GOST 19863.9-91
GOST 19863.9−91 Alloy of titanium. Methods for determination of niobium
GOST 19863.9−91
Group B59
STATE STANDARD OF THE USSR
ALLOYS OF TITANIUM
Methods for determination of niobium
Titanium alloys.
Methods for the determination of niobium
AXTU 1709
Date of introduction 1992−07−01
INFORMATION DATA
1. DEVELOPED AND INTRODUCED by the Ministry of aviation industry of the USSR
DEVELOPERS
V. G. Davydov, doctor of engineering. Sciences; V. A. Moshkin, PhD. tech. Sciences; G. I. Friedman, PhD. tech. Sciences; L. A. Tenyakova; M. N. Gorlova, PhD. chem. Sciences; A. I. Korolev, O. L. Sikorska, PhD. chem. Sciences
2. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee on management of quality and standards from 5.05.91 N 625
3. REPLACE GOST 19863.9−80
4. The frequency of inspection — 5 years
5. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS
| The designation of the reference document referenced |
Item number |
| GOST 3118−77 |
2.2; 3.2; 4.2 |
| GOST 3759−75 |
4.2 |
| GOST 4204−77 |
2.2; 3.2 |
| GOST 4461−77 |
4.2 |
| GOST 5456−79 |
2.2; 3.2 |
| GOST 5457−75 |
4.2 |
| GOST 5817−77 |
2.2; 3.2 |
| GOST 7172−76 |
2.2; 3.2 |
| GOST 9656−75 |
4.2 |
| GOST 10484−78 |
4.2 |
| GOST 10652−73 |
2.2; 3.2 |
| GOST 10929−76 |
4.2 |
| GOST 16100−79 |
4.2 |
| GOST 17746−79 |
2.2; 3.2 |
| GOST 25086−87 |
1.1 |
| THAT 6−09−1678−86 |
2.2; 3.2 |
This standard specifies the photometric (with a mass fraction of from 0.1 to 5.0%) and atomic absorption (at a mass fraction of from 0.5 to 5.0%) methods for determination of niobium.
1. GENERAL REQUIREMENTS
1.1. General requirements for methods of analysis GOST 25086 with the Supplement.
1.1.1. For the results analysis be the arithmetic mean of results of two parallel measurements.
2. The PHOTOMETRIC METHOD for the DETERMINATION of NIOBIUM WITH the REAGENT 1-(2-pyridyl-A30)-RESORCINOL (PAR) (for the mass concentration of niobium is from 0.5 to 5.0%)
2.1. The essence of the method
The method is based on dissolving the sample in sulfuric acid solution, education solution hydrochloric acid 0.75 mol/DMcolored orange-red complex with PAR and measuring the optical density of the solution at a wavelength of 536 nm.
2.2. Apparatus, reagents and solutions
Spectrophotometer or photoelectrocolorimeter.
Muffle furnace with thermostatic control.
Filters obestochennye on the other 6−09−1678.
Sulfuric acid according to GOST 4204 density 1.84 g/cm, a solution of 1:2.
Hydrochloric acid according to GOST 3118 density of 1.19 g/cm, solution 1 mol/DM
.
Tartaric acid according to GOST 5817, a solution of 200 g/DM.
Hydroxylamine hydrochloride according to GOST 5456, solution 100 g/DM.
Potassium preservatory according to GOST 7172.
Salt is the disodium Ethylenediamine — N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652, a solution of 0.0125 mol/DM: 4.65 g Trilon B, is placed in a conical flask with a capacity of 250 cm
, 100 cm poured
water and dissolve in low heat. The solution was cooled to room temperature, filtered into a measuring flask with volume capacity of 1000 cm
, made up to the mark with water and mix.
Titanium sponge according to GOST 17746* stamps TG-100.
_______________
* On the territory of the Russian Federation GOST 17746−96, here and hereafter. — Note the manufacturer’s database.
Pentoxide of niobium.
A standard solution of niobium: 0,0715 g of niobium pentoxide is fused in a quartz or platinum crucible with 3 g of potassium peacemaking at a temperature of (800±10) °C in a muffle furnace. After cooling, the crucible was placed in a beaker with a capacity of 400 cm, flow 75 cm
of tartaric acid solution and leach the melt when heated. The solution was cooled to room temperature, poured into a volumetric flask with a capacity of 500 cm
, made up to the mark with water and mix.
