GOST R 50429.9-92
«HH *n"71.M».M.away.354
Pear BSP
GOSUDARSTVENIY STANDARD ROSSISKAYA FEDERATION
GALLIUM Method of determining posford
Gallium.
Method for the determination of phosphorus
GOST P 50429.9−92
AXTU 1709
Date of introduction 01.01.94
This standard specifies the methods of extraction-photometric and visual-photometric determination of phosphorus in Gaul in the range of mass fraction from 1 • 10~5 to 1 • 10~4%.
1. GENERAL REQUIREMENTS
General requirements for methods of analysis and security requirements — according to GOST R 50429.0.
2. METHOD EXTRACTION-PHOTOMETRIC DETERMINATION OF PHOSPHORUS
2.1. The essence of the method
The method is based on the provisional transfer of gallium to the solution in the analytical autoclave, the extraction of gallium chloride by ether, selective extraction of phosphorus with a mixture of «-butanol with chloroform and subsequent determination in the restored molybdophosphoric of heteroalicyclic.
2.2. Apparatus, reagents and solutions
Autoclave analytical М167 design Giredmet or similar (drawing). When working with the autoclave should be strictly adhered to attached the manual.
Laboratory scales 1 grade according to GOST 24104.
Edition official
This standard may be fully or partially reproduced, duplicated or distributed without the permission of Gosstandart of Russia
GOST R C. 2
1 — housing of the autoclave, 2 — reaction capacity, 3 — collector, 4 — the lid of the reaction vessel 5 — housing cover of the autoclave, 6 locking device 7 is a tension nut, 8 — bottom refrigerator
Drying oven with thermostatic control, ensuring the heating temperature up to 250 °C*
The fan room.
The tweezers are made of Plexiglas or Teflon.
Phototechnologies FEK-56 or similar.
Separating funnel with a capacity of 50 Cm3.
Volumetric flasks with a capacity of 25; 100 cmand 1 DM3.
Pipettes with volume capacity of 1; 5 and 10 cm3.
The paper filter «red ribbon» with a diameter of 70 mm. Cylinder measuring capacity 10;. 25 cm3.
Hydrochloric acid of high purity according to GOST 14261, concentrated and the concentration is 6 mol/DM3.
Water deionized with a specific resistivity of 10 — 20 Mω-cm
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Ammonium molybdate according to GOST 3765, aqueous solution concentration of 100 g/DM3.
Chloroform technical according to GOST 20015.
Normal technical butyl alcohol according to GOST 5208.
Diethyl ether saturated with hydrochloric acid concentration is 6 mol/DM3.
Mixture for extraction: mixture of butyl alcohol and chloroform in a volume ratio of 3:7.
Glycerin according to GOST 6259.
Tin dichloride 2-water, a solution of glycerol concentration of 100 g/DM3 (dissolution is carried out by heating in a water bath).
Odnosemjannyj potassium phosphate according to GOST 4198.
Solution.phosphorus main: 0,438 g of single potassium phosphate is dissolved in water, transferred to a volumetric flask with a capacity of 1 DM3, was adjusted to the mark with water and mix.
1 cm3 of solution contains 100 µg of phosphorus.
A solution of phosphorus production: 10 cm3 the basic solution of phosphorus poured into a measuring flask with a capacity of 100 cm3, made up to the mark with water and mix.
1 cm3 the working solution contains 10 µg of phosphorus.
More dilute working solutions of phosphorus is prepared by successive dilution with water in volumetric ratio of 1:9 on the day of use.
2.3 analysis
2.3.1. Weighed samples of gallium by mass of 2 g is placed in the Teflon liner-the collection of analytical autoclave (see drawing), pour 5 cm3 of water. The liner with the contents set with tweezers in a reaction container in which a pre-zasirayut 20 cm3 of hydrochloric acid concentrated. Reaction capacity close lid and seal in a metal housing of the autoclave. The autoclave was placed in a preheated drying Cabinet and kept at a temperature of 200 °C for 3 h. the Autoclave is removed from the oven, cooled to room temperature using bottom of the refrigerator, razvernetsya, remove the reaction container, wipe the outside with cotton wool soaked with water and then with alcohol. Open the lid; take the tweezers liner-collection.
