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GOST 18385.5-89

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 18385.5−89 Niobium. Method for determination of silicon


GOST 18385.5−89

Group B59


STATE STANDARD OF THE USSR


NIOBIUM

Method for determination of silicon

Niobium. Method for the determination of silicon


AXTU 1709

Valid from 01.01.91
before 01.01.96*
_______________________________
* Expiration removed
Protocol 5−94 N Interstate Council
for standardization, Metrology and certification
(IUS N 11/12, 1994). — Note the manufacturer’s database.


INFORMATION DATA

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

DEVELOPERS

A. V. Elyutin, L. N. Filimonov, E. S., Blinov, D. I. Guzeev, A. S. Terekhov

2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 11.12.89 N 3644

3. INTRODUCED FOR THE FIRST TIME

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
 Item number
GOST 4212−76
 Sec. 2
GOST 4640−84
 Sec. 2
GOST 10157−79
 Sec. 2
GOST 13079−81
 Sec. 2
GOST 18289−78
 Sec. 2
GOST 18300−87
 Sec. 2
GOST 18385.0−89
 1.1



This standard establishes the atomic absorption method for determination of silicon in metallic niobium from 1·10ГОСТ 18385.5-89 Ниобий. Метод определения кремнияto 1·10ГОСТ 18385.5-89 Ниобий. Метод определения кремния%.

The method is based on the electrothermal atomization of silicon direct loading of metallic niobium sample into the furnace atomizer (cell).

1. GENERAL REQUIREMENTS

1.1. General requirements for method of analysis according to GOST 18385.0.

2. APPARATUS, MATERIALS, REAGENTS AND SOLUTIONS


Spectrophotometer atomic absorption the Perkin-Elmer model 300 or a similar device designed for work with graphite (cuvette) oven.

The hollow cathode lamp for silicon type of LSP or similar.

Analytical scale.

Volumetric flasks 2−50−2, 2−100−2, 2−1000−2.

The beakers capacity 50, 100 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния.

Pipette 2−2-5, 2−2-10, 2−2-25.

Distilled water, double-distilled.

Filter paper.

Argon according to GOST 10157.

Sodium silicate according to GOST 13079.

Sodium volframovich 2-water according to GOST 18289, a solution with a mass fraction of 5%: suspension of sodium volframovich 2-water 5.0 g of sodium dissolved in distilled water and transferred into a flask with a volume of 100 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния.

The technical rectified ethyl alcohol according to GOST 18300.

Mineral wool GOST 4640*.
______________
* On the territory of the Russian Federation GOST 4640−93. — Note the manufacturer’s database.

Solutions comparison

Solution a (spare): the hitch weight 2,6522 g previously calcined and brought to constant weight of sodium silicate dissolved in distilled water and transferred to volumetric flask 1000 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния. The solution was adjusted to the mark with bidistilled water and mix; 1 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof solution contains 1 mg of silicon; test according to GOST 4212.

Solution B: aliquot part of the solution And a volume of 10 cm,ГОСТ 18385.5-89 Ниобий. Метод определения кремнияtransferred to a volumetric flask with a capacity of 100 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния, made up with bidistilled water to the mark and mix; 1 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof a solution contains 0.1 mg of silicon.

Solution: aliquot part of a solution with a volume of 10 cm,ГОСТ 18385.5-89 Ниобий. Метод определения кремнияtransferred to a volumetric flask with a capacity of 100 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния, adjusted to the mark with bidistilled water and mix; 1 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof the solution contains 0.01 mg of silicon.

Solutions comparison of silicon (ГОСТ 18385.5-89 Ниобий. Метод определения кремния), containing 0,0005; 0,001; 0.002 mg/cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof silicon at three volumetric flasks with a capacity of 100 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияis administered 5, 10, 20 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияsolution, poured with bidistilled water to the mark and mix.

Solution comparison of silicon ГОСТ 18385.5-89 Ниобий. Метод определения кремнияcontaining 0.005 mg/cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof the silicon: selected 25 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияof the solution, place it in a flask with a capacity of 50 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния, mediterreano poured water up to the mark and mix.

Solutions comparison of silicon ГОСТ 18385.5-89 Ниобий. Метод определения кремнияprepared on the day of analysis samples. The analysis for the unit of measurement is consumed of 0.02 cmГОСТ 18385.5-89 Ниобий. Метод определения кремнияsolution comparison. The absolute amount of silicon in the volume ГОСТ 18385.5-89 Ниобий. Метод определения кремния, ГОСТ 18385.5-89 Ниобий. Метод определения кремния, ГОСТ 18385.5-89 Ниобий. Метод определения кремния, ГОСТ 18385.5-89 Ниобий. Метод определения кремнияis 1·10ГОСТ 18385.5-89 Ниобий. Метод определения кремния, 2·10ГОСТ 18385.5-89 Ниобий. Метод определения кремния, 4·10ГОСТ 18385.5-89 Ниобий. Метод определения кремния, 1·10ГОСТ 18385.5-89 Ниобий. Метод определения кремнияg, respectively.

