GOST 13637.9-93
GOST 13637.9−93 Gallium. Method of determination of phosphorus
GOST 13637.9−93
Group B59
INTERSTATE STANDARD
GALLIUM
Method of determination of phosphorus
Gallium.
Method for the determination of phosphorus
AXTU 1709
Date of introduction 1995−01−01
Preface
1. DEVELOPED by the Interstate technical Committee 104 «of the Semiconductor and rare metals products. Especially pure metals», State Institute of rare metals (Giredmet).
INTRODUCED by Gosstandart of Russia
2. ADOPTED by the Interstate Council for standardization, Metrology and certification (Protocol No. 4−93 of 19 October 1993)
The adoption voted:
| The name of the state | The name of the national authority standardization |
| The Republic Of Armenia |
Armastajad |
| The Republic Of Belarus |
Belstandart |
| The Republic Of Kazakhstan |
Gosstandart Of The Republic Of Kazakhstan |
| The Republic Of Moldova |
Moldovastandart |
| Russian Federation |
Gosstandart Of Russia |
| Turkmenistan |
Turkmenistanand |
| The Republic Of Uzbekistan |
Standards |
| Ukraine |
Gosstandart Of Ukraine |
3. Resolution of the Committee of the Russian Federation for standardization, Metrology and certification from
4. REPLACE GOST 13637.9−77
INFORMATION DATA
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 5208−81 |
2.2 |
| GOST 5830−79 |
2.2, 3.2 |
| GOST 6259−75 |
2.2 |
| GOST 11125−78 |
2.2, 3.2 |
| GOST 13637.0−93 |
Sec. 1 |
| GOST 14261−77 |
2.2, 3.2 |
| GOST 20015−88 |
2.2 |
| GOST 24104−88 |
2.2 |
| GOST 25086−87 |
4.3 |
This standard specifies the methods of extraction-fotometricheskogo and visual-photometric determination of phosphorus in Gaul in the range of mass fraction from 1·10to 1·10
%.
1. GENERAL REQUIREMENTS
General requirements for methods of analysis and security requirements — according to GOST 13637.0.
2. METHOD OF 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.
1 — housing of the autoclave, 2 — reaction capacity, 3 — collector, 4 — the lid of the reaction vessel
5 — housing cover of the autoclave, 6 — shut-off device 7 is a tension nut,
8 — bottom refrigerator
Laboratory scales of the 1st class according to GOST 24104*.
_______________
* On the territory of the Russian Federation GOST 24104−2001. — Note the manufacturer’s database.
Drying oven with thermostatic control, ensuring the heating temperature up to 250 °C.
The fan room.
The tweezers are made of Plexiglas or Teflon.
Photoelectrocolorimeter FEK-56 or similar.
Separating funnel with a capacity of 50 cm.
Volumetric flasks with a capacity of 25; 100 cmand 1 DM
.
Pipettes with volume capacity of 1; 5 and 10 cm.
The paper filter «red ribbon» with a diameter of 70 mm.
Cylinder measuring capacity 10; 25 cm.
Hydrochloric acid of high purity according to GOST 14261, concentrated and the concentration is 6 mol/DM.
Water deionized with a specific resistivity of 10−20 Mω·cm.
Ammonium molybdate according to GOST 3765, aqueous solution concentration of 100 g/DM.
Chloroform technical according to GOST 20015.
Normal technical butyl alcohol according to GOST 5208.
Diethyl ether saturated with hydrochloric acid concentration is 6 mol/DM.
Mixture for extraction: mixture of butyl alcohol and chloroform in the volume ratio 3:7.
Glycerin according to GOST 6259.
Tin dichloride 2-water, a solution of glycerol concentration of 100 g/DM(dissolution is carried out by heating in a water bath).
Potassium phosphate according to GOST odnosemjannyj 4198.
A solution of phosphorus main: 0,438 g of single potassium phosphate is dissolved in water, transferred to a volumetric flask with a capacity of 1 DM, adjusted to the mark with water and mix.
1 cmof the solution contains 100 µg of phosphorus.
A solution of phosphorus production: 10 cmbasic solution of phosphorus poured into a measuring flask with a capacity of 100 cm
, made up to the mark with water and mix.
1 seethe 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 DMG
ellenia.
