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GOST 8775.2-87

GOST 33729-2016 GOST 20996.3-2016 GOST 31921-2012 GOST 33730-2016 GOST 12342-2015 GOST 19738-2015 GOST 28595-2015 GOST 28058-2015 GOST 20996.11-2015 GOST 9816.5-2014 GOST 20996.12-2014 GOST 20996.7-2014 GOST P 56306-2014 GOST P 56308-2014 GOST 20996.1-2014 GOST 20996.2-2014 GOST 20996.0-2014 GOST 16273.1-2014 GOST 9816.0-2014 GOST 9816.4-2014 GOST P 56142-2014 STATE STANDARD P 54493-2011 GOST 13498-2010 STATE STANDARD P 54335-2011 GOST 13462-2010 STATE STANDARD P 54313-2011 GOST P 53372-2009 GOST P 53197-2008 GOST P 53196-2008 GOST P 52955-2008 GOST P 50429.9-92 GOST 6836-2002 GOST 6835-2002 GOST 18337-95 GOST 13637.9-93 GOST 13637.8-93 GOST 13637.7-93 GOST 13637.6-93 GOST 13637.5-93 GOST 13637.4-93 GOST 13637.3-93 GOST 13637.2-93 GOST 13637.1-93 GOST 13637.0-93 STATE STANDARD 13099-2006 GOST 13098-2006 GOST 10297-94 GOST 12562.1-82 GOST 12564.2-83 GOST 16321.2-70 GOST 4658-73 GOST 12227.1-76 GOST 16274.0-77 GOST 16274.1-77 GOST 22519.5-77 GOST 22720.4-77 GOST 22519.4-77 GOST 22720.2-77 GOST 22519.6-77 GOST 13462-79 GOST 23862.24-79 GOST 23862.35-79 GOST 23862.15-79 GOST 23862.29-79 GOST 24392-80 GOST 20997.5-81 GOST 24977.1-81 GOST 25278.8-82 GOST 20996.11-82 GOST 25278.5-82 GOST 1367.7-83 GOST 26239.9-84 GOST 26473.1-85 GOST 16273.1-85 GOST 26473.2-85 GOST 26473.6-85 GOST 25278.15-87 GOST 12223.1-76 GOST 12645.7-77 GOST 12645.1-77 GOST 12645.6-77 GOST 22720.3-77 GOST 12645.4-77 GOST 22519.7-77 GOST 22519.2-77 GOST 22519.0-77 GOST 12645.5-77 GOST 22517-77 GOST 12645.2-77 GOST 16274.9-77 GOST 16274.5-77 GOST 22720.0-77 GOST 22519.3-77 GOST 12560.1-78 GOST 12558.1-78 GOST 12561.2-78 GOST 12228.2-78 GOST 18385.4-79 GOST 23862.30-79 GOST 18385.3-79 GOST 23862.6-79 GOST 23862.0-79 GOST 23685-79 GOST 23862.31-79 GOST 23862.18-79 GOST 23862.7-79 GOST 23862.1-79 GOST 23862.20-79 GOST 23862.26-79 GOST 23862.23-79 GOST 23862.33-79 GOST 23862.10-79 GOST 23862.8-79 GOST 23862.2-79 GOST 23862.9-79 GOST 23862.12-79 GOST 23862.13-79 GOST 23862.14-79 GOST 12225-80 GOST 16099-80 GOST 16153-80 GOST 20997.2-81 GOST 20997.3-81 GOST 24977.2-81 GOST 24977.3-81 GOST 20996.4-82 GOST 14338.2-82 GOST 25278.10-82 GOST 20996.7-82 GOST 25278.4-82 GOST 12556.1-82 GOST 14339.1-82 GOST 25278.9-82 GOST 25278.1-82 GOST 20996.9-82 GOST 12554.1-83 GOST 1367.4-83 GOST 12555.1-83 GOST 1367.6-83 GOST 1367.3-83 GOST 1367.9-83 GOST 1367.10-83 GOST 12554.2-83 GOST 26239.4-84 GOST 9816.2-84 GOST 26473.9-85 GOST 26473.0-85 GOST 12645.11-86 