Determination of Zirconium by Precipitation from Homogeneous Solution

Willard, H. H.; Hahn, Richard B.

doi:10.1021/ac60026a015

Cited by 26 publications

(12 citation statements)

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“…1 (A) Sol/Solution Characterization: Lanthanum nitrate and trimethyl phosphate were dissolved in 20% nitric acid. 45,65 Solutions with La:PO 4 ratios of 1:1, 1:1.12, 1:1.20, 1:1.60, 1:1.80, and 1:3 were made. The viscosity and density of the 1:1 mixture changed from 0.90 to 1.07 mPa⅐s and 1.02 to 1.06 g/cm 3 , respectively, as concentration changed from 20 to 80 g/L.…”

Section: Resultsmentioning

confidence: 99%

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Continuous Coating of Oxide Fiber Tows Using Liquid Precursors: Monazite Coatings on Nextel 720™

Boakye

Hay

Petry

1999

Journal of the American Ceramic Society

114

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Seven different aqueous or ethanolic precursors were used to continuously coat monazite (LaPO 4 ) on Nextel 720™ fiber tows. Immiscible liquid displacement was used to minimize bridging of coating between filaments. Precursor viscosities, densities, and concentrations were measured, and solids were characterized by DTA / TGA and X-ray. Coatings were cured in-line at 1200°-1400°C and characterized for thickness, microstructure, and composition by optical microscopy, SEM, and TEM. Tensile strengths of the coated fibers varied with the precursor used and were 25% to >50% lower than those of the as-received fiber. The coating stoichiometry and coating thickness of a particular precursor did not correlate with tensile strength. Median coating thicknesses were typically ∼50-100 nm for precursors with 40-80 g / L monazite, much larger than thicknesses predicted by theory for 12 mm diameter monofilaments. There were significant thickness variations from filament to filament, but usually little variation in composition or microstructure. Amorphous AlPO 4 layers formed from phosphate-rich precursors. Factors that could affect coating characteristics and tensile strength reduction were discussed.

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Section: Resultsmentioning

confidence: 99%

“…If this behavior was similar to that for other mixed nitrate phosphates, the product could have been lanthanum methyl phosphate, (LaO(H(CH 3 )(PO 4 ))⅐1H 2 O). 45,65 A DTA exotherm suggested that this intermediate converted to monazite above 540°C ( Fig. 10).…”

Section: Resultsmentioning

confidence: 99%

Continuous Coating of Oxide Fiber Tows Using Liquid Precursors: Monazite Coatings on Nextel 720™

Boakye

Hay

Petry

1999

Journal of the American Ceramic Society

114

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“…For small amounts the phosphate precipitate can be ignited and weighed as ZrP207 (4; 65, p. 321). Willard determined larger amounts by precipitation from homogeneous solution by heating with triethyl phosphate ( 66).…”

Section: Gravimetricmentioning

confidence: 99%

Titrimetric Determination of Zirconium

Fritz¹,

Fulda²

1954

Anal. Chem.

