By visiting this site, you accept the use of cookies. More about our cookie policy.

GOST R 50424-92

GOST R ISO 15353-2014 GOST P 55080-2012 GOST R ISO 16962-2012 GOST R ISO 10153-2011 GOST R ISO 10280-2010 GOST R ISO 4940-2010 GOST R ISO 4943-2010 GOST R ISO 14284-2009 GOST R ISO 9686-2009 GOST R ISO 13899-2-2009 GOST 18895-97 GOST 12361-2002 GOST 12359-99 GOST 12358-2002 GOST 12351-2003 GOST 12345-2001 GOST 12344-88 GOST 12350-78 GOST 12354-81 GOST 12346-78 GOST 12353-78 GOST 12348-78 GOST 12363-79 GOST 12360-82 GOST 17051-82 GOST 12349-83 GOST 12357-84 GOST 12365-84 GOST 12364-84 STATE STANDARD P 51576-2000 GOST 29117-91 GOST 12347-77 GOST 12355-78 GOST 12362-79 GOST 12352-81 GOST P 50424-92 STATE STANDARD P 51056-97 GOST P 51927-2002 GOST P 51928-2002 GOST 12356-81 GOST R ISO 13898-1-2006 GOST R ISO 13898-3-2007 GOST R ISO 13898-4-2007 GOST R ISO 13898-2-2006 STATE STANDARD P 52521-2006 GOST P 52519-2006 GOST R 52520-2006 GOST P 52518-2006 GOST 1429.14-2004 GOST 24903-81 GOST 22662-77 GOST 6012-2011 GOST 25283-93 GOST 18318-94 GOST 29006-91 GOST 16412.4-91 GOST 16412.7-91 GOST 25280-90 GOST 2171-90 GOST 23401-90 GOST 30642-99 GOST 25698-98 GOST 30550-98 GOST 18898-89 GOST 26849-86 GOST 26876-86 GOST 26239.5-84 GOST 26239.7-84 GOST 26239.3-84 GOST 25599.4-83 GOST 12226-80 GOST 23402-78 GOST 1429.9-77 GOST 1429.3-77 GOST 1429.5-77 GOST 19014.3-73 GOST 19014.1-73 GOST 17235-71 GOST 16412.5-91 GOST 29012-91 GOST 26528-98 GOST 18897-98 GOST 26529-85 GOST 26614-85 GOST 26239.2-84 GOST 26239.0-84 GOST 26239.8-84 GOST 25947-83 GOST 25599.3-83 GOST 22864-83 GOST 25599.1-83 GOST 25849-83 GOST 25281-82 GOST 22397-77 GOST 1429.11-77 GOST 1429.1-77 GOST 1429.13-77 GOST 1429.7-77 GOST 1429.0-77 GOST 20018-74 GOST 18317-94 STATE STANDARD P 52950-2008 GOST P 52951-2008 GOST 32597-2013 GOST P 56307-2014 GOST 33731-2016 GOST 3845-2017 STATE STANDARD P ISO 17640-2016 GOST 33368-2015 GOST 10692-2015 GOST P 55934-2013 GOST P 55435-2013 STATE STANDARD P 54907-2012 GOST 3845-75 GOST 11706-78 GOST 12501-67 GOST 8695-75 GOST 17410-78 GOST 19040-81 GOST 27450-87 GOST 28800-90 GOST 3728-78 GOST 30432-96 GOST 8694-75 GOST R ISO 10543-99 GOST R ISO 10124-99 GOST R ISO 10332-99 GOST 10692-80 GOST R ISO 17637-2014 GOST P 56143-2014 GOST