m-Nitrobenzoes�ure als Reagens zur Zirkoniumbestimmung

Venkataramaniah, M.; Rao, Bh. S. V. Raghava

doi:10.1007/bf00452275

Cited by 4 publications

(3 citation statements)

References 3 publications

Supporting

Mentioning

Contrasting

Order By: Relevance

“…In our work, the acidity was about 0.25 N after the addition of the precipitant. When the zirconium m-nitrobenzoate is to be ignited t o zirconiunl dioxide in a gravimetric determingtion, a double precipitation may be necessary to eliminate coprecipitated ions of thorium and of certain other elements (5). The reagent will precipitate plutonium as plutonium (IV) but not a s plutonium (111) (2).…”

Section: Discussionmentioning

confidence: 99%

“…

…”

mentioning

confidence: 99%

“…of ammonium nitrate, water to give a volume of about 100 ml., and then, a t the boiling point with stirring, about 100 ml. of a hot 1% aqueous solution of m-nitrobenzoic acid (5). The mixture is boiled gently for five minutes and then filtered hot through a Gooch crucible.…”

mentioning

confidence: 99%

See 2 more Smart Citations

Note on the Polarographic Determination of Zirconium

Graham¹,

VanDalen²,

Upton³

1952

Can. J. Chem.

View full text Add to dashboard Cite

We have found that a useful polarographic method for the determination of zirconium can be based on the findings that m-nitrobenzoic acid is polarographically reducible (1,4) and that this compound is a highly selective precipitant for zirconium (3,5). In principle, the method consists of precipitating zirconium with m-nitrobenzoic acid, dissolving the filtered and washed precipitate in hydrochloric acid, and measuring the height of the polarographic wave corresponding to the reduction of the m-nitrobenzoic acid (to the hydroxylamine stage) in a suitable supporting electrolyte. The method is accordingly an indirect one for zirconium, and depends on the specificity of m-nitrobenzoic acid as a precipitant. We have applied the method successfully to the determination of zirconi~~m in magnesium-base alloys. PROCEDURETo a 5-gm. sample of the alloy, about 25 ml. of water is added followed by sufficient 16 M nitric acid (about 35 ml., in small portions) to cause ready dissolution, except for the relatively small residue which contains the so-called "insoluble" zirconium. The mixture is filtered through paper (Whatman No. 42) and the residue washed with 2.0 M nitric acid. The filtrate and washings are caught in a 250 ml. volumetric flask, from which, after making up to the mark with 2.0 M nitric acid, one or more 25 ml. aliquot samples are taken. T o each of these is added aqueous ammonia (1 :I) to the Congo red end point, with care being taken to avoid precipitation of zirconium. There are then added 20 ml. of 2.0 M hydrochloric acid, 10 gm. of ammonium nitrate, water to give a volume of about 100 ml., and then, a t the boiling point with stirring, about 100 ml. of a hot 1% aqueous solution of m-nitrobenzoic acid (5). The mixture is boiled gently for five minutes and then filtered hot through a Gooch crucible. The precipitate is washed with hot water and then dissolved in 25 ml. of 6.0 M hydrochloric acid by placing the crucible and acid in the original beaker and warming the mixture. The crucible, after it is washed down with water, is re~noved from the beaker and the contents of the beaker are neutralized to theCongo red end point wit11 aqueous ammonia (1:l) and washed with water into a 250 ml. volumetric flask. One or more 25 ml. aliquot samples are then pipetted into 100 ml. volumetric flasks, and, to each, 50 ml. of a 0.20 M solution of potassium chloride, 10 ml. of 0.20 M hydrochloric acid (by pipette), and 1 ml. of 0.75% gelatin solution (as a ~naxinlum suppressor) are added. The solution is made up to volume with water, a portion is decanted into the polarographic cell, bubbled with purified nitrogen for 15 min., and then polarographed.The polarographic wave for the first reduction step of nz-nitrobenzoic acid For personal use only.

show abstract

Section: Discussionmentioning

confidence: 99%

“…

…”

mentioning

confidence: 99%