GOST 18904.8-89

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-189048-89.pdf (215.92 KiB)
ГОСТ 18904.8-89

GOST 18904.8−89 Tantalum and its oxide. Spectral method for the determination of tungsten, calcium, cobalt, copper, molybdenum and sodium

GOST 18904.8−89
Group B59

STATE STANDARD OF THE USSR

TANTALUM AND ITS OXIDE

Spectral method for the determination of tungsten, calcium, cobalt,
copper, molybdenum and sodium

Tantalum and its oxide. Spectral method for determination of tungsten,
calcium, cobalt, copper, molybdenum and sodium

AXTU 1709

Valid from 01.01.90
to 01.01.95*
__________________________________
* Expiration removed
Protocol N 4−93 inter-state Council
for standardization, Metrology and certification
(IUS N 4, 1994). — Note the manufacturer’s database.

INFORMATION DATA

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

PERFORMERS

M. V. Vladimirova, N. Arakelian, B. M. Dobkin, R. F. Makarov, A. S. Terekhov

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 20.03.89 N 563

3. REPLACE GOST 18904.7−73, GOST 18904.8−73

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS


The designation of the reference document referenced	Section number, paragraph
GOST 4142−77	2
GOST 4145−74	2
GOST 4158−80	2
GOST 4210−77	2
GOST 4233−77	2
GOST 4467−79	2
GOST 5962−67	2
GOST 16539−79	2
GOST 18300−87	2
GOST 18904.0−89	1.1
GOST 18904.6−89	3.2
GOST 21241−77	2

This standard establishes a spectral method for the determination of impurities of tungsten, calcium, cobalt, copper, molybdenum, and sodium tantalum (previously translated into oxide) and their oxides.

The method is based on excitation and registration (photographic or photoelectric) arc emission spectra of analyzed samples and sample comparison.

Intervals determined by a mass fraction of impurities:


tungsten	from	1·10	to	1·10;

calcium	«	1·10	«	3·10;

cobalt	«	1·10	«	1·10;

copper	«	1·10	«	3·10;

molybdenum	«	1·10	«	1·10;

sodium	«	1·10	«	1·10.

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis and security requirements — according to GOST 18904.0 with the addition of: analysis result should be the arithmetic mean of two parallel definitions, each of which perform a separate sample.

2. APPARATUS, MATERIALS AND REAGENTS

The diffraction type spectrograph DFS-13 with the grating 600 gr/mm or similar.

Photovoltaic installation of DFS-DFS or 36 to 44.

Electronic computing machine «Iskra-1256» or «D-3−28» or similar type.

Generator UGE-4 or the rectifier 250 to 300 V, 20−30 A.

Microphotometer type MF-2 or similar.

Spectromancer PS-18 or similar.

Analytical scale.

Libra technical.

Shaker or other device for mixing and grinding samples.

Mortars and pestles of tantalum and organic glass.

Oven muffle.

Drying Cabinet.

Tile electric.

Grinding machine carbon electrodes.

Coals spectral high purity-7−3 or C-3, with a diameter of 6 mm.

Electrodes machined from the spectra of coals:

type «glass»: the crater diameter — 4 mm, the crater depth — 4 mm, height of outer wall — 5 mm, pin height — 3 mm leg diameter — 2.5 mm;

diameter — 4 mm, the height of the sharpened part is 10 mm.

Medical forceps according to GOST 21241.

Measurer stainless steel.

Barium carbonate according to GOST 4158.

Tungsten (VI) oxide.

Potassium sulfate according to GOST 4145.

Calcium nitrate 4-water according to GOST 4142.

Cobalt (II, III) oxide according to GOST 4467.

Copper (II) oxide according to GOST 16539.

Molybdenum (VI) oxide.

Sodium chloride according to GOST 4233.

Lead dichloride according to GOST 4210.

Rectified ethyl alcohol according to GOST 5962* or technical rectified ethyl alcohol according to GOST 18300.
_______________
* On the territory of the Russian Federation GOST R 51652−2000. — Note the manufacturer’s database.

Antimony (III) oxide.

The powdered tantalum of high purity or tantalum (V) oxide, pure for specific impurities.

Photographic plates of the spectral type I, type II, ES or equivalent, providing normal blackening photometrically lines and the background spectrum.

Developer contrast.

Fixer is acidic.

Standard solution of calcium with a mass concentration of 10 mg/cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия : sample nitrate calcium weight 5,8902 g dissolved in water, transferred to a volumetric flask of 100 cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия , adjusted to the mark with water and mix.

