Analysizing Tungsten Oxide Pyrochlore Type
A purity of more than 99.9% WO3 into a porcelain crucible, porcelain crucible and then placed in a muffle furnace and calcined at 800℃ 1 hour coolish placed in a desiccator, cool room temperature. Accurately weighed 0.25g tungsten trioxide into 100ml beaker, with 20% NaOH20ml, heating completely dissolved, after cooling into 250ml volumetric flask, dilute to the mark and shake, this solution was transferred to a plastic bottle dry spare.
Standard curve: accurate absorption 1.00mg / ml solution 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0ml Guarantee 100ml flask were placed with 0.85N ~ NaOH complement to 10ml, plus 50 percent potassium thiocyanate 5ml, plus 1: 1HCL50ml, plus 1% TiCl32ml, diluted with water to the mark and shake for 10 minutes, measured at 721 spectrophotometer extinction 0.5cm cuvette with a wavelength of 420 nm, as a reagent blank reference, drawing working curve, the measured slope of the curve K.
Solid phase analysis
Weigh a sample in 50ml of 0.200 ~ 0.500g iron crucible, adding sodium peroxide 4g, was stirred with dry round a glass rod, a small piece of filter paper Sassafras net glass rod, the filters were put in a crucible, in addition to the low temperature furnace H2O , add a muffle furnace at a temperature of 700 ~ 750 ℃ burn for about 10 minutes until pink, remove coolish, leaching into the 250ml beaker containing 100ml of hot water, and washed with water crucible, cooled to room temperature later, into 250ml volumetric flask, dilute to the mark, shake, filtration.Imbibe filtrate G2ml (tungsten oxide content may be) in 100ml volumetric flask, fill 0.85N sodium hydroxide to 10ml, following the same standard curve drawing methods.
Standard curve: accurate absorption 1.00mg / ml solution 0, 0.5, 1.0, 1.5, 2.0, 2.5, 3.0ml Guarantee 100ml flask were placed with 0.85N ~ NaOH complement to 10ml, plus 50 percent potassium thiocyanate 5ml, plus 1: 1HCL50ml, plus 1% TiCl32ml, diluted with water to the mark and shake for 10 minutes, measured at 721 spectrophotometer extinction 0.5cm cuvette with a wavelength of 420 nm, as a reagent blank reference, drawing working curve, the measured slope of the curve K.
Solid phase analysis
Weigh a sample in 50ml of 0.200 ~ 0.500g iron crucible, adding sodium peroxide 4g, was stirred with dry round a glass rod, a small piece of filter paper Sassafras net glass rod, the filters were put in a crucible, in addition to the low temperature furnace H2O , add a muffle furnace at a temperature of 700 ~ 750 ℃ burn for about 10 minutes until pink, remove coolish, leaching into the 250ml beaker containing 100ml of hot water, and washed with water crucible, cooled to room temperature later, into 250ml volumetric flask, dilute to the mark, shake, filtration.Imbibe filtrate G2ml (tungsten oxide content may be) in 100ml volumetric flask, fill 0.85N sodium hydroxide to 10ml, following the same standard curve drawing methods.
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