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GOST 14316-91

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 14316−91 Molybdenum. Methods of spectral analysis


GOST 14316−91

Group B59

STATE STANDARD OF THE USSR

MOLYBDENUM

Methods of spectral analysis

Molybdenum. Spectrum analysis methods

AXTU 1709

Date of introduction 1993−01−01

INFORMATION DATA

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

DEVELOPERS

Y. A. Abramov, A. I. Skrypnyk, S. N. Suvorova, N. With. Borodin 3.Isaev, L. P. Nikitina, V. E. Chebotarev, A. N. Galkova, A. I. Davydova, G. A. Matyushin

2. APPROVED AND promulgated by the Decree of Committee of standardization and Metrology of the USSR from 11.10.91 N 1609

3. REPLACE GOST 14316−82

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
Paragraph number section
GOST 83−79
Sec. 3
GOST 166−89
Sec. 3
GOST 195−77
Sec. 3
GOST 1770−74
9.2
GOST 2603−79
10.2
GOST 3118−77
Sec. 3, 10.2
GOST 3773−72
Sec. 3
GOST 4160−74
Sec. 3
GOST 4232−74
Sec. 3
GOST 4233−77
Sec. 3, 9.2, 10.2
GOST 4234−77
Sec. 3, 9.2
GOST 4331−78
Sec. 3
GOST 4461−77
Sec. 3, 10.2
GOST 4463−76
Sec. 3
GOST 4470−79
Sec. 3
GOST 4517−87
10.2
GOST 4526−75
Sec. 3, 10.2
GOST 4530−76
10.2
GOST 5457−75
10.2
GOST 5542−87
9.2
GOST 5556−81
Sec. 3
GOST 6563−75
Sec. 3
GOST 6709−72
Sec. 3
GOST 8677−76
Sec. 3
GOST 9147−80
Sec. 3
GOST 9428−73
Sec. 3
GOST 10216−75
Sec. 3
GOST 10262−73
Sec. 3
GOST 10929−76
Sec. 3, 9.2, 10.2
GOST 11120−75
Sec. 3
GOST 14919−83
Sec. 3, 10.2
GOST 16539−79
Sec. 3
GOST 17433−80
10.2
GOST 18300−87
Sec. 3, 10.2
GOST 19627−74
Sec. 3
GOST 19908−90
Sec. 3
GOST 22300−76
Sec. 3
GOST 23676−79
Sec. 3
GOST 23711−79
Sec. 3
GOST 23932−90
9.2
GOST 24147−80
10.2
GOST 25664−83
Sec. 3
GOST 27068−86
Sec. 3
GOST 29103−91
Section.1, 2, 4.5, 5.1.5, 7.5, 8.5, 9.5
TU 2.034 57 485 42.32−89
9.2
THAT 6−09−36−78
10.2
THAT 6−43−147−88
Sec. 3
THAT 14−5-203−89
Sec. 3
THAT 48−12−52−88
Sec. 3
THAT 95−175−78
10.2
THAT 95−337−79
10.2



This standard specifies methods for determining the spectral content of impurity elements: aluminum, bismuth, tungsten, hafnium, iron, cadmium, potassium, calcium, cobalt, silicon, magnesium, manganese, copper, arsenic, sodium, Nickel, niobium, tin, lead, antimony, tantalum, titanium, chromium, zinc, zirconium in the metallic molybdenum (powder, rod billet, rod, strip, foil, ribbon, wire), molybdenum oxide, ammonium molybdate, molybdenum carbide.

1. GENERAL REQUIREMENTS

General requirements for methods of analysis GOST 29103.

2. SAFETY REQUIREMENTS

Safety requirements — according to GOST 29103.

3. MEASUREMENT MEANS, AUXILIARY DEVICES, MATERIALS AND REAGENTS

Universal arc generator operating in the mode of DC arc UGE-4, or any rectifier that provides DC current of 15 a at A voltage of 220 V. the voltage on the electrodes should be at least 40 V.

The installation of a photovoltaic type MFS-8, MFS-6, MFS-4, or any other such type.

The quartz type spectrograph ISP-30, ES-22, ES-28, or any other medium variance.

The type of spectrograph DFS-13 or DFS-8 with grille 600 PCs/mm operating in the first order, or any other large dispersion.

Spectromancer types of SPP-2, DSP-1, or any other similar type.

Microphotometer geregistreerde type MF-2, MF-4 in unregistered mode, or any other similar type.

Muffle furnace with thermocouple, providing heating to a temperature of 1100 °C.

Tile electrical with closed spiral PE-600−2 according to GOST 14919, or any other such type.

Drying oven or infra-red lamp for drying and coal blends.

