GOST 14338.2-82
GOST 14338.2−82 Molybdenum. Method for the determination of sulphur (Change No. 1)
GOST 14338.2−82
Group B59
STATE STANDARD OF THE USSR
MOLYBDENUM
Method for the determination of sulfur
Molybdenum. Method for determination of sulphur
AXTU 1709
Valid from 01.01.84
before 01.01.92*
_______________________________
* Expiration removed
by the decree of Gosstandart of the USSR
from
Note the manufacturer’s database.
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of nonferrous metallurgy of the USSR
PERFORMERS
V. I. Veprintsev, S. N. Suvorova, Y. A. Abramov, L. V. Mikhailov, V. V., Sultanian
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from
3. REPLACE GOST 14338.2−74
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
The designation of the reference document referenced |
The number of the paragraph, subparagraph |
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 10262−73 | Sec. 2 |
GOST 14338.0−82 | 1.1 |
GOST 14338.1−82 | Sec. 2 |
GOST 18300−87 | Sec. 2 |
GOST 20292−74 | Sec. 2 |
GOST 25336−82 | Sec. 2 |
5. Validity extended till
6. REPRINT (August 1988) with amendment No. 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 molybdenum, molybdenum anhydride and ammonium molybdate.
The method is based on the combustion of weighed portion of the sample in flowing oxygen at 1200−1350 °C. the Sulfur in the sample is combusted to sulfur dioxide which is then in the absorption vessel is absorbed in water to form sulphurous acid, which octarepeat solution of iodine in potassium iodide in the presence of an indicator-starch.
1. GENERAL REQUIREMENTS
1.1. General requirements for method of analysis according to GOST 14338.0−82.
2. APPARATUS, REAGENTS AND SOLUTIONS
Setup for the determination of sulfur (hell.1) consists of a tank 1 with oxygen according to GOST 5583−78 with 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 furnace that provides heating to a temperature (1300±50) °C; capillary throttle 7; dust filter 8 and the analyzer 9, consisting of device type LMF-69 or other type with similar characteristics and the block of automatic titration BAHT or 15 BAHT-12ЛМ glass barbitalom (damn.2) and burette with an automatic valve or automatic burettes B-701.
Damn.1
Damn.2
The analyzer is placed in the absorption vessel according to GOST 25336−82, with a capacity of 150 cmwith a magnetic clasp.
Allowed to use any analyzer, to ensure accuracy not lower than specified in the standard.
Pumps porcelain LS-2 according to GOST 9147−80.
Refractory mullite tube with an inner diameter of 20−21 mm.
Microburette according to GOST 20292−74* with a capacity of 2−5 cm.
________________
* On the territory of the Russian Federation there are 29169−91 GOST, GOST 29227−91−29229−91 GOST, GOST 29251−91-GOST 29253−91. Here and further. — Note the manufacturer’s database.
Askari.
Bottles for washing gases according to GOST 25336−82.
Granulated manganese dioxide, prepared according to GOST 14338.1−82.
Potassium iodide according to GOST 4232−74.
Hydrochloric acid by the GOST 3118−77.
Zinc oxide according to GOST 10262−73.
Rectified ethyl alcohol GOST 18300−87.
The soluble starch according to GOST 10163−76, a 0.05% aqueous solution: 0,500 g of starch are dissolved in 50 cmof water is poured into 500 cmof hot water, boil, bring the volume of solution with water to 1000 cmand add 5 cmof hydrochloric acid.
Iodine GOST 4159−79, solution: the linkage of iodine with a mass of 0.6 g was placed in a volumetric flask with a capacity of 1000 cm, which had previously placed 4 g of potassium iodide, dissolve, add water to volume of 1000 cmand 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 nine or twelve batches.
Standard samples of categories of GEO, CCA, SOP, which certified the content of a component is not different from that analyzed more than two times.
(Changed edition, Rev. N 1).
3. PREPARATION FOR ASSAY
3.1. Porcelain boats and the zinc oxide is calcined in flowing oxygen at 1280 °C for 3 min.
In the absorption vessel pour 120 cmabsorption 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 cm/min.
The output of the LMF-69 is connected to the input Bat. On the way out of Bath connect the burette analyzer B-701 or magnetic valve, which is equipped with a BATH.
Only apply a silicone, fluoropolymer and polyethylene tubing with an inner 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 molybdenum metal to remove any dirt washed in 5−10 cmof alcohol.
The ammonium molybdate is calcined in a muffle furnace at 400−450 °C to complete oxidation.
4. ANALYSIS
4.1. Depending on the mass fraction of sulfur in the sample take the sample in accordance with table.1.
Table 1
Mass fraction of sulfur, % |
The mass of charge, 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 |
Put the hitch svezheproseyannuyu a porcelain boat. Mixed with the calcined zinc oxide in the ratio 1:2. A boat placed in a tube for combustion and automatic titration unit (BAHT) include a handle (button) «titration». After the device turns off automatically and calculate the volume of iodine consumed for titration. Then produce the following combustion of the 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 () in percent is calculated by the formula
,
where is the volume of iodine solution used for titration of the test solution, cm;
— the volume of iodine solution consumed for titration of the solution in the reference experiment, cm;
— the titer of the iodine solution, expressed in g/cmsulfur;
— weight of charge, g
.
5.2. Allowable absolute discrepancies in the results of parallel measurements at a confidence probability of 0.95 does not exceed the values given in table.2.
Table 2
Mass fraction of sulfur, % | Allowable absolute differences, % |
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 |