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), poured 5cmof water. The liner with the contents set with tweezers in a reaction container in which a pre-pour 20 cm
of concentrated hydrochloric acid. 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 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 out the tweezers liner-collection.
2.3.2. Solution of liner-collector is transferred to a measuring cylinder with a capacity of 10 cmand the volume was adjusted to 10 cm
solution of hydrochloric acid concentration is 6 mol/DM
. The solution from the cylinder is transferred to a separatory funnel. Gallium is extracted with three portions of ether at 10 cm
for 2 min. the Ether layer is discarded and the aqueous phase transferred to a separating funnel, poured 8 cm
of a solution of ammonium molybdate, 10 cm
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 solutions comparison used a 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 carried out two test 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 cmworking standard solution of phosphorus, which corresponds to 0,0; 0,2; 0,5; 1,0; 2,0; 5,0; 10,0 mcg phosphorus. Add up to 10 cm
of the hydrochloric acid concentration is 6 mol/DM
, 8 cm
ammonium molybdate, 10 cm
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, stirred. 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 the hydrochloric acid environment of ascorbic acid in the presence Armenonville potassium concentration of the extraction in isoamyl alcohol and 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 according to claim 2.2 with the addition of:
Tile laboratory electric power of 400 watts.
The quartz glasses with a capacity of 50 cm.
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 and the concentration of 2 and 6 mol/DM.
Ascorbic acid, an aqueous solution with a concentration of 17.6 g/DM.
Ammonium molybdate according to GOST 3765, aqueous solution with concentration of 40 g/DM.
Potassium armanavicius, an aqueous solution concentration of 3 g/DM.
Isoamyl alcohol according to GOST 5830.
Nitric acid of high purity according to GOST 11125*.
______________
* On the territory of the Russian Federation GOST 11125−84. — Note the manufacturer’s database.
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 claim 2.2.1
3.3.2. A portion of gallium by mass of 1 g was placed in a quartz beaker, pour 5 cmof the hydrochloric acid concentration is 6 mol/DM
, rinse the metal, the acid is carefully decanted and discarded.
In a glass pour 10 cmof a mixture of acid, cover with watch glass and hold the dissolution of the sample under low heat. The resulting solution was evaporated to dryness. The dry residue is dissolved in 5 cm
of hydrochloric acid concentration is 6 mol/DM
, the solution is transferred to a separatory funnel, the beaker rinsed another 5 cm
of hydrochloric acid of the same concentration, all transferred to a separating funnel.
Gallium is extracted 10 cmof 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
of hydrochloric acid of concentration 2 mol/DM
, the solution is transferred to a cylinder for colorimetrically, washing away a small amount of water, then add 0.25 cm
of a solution of ammonium molybdate, 0.5 cm
of a solution of ascorbic acid, 0.1 cm
of a solution of potassium Armenonville, bring the water volume up to 10 cm
. After adding each reagent, the contents thoroughly mixed. Add 1 cm
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
x experience.
3.3.3. Preparation of the scale comparison
In the cylinders to introduce colorimetrically 0,00; 0,05; 0,10; 0,15; 0,20; 0,40; 0,60; 1,00 cmworking solution of phosphorus (containing 1 µg/cm
of phosphorus), which corresponds to 0,00; 0,05; 0,10; 0,15; 0,20; 0,40; 0,60; 1,00 mcg phosphorus. Add 2 cm
of hydrochloric acid of concentration 2 mol/DM
, 0.25 cm
of a solution of ammonium molybdate, 0.5 cm
of a solution of ascorbic acid, 0.1 cm
of a solution of potassium Armenonville, bring the water volume up to 10 cm
. After adding each reagent, the contents thoroughly mixed. Add 1 cm
isoamyl alcohol, shaken for 30 s. the color Intensity of the organic layer scale solutions comparison used to determine the phosphorus in 5 min.
4. PROCESSING OF THE RESULTS
4.1. Mass fraction of phosphorus () in percent is calculated by the formula
where is the mass of phosphorus in the sample, µg,
— average mass of phosphorus in a control experiment, mcg,
the 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 of 0.95 is given in the table.
| Mass fraction of phosphorus, % |
Allowable difference, % |
1,0·10 |
0,3·10 |
5,0·10 |
2,0·10 |
1,0·10 |
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.