Analytical scale types of VLA-200M, VLR-200 or other similar type.

Libra torsion bar type W, which required weighing accuracy.

Libra technical VSC-2 according to GOST 23676* or GOST 23711.
______________
* On the territory of the Russian Federation GOST 29329−92. — Note the manufacturer’s database.

Stopwatch for NTD.

Scalpel stainless steel spatula or organic glass.

Tweezers stainless steel.

Compaction of organic glass.

Mortar with pestle made of organic glass, chalcedony, agate or Jasper.

Box table for sample preparation WITH (standard samples) any design, easy to use.

Cup quartz GOST 19908 or platinum according to GOST 6563, cups varicellae according to GOST 9147.

The quartz crucible according to GOST 19908 or platinum according to GOST 6563.

Mortar mechanical or any other device providing the necessary mixing of the sample.

Table lathe machine or any other device for grinding coal and graphite electrodes.

Vernier caliper 0−125 the price of division of 0.05 mm, 0−250 division value 0.1 mm according to GOST 166.

Carbon electrodes with a diameter of 6 mm grades b-3, C-2, OS.h. 7−4.

Coal powder obtained by grinding coal, graphite electrodes, or powder grade OS.h. 7−4.

Graphite on the other 48−12−52−88 or the 14−5-203−89.

Photographic plates PFS-01, the SFC-02, the SFC-03, PFS-05, PFI-01 size 9x12, 9х24, 13x18 cm on the other 6−43−147−88 or other contrasting photographic plates.

Reliever quartz nine-and three-stage.

Medical absorbent cotton wool GOST 5556.

Nitric acid according to GOST 4461.

Aluminum oxide, anhydrous, h.d. a.

Vanadium oxide, H. h

Of hafnium oxide, H. h

Tungsten oxide spectral-clean

Molybdenum oxide spectral-net.

Bismuth oxide according to GOST 10216.

Hydrogen peroxide according to GOST 10929.

Iron oxide.

Cadmium oxide according to GOST 11120.

Calcium oxide according to GOST 8677.

Silicon oxide according to GOST 9428.

Potassium iodide according to GOST 4232.

Potassium chloride according to GOST 4234.

Magnesium oxide according to GOST 4526.

Manganese oxide according to GOST 4470.

The powdered copper oxide according to GOST 16539

Arsenic oxide, H. h

Sodium chloride according to GOST 4233.

Sodium fluoride according to GOST 4463.

Nickel oxide according to GOST 4331 or OS.h.

Of niobium oxide, OS.h.

Tin oxide, h.d. a.

Hydrochloric acid according to GOST 3118 surpassed.

The technical rectified ethyl alcohol according to GOST 18300.

Of lead oxide.

Antimony oxide, h.d. a.

Titanium oxide, h.d. a.

Chromium oxide anhydrous, h.d. a.

Zinc oxide according to GOST 10262.

Zirconium oxide, h.d. a.

The ethyl ether according to GOST 22300.

Possible to use other compounds with oxygen and reactants of brand h. d. a., OS.h. or H. h ensure the quality of the analyses.

Developer:

Solution I:

metol (pair-metilaminofenazon) according to GOST 25664 — 2 g;

hydroquinone (paradoxians) according to GOST 19627 — 10 g;

sodium sanitarily according to GOST 195 — 52 g;

potassium bromide according to GOST 4160 — 2 g;

distilled water according to GOST 6709 — up to 1000 cmГОСТ 14316-91 Молибден. Методы спектрального анализа.

Solution II:

the anhydrous sodium carbonate according to GOST 83 — 44 g;

distilled water according to GOST 6709 — up to 1000 cmГОСТ 14316-91 Молибден. Методы спектрального анализа.

The same volumes I and II solutions were poured together before manifestation, which is carried out at (20±1) °C.

Fixer:

Chernovetskiy sodium (sodium thiosulfate GOST 27068 — 300 g);

ammonium chloride according to GOST 3773 — 60 g;

sodium sanitarily according to GOST 195 — 45 g;

distilled water according to GOST 6709 — up to 1000 cmГОСТ 14316-91 Молибден. Методы спектрального анализа.

Allowed to use other contrast developer.

4. THE METHOD OF DETERMINING THE MASS FRACTION OF ALUMINUM, IRON, CALCIUM, SILICON, MAGNESIUM, MANGANESE, SODIUM AND NICKEL

4. THE METHOD OF DETERMINING THE MASS FRACTION OF ALUMINIUM (1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%),
IRON (4·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%), CALCIUM (2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%), SILICON (3·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%),
MAGNESIUM (2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%), MANGANESE (1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%), SODIUM (4·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%)
AND NICKEL (2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа%)

4.1. The essence of the method

The method is based on the excitation spectrum of the sample and standard sample, measuring the relative intensity of analytical lines defined by impurity elements. To mitigate the spectrum of foundations in the standard samples and test sample pre-injected coal powder, and to enhance the analytical lines — copper oxide.

