Extraction from marine sediment

Montagna, P.A., 1982. Sampling design and enumeration statistics for bacteria extracted from marine sediments. Appl. Environ. Microbiol., 43 1366-1372. 

Bates, T.S. and Carpenter, R., 1979a. Determination of organosulfur compounds extracted from marine sediments. Anal. Chem., 51 551—554. 

Work is in progress to validate the MAE method, proposed for EPA, in a multi-laboratory evaluation study. Nothing similar has been reported for additives in polymeric matrices. Dean el al. [452] have reviewed microwave-assisted solvent extraction in environmental organic analysis. Chee et al. [468] have reported MAE of phthalate esters (DMP, DEP, DAP, DBP, BBP, DEHP) from marine sediments. The focus to date has centred on extractions from solid samples. However, recent experience suggests that MAE may also be important for extractions from liquids. 

Magni et al. [857] studied the optimisation of the extraction of metal-humic acid complexes from marine sediments. Polyarylamide gels have been... 

Hennig [40] has applied ultraviolet spectroscopy to the determination of aromatic constituents of residual fuel oil in hexane extracts of marine sediment samples. Examination of the ultraviolet spectra of samples of an oil pollutant from a beach and crude oil, at various concentrations, revealed strong absorption maxima at approximately 228nm and 256nm. The ratio of the peak heights at these wavelengths is constant for a particular oil, and is independent of concentration. These permit quantitative analysis of sediment samples many months after an oil spill. 

Supercritical carbon dioxide modified with methanol has been used to extract ditallowdimethylammonium from marine sediments [8]. 

In a method described by Bates and Carpenter [8] for the characterization of organosulphur compounds in the lipophilic extracts of marine sediments these workers showed that the main interference is elemental sulphur (S8). Techniques for its elimination are discussed. Saponification of the initial extract is shown to create organosulphur compounds. Activated copper removes S8 from an extract and appears neither to create nor to alter organosulphur compounds. However, mercaptans and most disulphides are removed by the copper column. The extraction efficiency of several other classes of sulphur compounds is 80-90%. Extracts are analyzed with a glass capillary gas chromatograph equipped with a flame photometric detector. Detection limit is lg S and precision 10%. 

Pontanen and Morris [8] compared the structure of humic acids from marine sediments and degraded diatoms by infrared and C13 and proton NMR spectroscopy. Samples of marine sediments taken from the Peru continental shelf were extracted with water, sodium hydroxide (0.05mol 1 J) and sodium pyrophosphate (0.05mol l-1) under an atmosphere of nitrogen and fractionated by ultrafiltration. Humic acids of molecular weight 300000 and above were examined. Diatoms were collected from... 

Kiss [8] examined various techniques for the efficient separation and preconcentration of boron from marine sediments. Alkaline fusion with potassium carbonate was used to render boron reactive, even in the most resistant silicate minerals. Fusion cakes were extracted with water and borate was isolated by Amberlite XE-243 boron-selective resin. Borate was determined spectrophotometrically, following elution with 2 mol L 1 hydrochloric acid. Either the carminic acid complex (620nm), formed in sulphuric acid (94%) or sulphuric acetic acid (1 4), or the azomethine hydrogen ion association complex (415nm) formed at pH5.2, were used for borate measurement. 

Chen et al. [Ill] extracted elemental sulphur from marine sediments with aromatic solvents and determined sulphur in the extract by gas chromatography. 

Chau et al. [f6] described a hexane extraction procedure to extract tetramethyllead, trimethylethyllead, methyltriethyllead, dimethyldiethyllead and tetraethyllead from marine sediments. The extracted compounds were analysed in their authentic forms by a gas chromatographic-atomic absorption spectrometric system. Other forms of organic and inorganic lead do not interfere. The detection limit was O.Ofmg kg-1 as lead. 

Jayaraman, S., R.J. Pruell, and R. Me Kinney. 2001. Extraction of organic contaminants from marine sediments and tissues using microwave energy. Chemosphere 44 181-191. 

Many microwave extractions can reach maximum recovery in 10 to 20 minutes. Longer extraction time is not necessary and may lead to the decomposition of thermolabile analytes. It was reported that the recovery of sulfonylurea from soil was not affected by extraction time in the range 5 to 30 minutes [79], Similar observation was made in the extraction of PAHs from soils and sediments [6], In the extraction of PAHs and LAHs (linear aliphatic hydrocarbons) from marine sediments, the extraction time was found to be dependent on the irradiation power and the number of samples extracted per run [81], When the irradiation power was 500 W, the extraction time varied from 6 minutes for one sample to 18 minutes for eight samples [74], The recovery of OCPs from spiked marine sediments increased from 30% at 5 and 10 minutes to 60% at 20 minutes and to 74 to 99% at 30 minutes [82],... 

Letellier, M. Budzinski, H. Charrier, L. Capes, S. Dorthe, A.M. 1999. Optimization by factorial design of focused microwave assisted extraction of polycyclic aromatic hydrocarbons from marine sediment. Fres. J. Anal. Chem. 364 228-237. 

Extraction of Humic Substances from Marine Sediments... 

Ambient-Temperature Extraction of Hydrocarbons From Marine Sediment-Comparison with Boiling-Solvent Extractions... 