1 cmof the solution contains 0.0001 g of niobium.
1-(2-pyridyl-azo)-resorcinol monosodium salt (PAR), a solution of 1 g/DM: 0.1 g of the reagent dissolved in 100
cmwater.
2.3. Analysis
2.3.1. A portion of sample weighing 0.1 g was placed in a conical flask with a capacity of 100 cm, flow 15 cm
of sulfuric acid solution and heated to complete dissolution.
To carry out control experience in the same way dissolve 0.1 g of titanium.
The solution was added dropwise a solution of hydroxylamine hydrochloride to the disappearance of a purple color, ten drops in excess, and boil for 1−2 min. the Solution was cooled to room temperature, pour 15 cmof a solution of tartaric acid, poured into a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
2.3.2. Aliquot part of the solution according to the table.1 is placed in a volumetric flask with a capacity of 50 cm, pour 1 cm
of tartaric acid solution, 1 cm
of solution Trilon B, 38.5 cm
hydrochloric acid solution, 1 cm
of solution PAIRS, made up to the mark with water and mix.
Table 1
| Mass fraction of niobium, % |
The volume aliquote part, see |
| From 0.5 to 2.5 incl. |
2,5 |
| SV. Of 2.5 «and 5.0 « |
1 |
2.3.3. Optical density of the solution is measured after 1 hour at a wavelength of 536 nm in a cuvette with a layer thickness fotometricheskogo 30 mm.
Solution comparison is the solution of the reference experiment with all used in the analysis reagent according to claim.2.3.1,
2.3.4. Mass fraction of niobium is calculated according to the calibration schedule.
2.3.5. Construction of calibration curve
2.3.5.1. For the mass concentration of niobium is from 0.5 to 2.5%
Eight volumetric flasks with a capacity of 50 cmpour 2.5 cm
of a solution of Titan, seven of them measure 0,1; 0,2; 0,3; 0,4; 0,5; 0,6; 0,7 cm
standard solution niobium, which corresponds to 0,00001; 0,00002; 0,00003; 0,00004; 0,00005; 0,00006; 0,00007 g niobium.
2.3.5.2. When the mass fraction of niobium of 2.5 to 5.0%
Eight volumetric flasks with a capacity of 50 cmpour 1 cm
of a solution of Titan, seven of them measure 0,1; 0,2; 0,3; 0,4; 0,5; 0,6; 0,7 cm
standard solution niobium, which corresponds to 0,00001; 0,00002; 0,00003; 0,00004; 0,00005; 0,00006; 0,00007 g niobium.
2.3.5.3. The solutions in the flasks prepared according to PP.2.3.5.1 and of a solution of tartaric acid and further arrive at PP.2.3.2 and
Solution comparison is the solution in which niobium is not entered.
According to the obtained values of optical density of the solutions and their corresponding masses of niobium build the calibration graph.
2.4. Processing of the results
2.4.1. Mass fraction of niobium () in percent is calculated by the formula
where is the mass of niobium in the sample solution found by the calibration schedule g;
— the weight of the portion of the sample in the appropriate aliquote part of the solution,
2.4.2. Discrepancies in the results must not exceed the values given in table.2.
Table 2
| Mass fraction of niobium, % |
The absolute allowable difference, % | |
| results of parallel measurements |
the results of the analysis | |
| From 0.50 to 1.00 incl. |
0,04 |
0,05 |
| SV. Of 1.00 «to 2.50 « |
0,06 |
0,07 |
| «Of 2.50» and 5.00 « |
0,12 |
0,15 |
3. The PHOTOMETRIC METHOD for the DETERMINATION of NIOBIUM WITH SULFOCHLORINATED (at the mass fraction of niobium of 0.1 to 1.5%)
3.1. The essence of the method
The method is based on dissolving the sample in sulfuric acid solution, education solution hydrochloric acid 1 mol/DMblue-violet complex compound of niobium — sulfochloride-tartrate, and measurement of optical density of the solution at a wavelength of 650 nm.
The effect of titanium, Zirconia and iron can be eliminated by introducing, respectively, tartaric acid, Trilon B and hydroxylamine hydrochloride.
3.2. Apparatus, reagents and solutions
Spectrophotometer or photoelectrocolorimeter.
