Determination in Sediment

First method about 2000 mg of sample were treated with HCl and extracted into toluene and cysteine, and back-extracted into toluene (88 5)% recovery assessed by two spikings of a CRM (PACS-1). The extract was dried with anhydrous Na2S04. The separation was by capillary gas chromatography (column of 25 m length, internal diameter of 0.53 mm stationary phase BP-1 (methylsilicone), 1.0 pm film thickness injection of 1 pL temperature of the injector of 200 °C, temperature of the ECD detector of 250 °C, colunm temperature of 90°C N2 as carrier gas at 12 mLmin and makeup gas type at 50.5 mLmin ). Calibration was by calibration graph with MeHgCl in toluene verified with a MeHgCl2 solution. 

Second method about 250 mg sample were treated with HCl and extracted into toluene, repeating the operation twice EtHgCl was added as internal standard the recovery [(96 2)%] was verified by spiking the RM used in the intercomparison. Clean-up was performed by equilibration of the MeHg into 

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A rapid and simple method for PBDE and HBCD determinations in sediment and fish samples was used. The analytical method was based in selective pressurized liquid extraction (SPLE) [21] without further cleanup step and analysis by gas chromatography coupled to mass spectrometry (GC-MS), working with negative ion chemical ionization (NCI) [22, 23],... 

Petroleum pollution monitoring laboratories in the Mediterranean region participated (1984-1986) in two intercalibration exercises (MEDCALI and II) to evaluate the International Oceanographic Commission (IOC) Manual for petroleum hydrocarbon determination in sediment (IOC, Manuals and Guides, No. 11). The main source of error in the analysis was the extraction/ partition step. When the results were corrected for recoveries, relative standard deviations for w-alkancs, UCM (unresolved complex mixture) and total aromatics, which had previously been 60, 56 and 49%, respectively, were reduced to 17, 30 and 6%, respectively. 

Table 12.9 compares results for phosphorus determinations in sediments obtained by methods I and II. 

Table 12.15 Comparison of arsenic determination in sediments by different analytical methods (pg/g dry weight)...

Few data have been published on cationic surfactants in aquatic sediments. Levels from 3 to 67 mg kg-1 were determined in sediment samples from Rapid Creek [54] and 6-69 mg kg-1 concentrations were found in sediment samples from Japan [4]. DTD MAC was reported in digested sewage sludge at levels ranging from 0.15 to 5.87 gkg-1 [22]. Also, cationic surfactants were determined in urban coastal environments and they were reported as markers [18,55]. In our work, concentrations of BAC ranged from 23 to 206 p,gkg 1 in sediment samples from different rivers near to wastewater treatment plants,... 

In summary, neutral hydrolysis rate constants for six different compounds which hydrolyze by four different hydrolysis mechanisms were determined in sediment/water systems using seven... 

E. M. M. Flores, J. N. G. Paniz, A. P. F. Saidelles, E. 1. Muller and A. B. da Costa, Direct cadmium determination in sediment samples by flame atomic absorption spectrometry using multivariate calibration procedures, J. Anal. At. Spectrom., 18, 2003, 769-774. 

PCDD/Fs were determined in sediments from a harbor near a wood-pre-serving plan in Thunder Bay, Lake Superior, 1988. The plant used pentachloro-phenol [49]. TeCDDs and PnCDDs were below detection, 0.02-0.9 ngg 1 dw. Most important PCDD/Fs were OCDD (< 0.4-980ngg x), HpCDDs (< 0.4-320 ngg x), and OCDF (< 1-400 ngg-1). Lesser concentrations of HxDDs, HxCDFs, and HpCDFs were frequently present (< 0.03-36 ngg ). The contamination was highly associated with oil/grease and PAH concentrations, suggesting a common source. There is no indication from Lake Superior sedi-... 

Pu determinations in sediments using on-line tandem Sr-Resin and TEVA-Resin columns in PrepLab system SF-ICP-MS 56... 

Uncontrolled species transformations during analysis form another source of error. For methylmercury determinations in sediments it was demonstrated that errors of up to 80% resulted from the formation of the compound from inorganic mercury during separation and analysis [28, 29], For the study of possible species transformations during analysis multiple isotope dilution could be used as a diagnostic tool for identifying the error and bias inherent in specific methods of storage, sample preparation and measurement [30, 31]. 

P. Quevauviller, M. Astruc, R. Morabito, F. Ariese, L. Ebdon, Collaborative evaluation of methods for tributyltin determinations in sediments and mussel tissue, Trends Anal. Chem., 19 (2000), 180D188. 

J. S. Landaluze, A. de Diego, J. C. Raposo, J. M. Madariaga, Methylmercury determination in sediments and fish tissues from the Nerbioi-Ibaizabal estuary (Basque Country, Spain), Anal. Chim. Acta, 508 (2004), 107-117. 

For mercury determination in sediments or fish tissues, samples were oxidized with boiling nitric acid. After reagent addition the methyl mercury derivate was extracted by benzene. The results of gas-chromatographic determination were higher than those obtained by wet-oxidation and atomic absorption methods . ... 

ORGANOMERCURY DETERMINATIONS IN SEDIMENTS AND SEUDGE WITH HEADSPACE— GAS CHROMATOGRAPHY—MICROWAVE INDUCED... 

Table 5.4 Summary of the various methods used for butyltin determination in sediments [16]... 

Characterisation of the Sample Matrix for Determinations in Sediments (All Types of... 

CHARACTERISATION OF THE SAMPLE MATRIX FOR DETERMINATIONS IN SEDIMENTS (ALL TYPES OF CHEMICAL)... 

Examples of Experimental Conditions for Derivatization Reactions Used in Butyltin Determinations in Sediment... 

Baldi F, Bianchi M and Muntau H (1996) Interlaboratory study to improve the quality control of mcthylmercury determination in sediment. Appl Organomet Chem 10 537-544. 

Fiedler, H. D., R. Rubio, G. Rauret 1. Casals, 1999. Acid volatile sulfide determination in sediment using elemental analyzer with thermal conductivity detector. Talanta 48 403-407. 

While the 15 halogenated POPs and PAHs are best analysed by GC-ECD and GC-MS, many other organic compounds in current use have similar physical properties and can be expected to partition to sediments in aquatic systems although they may be less persistent. The nony 1 phenol ethylate surfactants have been shown to be relatively persistent in sediments. Analysis by HPLC-triple quad MS permitted the ethoxylates and nonyl phenol to be determined simultaneously (Shang et al., 1999). The short and medium chain chlorinated paraffins, which are complex mixtures of C10-C17 chlorinated n-alkanes, have been determined in sediments by GC-high resolution ECNI MS (Tomy et al., 1997, Tomy Stern, 1999) following conventional extraction and cleannp procedures (Fig. 1). 

Butylated Sn compounds have been determined in sediments by exploiting microwave technology to simultaneously extract and derivatize Sn compounds... 

M.J. Marques, A. Salvador, A.E. Morales-Rubio, and M. de la Guardia. Trace element determination in sediments a comparative study between neutron activation analysis (NAA) and inductively coupled plasma-mass spectrometry (ICP-MS). Microchemical Journal 65 177-187, 2000. 

QuevauvUler, Ph., Fortunati, G. U., FillipeUi, M., Baldi, F., Bianchi, M., and Muntau, H. (1996) Interlaboratory study to improve the quality control of methylmercury determination in sediment. Appl Organomet. Chem., 10, 537 14. 

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