GOST 29103-91
GOST 29103−91
INTERSTATE STANDARD
TUNGSTEN, MOLYBDENUM
GENERAL REQUIREMENTS FOR METHODS OF CHEMICAL AND SPECTRAL ANALYSIS
Edition official
BZ I
And PC PUBLISHING house of STANDARDS, Moscow
UDC 669.27:543.06:006.354 Group B59
INTERSTATE STANDARD
TUNGSTEN, MOLYBDENUM
General requirements for methods of chemical
and spectral analysis GOST
29103−91
Tungsten, molybdenum.
General requirements for methods of chemical and spectral analysis
MKC 77.120.99
ОКС1У 1709_
Date of introduction 01.01.93
This standard specifies the General requirements for methods of chemical and spectral analysis in the metallic tungsten and molybdenum (powder, Fort. wire, rod, strip, foil), the oxide wool}) of frames, and molybdenum, tungsten acid, paravol Imamate ammonium, ammonium molybdate, molybdenum carbide.
I. GENERAL REQUIREMENTS
I… For tests and the preparation of solutions, reagents used distilled water according to GOST 6709. except where indicated to the application bendistillery-tion of water, and the chemicals qualifying OS.CH., H. h, h.d. a.
1.2. Sampling is carried out according to normative-technical documentation for this product.
1.3. Under the mass share solutions in the interest to understand the amount of a substance in grams in 100 g of solution.
1.4. In the expression «diluted 1:1, 1:2, etc.* the first digits stand for the volumetric part of concentrated acid, or any solution, the second volume of the water.
1.5. Mass fraction of a solution set not less than three batches of starting material and find the average value of three closely matching results.
1.6. The phrase «dissolution at high temperatures* indicates that an electric stove provides a temperature of 500 'C, «at the moderate heating* — 350' — 400 «, «under low heat* — 100 '-200 'C.
1.7. Weighing of batches is carried out with a maximum error of 0.0002 g.
1.8. The purity of the metals used for the preparation of standard solutions should be not less than 99.95%.
1.9. When photoelectrocolorimetry definitions, impurities build calibration graphs. on the x-axis which lay the contents of the element in grams, and the y — axis the value of the optical densities of the respective solutions.
1.10. The basis for the preparation of standard samples (CO) for the spectral analysis are oxides of tungsten and molybdenum. WITH prepared based on the content of metal impurities in the metallic tungsten and molybdenum. When calculating the content of impurities in the analyzed product is calculated the same way — metal to metal.
Before cooking WITH the metal oxides and the chlorides of sodium and potassium is calcined to constant weight at temperatures given in the table.
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C. 2 GOST 29103−91
| The name of the oxides and chlorides | Temperature about cal Icahn. • |
The name of the oxides and chlorides | Temperature nakali&Anija. • |
| Aluminum oxca (AljOs> | 10 (10−1100 | Calcium oxide (Cao) | 1100 |
| Vanadium oxide (VjOj) | 500 | Cobalt oxide (Co2 Oj) | 800 |
| Of bismuth oxide (BijOj) | 1000 | Silicon oxide (SiO?) | 1000−1100 |
| Tungsten oxide (WOj) | 650 | Magnesium oxide (MgO) | 900 |
| Hafnium oxide (Ngog's clock) | 900 | Manganese oxide (MnOj) | 500 |
| Iron oxide (Fe>Os) | 800 | Copper oxide (CuO) | 600 |
| Molybdenum oxide (Moos) | 450−550 | Lead oxide (RGO) | 250 |
| Arsenic oxide (As:Oj) | 100 | Of antimony oxide (Sb'Oj) | 600 |
| Sodium chloride (NaC'l) | 100−120 | Tantalum oxide (Tog) | 900 |
| Nickel oxide (Ni O?) | 400−500 | Titanium oxide (ThOs) | 900−1100 |
| Of niobium oxide (Nb^Os) | 900 | Chromium oxide (CR 03> | 900−1000 |
| Tin oxide (SnO) | 900−950 | Zinc oxide (ZnO) | 1000 |
| Cadmium oxide (C dO) | 900−1000 | Zirconium oxide (2W') | 900 |
| Potassium chloride (CC'1) | 100−120 |
1. 11. Based on the results of electrophoretic analytical line pairs and the build calibration curve for each analyzed element method (three standards), which find the mass percent of impurities in the sample.