Muffle furnace with thermostatic control.
Filters obestochennye on the other 6−09−1678.
Sulfuric acid according to GOST 4204 density 1.84 g/cm, a solution of 1:3.
Hydrochloric acid according to GOST 3118 density of 1.19 g/cmand a solution of 1:1.
Tartaric acid according to GOST 5817, solutions of 30 g/DMand 200 g/DM
.
Hydroxylamine hydrochloride according to GOST 5456, solution 100 g/DM.
Potassium preservatory according to GOST 7172.
Salt is the disodium Ethylenediamine — N, N, N', N'-tetraoxane acid, 2-water (Trilon B) according to GOST 10652, a solution of 0.0125 mol/DM(prepared according to claim 2.2).
Titanium sponge according to GOST 17746 grade TG-100.
Pentoxide of niobium.
Standard solutions of niobium
Solution a is prepared according to claim 2.2.
1 cmof the solution contains 0.0001 g of niobium.
Solution B (freshly prepared): 10 cmsolution And transferred with a pipette into a measuring flask with a capacity of 100 cm
, is poured the solution of tartaric acid 30 g/DM
up to the mark and mix.
1 cmof solution B contains 0,00001 g of niobium.
Sulfochlorides With a solution of 10 g/DM: 0.13 g of reagent are thoroughly ground in an agate mortar, placed in a beaker with a capacity of 100 cm
, 80 cm pour the
water and dissolve in low heat. After 1 h the solution was filtered through a filter (the"blue ribbon») in a volumetric flask with a capacity of 100 cm
, made up to the mark with water and the feather
meshivat.
3.3. Analysis
3.3.1. A sample of alloy weighing 0.1 g was placed in a conical flask with a capacity of 100 cm, flow 25 cm
of sulfuric acid solution and heated to complete dissolution.
To carry out control experience in the same way dissolve 0.1 g of titanium.
The solution was added dropwise a solution of hydroxylamine hydrochloride until the disappearance of the purple coloring, ten drops in excess, and boil for 1−2 min. the Solution was cooled to room temperature, poured 10 cmof a solution of tartaric acid, poured into a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix.
3.3.2. To aliquote part of the solution in accordance with the table.3 in a volumetric flask with a capacity of 50 cmpour 1 cm
of the solution Trilon B, 10 cm
of hydrochloric acid solution, 1 cm
of solution With sulfochloride, made up to the mark with water and mix.
Table 3
| Mass fraction of niobium, % |
The volume aliquote part, see |
| From 0.1 to 0.5 incl. |
5 |
| SV. 0,5 «1,0 « |
2 |
| «1,0» 1,5 « |
1 |
3.3.3. Optical density of the solution is measured after 1 hour at a wavelength of 650 nm in a cuvette with a layer thickness fotometricheskogo 30 mm.
Solution comparison is the solution of the reference experiment with all used in the analysis reagents.
3.3.4. Mass fraction of niobium is calculated according to the calibration schedule.
3.3.5. Construction of calibration curve
In six volumetric flasks with a capacity of 50 cmpour 2 cm
of the solution in the reference experiment, five of them measure 0,5; 1,0; 2,0; 2,5; 3,0 cm
standard solution B, which corresponds to 0,000005; 0,00001; 0,00002; 0,000025; 0,00003 g of niobium and do PP.3.3.2 and
Solution comparison is the solution in which niobium is not entered.
According to the obtained values of optical density of the solutions and their corresponding masses of niobium build the calibration graph.
3.4. Processing of the results
3.4.1. Mass fraction of niobium () in percent is calculated by the formula
where is the mass of niobium in the sample solution found by the calibration schedule g;
— the weight of the portion of the sample in the appropriate aliquote part of the solution,
3.4.2. Discrepancies in the results must not exceed the values given in table.4.
Table 4
| Mass fraction of niobium, % |
The absolute allowable difference, % | |
| results of parallel measurements |
the results of the analysis | |
| From 0.10 to 0.30 incl. |
0,02 |
0,03 |
| SV. Of 0.30 «to 0.50 « |
0,04 |
0,05 |
| «Of 0.50» to 1.50 « |
0,06 |
0,07 |
4. ATOMIC ABSORPTION METHOD FOR THE DETERMINATION OF NIOBIUM
4.1. The essence of the method
The method is based on dissolving the sample in hydrochloric and bridgestation acids and measuring the nuclear absorption of niobium at a wavelength of 334,4 nm in a flame acetylene — nitrous oxide.
