US EPA

1439885 

Journal Article 

Determination of total and extractable hydrogen peroxide in organic and aqueous solutions of uranyl nitrate 

Goodall, P 

1999 

Yes 

Journal of Radioanalytical and Nuclear Chemistry
ISSN: 0236-5731
EISSN: 1588-2780 

240 

1 

5-13 

10.1007/bf02349129 

WOS:000080027500002 

The development of a spectrophotometric method for the
determination of hydrogen peroxide in uranyl nitrate solutions is reported. The method involves
the measurement of the absorbance at 520 nm of a vanadyl peroxide species. This species was
formed by the addition of a reagent consisting of vanadium (V) (50 mmol.dm(-3)) in dilute
sulphuric acid (2 mol.dm(-3) H2SO4) This reagent, after dilution, was also used as an extractant
for organic phase samples. The method is simple and robust and tolerant of nitric acid and U(VI).
Specificity and accuracy were improved by the application of solid phase extraction techniques to
remove entrained organic solvents and Pu(IV). Reverse phase solid phase extraction was used to
clean-up aqueous samples or extracts which were contaminated with entrained solvent. A solid
phase extraction system based upon an extraction chromatography system was used to remove Pu(IV).
Detection limits of 26 mu mol.dm(-3) (0.88 mu g.cm(-3)) or 7 mu mol.dm(-3) (0.24 mu g.cm(-3))
for, respectively, a 1 and 4 cm path length cell were obtained. Precisions of RSD = 1.4% and
19.5% were obtained at the extremes of the calibration curve (5 mmol.dm(-3) and 50 mu mol.dm(-3)
H2O2, 1 cm cell). The introduction of the extraction and clean-up stages had a negligible effect
upon the precision of the determination. The stability of an organic phase sample was tested and
no loss of analyte could be discerned over a period of at least 5 days. The presence of trace
levels of reductants interfered with the determination, e.g., hydrazine (<2 mmol.dm(-3)), but
this effect was ameliorated by increasing the concentration of the colormetric reagent.