GOST 14316-91

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  ГОСТ 14316-91

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

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 cm.

Solution II:

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

distilled water according to GOST 6709 — up to 1000 cm.

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 cm.

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 (1·10-6·10%),
IRON (4·10-6·10%), CALCIUM (2·10-6·10%), SILICON (3·10-6·10%),
MAGNESIUM (2·10-6·10%), MANGANESE (1·10-6·10%), SODIUM (4·10-6·10%)
AND NICKEL (2·10-6·10%)

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 (Moo).

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 cmof 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 (Moo).

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.

Damn.1

Table 1

mm

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 cmof 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 Mooand 100 g of coal mix; mortar and pestle is rubbed with cotton wool soaked with alcohol after each mixing (1 cmper 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 75 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

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* 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 and average for. According to table.27, are given in Appendix 2, determine for 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 .

To determine the calcium calibration curve constructed in the coordinates

.

For each of the three obtained values , for the analyzed elements using the calibration curve find the corresponding mass fraction . 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