4.2. Apparatus, reagents and solutions
Spectrophotometer of atomic absorption with a radiation source for niobium.
Acetylene according to GOST 5457.
Nitrous oxide medical.
Hydrochloric acid according to GOST 3118 density of 1.19 g/cmand a solution of 2:1, 1:1.
Nitric acid according to GOST 4461 density of 1,35−1,40 g/cm.
Boric acid according to GOST 9656 and a saturated solution.
Hydrofluoric acid according to GOST 10484.
Acid bridgestation: 280 cmhydrofluoric acid at a temperature of (10±2) °C add portions 130 g of boric acid and stirred. The solution is prepared and stored in a plastic container.
Hydrogen peroxide according to GOST 10929.
Aluminium chloride according to GOST 3759.
Niobium GOST 16100 brand SNB-00.
Standard solutions of niobium
Solution a: 2.5 g of niobium metal is placed in a Teflon beaker with a capacity of 100 cmand dissolved in 20 cm
of a mixture of hydrofluoric and nitric acids in the ratio 1:1. The dissolution is conducted at room temperature, the mixture of acids is added in small portions. After dissolution of the sample add 30 cm
of a saturated solution of boric acid and allowed to stand for 10 min. Then add 5 cm
of hydrogen peroxide and 10 cm
of hydrochloric acid.
The solution was transferred to volumetric flask with a capacity of 100 cm, made up to the mark with water, mixed and poured in Teflon beaker in which the dissolution was carried out.
1 cmof the solution contains 0.025 g of niobium.
Solution B: 10 cmsolution And placed in a volumetric flask with a capacity of 100 cm
, add 1 cm
of hydrogen peroxide solution, 10 cm
of hydrochloric acid, made up to the mark with water and mix.
1 cmof solution B contains 0,0025
g niobium.
4.3. Analysis
4.3.1. A portion of sample weighing 0.5 g is placed in a conical flask with a capacity of 100 cm, flow 20 cm
of a hydrochloric acid solution of 2:1, 1 cm
bridgestation acid and dissolved with moderate heating. The solution was cooled to room temperature, add 1 cm
of hydrogen peroxide solution, 10 cm
bridgestation acid and 20 cm
of a solution of aluminum chloride. After each addition of reagent solution mix thoroughly. The solution was then transferred to a volumetric flask with a capacity of 100 cm
, made up to the mark with water and mix
.
4.3.2. The solution in the reference experiment is prepared according to claim
4.3.3. Construction of calibration curve
Five conical flasks with a capacity of 100 cmis placed 0.5 g of the alloy, similar in composition analyzed, but does not contain niobium, four of them measure 1,0; 4,0; 7,0; 10,0 cm
standard solution B, which corresponds to 0,0025; 0,01; 0,0175; 0.025 g of niobium and conduct dissolution according to claim
4.3.4. The sample solution, solution control experience and solutions to build the calibration curve is sprayed into the flame of acetylene — nitrous oxide (recovery) and measure the atomic absorption of niobium at a wavelength of 334,4 nm.
According to the obtained values of atomic absorption and corresponding mass concentrations of niobium build a calibration curve in the coordinates «Value of atomic absorption — Mass concentration of niobium, g/cm».
The mass concentration of niobium in the sample solution and the solution of control and experience determined by the calibration schedule.
4.4. Processing of the results
4.4.1. Mass fraction of niobium () in percent is calculated by the formula
where is the mass concentration of niobium in the sample solution found by the calibration schedule, g/cm
;
— mass concentration of niobium in solution in the reference experiment, was found in the calibration schedule, g/cm
;
— the volume of the sample solution, cm
;
— the weight of the portion in the sample solution, g
.
4.4.2. Discrepancies in the results must not exceed the values given in table.5.
Table 5
| Mass fraction of niobium, % |
The absolute allowable difference, % | |
| results of parallel measurements |
the results of the analysis | |
| From 0.50 to 1.00 incl. |
0,05 |
0,10 |
| SV. Of 1.00 «to 2.50 « |
0,10 |
0,15 |
| «Of 2.50» and 5.00 « |
0,15 |
0,20 |