3. ANALYSIS


Graphite furnace prepare: in a glass with a solution of tungstate of sodium is placed vertically 8−10 graphite a ditch, soaked for 2−3 h. Then the cuvette is removed from the solution and dried in a drying Cabinet at a temperature of 120 °C, positioning a boot up the hole. After drying, the cell was calcined under the conditions of 100 °C — 30 s, 1000 °C — 10 s, 2600 °C 30 s. the Entire operation is repeated twice.

After preparing the device for use according to instructions the sample with a mass of 15−30 mg were placed in a cuvette with a syringe-spatula, turn the flow of water and argon, and then include the heating of the cuvette in accordance with the following modes in the table. The same operation is done for comparison solutions used to build calibration curve.

     
The parameters of the device
 Mode
  Solution comparison
 The analyzed sample
Supply current, mA (lamp LSP)
 30
 30
Wavelength, nm
 251,61
 251,61
Temperature, °C
 110
 -
Drying time,
 30
 -
The atomization temperature, °C
 2400
 2400
The time of atomization, with
 60
 120
Time of cooling of the graphite furnace with
 40
 40



Alcohol consumption before installation of the cell and replacement of the graphite contacts is 5 cmГОСТ 18385.5-89 Ниобий. Метод определения кремния.

The cuvette is recommended to be changed after every 50 samples.

4. PROCESSING OF THE RESULTS

4.1. The area of the absorption signal, obtained from the solution of the comparison calculated by the formula of area of triangle. Measurement solutions comparison build the calibration curve: area under the curve of absorption — mass of the element.

In the analysis of niobium metal, the absorption signal of silicon markedly tightened, so the area under the curve (ГОСТ 18385.5-89 Ниобий. Метод определения кремнияmm)ГОСТ 18385.5-89 Ниобий. Метод определения кремния, calculated by the formula

ГОСТ 18385.5-89 Ниобий. Метод определения кремния,


where ГОСТ 18385.5-89 Ниобий. Метод определения кремния — the maximum height of the signal absorption, mm;

ГОСТ 18385.5-89 Ниобий. Метод определения кремнияand ГОСТ 18385.5-89 Ниобий. Метод определения кремния — time corresponding to the distance of registerme from the moment the signal absorption up to 40 and 120 s, respectively:

ГОСТ 18385.5-89 Ниобий. Метод определения кремнияand ГОСТ 18385.5-89 Ниобий. Метод определения кремния — height of the absorption signal at time ГОСТ 18385.5-89 Ниобий. Метод определения кремнияand ГОСТ 18385.5-89 Ниобий. Метод определения кремния, respectively, mm

.

4.1.1. According to the calibration schedule find a lot of silicon in the sample. Mass fraction of silicon (ГОСТ 18385.5-89 Ниобий. Метод определения кремния) in percent is calculated by the formula

ГОСТ 18385.5-89 Ниобий. Метод определения кремния,


where ГОСТ 18385.5-89 Ниобий. Метод определения кремнияis the mass of silicon was found in the calibration schedule, the sample mass ГОСТ 18385.5-89 Ниобий. Метод определения кремния, g.

For the result analysis (aГОСТ 18385.5-89 Ниобий. Метод определения кремния) taking the arithmetic average of results of five parallel measurements. The absolute value of the difference between the maximum and minimum results with a confidence probability ГОСТ 18385.5-89 Ниобий. Метод определения кремнияof 0.95 should not be more ГОСТ 18385.5-89 Ниобий. Метод определения кремния. The absolute value of the difference between two tests with confidence probability ГОСТ 18385.5-89 Ниобий. Метод определения кремнияof 0.95 should not be more ГОСТ 18385.5-89 Ниобий. Метод определения кремния.

5. VALIDATION RESULTS


The correctness of the results of the analysis check method variable sample. Three sample samples weighing approximately 10 mg and three sample twice analyzed in sect.3 and 4.

The difference between the highest and lowest of the arithmetic average of the results of two determinations from a sample weight of approximately 10 and 20 mg should not exceed the value permissible discrepancies in the results of the two analyses for the mass fraction of the element corresponding to the average result of all definitions.