3. PREPARATION FOR ASSAY

3.1. Preparation of the buffer mixture

A portion of chloride of lead with a mass of 7.4 g of potassium sulfate with a mass of 2.5 g, barium carbonate with a mass of 0.25 grams of antimony oxide with a mass of 0.1 g of thoroughly triturated in a mortar for 1.5−2 h on the shaker for 40−50 min.

3.2. Sample preparation comparison (OS)

References are prepared according to GOST 18904.6.

3.2.1. The head sample comparison (GOS) is prepared by mixing the base with the solution of calcium, previously calcined oxides of tungsten, cobalt, copper, molybdenum, and chloride of sodium.

The platinum Cup is placed 11,4775 g bases, injected 18 cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия standard solution of calcium on the tile are dried and calcined in a muffle furnace at 750 °C for 1 h. After cooling, transferred into tantalum mortar, add 0,1261 g of an oxide of tungsten (VI), 0,1362 g of cobalt oxide (II, III) 0,1252 g of copper oxide (II), 0,1500 g of an oxide of molybdenum (VI) and 0,2540 of sodium chloride, thoroughly grind the tantalum pestle for 1.5−2 h on the shaker for 40−50 min.

The received STATE is stored in a hermetic glass jar.

Other operating systems prepare serial dilution of GOS and subsequent OS basis. The mass fraction of the designated impurities in the percentage of the sum of the metals tantalum and impurities and added to the mixture sample diluted basis and OS are shown in table.1.

Table 1


Marking sample	Mass fraction of tungsten, calcium, cobalt, copper, molybdenum, sodium, %	The mass of charge, g
		the basics	diluted sample (marking sample)
STATE	1,0	-	-
OS-1	1·10	8,8521	1,0000 (STATE)
OS-2	3·10	31,8031	1,0000 (STATE)
OS-3	1·10	8,9852	1,0000 (OS-1)
OS-4	3·10	8,9955	1,0000 (OS-2)
OS-5	1·10	8,9985	1,0000 (OS-3)
OS-6	3·10	9,0000	1,0000 (OS-4)
OS-7	1·10	9,0000	1,0000 (OS-5)

Each reference sample is mixed with a buffer mixture in the ratio of 5:1 by weight in a mortar for 1 h on the shaker for 30 min. Ready OS stored in tightly closed glass jars.

Allowed trade OS using other quantities of the mixed substances by storing values of the mass fraction specified in the standard.

4. ANALYSIS

4.1. Preparation of samples for analysis

A sample of the metal converted into oxide according to GOST 18904.6. The analyzed oxide is mixed with the buffer mixture in the ratio of 5:1 by weight in a mortar or on the shaker for 10−15 min.

When taking batches boats, spatulas and other tools rubbing alcohol (0.5 cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия per sample).

When mixing mortars, pestles or part of vibrostanok washed with water and rubbing alcohol (2 cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия per sample).

4.2. Excitation spectra

The analyzed samples and the OS mixed with the buffer mixture, with the measuring device placed in the form of briquettes weighing 50 mg in craters of the carbon electrodes of the type «glass». The height of the briquette is 3.4−3.6 mm. not getting particles in the sample on the end of the electrode.

After each sample the dipstick clean with a cotton swab moistened with alcohol (0.5 cm ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия ).

The electrodes with the samples serve as the anode. The upper electrode machined to a diameter of 4 mm, serves as a cathode. The amperage of the arc And 11−13, the time of exposure was 20 s, in the interelectrode gap is 2.5 mm, the lighting system is being.

4.3. Check spectra

4.3.1. While photographic registration, the slit width of the spectrograph DFS-13 12−15 µm, photographed spectral range 300−400 nm. On the plate 3 photograph of the spectrum of each sample and of each OS. Photographing is repeated twice.

Take pictures of every portion of the prepared (mixed with the buffer mixture) from one sample to the original sample of oxide (or oxidized metal samples), two photos three times on each plate.

After photographing the spectra show photographic plates, washed, fixed, washed in running water and dried.

4.3.2. With the photoelectric registration of the width of the entrance slit of a photovoltaic plant DFS-36 (DFS-44) of 0.15−0.20 microns, and lighting system — two -.

Register two spectrum one portion is prepared (mixed with the buffer mixture) from one sample to the original sample of oxide (or oxidized samples of the metal).

5. PROCESSING OF THE RESULTS

5.1. Photographic plates photometrist on microphotometer. On each spectrogram to measure the blackening of analytical lines and lines of comparison, calculate the difference of pucheranii ( ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия ), find the arithmetic average for the three spectrograms obtained from the same sample. The wavelengths of the analytical lines and lines of comparison are shown in table.2.

