The isolation of some polynuclear aromatic hydrocarbons from aqueous samples by means of reversed-phase concentrator columns

The results for some polynuclear aromatic hydrocarbons (PAH) in canal water and rain water differ depending on whether the PAH are concentrated directly on Sep- Pak C-18 cartridges or concentrated after filtration with further analysis of the particulate matter. For canal waters, higher total PAH concentrations are obtained when the suspended material is also analyzed.     

喷气燃料中悬浮物的分离和分析

通过过滤分离出喷气燃料中的悬浮物,并用正己烷和二氯甲烷提取,利用扫描电镜、X射线能潜仪、X射线衍射仪、红外光谱仪和气相色谱-质谱仪分析悬浮物的组成;得出喷气燃料的悬浮物中同时含有烃类物质．极性成分和小粒径颗粒物。实验结果为进一步研究喷气燃料中的悬浮物来源和机理奠定了基础。     

Charakterisierung des organischen Anteils von Schwebstoffen aus Flu?wasserproben durch Elementaranalyse mit einem automatischen CHN-Analysator

Zusammenfassung Es wird über eine Methode berichtet, die unter Einsatz eines automatischen CHN-Analysators die Bestimmung der Menge und Elementzusammensetzung des organischen Anteils in Schwebstoffen aus Wasserproben ermöglicht. Die zur Analyse erforderliche Anreicherung der Schwebstoffe erfolgt mittels Filtration durch binderfreie Glasfaserfilter. Bekannte Flächenanteile der belegten Filter werden unmittelbar zur Analyse eingesetzt.

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Characterization of the organic constituents of suspended matter from river water samples by means of elemental analysis using an automatic CHN-analyzer

Summary A method is presented which permits screening of the amount and composition of the organic constituents in suspended matter from water samples by means of an automatic CHN analyzer. The enrichment of sediment required for analysis is accomplished by filtration through binder-free glass-fibre filter paper. Known square aliquots of the loaded filters are directly subjected to analysis.

     

Phthalates in surface water — a method for routine trace level analysis

Summary A routine method for the determination of phthalates in water is presented. It is suitable for all kinds of water like surface water, waste water, landfill leachate, rain water and ground water. Unfiltered water samples including all suspended particulate matter are extracted by solid-phase extraction in an all-glass apparatus using RPC-18. The extracts are measured by GC/MSD in the SIM mode. Due to an easy but efficient decontamination technique, method blanks could be decreased below 0.02 g/l for all phthalates. The detection limits are 0.01 to 0.02 g/l, the determination limits are 0.02 to 0.05 g/l. Recovery for all phthalates is about 98% (±5%). Phthalates were measured in about 400 samples of water of the river Rhine and its main affluents in Northrhine-Westfalia.     

Radium isotopes in suspended matter in an estuarine system in the southwest of Spain

The presence of²²⁶Ra and²²⁴Ra in suspended matter from an estuarine system which surrounds a phosphate fertilizer complex has been investigated. The results have confirmed an important radioactive impact from the industrial complex, since up to 2.5 Bq²²⁶Ra/g suspended matter (dry) has been measured. The influence of tides and seasonal conditions, through changes in salinity, has been found to be relevant. The distribution coefficients for²²⁶Ra between the suspended matter and the river water have been calculated. The values are in agreement by order of magnitude with those found in the literature, but they clearly depend on tidal state and seasonal conditions.     

Titanium in natural surface waters: The content and coexisting forms

Results obtained in studying the content and coexisting forms of titanium in surface waters are given. It was established that the titanium concentration lies within 0.0–1180 μg/L in the world’s surface water and within 0.0–573 μg/L in the studied water bodies of Ukraine. The concentration of dissolved and suspended titanium in the water bodies studied also varies within the wide range, 0.0–86.0 and 0.0–534.6 μg/L, respectively. The concentration of its dissolved form in world’s surface water is 0.0–68.7 μg/L. The ratio of dissolved to suspended titanium in water bodies depends on the content of suspended matter and its nature. In river waters, the suspended titanium mostly dominates over the dissolved form. We found that in rivers with the high concentration of suspended matter (6.0–140.6 mg/L), mostly of mineral nature, a fraction of the suspended titanium reaches 62.3–88.6% on the average. A strong correlation between the mass of suspended matter and the concentration of suspended titanium in these surface waters shows that the nature of suspended matter affects the concentration of suspended titanium. The correlation coefficient is between 0.81–0.99 at a significance level of 0.01. The titanium content in the suspended matter and bottom sediments of world’s water bodies makes 0.2–19.8 and 0.1–24.6 mg/g of dry weight of the suspended matter, respectively. In the surface waters studied, its content ranges within 0.0–16.5 mg/g of dry weight of the suspended matter. Taking into account the average values, the titanium content in the suspended matter of the studied rivers, water reservoirs, lakes, and ponds is (mg/g in terms of dry mass): 1.0–7.5, 1.0–4.9, 1.3–3.9, and 1.2–1.3, respectively. The percentage of the adsorbed titanium in the suspended matter of the Kilia Danube delta, Kanev Reservoir, and the Lybid’ River is 91.6–97.3, 67.6–74.4, and 57.1–99.4%, respectively. The acidic (anionic), basic (cationic), and neutral fractions of the dissolved organic substances in the surface waters contained 15.7–89.4, 0.0–33.8, and 0.0–80.7% of dissolved titanium (Ti_diss) (i.e., 44.4, 13.2, and 42.4% of Ti_diss on the average). The presence of dissolved titanium in the anionic fraction shows that titanium forms complexes with humic substances or exists in the form of TiO₂ colloidal particles (nanoparticles) coated with humic substances. In the neutral fraction, a hydrated titanium oxide TiO(OH)₂ may exist as a form of its migration in natural surface waters.     