1.12. To obtain three parallel measurements they take three sample and test portion prepared in the form of oxides, which fill the craters of the electrodes, and photographed spectra.
1.13. The final result of the analysis taking the arithmetic mean of results of three parallel definitions, the difference between them at a confidence probability P = 0.95 does not exceed specified in the standards of permissible differences.
1.14. For the result of spectral analysis taking the arithmetic mean of three parallel measurements with a confidence probability P= 0,95 when the condition
c,nJ v-c m.n5 z. z • s. Z
max mm ' '
where Cralft, Cmln — limit values of determined concentrations;
5 — relative standard deviation, specified in relevant tables _ standards for spectral analysis;
7 — arithmetic mean value of three parallel measurements.
If the condition is not met, the analysis is repeated and the result of the analysis taking the arithmetic mean of six parallel measurements. If the condition is not met in this case, carry out an additional averaging of samples weighing 2−5 g in a mortar with ethanol for 30−40 min.
1.15. The correctness of analysis results control using standard samples of similar chemical composition to the analyzed samples. The results of the analysis are considered correct if the difference between the certified content in the standard sample (Withя7) module and the mean value of parallel measurements does not exceed ' / allowed discrepancies (
A1-C) <4*
where d = 3,3 Sr C =" 3,3 S.
1.16. The entire analysis should be carried out under conditions that exclude the possibility of contamination. samples and sample comparison.
1.17. Allowed use of the equipment, materials, utensils and reagents, subject to obtaining the metrological characteristics are not worse than specified in Sool"estouy the standard methods of analysis.
GOST 29103−91 C. 3
2. SAFETY REQUIREMENTS
2.1. Chemical and spectral (emission and atomic absorption) methods of analysis must be performed in accordance with regulatory and technical documentation on safe conducting works in the chemical and spectral laboratories.
2.2. Laboratory facilities in which to conduct tests, including premises, which carry out the selection and study of samples must be equipped with exhaust ventilation in accordance with the requirements of GOST
2.3. General hygiene requirements for temperature, humidity, air velocity and contents of harmful substances in the air of the working area and laboratory facilities must meet the requirements of GOST 12.1.005 and GOST
2.4. Fire safety requirements when working in a chemical laboratory must comply with GOST
2.5. Requirements when working with flammable and explosive gases (acetylene, propane-butane, oxygen) should comply with GOST 12.1.010 and GOST 12.1.004, as well as safety regulations in the gas sector, approved by Gosgortekhnadzor of the USSR.
2.6. When you use gases in cylinders must comply with the rules for arrangement and safe operation vessels working under pressure, approved by Gosgortekhnadzor of the USSR.
2.7. The types of fire fighting equipment and extinguishing media must comply with GOST
2.8. Analytical room should be equipped with a heating furnace with ventilation cabinets, running water, Sewerage, chemical utensils, and work desks.
2.9. Work tables, cupboards and other laboratory furniture guy must have Gladky Yu surface coating which prevents contamination of the samples, and be mounted on legs with the preservation of free space to allow free cleaning of the floor beneath them.
2.10. It is necessary to provide a separate room for spectrographs, spectrophotometers. photoelectrocolorimeters, atomic absorption installations, photographic works, works on sample preparation and grinding of carbon electrodes.
2.11. In the room where the spectrographs, microphotometry, spectrometry and balance, not allowed to work with chemicals to prevent corrosion of metal parts of the instrument and damaging the optical components. Areas should be dry.
2.12. Used when performing spectral analysis equipment shall comply with the requirements of normative-technical documentation for its production.
2.13. Tripods spectrographs should have screens for protection against UV radiation, suction devices for removing from the air ozone, metal oxides, and carbon monoxide emitted in the sources of spectra excitation and bad acting on the body working. The machine tool for sharpening of electrodes should also have a suction device for removing dust prestigiosa.
