By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST 14339.1-82

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 14339.1−82 Tungsten. Methods for determination of carbon (Change No. 1)


GOST 14339.1−82

Group B59

INTERSTATE STANDARD


TUNGSTEN

Methods for determination of carbon

Tungsten. Methods for the determination of carbon


AXTU 1709

Date of introduction 1984−01−01


INFORMATION DATA

1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR

DEVELOPERS

V. I. Veprintsev, S. N. Suvorova, N. With. Borodin, L. V. Mikhailov, V. V., Sultanian, N. P. Anikeeva, S. A. Isaev, V. I. Vinogradov, V. E. Chebotarev, V. A. Prilepskaya, A. Y. Abramov, N. B. Denisov, L. M. Efimov, K. Z. Stegenga

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 30.09.82 N 3868

3. REPLACE GOST 14339.1−74

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
Item number
GOST 435−77
2.2
GOST 3760−79
2.2
GOST 4107−78
2.2
GOST 4108−72
2.2
GOST 4234−77
2.2
GOST 5583−78
2.2
GOST 9147−80
2.2, 3.2
GOST 18300−87
2.2, 3.2
GOST 20478−75
2.2
GOST 29103−91
1.2

5. The expiration time limit is removed by the Resolution of Gosstandart from 27.09.91 N 1525

6. REVISED (June 1999) Change 1, approved in April 1988 (I & C 7−88)


This standard specifies the potentiometric and coulometric methods for determination of carbon in metallic tungsten, tungsten oxide, ammonium paratungstate and tungsten acid (when the mass fraction of carbon from 0.0005 to 0.5%).

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 29103.

2. POTENTIOMETRIC METHOD FOR DETERMINATION OF CARBON

2.1. The essence of the method

The method is based on the combustion of a test sample in flowing oxygen in a tube furnace at 1250−1350 °C with subsequent absorption of the formed carbon dioxide electrolyte solution.

Carbon dioxide, absorbed in the electrolyte changes the pH of the solution and thus changes the potential of the electrodes, then electrolyte titrated with a solution of hydroxide of barium to the original pH (9,7−10).

(Changed edition, Rev. N 1).

2.2. Apparatus, reagents and solutions

Setup for determination of carbon, shown in the drawing, consists of a cylinder 1 with a pressure reducing valve and oxygen (GOST 5583); flowmeter type RS-ZL or RM- 2; flask 3 with Astarita; startup shutter 4; dogtramadol furnace 5 with sheltowee heaters providing heat to (1300±20) °C; dust filter 6; a capillary choke 7; flask 8filled with granular manganese dioxide; electrolytic cell 9; the agitator 10; the electrode system 11; dropper 12 to enter into the cell volume of the titrant used; electric motor 13; burette 14 with a capacity of 10−25 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1); magnetic valve 15; pH meter 16of the type pH 340 or pH 121; normal item 17; block of automatic titration 18(BAT 15, BAT-12ЛМ).

ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)

Note. Instead of a burette 14, the magnetic valve 15 can be to use the automatic burette dispenser B-701. Electrolytic cell 9 with a capacity of 200 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)can be replaced by a vessel with a porous filter N 2 or 3 with a capacity of 100 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1).


Allowed to use the analyzer to ensure accuracy not lower than specified in the standard.

Normal element connected in case of use of pH meter pH-340 BAHT 12ЛМ.

Manganese sulfate according to GOST 435.

Ammonia according to GOST 3760.

Granulated manganese dioxide and 200 g of manganese sulfate is dissolved in 2500 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of hot water, then in the solution add 25 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of ammonia; add 1000 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)to 22.5% strength solution naternicola ammonium and the mixture boiled for 10 min. while boiling, add ammonia to alkaline reaction, then the solution to stand until complete precipitation of manganese dioxide. The precipitate was filtered off, washed and dried at 110 °C.

Askari.

The lime soda.

Ammonium neccersarily according to GOST 20478, 22,5% solution.

Pumps porcelain LS-2, LS-4 according to GOST 9147.

Tube refractory mullite inner diameter of 20−21 mm.

Potassium chloride according to GOST 4234, saturated solution.

Barium chloride according to GOST 4108, electrolyte solution: 10 g of barium chloride dissolved in 1000 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of distilled water and to the obtained solution poured 10 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of ethanol.

Barium hydroxide according to GOST 4107, a saturated solution of the hydroxide of barium is dissolved in distilled water (pre-boiled for 2 h and cooled to room temperature). The resulting solution is diluted 30 times. The solution is stored in bottles fitted with tubes with soda lime.

The technical rectified ethyl alcohol according to GOST 18300.

Standard samples of category, GEO, CCA, SOP, in which the content of component is not different from that analyzed more than two times.

(Changed edition, Rev. N 1)

.

2.3. Preparation for assay

To the output of the pH meter is connected to the block automatic titration series using normal element. Set up a pH meter and an automatic titration unit according to the attached instructions to these devices.