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1~c-382 T h i s r e p o r t i s d i s t r i b u t e d a c c o r d i n g t o t h e c a t e g o r y Chemistry-General a s l i s t e d i n M-3679, April 15, 1953. Macro amounts of zirconium a r e u s u a l l y d e t e r m i n e d g r a v i m e t r ic a l l y o r by t i t r i m e t r i c means f o l l o w i n g q u a n t i t a t i v e i s o l a t i o n o f a p r e c i p i t a t e . T h i s i s time-consuming. T h i s p a p e r d e s c r i b e s a q u i c k , d i r e c t t i t r i m e t r i c method f o r zirconium. The t i t r a t i o n i s Carrie3 o u t i n a c i d s o l u t i o n w i t h Versene (disodium dihydrogen ethylenediaminetetraacetate), a s t a b l e , s o l u b l e complex b e i n g formed. -A v i s u a l i n d i c a t o r g i v e s a s h a r p end p o i n t . Ir,on, thorium, mol-y-bdenum and bismuth c o n s t i t u t e i m p o r t a n t i n t e r f e r e n c e s , b u t most o t h e r metals do n o t a f f e c t t h e r e s u l t s . .Tin and t i t a n i u m , r e d u c e t h e s h a r p n e s s of t h e end p o i n t b u t d o n o t o t h e r w i s e i n t e rf e r e . T h i s method s h o u l d be a p p l i c a b l e t o many s p e c i f i c problems w ISC-382 i t h o u t m o d i f i c a t i o n . I t a l s o c o n s t i t u t e s a new approach t o t h e d e t e r m i n a t i o n o f z i r c o n i u m i n more d i f f i c u l t samples.Most of t h e r e c e n t p r o g r e s s i n a n a l y t i c a l methods f o r macro amounts o f z i r c o n i u m has be,en due t o t h e development o f p r e c i p i t a n t s s u c h a s c u p f e r r o n , mandelic a c i d , and a r s o n O f t h e s e , mandelic a c i d and its d e r i v a t i v e s (6,8,9) a r e p r o b a b l y t h e most s u c c e s s f u l . They p o s s e s s e x c e l l e n t s e l e c t i v i t y f o r z i rconium and under p r o p e r c o n d i t i o n s form p r e c i p i t a t e s o f d e f i n i t e composition. (7) have r e p o r t e d a n amperomet c t i t r a t i o n of zirconium, thorium, t i n and uranium w i t h m-nitropheny s o n i c a c i d . W h i t e (10) developed a t i t r i m e t r i c method f o r zirconium f o l l o w i n g t h e q u a n t i t a t i v e i s o l a t i o n o f zirconium mandelate. Dhar and Das Gupta (1) d e t e r m i n e d zirconium by e i t h e r c o l o r i m e t r i c o r t i t r i m e t r i c means f o l l o w i n g p r e c i p i t a t i o n w i t h oxalohydroxamic a c i d . The d i r e c t $ i t r a t i o n of thorium i n a c i d s o l u t i o n w i t h e t h y l e n e d i a m i n eu s i n g A l i z a r i n Red S i n d i c a t o r has r e c e n t l y been r e p o r t Zirconium i n t e res i n t h i s t i t r a t i o n t e t r a a c e t i c a c i d (Ve b u t cannot i t s e l f be t i t r a t e d , by t h e t h o r i u r o c e d u r e . MOW9 however, new i n d i c a t o r s have'bee'n found, which p e r m i t t h e r a p i d andThe method proposed t i v e and s h o u l d b e -o f use i n numerous cases. ,omplex must be less s t a b l e t h a n t h e zirconium-Versene complex. F u r t h e r , r e a c t...

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“…This reaction was applied to the quantitative determination of zirconium by Hahn (17). It was found entirely feasible, to determine zirconium by igniting the precipitate to zirconium pyrophosphate, ZrP2C>7, and to separate it from large amounts of other elements; only antimony, bismuth, cerium, and stannic ions'interfered.…”

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Separation by Precipitation from Homogeneous Solution

Willard¹

1950

Anal. Chem.

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When a precipitating ion is added to a solution in which a substance is to be precipitated, the local concentration of the former at the point where the solutions mix often causes coprecipitation of other ions which may remain adsorbed when the solution subsequently becomes uniform. This error is avoided by adding a substance which does not contain the desired precipitating ion as such, so that no immediate precipitation results, and the solution is homogeneous. Heat is then applied and the proper ion is formed by hydrolysis in the solution.If neutralization of an acid solution is required, the hydrolysis of urea to form carbon dioxide and ammonia is a convenient process.If a weak base is thus precipitated in the presence of the proper anion, a dense basic salt is formed. With aluminum, succinate is best; with iron, formate. Errors due to adsorption are therefore greatly decreased and far more effective separations are accomplished. Data for such separations are presented. Oxalate ion is

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Determination of Zirconium by Precipitation from Homogeneous Solution

Cited by 26 publications

References 5 publications

Continuous Coating of Oxide Fiber Tows Using Liquid Precursors: Monazite Coatings on Nextel 720™

Continuous Coating of Oxide Fiber Tows Using Liquid Precursors: Monazite Coatings on Nextel 720™

Titrimetric Determination of Zirconium

Separation by Precipitation from Homogeneous Solution

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