The determination and phase control of Ca-containing inclusions are important for the successful production of Ca-treated steels such as hydrogen induced cracking resisted steels. In this work, the quantitative isolation of calcium aluminate (mCaO·nAl
2O
3), CaS and CaO in Ca-treated steels has been investigated. All operations of isolation procedure from matrix dissolution to filtration were carried out in a glovebox with an Ar atmosphere. The atmosphere was controlled to a relative humidity of 25% to prevent H
2O from attacking the inclusions. Using this protection, 10% bromine-methanol method was capable of the quantitative isolation of mCaO·nAl
2O
3, whose reactivity with H
2O was found to be increased with increasing the ratio of m/n. Constant current electrolysis in 10% acetylacetone-1% tetramethylammonium chloride-methanol electrolyte (AA electrolysis method) was capable of the quantitative isolation of mCaO·nAl
2O
3 and CaS. However, CaO was not isolated. On the basis of these results, the method for evaluating the amounts of the Ca-containing inclusions has been developed. The amount of mCaO·nAl
2O
3 was evaluated by converting the analytical values of metal elements in the residue isolated by 10% bromine-methanol method into oxide forms. The amount of CaS was calculated from the difference between the amounts of Ca isolated by AA electrolysis method and 10% bromine-methanol method. The amount of CaO was calculated from the difference between the amounts of total oxygen and oxygen as mCaO·nAl
2O
3.
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