Table 2


The designated element	Wavelength, nm		Element comparison	The interval defined by the mass fraction of impurities, %
	analytical lines	comparison lines
Tungsten	400,87	323,25	Antimony	1·10 — 3·10
	397,93	323,25	Antimony	1·10 — 1·10
	400,87*	287,8*	Antimony	1·10 — 1·10
Copper	324,75	323,25	Antimony	1·10 — 3·10
	327,40	323,25	Antimony	3·10 — 1·10
	324,75*	287,8*	Antimony	1·10 — 3·10
Molybdenum	390,29	323,25	Antimony	1·10 — 3·10
	319,40	323,25	Antimony	1·10 — 3·10
	320,88	323,25	Antimony	1·10 — 1·10
	319,40*	287,8*	Antimony	1·10 — 1·10
	390,30*	287,8	Antimony	1·10 — 1·10
Calcium	399,85	399,34	Barium	1·10 — 3·10
	422,67*	393,6*	Barium	1·10 — 1·10
Cobalt	345,35	323,25	Antimony	1·10 — 3·10
	340,51	323,25	Antimony	1·10 — 1·10
	345,35*	287,8*	Antimony	1·10 — 1·10
Sodium	330,30	323,25	Antimony	1·10 — 3·10
	330,23	323,25	Antimony	1·10 — 1·10
	330,30*	287,8*	Antimony	1·10 — 1·10
	330,23*	287,8	Antimony	1·10 — 1·10

_______________
* Lines used in photoelectric registration.

5.2. At the output of the photovoltaic installation (display of digital voltmeter or tape tsifropechatayuschee device), get values ( ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия ), which is proportional to the logarithm of the relative intensity of the analytical lines and comparison lines (tab.2).

5.3. For each user-defined impurities build a calibration curve: the abscissa shows the delay value ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия , where — mass fraction determined by the impurities in the OS, the axis of ordinate delay averaged values of the analytical signal ( ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия or ) of the respective OS. The graphs and average values of the analytical signal obtained for the spectra of samples, find the values of the mass fraction of the designated impurities in the analyzed samples.

5.3.1. While photographic registration of the spectrum for the result of one of parallel measurements take the average of the results obtained on two photographic plates, each of which is the average of the three spectrograms.

5.3.2. By the photoelectric registration of spectrum for the result of one of parallel measurements take average of the results of measurements of analytical signals of the two spectra.

5.4. Allowed to carry out the analytical signals with the help of computers «Iskra-1256» or similar programs approved in the prescribed manner.

5.5. The absolute value of the difference of the two results of parallel measurements (rate of convergence) and two test results (index of reproducibility), which is numerically equal, with a probability ГОСТ 18904.8-89 Тантал и его окись. Спектральный метод определения вольфрама, кальция, кобальта, меди, молибдена и натрия of 0.95, should not exceed the values of permissible differences given in table.3.

Table 3


The designated element	Mass fraction, %	Allowable difference, %
		when the spectrophotometer photographic analysis	when the spectrophotometer photovoltaic analysis
Sodium	1·10	7·10	4·10
	1·10	7·10	4·10
	1·10	5·10	4·10
	1·10	5·10	4·10
Tungsten, calcium, cobalt, copper, molybdenum	1·10	5·10	4·10
	1·10	5·10	4·10
	1·10	5·10	4·10
Calcium, copper	3·10	1,4·10	1·10
Tungsten, cobalt, molybdenum	1·10	5·10	4·10

Allowable differences for intermediate values of mass fraction are calculated by using linear interpolation.

5.6. Allowed the use of other techniques of analysis on metrological characteristics are not inferior to mentioned in the standard.

GOST 18904.8-89

GOST 18904.8−89 Tantalum and its oxide. Spectral method for the determination of tungsten, calcium, cobalt, copper, molybdenum and sodium

2. APPARATUS, MATERIALS AND REAGENTS

3. PREPARATION FOR ASSAY

4. ANALYSIS

5. PROCESSING OF THE RESULTS

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GOST 18904.8-89

GOST 18904.8−89 Tantalum and its oxide. Spectral method for the determination of tungsten, calcium, cobalt, copper, molybdenum and sodium

2. APPARATUS, MATERIALS AND REAGENTS

3. PREPARATION FOR ASSAY

4. ANALYSIS

5. PROCESSING OF THE RESULTS

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