Fluoride gravimetric analysis

Using this chemical phenomenon, heavy-metal fluoride glasses were prepared using trifluoroacetates of zirconium, barium, lanthanum, aluminum and sodium [21]. Eigure 10.2 shows thermal gravimetric analysis of the ZBLAN powder in this process. A drastic decrease in weight (47.4%) was observed in the range of 220-300 °C, which was attributed to the decomposition from the trifluoroacetate to the sohd ZBLAN fluoride. 

Fluoride ion, and weak acids and bases do not interfere, but nitrate, nitrite, perchlorate, thiocyanate, chromate, chlorate, iodide, and bromide do. Since analysis of almost all boron-containing compounds requires a preliminary treatment which ultimately results in an aqueous boric acid sample, this procedure may be regarded as a gravimetric determination of boron. 

For the analysis of molybdenum, the sample is decomposed by fuming with a few drops of nitric acid and sulfuric acid in a platinum crucible and the molybdenum is determined gravimetrically7 as the 8-quinolinol complex. From the filtrate, potassium is determined gravimetrically as K2S04. Fluoride is determined by titration with a standard solution of thorium nitrate using sodium alizarinsulfonate as indicator, after steam distillation of fluorosilicic acid.8 The determination of the oxidation state of molybdenum is carried out by oxidizing a known amount of the compound with a known amount of potassium dichromate in hot 2 N sulfuric acid and titrating the excess dichromate with standard Fe2+ solution. 

Using the proper choice of separation column, ion chromatography appears to be applicable for the sequential multicomponent analysis of other anions such as sulfate, chloride, fluoride and nitrate. The detection limits will be substantially lower than the classical gravimetric and potentiometric methods currently used. Ion selective electrodes are available for chloride and fluoride. 

Like cements, the elemental composition is determined by XRF or AAS techniques. The XRF bead is made using lithium tetraborate at 1050°C. Sulfide content cannot be determined by XRF. Sulfite, SO3 , and sulfate, S04 , are safely analyzed by XRF. Na2C03 -I- K2CO3 fusion is carried out for Ca, Mg, Fe, and A1 analysis by AAS. Lanthanum chloride is used as a sulfate interference suppressant. Gravimetric sulfate determinations are also carried out by precipitation as barium sulfate. The Leco Carbon-Sulfur Analyzer can also be used for quality control purposes. The fluoride is determined by XRF or a pyrohydrolysis method. The measurement of particle size distribution is carried out in a manner similar to that for cements and clays. 

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