R ISO 16918-1-2013 GOST R ISO 14250-2013 GOST P 55724-2013 GOST R ISO 22826-2012 GOST P 55143-2012 GOST P 55142-2012 GOST R ISO 17642-2-2012 GOST R ISO 17641-2-2012 GOST P 54566-2011 GOST 26877-2008 GOST R ISO 17641-1-2011 GOST R ISO 9016-2011 GOST R ISO 17642-1-2011 STATE STANDARD P 54790-2011 GOST P 54569-2011 GOST P 54570-2011 STATE STANDARD P 54153-2010 GOST R ISO 5178-2010 GOST R ISO 15792-2-2010 GOST R ISO 15792-3-2010 GOST P 53845-2010 GOST R ISO 4967-2009 GOST 6032-89 GOST 6032-2003 GOST 7566-94 GOST 27809-95 GOST 22974.9-96 GOST 22974.8-96 GOST 22974.7-96 GOST 22974.6-96 GOST 22974.5-96 GOST 22974.4-96 GOST 22974.3-96 GOST 22974.2-96 GOST 22974.1-96 GOST 22974.13-96 GOST 22974.12-96 GOST 22974.11-96 GOST 22974.10-96 GOST 22974.0-96 GOST 21639.9-93 GOST 21639.8-93 GOST 21639.7-93 GOST 21639.6-93 GOST 21639.5-93 GOST 21639.4-93 GOST 21639.3-93 GOST 21639.2-93 GOST 21639.0-93 GOST 12502-67 GOST 11878-66 GOST 1763-68 GOST 13585-68 GOST 16971-71 GOST 21639.10-76 GOST 2604.1-77 GOST 11930.7-79 GOST 23870-79 GOST 11930.12-79 GOST 24167-80 GOST 25536-82 GOST 22536.2-87 GOST 22536.11-87 GOST 22536.6-88 GOST 22536.10-88 GOST 17745-90 GOST 26877-91 GOST 8233-56 GOST 1778-70 GOST 10243-75 GOST 20487-75 GOST 12503-75 GOST 21548-76 GOST 21639.11-76 GOST 2604.8-77 GOST 23055-78 GOST 23046-78 GOST 11930.11-79 GOST 11930.1-79 GOST 11930.10-79 GOST 24715-81 GOST 5639-82 GOST 25225-82 GOST 2604.11-85 GOST 2604.4-87 GOST 22536.5-87 GOST 22536.7-88 GOST 6130-71 GOST 23240-78 GOST 3242-79 GOST 11930.3-79 GOST 11930.5-79 GOST 11930.9-79 GOST 11930.2-79 GOST 11930.0-79 GOST 23904-79 GOST 11930.6-79 GOST 7565-81 GOST 7122-81 GOST 2604.3-83 GOST 2604.5-84 GOST 26389-84 GOST 2604.7-84 GOST 28830-90 GOST 21639.1-90 GOST 5640-68 GOST 5657-69 GOST 20485-75 GOST 21549-76 GOST 21547-76 GOST 2604.6-77 GOST 22838-77 GOST 2604.10-77 GOST 11930.4-79 GOST 11930.8-79 GOST 2604.9-83 GOST 26388-84 GOST 14782-86 GOST 2604.2-86 GOST 21639.12-87 GOST 22536.8-87 GOST 22536.0-87 GOST 22536.3-88 GOST 22536.12-88 GOST 22536.9-88 GOST 22536.14-88 GOST 22536.4-88 GOST 22974.14-90 GOST 23338-91 GOST 2604.13-82 GOST 2604.14-82 GOST 22536.1-88 GOST 28277-89 GOST 16773-2003 GOST 7512-82 GOST 6996-66 GOST 12635-67 GOST 12637-67 GOST 12636-67 GOST 24648-90