The ability of several methods to extract polycyclic aromatic hydrocarbons (PAHs) and other petroleum hydrocarbons from marine sediments was examined. Comparisons of soxh-let and methylene chloride reflux methods gave extraction efficiencies that showed no statistical difference in the return of PAHs however, the return when using ball-mill tumbling was significantly lower. The relative content of individual parent PAH compounds, parent compound distributions (PCDs), and alkyl homologue distributions (AHDs) of PAHs was calculated using capillary column GC-MS. The similarities of the distributions showed that any of the three methods could have been used to calculate these distributions. An examination of several extraction methods commonly used for the extraction of petroleum hydrocarbon material from sediment samples showed differences in results that depended on the extraction method employed. In addition, the methods varied in their ability to extract resolved versus unresolved material and to return aliphatic and aromatic hydrocarbon compounds. 

Several studies have examined the total PAH content, the relative content of individual parent PAH compounds, that is, parent compound distributions (PCDs), and the alkyl homologue distributions (AHDs) of PAHs from extracts of marine sediments (1-9). The analytical methods used in these studies were generally complex and lengthy, and consisted of an extraction, an isolation of the PAH material (by either complex formation or chromatographic separation), and an analysis. Based on comparisons of PCDs and AHDs of the sediment samples with those of samples from known origins (e.g., petroleum, combustion products), these studies discussed the origins of PAH compounds found in sediments. 

This chapter reports the results of experimentation designed to examine the extraction and characterization of petroleum hydrocarbons, including PAHs, from marine sediments. The efficiencies of several methods for the extraction of PAHs from marine sediments were compared, and the ability of these extraction methods [followed by gas chromatographic-mass spectrometric (GC-MS) analysis] to reproduce consistently AHDs and PCDs from contaminated sediments was exam-... 

The present study compared the ability of three techniques to extract PAH compounds and their alkylated homologues from marine sediments. Specifically, this study was designed to determine if the results of a shorter and simpler extraction (CH2C12 reflux) were comparable with those from longer yet more commonly used extraction methods (exhaustive soxhlet and ball-mill tumbling). 

Hydrocarbon Investigations. Since no standard method exists for the analysis of hydrocarbon material from marine sediment, the extraction and analytical procedures used to determine the level of hydrocarbons in... 

The results of Experiment 3 are shown in Table IV. This experiment compared the ability of different methods (III and V) to extract recently added petroleum hydrocarbons from marine sediment. The more vigorous extraction (Method V) increased the yield, but the additional material returned was unresolved. It appeared that the extractions were equally effective in returning the resolved hydrocarbons. In the unresolved portions of chromatograms, it was not possible to differentiate between recently added hydrocarbons and those from long-term inputs. This differentiation may be important for determining the extent of contamination from oil spills where extensive areas are impacted and control or prespill sediment samples (to determine background hydrocarbon levels) are not available. 

Librando, V., Hutzinger, O., Tringali, G., and Aresta, M., Supercritical fluid extraction of polycyclic aromatic hydrocarbons from marine sediments and soil samples, Chemosphere, 54,1189-1197,2004. 

A microwave-assisted solvent extraction (MASE) method was optimized by Chee et al. to extract phthalate esters from marine sediments, soils, and results were compared with those obtained by the same authors using conventional Soxhlet and sonication techniques. The analysis was performed by GC-ECD or GC-MS. The overall optimal conditions for the extraction of phthalate esters by MASE included the use of 1 1 acetone or hexane at 115°C for 10 min. Recoveries for six individual phthalate esters (DMP, DEP, DAP, DBP, BBP, DEHP) ranged from 71% to 91%, and were better than those obtained with Soxhlet (66% to 90%) or sonication (65% to 89%). The authors stated that advantages of MASE extraction over sonication or Soxhlet are larger sample throughput, lower usage of hazardous solvents, and less laborious cleanup steps. 

Fig. 3.13 Application of a high-momentum gravity corer (Meischner and Rumohr 1974) to obtain samples from marine sediments. The device can also be stationed on smaller vessels and is suited to extract almost unperturbed cores measuring 1 m in length to be applied in pore water analysis.

Fig. 3.18 Extraction of pore water from marine sediments with rhizons. (A) Basic construction of a rhizon including three different techniques to apply a vacuum. (B) Insertion into an opened core section. (C) Insertion into a multicorer core. (D) Application in the intertidal flat region, from the sediment surface (from Seeberg-Elverfeldt...

De Lange, G.J., Cranston, R.E., Hydes, D.H. and Boust, D., 1992. Extraction of pore water from marine sediments A review of possible artifacts with pertinent examples from the North Atlantic. Marine Geology, 109 53-76. 

Bulleid, N.C., 1978. An improved method for the extraction of ATP from marine sediment and seawater. Limnol. Oceanogr., 23 174—178. 

Hgure 2 Percentage metal extracted, relative to the total concentration, from marine sediments by different reagents, enzymes, and the gut fluid from cod. HCI = 1 mol I HCI HOAc=25% glacial acetic acid NaOH =0.1 mol I NaOH Pepsin = Pepsin A pH 2 Trypsin = Trypsin ll-S pH 7.6 Gut fluid (1) = natural filtered intestinal fluid, pH 7 Gut fluid (2) = natural filtered intestinal fluid, pH 2. (A) Cu and (B) Zn. (Adapted from Turner A and Olsen YS (2000) Chemical versus enzymatic digestion of contaminated estuarine sediment Relative importance of iron and manganese oxides in controlling trace metal bioavailability. Estuarine, Coastal and Shelf Science 51 717-728.)... 

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