Determinação entalpimétrica de cálcio e magnésio em calcários usando-se um entalpímetro de fluxo contínuo

Abstract

Determination of calcium and magnesium in limestone using a flow enthalpimeter is described. The apparatus consists of a peristaltic pump, a proportional injector, two twin thermistors, a Wheatstone bridge and a strip-chart recorder. The injector, the 'flow manifolds and the emperature-sensing elqments are immersed in San insulated water bath. For the determination of calcium, preliminary studies were undertaken using the precipitation reaction with ammonium oxalate and the complaxation with Na2-EDTA and Mg-EDTA. After these studies, the experimental procedure chosen was based on complexation with Mg-EDTA. In order to test the method, determination of calcium was performed in synthetic, certified and other samples. Precision and accuracy was found to be equal to 1.0% and the analytical rate was 100 samples per hour. For the determination of magnesium, initial tests were conducted investigating the possibility of using the complexation reaction with Na2-EDTA and the previous separation of calcium by means of precipitation with ammonium oxalate and ammonium molybdate. In the final procedure, the complexation reaction with Na2-EDTA was chosen to give the amount of both calcium and magnesium. Then, magnesium is found by difference, since the percentage of calcium is known. Resuls of several determinations indicate an average error around 4% for samples with MgO higher than 10%. The uncertainty increases for samples having MgO lower than 10%. The analytical rate is about 100 samples per hour. The results of the enthalpimetric method were compared with those found by other techniques such as volumetry ( by complexation) atomic absorption and flame photometry.