Is 12308-4 - 1988 - 3
Is 12308-4 - 1988 - 3
Is 12308-4 - 1988 - 3
Indian Standard
METHODSFOR
CHEMICALANALYSISOFCASTIRON
ANDPIGIRON
P/ART 4 DETERMINATION OF TOTAL CARBO~N, CRAPHITIC CARBON
AND COMBINED CARBON BY GRAVIMETRIC METHOD
1.1 This standard ( Part 4 ) -covers the gravi; The difference between the percentage of total
metric method for determination of total carbon, carbon and graphite carbon represents the com-
graphitic carbon and combined carbon in cast bined carbon.
iron, alloyed cast iron and pig iron. 5.2 Reagents
2 REFERENCE 5.2.1 Tower Packed with Granulated Manganese
Dioxide
IS 6626 ( Part 1 ) : 1971 Recommendations for
apparatus for chemical analysis of metals; 5.2.2 Tower Packed with Magnesium Per&orate
Part 1. Determination of carbon by direct corn- 5.2.3 Absorption Tower Packed with Soda Aspirate
bustion, is a necessary adjunct to this standard. and Magnesium Perchlorate
3.1 The sample shall be drawn and prepared as 5.2.5 Hydro_Ruoric acid, 40 percent
prescribed in the relevant Indian Standard. 5.2.6 Preignited Asbestos for Gooch Crucible,
( preserved in a desiccator )
3.2 The sample is to be cleaned with analar
grade organic solvent ( like acetone, benzene or 5.3 Apparatus
ether ) by washing it thrice and dried in an air
oven at 100 I-lr5°C. The apparatus recommended in 1s 6626 ( Part
1): 1971 Recommendations for apparatus for
4 QUALITY OF REAGENTS chemical analysis of metals: Part 1 Determina-
tion of carbon by direct combustion may be used.
Unless specified otherwise, analytical grade
reagents and distilled water shall be employed in 5.4 Procedure
the test.
5.4.1 For Total Carbon
5 DETERMINATION OF TOTAL CARBON,
GRAPHITIC CARBON AND COMBINED Weigh 1’00 g of sample on a preignited combus-
CARBON BY GRAVIMETRIC METHOD tion boat and introduce the same into the
combustion tube maintained at a temperature of
5.1 Outline of the Methods 1 100°C or above.
5.1.1 Total Carbon Stopper the combustion tube inside the furnace
and allow the sample to heat for I to 2 minutes.
The sample is burnt in the presence of oxygen. Then pass oxygen at the rate of 800-l 000 ml per
The carbon dioxide formed is absorbed in a tube minute while combustion is going on and allow
containing ascarite or soda asbestos and weighed. the evolved gases to pass through the tower of
granular manganese ~dioxide and magnesium
5.1.2 Graphitic Carbon perchlorate and fina.lly to the absorption tower
( 5.2.3 ) ( tube A 1 kept in series. When the com-
The sample is dissolved in nitric acid and hydro- bustion is complete ( about 2 minutes >, reduce
fluoric acid. The graphitic carbon is filtered off the rate of flow of oxygen to 400-500 ml/minute
in preignited asbestos in a fused silica gooch and continue for another 7-8 minutes in order to
crucible and dried and ignited in a combustion sweep off the carbon dioxide. Withdraw the
furnace. Carbon dioxide so formed is absorbed absorption tower ( tube A) filled with oxygen
in a tower of soda aspirate and weighed. and place it in the balance case for 10 minutes,