GOST R 50424−92 Steel and cast iron. Method of determination of calcium


GOST R 50424−92

Group B39


STATE STANDARD OF THE RUSSIAN FEDERATION


STEEL AND CAST IRON

Method of determination of calcium

Steel and cast iron. Method for determination of calcium


OKS 77.080.01
AXTU 0809

Date of introduction 1994−07−01


INFORMATION DATA

1 DEVELOPED AND SUBMITTED by the Technical Committee for standardization TC 145 «monitoring Methods of steel products"

2 APPROVED AND put INTO effect by the Resolution of Gosstandart of Russia from December 2, 1992 N 1529

3 INTRODUCED FOR THE FIRST TIME

4 REFERENCE NORMATIVE AND TECHNICAL DOCUMENTS

   
The designation of the reference document referenced
The partition number
GOST 4517−87
2
GOST 11125−84
2
GOST 14261−77
2
GOST 19908−90
2
GOST 28473−90
1
THAT 6−09−895−85
2
TU 6−09/3678−86
2

5 REISSUE


This standard specifies atomic absorption (in mass fractions of from 0.001 to 0.20%) method for the determination of calcium in steels and cast iron.

The method is based on dissolving the sample in hydrochloric, nitric, fluoric hydrogen and chloric acid; the addition of solutions of potassium chloride and lanthanum nitrate as a spectrochemical buffer, spraying the test solution into the flame dinitroazetidine; spectrometric measuring the absorption values of the radiation emitted by the lamp with hollow cathode, free of calcium atoms at a wavelength 422,7 nm.

1 General requirements


General requirements for methods of analysis GOST 28473.

2 Equipment, reagents and solutions


The atomic absorption spectrometer.

Lamp with hollow cathode for the determination of calcium.

Cylinders dinitrourea and acetylene not containing water, oil and calcium (acetylene purified by passing through geratol or other suitable method).

Beakers, flasks, funnels made of transparent quartz glass according to GOST 19908.

The glasses are made of PTFE with a capacity of 250−300 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция.

Volumetric flasks made of fluoroplastic 4MB with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияon the other 95−337.

The cylinders of fluoroplastic 4MB.

Note — All used utensils should be thoroughly washed with hot hydrochloric acid (1:2), and then double-distilled water (tap water for intermediate rinsing is used).


Conventional laboratory equipment.

Bidistilled water according to GOST 4517 or equivalent purity (stored in a vessel made of polyethylene).

Iron is very pure, containing not more than 0.0005% of calcium.

Diethyl ether (ethyl ether medical).

Acid hydrochloric GOST 14261, optionally purified, and diluted 1:2 and 1:9.

Cleaning method: in the desiccator, pour hydrochloric acid on a support is placed a glass made of polyethylene or PTFE, filled with double-distilled or deionized water.

The volume ratio of water and acid should be 1:6. The desiccator tightly closed ground cover. After about four days to get a solution of hydrochloric acid, free from impurities of calcium, with a density of 1.15. Store in polyethylene bottle.

Nitric acid, OS.h. according to GOST 11125.

Perchloric acid, OS.h.

Acid fluoride-hydrogen, the OS.CH., of the highest category.

Potassium chloride, OS.h. on the other 6−09−3678.

Lanthanum nitrate, OS.h.

Spectrochemical buffer: dissolve 95,34 g of potassium chloride and 62,35 g setevogo lanthanum nitrate (La (NOГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция)ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияx6HГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияO) in water and diluted to 1000 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияand mixed. Store the solution in polyethylene bottles.

Calcium carbonate, OS.h. on the other 6−09−895.

Standard solutions of calcium

Solution a: 0,2497 g of calcium carbonate dried at 100 °C for 1 h and cooled in a desiccator to room temperature, placed in a beaker, carefully add 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid (1:2), covered with a glass watch glass and dissolve with a moderate heat. The solution was cooled, transferred to a measuring flask with volume capacity of 1000 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция, made up to the mark with water and mix. Store the standard solution in a sealed plastic container.

1 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof the solution contains 100 mg of calcium.

Solution B: placed 10.0 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof solution A in a volumetric flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция, add 5 cm ofГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияhydrochloric acid (1:9), dilute to the mark with water and mix. The solution is prepared immediately before use.

1 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof solution contains 10 mcg of calcium.

Note — For the preparation of all series of the analyzed samples in the reference experiment and the calibration solutions used reagents, including water, from the same batch.