The electrode system set up against the buffer solution of 9.18 pH-9,22 (fixanal 0.01 M solution of potassium tetraborate).

The porcelain boat was calcined in flowing oxygen at 1280 °C for 3 min.

Electrolytic cell filled with electrolyte 200 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1), and in the case of a cell with a porous partition 100 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1).

Set the oxygen flow rate is 700 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)in 1 min. Include the BAT in the titration and the pH adjusted to 10.

Burning 3−4 sample standard sample, set the caption of the hydroxide of barium.

Samples of tungsten acid is calcined for 4 h at (650±10) °C to tungsten trioxide.

Samples of ammonium paratungstate is transferred to the tungsten oxide by calcination (650±10) °C for 1.5 h.

Tungsten dioxide is burned in a current of oxygen without pre-treatment.

Samples of metal tungsten is cleaned from possible contamination by washing with 5−10 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of alcohol.

2.4. Analysis

Depending on the mass fraction of carbon in the sample take a different sample in accordance with table.1.

Burnt the boat with a weighed test portion is placed in a tube for burning, close the shutter and include a block of automatic titration for titration.

The end of the analysis of the fixed block automatic titration burette and the measured amount of a solution of hydroxide of barium, used for titration.

Burning a standard sample for determining the titer done after every fifth sample analyzed.

Table 1

   
Mass fraction of carbon, %
The mass of charge, g
From 0.0005 to 0.001 Of 2.00
SV. Of 0.001 «to 0.005 Of 1.00
«Of 0.005» to 0.05 0,50
«0,05» 0,5
0,25

2.5. Processing of the results

2.5.1. Mass fraction of carbon (ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)) in percent is calculated by the formula

ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1),


where ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1) — volume of the solution of hydroxide of barium, used for titration of the test solution, cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1);

ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)the volume of the solution of hydroxide of barium, used for titration of the solution in a control experiment, cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1);

ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)the titer of a solution of hydroxide of barium, expressed in g/cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)carbon;

ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1) — weight of charge, g

.

2.5.2. Allowable absolute differences of the results of three parallel measurements at a confidence level ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)=0.95 does not exceed the values specified in table.2.

Table 2

   
Mass fraction of carbon, %
The absolute allowable difference, %
From 0.0005 to 0.001
0,0003
SV. Of 0.001 «to 0.003 to
0,0004
«Of 0.003» to 0.01
0,001
«Is 0.01» to 0.03
0,002
«0,03» 0,1
0,004
«0,1» 0,3
0,015
«0,3» 0,5
0,025



(Changed edition, Rev. N 1).

3. COULOMETRIC METHOD FOR DETERMINING CARBON

3.1. The essence of the method

The method is based on the combustion of a test sample in flowing oxygen in a tube furnace at 1200−1250 °C with subsequent absorption of the formed carbon dioxide electrolyte solution.

Then the electrolyte electrolyzed to restore the original pH, and the amount of consumed electricity in the electrolysis process to measure the carbon content.

3.2. Equipment, reagents, solutions

Coulometric analyzer an-7560 or any other type for that range, determine carbon content.

Resistance furnace providing heating up to (1300±20) °C.

Cylinder with reducing valve with oxygen according to GOST 5583.

Pumps porcelain LS-2 and LS-4 according to GOST 9147.

Tube refractory mullite inner diameter of 20−21 mm.

The technical rectified ethyl alcohol according to GOST 18300.

Standard samples of category, GEO, CCA, SOP, in which the content of component is not different from that analyzed more than two times.

(Changed edition, Rev. N 1).

3.3. Preparation for assay

The porcelain boat was calcined in flowing oxygen at 1280 °C for 3 min.

Include the analyzer to the network and configured. The analyzer is calibrated by standard samples.

Samples of tungsten acid is dehydrated and calcined for 4 h at (650±10) °C to tungsten trioxide.

Samples of ammonium paratungstate is transferred to the tungsten oxide by calcination (650±10) °C for 1.5 h.

Tungsten dioxide is burned in a current of oxygen without pre-treatment.

Samples of metal tungsten is cleaned from possible contamination by washing with 5−10 cmГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)of alcohol.

3.4. Analysis

Depending on the mass fraction of carbon in the sample take a different sample in accordance with table.1.

A boat with prepared breakdown is placed in a tube for burning, close the shutter and turn on the device for titration.

(Changed edition, Rev. N 1).

3.5. Processing of the results

3.5.1. Mass fraction of carbon in percent less carbon content found in the control experiment corresponds to the indication of the digital display device.

3.5.2. Allowable absolute discrepancies in the results of parallel measurements at a confidence level ГОСТ 14339.1-82 Вольфрам. Методы определения углерода (с Изменением N 1)=0.95 does not exceed the values specified in table.2.

(Changed edition, Rev. N 1).

3.5.3. The method used in the disagreement in assessing the quality of tungsten.