Carboxylic Biointermediates of LAS and NPEO: Synthesis, Characterization and RP-HPLC Determination

Marcomini, Antonio; Busetti, S; Sfriso, Adriano; Capri, Silvio; Noce, T. La; Liberatori, A.

doi:10.1007/978-94-011-3356-2_27

Cited by 7 publications

(8 citation statements)

References 13 publications

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“…The quantification limit was 0.1 μg L -1 . OP1EC was prepared using a method reported previously ( , ). Compound identity and purity were verified using 1 H NMR and elemental analysis.…”

Section: Experimental Design and Analytical Methodsmentioning

confidence: 99%

Biodegradation Residual of 4-Octylphenoxyacetic Acid in Laboratory Columns under Groundwater Recharge Conditions

Wild

Reinhard

1999

Environ. Sci. Technol.

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The biodegradation of 4-octylphenoxyacetic acid (OP1EC) was studied in laboratory columns to determine the residual concentration that can persist during groundwater recharge or transport. Biofilm models predict residual concentrations are independent of the initial concentration and residence time. Two column trains, constructed with glass beads and providing a residence time of 280 min were fed continuously with lake water (LW) containing biodegradable dissolved organic carbon (DOC) and groundwater (GW) containing no biodegradable DOC. The feedwater was amended with OP1EC first at high (1 mg/L) and then at low (50 μg L-1) concentration. To simulate mixing of recharged LW and regional GW, the effluents of the GW and LW train were blended and fed to a column (BW) with 114 min residence time. When the influent OP1EC concentration was 1000 μg/L the residual concentra tions in the LW and GW trains ranged from 0.3 to 3 and 0.8 to 3 μg L-1, respectively. When the feed concentrations were decreased to 50 μg L-1, the residual concentration in the LW decreased to below the detection limit (<0.1 μg L-1) but stayed above 0.2 μg L-1 in the GW train effluent. Mixing the two LW and GW column effluents stimulated additional (up to 11%) dissolved organic carbon (DOC) removal but no additional OP1EC degradation.

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“…The quantification limit was 0.1 μg L -1 . OP1EC was prepared using a method reported previously ( , ). Compound identity and purity were verified using 1 H NMR and elemental analysis.…”

Section: Experimental Design and Analytical Methodsmentioning

confidence: 99%

Biodegradation Residual of 4-Octylphenoxyacetic Acid in Laboratory Columns under Groundwater Recharge Conditions

Wild

Reinhard

1999

Environ. Sci. Technol.

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“…Soxhlet extractions are mostly carried out with dried samples. For this the samples are either dried at 60 °C − or freeze-dried 42,59 and then pulverized. In a typical procedure 0.5 g of detergent powder, 2 g of sewage sludge, and 20 g of soil or sediment are transferred into the preextracted paper thimble of the Soxhlet apparatus.…”

Section: Extraction From Solid Matricesmentioning

confidence: 99%

“…Quantification of LAS and NPEOs was performed by external standard calibration graphs. , A similar method was developed for determining simultaneously LAS and NPEOs as well as their corresponding metabolites sulfophenyl carboxylate (SPC) and alkylphenol ether carboxylates (APECs), respectively. These analytes were quantitatively determined using calibration graphs or the standard addition method. , …”

Section: High-performance Liquid Chromatography (Hplc) and Liquid Chr...mentioning

confidence: 99%

“…NPEO concentrations in samples from STP near Prato, Italy, dealing with textile waste waters ranged from 5700 to 9000 μg L -1 in influent water and from 400 to 480 μg L -1 in effluent water, while NPEC concentrations were 600−1100 μg L -1 in influents and 500−1600 μg L -1 in effluents. NPEOs, therefore, was remarkably biodegraded before reaching the STP since NPECs was already present in the influents . The situation was different in case of sewages of prevailing domestic origin.…”

Section: A Sewage Treatment Plantsmentioning

confidence: 99%

“…These analytes were quantitatively determined using calibration graphs or the standard addition method. 36,81 Electrospray (ES) LC/MS currently provides the most sensitive and selective analysis of NPEOs. This method allows the determination of NPEOs from influents and effluents of sewage treatment plants, river water, and drinking water with detection limits of 0.6, 0.02, 0.002, and 0.0002 µg L -1 , respectively, using an alcohol ethoxylate (C-10 EO 6 ) as an internal standard.…”

Section: Mass Spectrometrymentioning

confidence: 99%

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Alkylphenol Ethoxylates: Trace Analysis and Environmental Behavior