2.3.2. Solution of liner-collector is transferred to a measuring cylinder with a capacity of 10 cm3 and the volume was adjusted to 10 cm3 solution of hydrochloric acid concentration is 6 mol/DM3. The solution from the cylinder is transferred to a separatory funnel. Gallium is extracted with three portions of ether 10 cm3 within 2 min. of the Ethereal layer, Ambra-
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GOST R 50429.9−92 p. 4
charge, and the aqueous phase transferred in a separating funnel, poured in 8 cm3 of a solution of ammonium molybdate, 10 cm3 of the mixture for extraction. Shake the funnel for 2 min. Organic phase (lower layer) was filtered through a paper filter into a flask, add one drop of a solution of tin dichloride and stirred. Measure the optical density of the solution on the photoelectrocolorimeter in a ditch with thickness of the absorbing layer 50 mm at a wavelength of 630 nm. As a comparison, using a solution mixture for extraction. The mass of phosphorus in the sample is determined according to the calibration schedule.
In parallel through all stages of the analysis performed give control of the experience. The correction control experience should not exceed 0.02 mg of phosphorus.
2.3.3. Construction of calibration curve
In a series of separating funnels make 0-.00; 0,02; 0,05; 0,10; 0,20; 0,50; 1,0 cm3 working standard solution of phosphorus, which corresponds to 0,0; 0,2; 0,5; 1,0; 2,0; 5,0; 10,0 mcg phosphorus. Added to 10 cm3 solution of hydrochloric acid concentration is 6 mol/DM3, 8 cm3 of ammonium molybdate, 10 cm3 of the mixture for extraction. Shake the funnel for 2 min. Organic phase was filtered into a flask, add 1 drop of a solution of tin dichloride; mix. The optical density of the resulting solutions is measured as in section
Treatment results are in accordance with clause 4.
3. METHOD VISUAL-PHOTOMETRIC DETERMINATION OF PHOSPHORUS
3.1. The essence of the method
The method is based on the reaction of formation of molybdophosphoric heterophilically with the subsequent recovery in hydrochloric acid environment of ascorbic acid in the presence of potassium Armenonville, extraction concentration in isoamyl-tion of alcohol and the subsequent visual-photometric determination of phosphorus.
Gallium previously removed from the solution by extraction of its ether chloride.
3.2. Apparatus, reagents and solutions
Apparatus, reagents and solutions for section 2.2 with the addition of:
Tile laboratory electric power of 400 watts.
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C. 5 GOST R 5в429.9-Yes
The quartz glasses with a capacity of 50 cm3.
Glass clock with a diameter of 50 mm.
Cylinders for colorimetrically with a height of 180 mm and a Diameter of 15 mm,
Hydrochloric acid of high purity according to GOST 14261, concentrated, concentration 2 and 6 mol/DM3.
Ascorbic acid, an aqueous solution with a concentration of 17.6 g/DM3.
Ammonium molybdate according to GOST 3765, aqueous solution with concentration of 40 g/DM®.
Potassium armanavicius, an aqueous solution concentration of 3 g/DM3.
Isoamyl alcohol according to GOST 5830.
Nitric acid of high purity according to GOST 11125.
Mixture of nitric and hydrochloric acids: prepared before use by mixing the volumes of the acids taken in a ratio of 1:5.
3.3. Analysis
3.3.1. A portion of gallium by mass of 1 g is dissolved as specified in 2.2.1 or I.
3.3.2. A portion of gallium by mass of 1 g was placed in a quartz beaker, pour 5 cm3 of hydrochloric acid concentration is 6 mol/DM®, rinse the metal, the acid is carefully decanted and discarded.
In a glass pour 10 cm3 of the mixture of acids, a daily hour stackvm and conduct dissolution of the sample under low heat. The resulting solution was evaporated to dryness. The dry residue is dissolved in 5 cm3 of hydrochloric acid cocentrate 6 mol/DM®, the solution was transferred to a separatory funnel, the beaker is rinsed 5 cm3 of hydrochloric acid solution of the same concentration all translate into dividing1 funnel.
