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Measurement of water by oven evaporation using a novel oven design.
Authors:Sam A Margolis  Kevin Vaishnav  John R Sieber
Institution:(1) Analytical Chemistry Division, Chemical Science and Technology Laboratory, National Institute of Standards and Technology, 100 Bureau Drive, MS 8392, Gaithersburg, MD 20899-8392, USA;(2) 5902 Roosevelt Street, Bethesda, MD 20817, USA
Abstract:Using an automated oven evaporation technique combined with the coulometric Karl Fischer method, the mass fraction of water has been measured in cement, coal, and refined oil samples. The accuracy of this method was established by using SRM 2890, water-saturated 1-octanol that was added to white oil. The samples were analyzed for total reactive Karl Fischer reagent (KFR) material, for interfering materials, and for material that does not react with the aldehyde–ketone KFR. All of the samples yielded volatile material that reacted with the standard KFR. None of the samples contained significant masses of material that reacted with iodine. The cement and coal SRMs contained no material that reacted with methanol and very little material that did not volatilize at 107°C. The refined oils contained some material that was volatile at 107°C and some at 160°C. However, none of this material reacted with the aldehyde–ketone reagent. These results show that the material in the solid samples is water and that the material in the refined oils is a material other than water which reacts with methanol to form water.
Keywords:Water  Karl Fischer  Oven evaporation  Coal  Portland cement  Solvent neutral oils
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