1997

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APEOs, the reader is referred to other books and reviews. [24][25][26][27][28][29] II. Analysis A. Sampling and StorageAnalytical results significantly depend on the homogeneity of the samples and accurate storage procedures which guarantee that no changes take place in the composition of the samples. The main problem of surfactants in general is their tendency to adsorb on all phase boundaries due to their amphiphilic nature. Consequently losses to surfaces or suspended solids from aqueous solutions are commonplace. Especially for matrices like sewage sludge, sediment, or soils, quantitative recovery of analytes turns out to be very difficult. Therefore, internal standards are added to the samples to correct for nonquantitative recovery during isolation and quantification of the analytes. Giger et al. used n-nonylbenzene 11,30 and 2,4,6-tribromophenol 8 in gas chromatographic determinations of APs/APEOs from sludge and water, respectively. 4-n-Nonylphenol, which is not included in technical NP, is applied to the quantification of NP in soils by GC. 31 For water analysis by HPLC 2,4,6-trimethylphenol is well suited. 32 This approach, however, is useless for nonspecific methods since they cannot discriminate analytes initially present from added internal standards.Environmental samples have to be preserved immediately upon collection with chemical biocides to minimize and prevent microbial degradation of the surfactant present. Water samples from sewage treatment plants, rivers, or seas are generally collected in glass bottles, preserved with 1% formaldehyde, and stored at 4 °C. [33][34][35][36][37] A less common preservation method for aqueous samples is the addition of methylene chloride and acidification to pH 2 with hydrochloric acid. 38 Kubeck et al. showed that refrigeration alone was sufficient to stabilize river water samples for up to 4 weeks. 35 Due to diurnal variations of APEO concentrations in the influents and effluents of sewage treatment plants, 24-h and 2-h composite samples should be collected, ideally, with automatic sampling devices. 39 Sewage sludges are dealt with in the same way as water samples, i.e. preservation with 1% formaldehyde and storage at 4 °C. 39,40 Jobst et al. preferred aluminium vessels to store the sludge samples. 41 Sediment samples are collected from the upper 2 cm using a grab sampler and frozen at -20 °C until analysis. 33,[42][43][44] In the laboratory, samples are freezedried 44 or air-dried at 21 °C43 .The application of sewage sludges to agricultural land has resulted in the need to monitor concentrations of detergents in sludge-amended soils. Soil samples are collected from the upper 5 cm with a stainless steel corer, dried at 60 °C, pulverized, and stored in the dark at 4 °C. 40 Biological matrices represent a difficult problem with regard to a representative sampling and a unchanged composition of the samples during storage. The Environmental Specimen Bank (ESB) of Germany has developed a method for collection and preparation of fresh biological materials. 45,46 ...

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LAS removal and biodegradation in a wastewater treatment plant

Cavalli¹,

Gellera²,

Landone³

1993

Enviro Toxic and Chemistry

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Linear alkylbenzene sulfonate (LAS) biodegrades easily and loses its tensioactive properties quickly through a primary biodegradation process, as many works of literature testify. Many studies have been carried out in laboratories or in pilot plants, whereas few have been undertaken in a wastewater treatment plant (WWTP). In Italy, unlike in other countries, no detailed investigation has been made so far to establish LAS biodegradation in real WWTP conditions. EniChem Augusta (EA) and Consorzio Po‐Sangone (CPS) have worked together for over two years on this problem, taking into consideration the large (flow rate: approximately 400 × 103 m3/d) and central active sludge WWTP of the metropolitan area of Torino, north of Italy. Specific LAS data have been obtained, using established HPLC techniques, in influent and effluent streams, in the dissolved (waters) and adsorbed (suspended solids and sludges) phases, to reach a complete mass balance. LAS removal >99% and LAS biodegradation of approximately 85% have been observed. Attention also has been given to LAS intermediates of biodegradation, namely the sulfophenyl carboxylates (SPC), using HPLC and GC‐MS techniques, the latter after derivatization. The SPCs have been found present only in the waters and not in the adsorbed phases (SS and sludges).

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Carboxylic Biointermediates of LAS and NPEO: Synthesis, Characterization and RP-HPLC Determination

Cited by 7 publications

References 13 publications

Biodegradation Residual of 4-Octylphenoxyacetic Acid in Laboratory Columns under Groundwater Recharge Conditions

Biodegradation Residual of 4-Octylphenoxyacetic Acid in Laboratory Columns under Groundwater Recharge Conditions

Alkylphenol Ethoxylates: Trace Analysis and Environmental Behavior

LAS removal and biodegradation in a wastewater treatment plant

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