4.2. Measuring instruments, accessories, reagents and materials

For the analysis of used equipment, materials and reagents is given in sect.3.

4.3. Preparation for assay

4.3.1. Preparation of samples for analysis

Samples of molybdenum and its compounds prior to analysis is transferred to the oxide of molybdenum in two ways.

4.3.1.1. First method: calcination in a muffle furnace.

Samples of molybdenum in the form of shavings, small pieces of rod billet, rod, ribbon or wire, pre-washed with ether to remove traces of grease and dried in air or at temperatures above 50 °C. To remove mechanical impurities introduced during grinding, the sample is treated in a distilled hydrochloric acid (1:1) by heating for 5−10 min. From the aquadag surface of the wire is cleaned by etching in a boiling hydrogen peroxide solution with a mass fraction of 3%. Then washed twice with distilled water.

Clean shavings, pieces of wire, metal alloy powder and molybdenum carbide calcined in a muffle furnace at 500−550 °C until complete transfer of samples in the molybdenum oxide. The calcination is carried out in quartz or platinum crucibles or cups.

Samples of ammonium is placed in a cold muffle furnace, set the thermostat at 400−450 °C and include. The calcination is carried out for about 2 hours until complete decomposition of the ammonium molybdate and the formation of molybdenum oxide (MooГОСТ 14316-91 Молибден. Методы спектрального анализа).

4.3.1.2. The second method: dissolving the sample in acid or hydrogen peroxide. Samples from the molybdenum rod billet, rod, ribbon, metallic molybdenum in the form of small chips and a molybdenum wire with a diameter greater than 40 µm prior to oxidation is cleaned from surface contamination as specified in clause 4.3.1.1.

Next the samples are dissolved in a mixture of hydrochloric and nitric acids in the ratio 3:1 or the hydrogen peroxide solution with a mass fraction of 3% until completely dissolved at low heat (1−3 g of molybdenum by 10−30 cmГОСТ 14316-91 Молибден. Методы спектрального анализаof the mixture of acids).

The dissolution is carried out in platinum cups. The solutions were evaporated, the residue is calcined at about 20 min in a muffle furnace at temperature 400−450 °C to obtain a molybdenum oxide (MooГОСТ 14316-91 Молибден. Методы спектрального анализа).

Note. For dissolving use ultra-pure hydrochloric and nitric acid.

Hydrochloric acid, free from impurities, is obtained by saturation. To do this in a desiccator (or other sealed container), pour concentrated hydrochloric acid, then the stand is placed glass polyethylene, PTFE, filled with double-distilled water. The volume ratio of water and acid should be 1:6. The desiccator tightly closed ground cover. After 4−5 days the resulting hydrochloric acid solution is drained from the plastic Cup in a plastic flask.

Nitric acid ultra pure get in apparatus for the distillation-type PC in accordance with the instructions for the device.

4.3.2. Preparation of standard samples

Preparation of standard samples are given in Appendix 1.

4.3. Preparation of carbon electrodes and carbon mixtures

The electrodes are machined, as indicated on the devil.1 (a, in) and the table.1 (type I, V), and burn in the arc of a DC at a current of 10−15 And 15−20 C.

ГОСТ 14316-91 Молибден. Методы спектрального анализа


Damn.1

Table 1

mm

                       
Type

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

ГОСТ 14316-91 Молибден. Методы спектрального анализа

I
40−60
3±0,1
-
-
-
-

6ГОСТ 14316-91 Молибден. Методы спектрального анализа

3±0,1
-
-
-
II
40−60
3±0,1
-
-
-
-

6ГОСТ 14316-91 Молибден. Методы спектрального анализа

3,5±0,1
-
-
-
III
40−60
-
9±0,1
11±0,1
22±0,1
-

6ГОСТ 14316-91 Молибден. Методы спектрального анализа

-
4±0,1
3±0,1
-
IV
40−60
4±0,1
-
-
-
-

6ГОСТ 14316-91 Молибден. Методы спектрального анализа

4±0,1
-
-
-
V
40−60
-
-
-
-
10−12

6ГОСТ 14316-91 Молибден. Методы спектрального анализа

-
-
-
3±0,1



A coal mixture consisting of carbon powder and copper oxide with a mass fraction of 3%, prepared by mixing in a mortar: in the beginning the mixing is done dry for 20−30 min, then alcohol is added and stirred for another 75 min. the Alcohol is added several times as it evaporates, keeping the mixture in the form of thick cream. The mixture is then dried at a temperature not above 70 °C. thereafter, the mixture was stirred for 30−40 min and finally dried at (105±5) °C in a drying Cabinet or under an infrared lamp. To prepare 10 g of a mixture requires a 30−40 cmГОСТ 14316-91 Молибден. Методы спектрального анализаof alcohol.