3 analysis

3.1 the sample the sample washed in diethyl (ethyl) ether and dried, weighing 1,000 g was placed in a Teflon beaker, add 15 cm ofГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияhydrochloric acid, cover with a Teflon cap and dissolved with moderate heating the bulk sample, then add 3−5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof nitric acid. After the cessation of violent foaming, add 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof perchloric acid and 3.5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияfluoride-hydrogen. Continue a moderate heat to release the dense white fumes of perchloric acid.

Perchloric acid can explode in the presence of ammonia, vapour of nitrous acid and any organic reagents.

The solution was cooled, washed wall with water and heating was continued until the termination of allocation of vapors of perchloric acid. Salt dissolved in 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid, add 20 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof water, heated to boiling. The hot solution is filtered into a measuring flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияthrough a filter of medium density pre-washed 5−6 times with hot hydrochloric acid (1:2) and several times with bidistilled water. The filter cake is washed with hot hydrochloric acid (1:9), add it in small portions until the complete laundering of the filter from iron salts, then washed the filter 3 times more bitter with water and discarded. In the flask, if the expected calcium content does not exceed 0.01%, add 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияspectrochemical buffer, made up to the mark with water and mix. In the case that the expected calcium content exceeds 0.01%, the solution in the flask topped up to the mark with water and mix. Then select aliquot part of 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияin a volumetric flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция, add 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияspectrochemical buffer, made up to the mark with water and mix.

In parallel with the determination, performing all operations of the methods and using the same quantities of reagents, carry out a test

experience.

3.2 Preparation of the calibration solutions with the mass fraction of calcium to 0.01%

Put seven quartz glasses with a capacity of 250−300 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция1,000 g of iron, add 15 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid and 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof nitric acid. After complete dissolution of the iron solution was evaporated to wet salts and salt dissolved in 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid. Add 20 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof water, bring to the boil, then cooled and transferred to volumetric flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция. Add standard solution B in accordance with table 1, 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияspectrochemical buffer, made up to the mark with water and mix.


Table 1

         
The interval defined by the content of calcium, %

Volume of standard solution B, cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция

The appropriate concentration of calcium, mg/cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция

Mass fraction of calcium, %,
when mounting the sample, g
      1,0
0,1
From 0.001 to 0.01 incl. 0*
0 0 0
  1,0
0,1 0,001 0,01
  2,0
0,2 0,002 0,02
  4,0
0,4 0,004 0,04
SV. 0.01 to 0.10 incl. 6,0
0,6 0,006 0,06
  8,0
0,8 0,008 0,08
  10,0
1,0 0,01 0,1
«To 0.10» to 0.20 incl. 0*
0 0 0
  10,0
1,0 - 0,10
  12,0
1,2 - 0,12
  14,0
1,4 - 0,14
  16,0
1,6 - 0,16
  18,0
1,8 - 0,18
  20,0
2,0 - 0,20
* Zero solution.

3.3 Preparation of calibration solutions for the mass concentration of calcium above 0.01%

Put seven quartz glasses with a capacity of 250−300 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция1,000 g of iron, add 15 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid and 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof nitric acid. After complete dissolution of the iron is evaporated to wet salts and salt dissolved in 5 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof hydrochloric acid. Add 20 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof water, bring to the boil, then cooled and transferred to volumetric flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция. Topped up to the mark with water and mix. Select aliquot part of 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияin a volumetric flask with a capacity of 100 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция, add standard solution B in accordance with table 1, add 10 cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияspectrochemical buffer, made up to the mark with water and paramashiva

yut.

3.4 preparation of the device for measuring

The inclusion and configuration of the atomic absorption spectrometer is carried out according to the instructions supplied with the device.

Basic instrumental parameters

Analytical line 422,7 nm.

Flame — dinitrourea-acetylene. Transparent, stoichiometric with the height of the red cone 10−20 mm, adjusted to the maximum atomic absorption of radiation by atoms of calcium.

