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GOST 14339.2-82

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 14339.2−82 Tungsten. Method for the determination of sulphur (Change No. 1)


GOST 14339.2−82

Group B59

INTERSTATE STANDARD


TUNGSTEN

Method for the determination of sulfur

Tungsten. Method for the determination of sulphur


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 14339.2−74

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
 Item number
GOST 3118−77
 Sec. 2
GOST 4159−79
 Sec. 2
GOST 4232−74
 Sec. 2
GOST 5583−78
 Sec. 2
GOST 9147−80
 Sec. 2
GOST 10163−76
 Sec. 2
GOST 14339.1−82
 Sec. 2
GOST 18300−87
 Sec. 2
GOST 25336−82 Sec. 2
GOST 29103−91 1.1
GOST 29251−91 Sec. 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 politicalticker method for the determination of sulfur (with sulfur mass fraction of from 0.0005 to 0.05%) in the metal tungsten, tungsten dioxide, tungsten acid, ammonium paratungstate.

The method is based on the combustion of weighed portion of the sample in flowing oxygen at 1200−1350 °C. the Sulfur burns to sulfur dioxide, which is then in the absorption vessel is absorbed in water to form sulphurous acid. Sulfurous acid octarepeat solution of iodine in potassium iodide in the presence of an indicator — starch.

(Changed edition, Rev. N 1).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 29103.

2. APPARATUS, REAGENTS AND SOLUTIONS


Setup for the determination of sulfur (hell.1) consists of a tank 1 with oxygen according to GOST 5583 gear; flowmeter 2 type RS-3A or RM-A; bottle 3filled with a granular manganese dioxide; bottle 4filled with Astarita; startup shutter 5; dogtramadol furnace 6 with sheltowee heaters or any other tubular furnace that provides heat to 1200−1350 °C; capillary throttle 7; dust filter 8 and the analyzer 9, consisting of device type LMF-69, or any other type with similar characteristics and the block of automatic titration BAHT or 15 BAHT-12ЛМ with a glass bubble counter (DWG.2) and burette with an automatic valve or automatic burettes B-701.

Absorption vessel with GOST 25336 capacity of 150 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1), with a magnetic clasp.

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

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

Tube refractory mullite inner diameter of 20−21 mm.

Microburette according to GOST 29251 with a capacity of 2−5 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1).

Bottles for washing gases according to GOST 25336.

Askari.

Potassium iodide according to GOST 4232.

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)


Damn.1

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)


Damn.2

Granulated manganese dioxide, manufacturing manganese dioxide according to GOST 14339.1.

Hydrochloric acid according to GOST 3118.

The technical rectified ethyl alcohol according to GOST 18300.

The soluble starch according to GOST 10163, 0,05% absorption solution 0,500 g of starch are dissolved in 50 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)of water is poured into 500 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)of hot water, boil, and top up the solution with water to 1000 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)and add 5 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)of hydrochloric acid.

Iodine GOST 4159, solution: the linkage of iodine with a mass of 0.6 g was placed in a volumetric flask with a capacity of 1000 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1), which had previously placed 4 g of potassium iodide, dissolve, top up with water to 1000 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)and mixed. The solution was stored in a flask made of dark glass. The titer of the iodine solution sets for the standard sample and verify after burning ten or twelve batches.

Standard samples of categories of 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. PREPARATION FOR ASSAY


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

In the absorption vessel pour 120 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)absorption solution, place the vessel in the slot of the analyzer, is lowered into the vessel, the rod of the stirrer and adjust the stirring speed of the solution.

Set the oxygen flow rate is 1000 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)/min.

The output of the LMF-69 is connected to the input Bat. On the way out of Bath connect the burette dosing B-701 or magnetic valve attached to the BAT.

Use only silicone, PTFE and polyethylene tubing internal diameter of 2 mm. the portion of the tube, the magnetic pinch valve, replace the rubber nipple with a tube length of 15 mm.

Bring the color of the absorption vessel to blue (wavelength 440−460 nm). After that, burn two or three sample standard sample containing sulfur.

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 tungsten metal in order to remove any contaminants are washed in 5−10 cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)of alcohol.

4. ANALYSIS


Depending on the mass fraction of sulfur take a charge in accordance with table.1.

Table 1

   
Mass fraction of sulfur, %
 The weight of analyzed sample, g
From 0.0005 to 0.001
 Of 2.00
SV. Of 0.001 «to 0.01
 Of 1.00
«To 0.01» to 0.05
 0,50



Svezheproseyannuyu a porcelain boat with the appropriate charge placed in the tube for combustion and automatic titration unit (BAHT) include a handle (button) «titration». After the device automatically turns off, count the volume of iodine consumed for titration. Then carry out the combustion of the next sample.

At the end of the analysis, the burette and absorption vessel is rinsed with water.

5. PROCESSING OF THE RESULTS

5.1. Mass fraction of sulfur (ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)) in percent is calculated by the formula

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1),


where ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)is the volume of iodine solution used for titration of the test solution, cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1);

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1) — the volume of iodine solution consumed for titration of the solution in the reference experiment, cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1);

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1) — the titer of the iodine solution, expressed in g/cmГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)sulfur;

ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1) — weight of charge, g

.

5.2. Allowable absolute discrepancies in the results of parallel measurements at a confidence level ГОСТ 14339.2-82 Вольфрам. Метод определения серы (с Изменением N 1)=0.95 does not exceed the values given in table.2.

Table 2

   
Mass fraction of sulfur, %
 The absolute allowable difference, %
From 0.0005 to 0.001
 0,0002
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
«To 0.03» to 0.05
 0,004