Gallium is extracted 10 cm3 of ether for 2 min. repeat the Extraction, the ether layer is discarded and the aqueous phase was transferred to a beaker and evaporated to dryness. The dry residue is dissolved in 2 cm® hydrochloric acid of concentration 2 mol/DM3, the solution is transferred into the cylinder for colorimetrically, washing away a small amount of water, then add 0.25 cm3 of a solution' of ammonium molybdate, 0.5 cm3 of a solution of ascorbic acid, 0.1 cm3 of a solution of potassium Armenonville, bring in th ' volume up to 10 cm3. After adding each reagent, the contents thoroughly mixed. Add 1 cm3 of isoamyl alcohol, shaken for 30 s and comparing the color intensity of the organic layer with scale solutions comparison after 5 min. at the same time through all stages of the analysis carried out two test experience.
GOST 9 W"L-M S. in
3.3.3. Preparation of the scale comparison
Into the cylinders for colorimeters Enter 0,00; 0,05; 0,10; 0,15; 0,20; 0,40; 0,60; 1,00 cm* the working solution of phosphorus (containing 1 µg/cm3 of phosphorus), which corresponds to 0,00; 0,05; 0,10; 0,15; 0,20; 0.40; 0,60; 1,00 mcg phosphorus. OO add 2 cm3 of hydrochloric acid concentration of 2 mol/DM®, 0.25 cm3 of a solution of ammonium molybdate, 0.5 cm3 of a solution of ascorbic acid, 0,1 eat3 solution of potassium Armenonville, bring the water volume up to 10 cm3. After each addition of reagent the contents carefully peremeshayte. Add 1 cm3 of isoamyl alcohol, shaken for 30 s. the color Intensity of the organic layer scale solutions comparison used to determine the phosphorus using 5 miy.
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of phosphorus (X) in percent is calculated by the formula
x=. U-*
t 7
where mi is the mass of phosphorus in the sample, µg,
t2 is the average mass of phosphorus in a control experiment, mkg, t — weight of gallium,
4.2. The result of the analysis taking the arithmetic average of the two results of parallel measurements carried out from separate batches.
The allowable discrepancy of the two results of parallel measurements and the two results of the analysis (the difference between larger and smaller) with confidence probability P-0.95 is shown in the table.
| Mass fraction of phosphorus, % | Allowable difference, % |
| 1.0* 10"5 | OD-10-' |
| 5.0 to GO-5 | 2.0−10-' |
| 1.0−10-4 | 0.3−10-' |
The allowable discrepancy for the intermediate mass fraction of phosphorus calculated using linear interpolation.
4.3. Control of the correctness analysis is carried out by additives according to GOST 25086.
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P. 7 GOST R 50429.9−92
INFORMATION DATA
1. DEVELOPED AND SUBMITTED by the Technical Committee TC 104 «of the Semiconductor and rare metals products»
DEVELOPERS:
V. A. Orlov, L. N. Bakin
2. APPROVED AND put INTO effect by the Resolution of Gosstandart of Russia from
3. INSTEAD, GOST 18637.9−77
4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced | Paragraph number section |
| GOST 3765−78 | 2.2, 3.2 |
| GOST 4198−75 | 2.2 |
| GOST '51208−81 | 2.2 |
| GOST 5830−79 | 2.2, 3.2 |
| GOST, 6250−75 | 2.2 |
| GOST 11125−78 | 2.2, 3.2 |
| GOST R 504219.0−92 | Sec. 1 |
| GOST 14261−77 | 2.2, 3.2 |
| GOST 20016−88 | 2.2 |
| GOST 24104−88 | 22 |
| GOST 25086−87 | 4.3 |
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Editor Y. V. Vinogradsky Technical editor G, L. Terebinthina Concealer, T. A. Vasilyeva
Put in LO nab.OLES. Sneaky, PECs. &ОДЭ4.90. UEL.: p. L. 5,13% UEL. cu.-Ott. Of 5.66. UC.-ed. L. 6J35. Edition of 366 copies, Ц36._
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