GOST 12645.12-86 GOST 8775.3-87 GOST 27973.0-88 GOST 18904.8-89 GOST 18904.6-89 GOST 18385.0-89 GOST 14339.5-91 GOST 14339.3-91 GOST 29103-91 GOST 16321.1-70 GOST 16883.2-71 GOST 16882.1-71 GOST 12223.0-76 GOST 12552.2-77 GOST 12645.3-77 GOST 16274.2-77 GOST 16274.10-77 GOST 12552.1-77 GOST 22720.1-77 GOST 16274.4-77 GOST 16274.7-77 GOST 12228.1-78 GOST 12561.1-78 GOST 12558.2-78 GOST 12224.1-78 GOST 23862.22-79 GOST 23862.21-79 GOST 23687.2-79 GOST 23862.25-79 GOST 23862.19-79 GOST 23862.4-79 GOST 18385.1-79 GOST 23687.1-79 GOST 23862.34-79 GOST 23862.17-79 GOST 23862.27-79 GOST 17614-80 GOST 12340-81 GOST 31291-2005 GOST 20997.1-81 GOST 20997.4-81 GOST 20996.2-82 GOST 12551.2-82 GOST 12559.1-82 GOST 1089-82 GOST 12550.1-82 GOST 20996.5-82 GOST 20996.3-82 GOST 12550.2-82 GOST 20996.8-82 GOST 14338.4-82 GOST 25278.12-82 GOST 25278.11-82 GOST 12551.1-82 GOST 25278.3-82 GOST 20996.6-82 GOST 25278.6-82 GOST 14338.1-82 GOST 14339.4-82 GOST 20996.10-82 GOST 20996.1-82 GOST 12645.9-83 GOST 12563.2-83 GOST 19709.1-83 GOST 1367.11-83 GOST 1367.0-83 GOST 19709.2-83 GOST 12645.0-83 GOST 12555.2-83 GOST 1367.1-83 GOST 9816.3-84 GOST 9816.4-84 GOST 9816.1-84 GOST 9816.0-84 GOST 26468-85 GOST 26473.11-85 GOST 26473.12-85 GOST 26473.5-85 GOST 26473.7-85 GOST 16273.0-85 GOST 26473.3-85 GOST 26473.8-85 GOST 26473.13-85 GOST 25278.13-87 GOST 25278.14-87 GOST 8775.1-87 GOST 25278.17-87 GOST 18904.1-89 GOST 18904.0-89 STATE STANDARD P 51572-2000 GOST 14316-91 GOST P 51704-2001 GOST 16883.1-71 GOST 16882.2-71 GOST 16883.3-71 GOST 8774-75 GOST 12227.0-76 GOST 12797-77 GOST 16274.3-77 GOST 12553.1-77 GOST 12553.2-77 GOST 16274.6-77 GOST 22519.1-77 GOST 16274.8-77 GOST 12560.2-78 GOST 23862.11-79 GOST 23862.36-79 GOST 23862.3-79 GOST 23862.5-79 GOST 18385.2-79 GOST 23862.28-79 GOST 16100-79 GOST 23862.16-79 GOST 23862.32-79 GOST 20997.0-81 GOST 14339.2-82 GOST 12562.2-82 GOST 25278.7-82 GOST 20996.12-82 GOST 12645.8-82 GOST 20996.0-82 GOST 12556.2-82 GOST 25278.2-82 GOST 12564.1-83 GOST 1367.5-83 GOST 25948-83 GOST 1367.8-83 GOST 1367.2-83 GOST 12563.1-83 GOST 9816.5-84 GOST 26473.4-85 GOST 26473.10-85 GOST 12645.10-86 GOST 8775.2-87 GOST 25278.16-87 GOST 8775.0-87 GOST 8775.4-87 GOST 12645.13-87 GOST 27973.3-88 GOST 27973.1-88 GOST 27973.2-88 GOST 18385.6-89 GOST 18385.7-89 GOST 28058-89 GOST 18385.5-89 GOST 10928-90 GOST 14338.3-91 GOST 10298-79 GOST P 51784-2001 GOST 15527-2004 GOST 28595-90 GOST 28353.1-89 GOST 28353.0-89 GOST 28353.2-89 GOST 28353.3-89 STATE STANDARD P 52599-2006