4.4. Analysis

Prepared for analysis according to claim 4.3.1 sample and mixed for 5−6 min in a mechanical mortar or for 10 min by hand with a charcoal mixture (p.4.3.3) in a 1:1 ratio (100 mg of MooГОСТ 14316-91 Молибден. Методы спектрального анализаand 100 g of coal mix; mortar and pestle is rubbed with cotton wool soaked with alcohol after each mixing (1 cmГОСТ 14316-91 Молибден. Методы спектрального анализаper sample). Sample sample WITH and coal mixture for torsion or analytical balance. The resulting mixture was placed in craters of the electrodes and compacted to the brim with a scalpel or use other methods of compaction of the mixture.

Evaporation of the sample and the excitation spectrum is carried out in the arc DC. The electrode with the sample serves as the anode of the arc. Calcination is carried out for 5 s at a current of 5 A. the Spectra are photographed on the spectrograph medium dispersion at a current of 5 A with an exposure of 15−20 C. the illumination of the slit of a spectrograph — being with a round aperture in the intermediate or single-lens condenser with the condenser ГОСТ 14316-91 Молибден. Методы спектрального анализа75 mm.

Arc gap — 2 mm. Width of slit of a spectrograph of 0.1 to 0.012 mm.

Photographed in the spectrum 3 (3 electrode) of each and sample.

The cassette is placed a photographic plate type PFS-01. Allowed to use other photographic plates on which it is possible to obtain analytical lines in the region of normal pochernenija.

4.5. Processing of the results

The resulting spectrograms photometric blackening of analytical lines given in table.2. When the selected photography of the spectra of black lines must be within the scope of normal pochernenija.

Table 2

       
Identify the elements Wavelengths, nm
The ranges defined by mass fraction, %
  lines of impurity
lines of comparison
 
Aluminium
308,215
Copper 309,399

1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

  257,510
Copper 276,887

5·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Iron
259,837
Copper 276,887

2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

  302,064
Copper 303,610
 
Calcium
317,933
Molybdenum 317,681*

2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Silicon
251,432
Copper 276,887

3·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Magnesium
277,669
Copper 276,887

2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Manganese
294,921
Copper 288,293

1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

  293,306
Copper 288,293
 
Sodium
330,237
Copper 309,399

4·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Nickel
305,082
Copper 309,399

2·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-3·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

________________
* Measured blackening of the line of molybdenum 317,681 nm to account for the superimposing of molybdenum 317,932 nm as background in the line of calcium 317,933 nm.


Find the difference pucherani analytical lines and lines of comparison ГОСТ 14316-91 Молибден. Методы спектрального анализаand average for. According to table.27, are given in Appendix 2, determine ГОСТ 14316-91 Молибден. Методы спектрального анализаfor calcium.

If the lovers are in the field of neoteric (exaggerations), the transition intensities is carried out using a characteristic curve of photographic plates.

Calibration curve constructed in the coordinates ГОСТ 14316-91 Молибден. Методы спектрального анализа.

To determine the calcium calibration curve constructed in the coordinates

ГОСТ 14316-91 Молибден. Методы спектрального анализа.

For each of the three obtained values ГОСТ 14316-91 Молибден. Методы спектрального анализа, ГОСТ 14316-91 Молибден. Методы спектрального анализаfor the analyzed elements using the calibration curve find the corresponding mass fraction ГОСТ 14316-91 Молибден. Методы спектрального анализа. The final result of the analysis taking average value of three parallel measurements, if the condition specified in GOST 29103.

Wavelength of analytical line pairs and the mass fraction ranges shown in table.2.

The values of relative average squared deviations for the ranges of mass fraction of detectable elements are shown in table.3.

Table 3

       
Identify the elements

The values ГОСТ 14316-91 Молибден. Методы спектрального анализаfor the ranges of mass fraction

 

1·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-4·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

4·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-16·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

16·10ГОСТ 14316-91 Молибден. Методы спектрального анализа-6·10ГОСТ 14316-91 Молибден. Методы спектрального анализа

Aluminium
0,24
0,22
0,20
Iron
0,19
0,18
0,15
Calcium
0,24
0,20
0,18
Silicon
0,21
0,18
0,17
Magnesium
0,22
0,17
0,15
Manganese
0,21
0,19
0,18
Sodium
-
0,22
0,19
Nickel
0,15
0,13
0,12