2.14. Electrical appliances must conform to the rules of electrical devices approved by the Glavgosenergonadzora.
Electrical and electronic equipment shall meet the requirements of the standards, «Rules of technical operation and security services electrical industrial companies*, «electrical installation systems Rules» approved by Glavgosenergonadzora.
2.15. To prevent the possibility of accumulation of charges of static electricity, all equipment must be properly grounded in accordance with the requirements of the rules for electrical installations and devices grounding requirements GOST 1 '2.2.007.0 and GOST 21130.
2.16. Floors in all rooms that contain equipment with electric equipment (spectrographs, atomic absorption unit, etc.), should provide opportunities cleanliness of premises, equipment and electrical insulation. Sections of the floor at work at these devices should be covered with rubber mats.
2.17. Safety requirements when working with electronic equipment must comply with GOST 12.2.006**.
'On the territory of the Russian Federation GOST R IEC 60065−2002.
C. 4 GOST 29103−91
2. IS. Acid vapors and dry dust alkalis, acids, oxides and metals are irritating to the respiratory tract and mucous membranes of the eyes and nose. Acid and alkali, when applied to the skin, causing severe burns. According to GOST 12.1.005 mineral acids (hydrochloric acid, nitric acid) and alkali (calculated as sodium hydroxide and potassium) are to the 2nd class of hazard. The maximum allowable concentration of these substances in the air of working zone must meet the requirements of the FDI GOST
2.19. Control of content of harmful substances in the air of the working zone of production areas must be conducted in accordance with the requirements of GOST
2.20. Analysis of samples for harmful substances is carried out according to normative-technical documentation for methods of determination of harmful substances in the air, approved by the Ministry of health of the USSR.
2.21. Used in the spectral method of the analysis of gases, reagents and other raw materials must comply with the requirements of normative-technical documentation on them.
2.22. Storage of reagents and other raw materials must comply with the requirements of normative-technical documentation regulating their storage.
2.23. Sample preparation and standard samples is carried out in the pits.
2.24. Preliminary training in safe working practices in chemical (spectral) laboratory and rules for the treatment of protective equipment is conducted in accordance with GOST 12.0.004 and GOST
2.25. Depending on the analysis employed should be provided with bathrobes according to GOST 12.4.131 and GOST 12.4.132, rubber gloves according to GOST 20010, or GOST 3. aprons according to GOST 12.4.029, protective goggles according to GOST 12.4.0131, protective shields according to GOST 12.4.023 in accordance with the current normative-technical documentation for the provision of personal protective equipment.
1
On the territory of the Russian Federation GOST R 12.4.013−97.
GOST 29103−91 C. 5
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of metallurgy of the USSR
2. APPROVED AND promulgated by the Decree of Committee of standardization and Metrology of the USSR from
3. INSTEAD, GOST 14339.0−82, GOST 14338.0−82
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| Marking NTD, kogoro Dina link | Moyer paragraph |
| GOST 3−88 | 2.25 |
| GOST 12.0.004−90 | 2.24 |
| GOST 12.1.004−91 | 2.4: 2.5 |
| GOST 12.1.005−88 | 2.3: 2.18 |
| GOST 12.1.007−76 | 2.3: 2.19 |
| GOST 12.1.010−76 | 2.5 |
| GOST 12.2.006−87 | 2.17 |
GOST |
2.15 |
| GOST 12.4.009−83 | 2.7 |
| GOST 12.4.011−89 | 2.24 |
| GOST 12.4.013−85 | 2.25 |
| GOST 12.4.021−75 | 2.2 |
| GOST 12.4.023−84 | 2.25 |
| GOST 12.4.029 — 76 | 2.25 |
| GOST 12.4.131−83 | 2.25 |
| GOST 12.4.132−83 | 2.25 |
| GOST 6709−72 | 1.1 |
| GOST 20010−93 | 2.25 |
| GOST 21130−75 | 2.15 |
Editor L. I. Nakhimov Technical editor V. N. Prosacea Concealer L/.With. Kavasam/a DTP S. V. RHB+OI
ia. LII. N: 02354
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