphorus corresponding to aliquote part of the solution». Mass fraction of phosphorus in the sample is determined according to the calibration schedule.

5.3.5 allowed to set mass fraction of phosphorus by comparison. To do this, along with the analysis of the sample analyzing the sample comparison 5.3.1 and 5.3.2, which is used as a standard sample with a similar phosphorus content.

5.4 processing of the results

5.4.1 Mass fraction of phosphorus ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, %, is calculated by the formula

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, (2)


where ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораis the mass of phosphorus was found in the calibration schedule g;


ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — the weight of the portion of alloy, suitable aliquote part of the sample solution,

5.4.2 When using the method of comparison of mass fraction of phosphorus ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, %, is calculated by the formula

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора, (3)


where ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — mass fraction of phosphorus in the reference sample, %;


ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфораthe value of optical density of the analyzed solution;

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — the weight of the portion of the reference sample corresponding to aliquote part of the sample solution, g;

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — the value of the optical density of the solution of the comparison;

ГОСТ 6674.1-96 Сплавы медно-фосфористые. Методы определения фосфора — the weight of the portion of alloy, suitable aliquote part of the sample solution,

5.4.3 the differences between the results of parallel measurements and the results of the analysis shall not exceed allowable values in accordance with 4.4.2 and 4.4.3.