GOST 8775.2−87 Li. Method for the determination of sodium, potassium and calcium

GOST 8775.2−87

Group B59

STATE STANDARD OF THE USSR

LI

Method for the determination of sodium, potassium and calcium

Lithium.
Method for determination of sodium, potassium and calcium

AXTU 1709

Valid from 01.07.88
to 01.07.93*
__________________________
* Limit of validity
filmed on the Protocol, the Interstate Council
for standardization, Metrology and certification
(IUS N 2, 1993). — Note the manufacturer’s database.

INFORMATION DATA

1. APPROVED AND put INTO EFFECT by Decision of the USSR State Committee for standards from 28.09.87 N 3764

2. The term of the first test 1991

The frequency of inspection 5 years

3. REPLACE GOST 8775−75 (sect.3)

4. REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
Section number, paragraph
GOST 3118−77
2
GOST 4233−77
2
GOST 4234−77
2
GOST 4530−76
2
GOST 4919.1−77
2
GOST 5429−74
2
GOST 5457−75
2
GOST 6709−72
2
GOST 8774−75
3.3
GOST 8775.0−87
1.1; 5.2; 5.3.3; 5.4
GOST 14261−77
2
GOST 19908−80
2
GOST 20298−74
2
GOST 24104−80
2



This standard sets flame photometric method for the determination of impurities of sodium, potassium and calcium (when the mass fraction of sodium from 0.003 to 0.2%, potassium from 0.001 to 0.02%, calcium from 0.005 to 0.05%) to lithium.

The method is based on excitation in the air-acetylene flame emission spectrum of sodium, potassium and calcium and photoelectric registration of the intensities of analytical lines of sodium, potassium and calcium.

1. GENERAL REQUIREMENTS

1.1. General requirements for methods of analysis GOST 8775.0−87.

2. APPARATUS, REAGENTS AND MATERIALS

The fiery spectrophotometer C-115 or other type with similar or better metrological characteristics.

Laboratory scales according to GOST 24104−80*, of the 2nd accuracy class with the largest weighing limit of 200 g.
______________
* On the territory of the Russian Federation GOST 24104−2001. — Note the manufacturer’s database.

Quartz glasses according to GOST 19908−80*.
______________
* On the territory of the Russian Federation GOST 19908−90. — Note the manufacturer’s database.

Acetylene according to GOST 5457−75.

Hydrochloric acid according to GOST 14261−77, OS.CH., or according to GOST 3118−77, distilled in a quartz apparatus.

Methyl red indicator in 0.1% alcoholic solution prepared according to GOST 4919.1−77.

Sodium chloride according to GOST 4233−77.

Potassium chloride according to GOST 4234−77.

Calcium carbonate according to GOST 4530−76.

Strontium nitrate according to GOST 5429−74.

Lithium carbonate, the OS.h.

Carbon tetrachloride according to GOST 20298−74.

Distilled water GOST 6709−72, double-distilled.

3. PREPARATION FOR ASSAY

3.1. Preparation of solutions for calibration and control

3.1.1. Preparation of a 10% solution of strontium

242,0 g of strontium nitrate is weighed with an accuracy of at least 0.1 g, dissolved in water, transferred to a volumetric flask with a capacity of 1 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, the volume was adjusted solution with water to 1 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияand stirred.

3.1.2. Preparation of the solution of the base 1% strength solution of lithium

The 106.5 g of lithium carbonate are weighed with an error not more than 0.1 g was placed in a beaker with a capacity of 1 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, pour 200−300 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияof water, add two or three drops of the indicator and poured hydrochloric acid to acid reaction. Cooled to room temperature, the solution was transferred to a volumetric flask with a capacity of 2 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, the solution was adjusted to the mark with water and mix.

3.1.3. In solutions of bases and strontium to determine the concentration of sodium, potassium and calcium.

For this photometered at the same time solutions for the calibration and the basis of; according to the results of the photometry data to build calibration graphs.

The concentration of sodium, potassium and calcium in the basis determined by linear interpolation.

The concentration of each of the designated impurities in the solution framework shall not exceed 0.0002 g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, in the solution of strontium — 0.001 g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция.

3.1.4. Preparation of the starting solution for calibration

0,0165 g of sodium chloride, 0,7627 g of potassium chloride 0,9987 g of calcium carbonate and 106.5 g of lithium carbonate was placed in a quartz beaker, moistened with water and gently, drop by drop, poured hydrochloric acid until complete dissolution of salts. The solution was transferred to a volumetric flask with a capacity of 2 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, cooled, the volume was adjusted solution to the mark with water and mix. The starting solution contains 10 g of lithium and 0.2 g of sodium, potassium and calcium in a 1 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция.

