A colorimetric modification of the wickbold procedure for the determination of non ionic surfactants in biodegradation test liquors

Waters, J.; Longman, G. F.

doi:10.1016/0003-2670(77)80045-7

Cited by 13 publications

(5 citation statements)

References 3 publications

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“…The nonionic surfactant was determined using the nonspecific BiAS method in accordance with the procedure of Wickbold (28,29), using the ethylene diamine tetraacetic acid modification as proposed by other authors for the quantification of nonionic surfactants (30). The percentage of MBAS or BiAS elimination was based on the determination of MBAS and BiAS in the influent and effluent streams of the Husmann units using the OECD 303A calculation criteria (23).…”

Section: Methodsmentioning

confidence: 99%

Effect of temperature on the biodegradation of linear alkylbenzene sulfonate and alcohol ethoxylate

Prats

López

Vallejo

et al. 2006

J Surfact & Detergents

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The effect of temperature on the biodegradation of linear alkylbenzene sulfonate (LAS) and alcohol ethoxylate (AE) was evaluated using method OECD 303 A, Confirmatory test (Husmann units). The experiments were performed using an initial surfactant concentration of 10 mg/L and working temperatures of 25, 15, and 9°C, keeping the biodegradation units inside a thermostatic chamber. In all cases, the removal of both surfactants tested, LAS and AE, was higher than 90%, regardless of the temperature used in the test. We observed that longer acclimation periods were needed by the microorganisms at lower temperatures.Paper no. S1488 in JSD 9, 69-75 (Qtr. 1, 2006).The widespread use of surfactants in many household and industrial products, together with the high volume consumed worldwide, justifies the abundant and frequent scientific scrutiny of the environmental safety characteristics of these products. Among the variety of surfactants used in the industry, anionic linear alkylbenzene sulfonates (LAS) and nonionic alcohol ethoxylates (AE) are the most relevant families, representing 27 and 22% of the total volume used in the European Union in 1998 (1). The behavior of these surfactants during wastewater treatment operations has been thoroughly studied (2-5). Biodegradation begins in the sewer system (5-7), with reported removals higher than 60% for LAS and between 28 and 58% for AE (5). The LAS concentration in raw sewage varies from 1 to 10 mg/L (8), reaching 32 mg/L in some isolated peak cases (7). Reported concentrations for AE are in the range of 1-4 mg/L (4,9). The elimination of LAS in wastewater treatment plants (WWTP) depends on the type of operation used; in plants operated with trickling filter systems, removals higher than 85% have been reported (7,10), whereas in plants using activated sludge systems, removals higher than 98% are widely obtained (2,5). Treatments based on trickling filters are reported to provide more variable degrees of removal (11). In the case of AE, the published information indicates removals higher than 98% (3,4,9). The degree of mineralization observed with LAS and AE in WWTP operating with activated sludge has been reported to be higher than 90% (12-14).LAS and AE are removed by biological processes (biodegradation) as well as by physical processes (sorption-precipitation) (2,3). The mass balance for LAS elimination according to different studies conducted at real environmental conditions (15) indicates that approximately 90% is biodegraded, 10% is removed by sorption onto the sludge, and less than 1% leaves the treatment plants with the treated water. Adsorption of LAS on activated sludge increases with the length of the alkyl chain (16), and it has been reported that the adsorption coefficient increases 2.8 times per methylene group (17). The physical removal of AE with primary sludge has been found to be between 6 and 60% of the total for C 10 EO 9 and C 16 EO 9 , respectively. Physical removal is also influenced by the length of the ethoxy groups (3). Levels of AE on the sludge a...

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Section: Methodsmentioning

confidence: 99%

Effect of temperature on the biodegradation of linear alkylbenzene sulfonate and alcohol ethoxylate

Prats

López

Vallejo

et al. 2006

J Surfact & Detergents

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“…The BiAS procedure has been elaborated by Wickbold et al ,, using barium tetraiodobismuthate (modified Dragendorff reagent) to form an orange precipitate with nonionic surfactants in moderately to strongly acidic solutions. The precipitate is then dissolved with ammonium tartrate solution, and the released bismuth ions are determined colorimetrically, , by potentiometric titration, , or by X-ray fluorescence spectroscopy. , In its original scope, the procedure was designed for the analysis of contaminated water samples containing milligrams per liter levels of nonionic surfactants, after concentration by solvent sublation (see section II.B.2). Waters et al have shown that an optimized procedure involving unfiltered samples, four 10-min sublation steps, and a cation/anion exchange cleanup of the sublation extract (see section II.B.2) is required to obtain reliable BiAS levels .…”

Section: Determination Procedures1 Colorimetry/titrimetrymentioning

confidence: 99%

“…The BiAS procedure has been elaborated by Wickbold et al 64,85,86 using barium tetraiodobismuthate (modified Dragendorff reagent) to form an orange precipitate with nonionic surfactants in moderately to strongly acidic solutions. The precipitate is then dissolved with ammonium tartrate solution, and the released bismuth ions are determined colorimetrically, 87,88 by potentiometric titration, 64,85 or by X-ray fluorescence spectroscopy. 89,90 In its original scope, the procedure was designed for the analysis of contaminated water samples containing milligrams 67 The BiAS procedure fails to determine APEOs with less than five ethoxy groups because these compounds are not precipitated by the modified Dragendorff reagent.…”

Section: Colorimetry/titrimetrymentioning

confidence: 99%

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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“…The orange precipitate formed by the re action of nonionic surfactant with tetraiodobismuthate (modified Dragendroff reagent) is dissolved with ammonium tartrate solution and the liberated bismuth is determined by titration (Wickbold [31]), atomic absorption (HMSO) [32] or UV, (Waters and Longman) [33]. The surfactants analysed (in the range 250--800 Jig) must have 6-50 ethylene oxide groups although propoxylated surfactants also react.…”

Section: Bismuth Active Substances (Bias)mentioning

confidence: 99%