Current lamp in accordance with the instructions or 20−25 mA.

The width of the spectral band in accordance with the instructions or between 0.3 and 0.1 mm.

Corrector background — can be used in the case when the absorption is zero the solution has a meaningful value.

Burner — high temperature, with the length of the slit 5, see Before using the slot burner should be cleaned well with a mixture of acetone and ethanol (1:1).

3.5 Spectrometric analysis procedure

3.5.1 Set the lamp current, wavelength, pressure and the initial flow of gases, lit torch, heat it for 5 minutes, then spray water to establish stable results. Adjust flow rates of gases so that the flame was luminous and had a red cone height of about 10−20 mm. is Sprayed, alternately the most concentrated calibration solution and null, while adjusting the gas flow and the burner position (horizontal, vertical, and angled) relative to the light path as long as the difference in absorption value between these solutions will be a maximum. Check the accuracy of the output of the spectrometer at the desired wavelength. Set zero on the registered device unit relative to the water.

Sprayed a full set of calibration solutions, including zero, in ascending order, repeating this operation until the readings will not be stable. Choose two of the calibration solution with a value of absorption is a little lower and a little higher than the test solution. Spray these solutions in ascending or reverse order (the subject in the middle), measuring the absorbance in each case relative to water.

Again spray a complete set of calibration solutions in ascending or reverse order and use average values of absorption for constructing the calibration curve.

In the measurement process, if necessary, clean the burner of soot, if the results show the loss of precision due to contamination of the burner.

Be sure to spray water between the spraying of each solution was measured, making sure that the air intake was minimal.

Mass fraction of calcium in the test sample and the control solution experience find for the calibration schedule.

3.5.2 it is Necessary to prepare a new calibration curve for each series of definitions of calcium and for each interval of the designated contents.

According to the obtained average values of absorbance and corresponding concentrations of calcium, expressed in µg/cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof Sa, build a calibration curve.

Compare the values of the selected absorption of the calibration solutions, which were sprayed before and after test solution, and if these values do not differ from the graphics are more than acceptable standards of accuracy (see table 2), and the value of absorbance of test solution is considered acceptable for determining the calcium concentration, expressed in micrograms/cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияof Sa, according to the calibration schedule.


Table 2

           
    Allowable difference, %
Mass fraction of calcium,
%
Error analysis % two secondary results of the analysis performed
in various conditions
two Paral-
lennyh definitions
three Paral-
lennyh definitions
the results of the analysis of standard sample and certified values
From 0.001 to 0.002 incl.
0,0008 0,0010 0,0008 0,0010 0,0005
SV. Of 0.002 «to 0.005 «
0.0016 inch 0,0020 0,0017 0,0020 0,0010
«0,005» 0,01 «
0,0026 0,0033 0,0027 0,0034 0,0017
«0,01» 0,02 «
0,004 0,006 0,005 0,006 0,003
«0,02» 0,05 «
0,007 0,009 0,007 0,009 0,004
«0,05» 0,10 «
0,012 0,015 0,012 0,015 0,008
«To 0.10» to 0.20 «
0,018 0,022 0,018 0,022 0,012

4 processing of the results

4.1 the Content of calcium (ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция) percentage in the test sample, expressed in mass fractions, calculated by the formula

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция


or in the case of using aliquote part of the solution

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция,


where ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияis the concentration of calcium in solution in the reference experiment, µ g/cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция;

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция — calcium concentration in the measured solution, µg/cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция;

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальцияthe volume of the measured solution, cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция;

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция — the volume of the test solution obtained after dissolution of sample, cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция;

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция — volume aliquote part of the solution, cmГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция;

ГОСТ Р 50424-92 Сталь и чугун. Метод определения кальция — the weight of the portion of samples

s,

4.2 the Norms of accuracy and norms control the accuracy of determining the mass fraction of calcium are shown in table 2.