Determination of total phosphate in waste waters by on-line microwave digestion incorporating colorimetric detection

Williams, Kathleen E.; Haswell, Stephen J.; Barclay, David; Preston, Gaynor

doi:10.1039/an9931800245

Cited by 49 publications

(15 citation statements)

References 4 publications

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“…McKelvie et al ( 1993) used gel filtration and FIA to determine low and high molecular weight phosphorus species in water, wastewater, and sediment extracts. Williams, K.E. et al ( 1993) developed a method for total phosphate determination in wastewater based on on-line microwave digestion and subsequent colorimetric detection.…”

Section: New Applicanonsmentioning

confidence: 99%

Chemical species

Jensen¹,

Dietrich²

1994

Water Environment Research

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Section: New Applicanonsmentioning

confidence: 99%

Chemical species

Jensen¹,

Dietrich²

1994

Water Environment Research

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“…These attempts included different flow techniques, as well as digestion and reaction conditions. Some methods have been developed for flow analysis of TDP in various mediums: soil leachate and runoff waters by Peat et al (1997), wastewaters by Aoyagi et al (1988), Hinkamp and Schwedt (1990) and Williams et al (1993). These methods generally use drastic digestion conditions and their limits of detection are inappropriate for unpolluted natural waters, especially seawater.…”

Section: Introductionmentioning

confidence: 99%

An automated photo-oxidation method for the determination of dissolved organic phosphorus in marine and fresh water

Aminot

Kérouel

2001

Marine Chemistry

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A segmented flow automated method with on-line photo-oxidation for the determination of dissolved organic phosphorus+soluble reactive phosphorus (DOP+SRP) in seawater and fresh water is described here. A low-power lamp was used for a compact, easy-to-handle and low-ozone-producing manifold. The influence of seawater matrix components was studied in detail using natural seawater and salt solutions spiked with DOP model compounds. Bromide was found to be the most inhibitory species in seawater. The work shows that most salt solutions referred to as artificial seawater are not satisfactory model matrices to test the actual seawater matrix effect. Since DOP recovered in undiluted seawater samples was about half that obtained in fresh water samples, the described method includes a 5-to 6-fold dilution of seawater samples. This simple procedure overcomes matrix effects and provides satisfactory DOP recovery. No pH effect was found in the 6-9 range corresponding to most natural waters. The standard deviation was 0.007 μmol l −1 and the limit of detection 0.02 μmol l −1 . Linearity was tested up to 5 μmol l −1 of DOP, i.e. far above naturally occurring values. A throughput of 20 samples per hour is easily achieved. ABSTRACTA segmented flow automated method with on-line photo-oxidation for the determination of dissolved organic phosphorus + soluble reactive phosphorus (DOP + SRP) in seawater and fresh water is described here. A low-power lamp was used for a compact, easy-to-handle and low-ozone-producing manifold. The influence of seawater matrix components was studied in detail using natural seawater and salt solutions spiked with DOP model compounds. Bromide was found to be the most inhibitory species in seawater. The work shows that most salt solutions referred to as artificial seawater are not satisfactory model matrices to test the actual seawater matrix effect. Since DOP recovered in undiluted seawater samples was about half that obtained in fresh water samples, the described method includes a 5 to 6-fold dilution of seawater samples. This simple procedure overcomes matrix effects and provides satisfactory DOP recovery. No pH effect was found in the 6-9 range corresponding to most natural waters. The standard deviation was 0.007 µmol l -1 and the limit of detection 0.02 µmol l -1 . Linearity was tested up to 5 µmol l -1 of DOP, i.e. far above naturally occurring values. A throughput of 20 samples per hour is easily achieved.

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“…In the PUREX process, where TBP exposed to acidic conditions (nitric acidaqueous phase) and gamma radiation (U, Th, and fission products), undergoes hydrolytic and radiolytic reactions resulting into formation of some undesired components mainly dibutyl phosphate (DBP) and to a lesser extent monobutyl phosphate (MBP). Numerous analytical methods like GC-FID [16][17][18][19], titrimetry [20], complex-gravimetry [21], ion pair chromatography [22][23][24], colorimetry [25,26], IR, UV-VIS, NMR spectroscopy [7,22], and AAS [27] exist to determine TBP at higher concentration level. High speed isotachophoresis [28] was successfully used to analyze degradation mixture of TBP.…”

Section: Introductionmentioning

confidence: 99%

Thermal Decomposition of Nitrated Tri-n-Butyl Phosphate in a Flow Reactor

Patil

Gaikar

Kumar

et al. 2012

ISRN Chemical Engineering

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Tri-n-butyl phosphate (TBP) is a universal nuclear extractant, commercially used in the PUREX process for the last 60 years. However, it is prone to nitration and thermal degradation, and as a consequence a red-oil event may be initiated under several operating conditions resulting in severe pressurization of vessel/cell if venting is inadequate. In this work, an attempt was made to understand the reaction pathway of thermal decomposition of nitrated TBP in a flow reactor at atmospheric pressure. Many reaction products were identified and quantified by instrumental methods like HPLC-RI and GC-TCD. The experimental data was analysed with a power law model and the apparent rate constants were estimated. The activation energy for thermal decomposition of nitrated TBP, assuming an Arrhenius type of temperature dependency, was estimated to be 47.39 ± 0.25 kJ·mol −1 . The effect of both varying temperature and concentration of nitric acid on conversion of TBP into degradation products and products distribution was experimentally studied. Based on the experimental observations, a reaction mechanism framework for thermal decomposition of nitrated TBP is proposed.

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Determination of total phosphate in waste waters by on-line microwave digestion incorporating colorimetric detection

Cited by 49 publications

References 4 publications

Chemical species

Chemical species

An automated photo-oxidation method for the determination of dissolved organic phosphorus in marine and fresh water

Thermal Decomposition of Nitrated Tri-n-Butyl Phosphate in a Flow Reactor

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