3.1.5. Preparation of solutions for calibration

In a volumetric flask with a capacity of 1 DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияplaced 1,5; 2,5; 5,0; 12,5; 25,0; 50,0; 100,0 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияinitial solution and 8 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияof a solution of strontium, bring the volume of solution in the flasks with a solution of lithium (10 g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция) up to the mark and mix.

The calibration solutions contain sodium, potassium and calcium (without regard to the content of these elements in the basis) 0,0003; 0,0005; 0,0010; 0,0025; 0,0050; 0,0100; 0,0200 g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция. The contents of sodium, potassium and calcium in solutions to calibration adjust based on the content of these elements in the basis.

3.2. Preparation of the spectrophotometer

Preparation of the spectrophotometer to the work carried out by the device attached to the user.

3.3. Sample preparation

Pieces of lithium metal stored in accordance with GOST 8774−75, remove the tweezers from the banks, degreased with carbon tetrachloride, cleaned with a knife from the oxides and on the plate of organic glass cut from each piece of the required amount of metal to total mass was approximately 1 g.

4. ANALYSIS

4.1. Weighed samples of lithium with a mass of 1.00 g is dissolved in water, contained in a quartz glass with a capacity of 200 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, with each piece lithium make glass after dissolution of the previous one, add 1−2 drops of indicator and dropwise poured hydrochloric acid to acid reaction. The sample solution is poured into a measuring flask with a capacity of 100 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, add 0.8 cmГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияof a solution of strontium, the volume was adjusted solution to the mark with water and mix. When the content in the samples of sodium, potassium and calcium more than 0.5% from the sample solution is diluted with a solution of the bases 10 times. If the aluminum content in the samples less than 0.01%, a solution of strontium in samples and calibration solutions can not be added.

4.2. Prepared to work the spectrophotometer photometric the analyzed sample solution and the corresponding concentrations of the calibration solutions.

Fotometrirovanie solutions is carried out at the analytical line wavelengths listed in table.1.

Table 1

   
The designated element
Wavelength of analytical lines, nm
Sodium
589,0−589,6
Potassium
766,5−769,9
Calcium
422,7



The solutions of samples and standards for calibration photometric three times and the result should be the arithmetic mean value of three measurements.

4.3. The results of the photometry of the calibration solutions to build calibration graphs by laying the abscissa shows the concentration of the element in g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция, y-axis affimations average value of three measurements of the analytical signal of the calibration solution. For the calibration chart to determine the concentration of sodium, potassium and calcium in the sample (ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция), g/DMГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция.

5. PROCESSING OF THE RESULTS

5.1. Mass fraction of sodium, potassium and calcium (ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция) in percent is calculated by the formula

ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция.

5.2. The result of the analysis taking the arithmetic mean of two parallel definitions (some definitions) under the conditions of the PP.2.5, 2.6, and 2.10 GOST 8775.0−87.

5.3. Accuracy metrics

5.3.1. Indicators of convergence and reproducibility of the definitions ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияand ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальцияshown in table.2.

Table 2

       
The designated element
Mass fraction of element

ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция

ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция

    no more
Sodium
From 0.003 to 0.01 incl.
0,05
0,07
  SV. The 0.01 «to 0.05 «
0,02
0,05
  «To 0.05» to 0.2 «
0,01
0,03
Potassium
From 0.001 to 0.005 incl.
0,05
0,10
  SV. Of 0.005 «to 0.02 «
0,05
0,06
Calcium
From 0.005 to 0.02 incl.
0,10
0,13
  SV. 0,02 «0,05 «
0,04
0,07

5.3.2. Non-excluded systematic error (ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция) is insignificant compared to the random error.

5.3.3. The value of error analysis result (ГОСТ 8775.2-87 Литий. Метод определения натрия, калия и кальция) is determined according to GOST 8775.0−87.

5.4. The control accuracy of the analysis

The control accuracy of the analysis carried out by the method of additives in accordance with GOST 8775.0−87, using as additives aliquote part of the calibration mixtures of sodium, potassium and calcium, prepared according to claim 3.1.5. Calibration solution the determined element is added to the weighed sample until it is dissolved.