A system for taking a representative sample from a large volume of turbid surface sea water for trace element determinations

The sampler is designed for use in routine monitoring of dissolved and particulate trace metals (Zn, Cd, Pb, Cu, Sb and Bi) in turbid sea water. By continuous horizontal sampling, the 5-l volume of sea water actually collected is representative of a very large volume (3000 1). The system includes pumping and filtration apparatus, suitable for use by unskilled operators, to collect small liquid and particulate samples in a closed system precluding atmospheric contamination. Filtration (0.45-μm filter) under pressure makes it possible to collect 50–100 mg of suspended matter from shallow water within 45 min. Tests under routine working conditions show satisfactory results.     

Sorption–Atomic Absorption Determination of Trace Elements in Natural Waters Using Simultaneous Atomization of a Solid Concentrate and Suspended Matter

A sorption–atomic absorption technique with dynamic preconcentration on DETATA adsorbents in a microcolumn crucible followed by the direct atomization of a solid matrix (concentrate + suspended matter) was used to determine the total dissolved and suspended Cd, Pb, and Tl (El_dis+ El_susp) in natural waters. The detection limits were 1–3 ng/L for Cd and 5–30 ng/L for Pb and Tl. The results of the sorption–filtration atomic absorption determination of the total dissolved and suspended elements can provide extra information for the speciation analysis of waters.     

Association of uranium with colloidal and suspended particulate matter in Arabian sea near the west coast of Maharashtra (India)

The purpose of the present study is the association of natural uranium in seawater with colloidal and suspended-particulate matter was determined. The separation of suspended particulate material (>0.45 µm) and colloidal fraction (as dissolved fractions) in seawater were done by suction and ultra filtration techniques. Seawater samples were collected at 1 km away from the shore and subjected to sequential fractionation in nine stages ranging from 2.7 µm to 1.1 nm. Suspended particulate matter were separated in three different size groups namely >2.7 µm, <2.7–>0.45 µm and <0.45–>0.22 µm by suction filtration using cellulose acetate and nitrate membranes filters. To concentrate the solution with colloidal particles <0.22 µm–1.1 nm (0.5 k Nominal Molecular Weight cut-off Limit {NMWL}), the solution obtained from filtration through <0.22 µm was passed through stirred ultra-filtration cell. The pH and conductivity at different stages of fractionation (dissolved) showed minor variations. The concentration of uranium was measured in suspended and dissolved fractions by using a pulsed nitrogen laser at 337.1 nm. In order to evaluate the role of mineral colloids in various stages of filtration, concentration of calcium, magnesium, potassium were measured by using ion chromatography and atomic absorption spectrometry. The clay mineral at seawater pH (approximately 8) behave as negative ions and provides binding site for the positively charge species of uranium. Among the dissolved fraction, the maximum concentrations of colloidal uranium was observed about 4 times higher than that compared to average concentration of 6.93±3.10 ppb in other fractions. In the case of suspended particulate matter, the concentration of uranium was below detection limits (<1 ppb). The maximum concentration of Ca, Mg and K in the dissolved fraction were in the <1.1 nm fraction, while for suspended particulate matter, the concentration of Ca, Mg and K decreased with the decrease in size and it is highest in the fraction of 0.22 –0.45 µm.This revised version was published online in November 2005 with corrections to the Cover Date.     

Separation and determination of dissolved and particulate humic substances in river water

Distribution of humic and fulvic acids in participate or dissolved form is studied by using simple leaching and sorption techniques. After filtration of water sample (100–200 ml), the filter along with suspended particles is treated with 5 ml of chloroform and 3 ml of 0.1 mol/l sodium hydroxide solution. The filter dissolves completely in the organic phase, while the suspended particles remain in the aqueous phase enabling a leaching of humic substances. The leaching is repeated once more with 2 ml of 0.1 mol/l sodium hydroxide solution. The humic and fulvic acids in the combined solution are fractionated at pH l by filtration, where the membrane filter is preliminarily coated with sodium dodecyl sulfate. On the other hand, dissolved humic substances are concentrated from a 50-ml filtered sample by sorption on a DEAE-cellulose column. They are desorbed with 5 ml of 0.1 mol/l sodium hydroxide solution and fractionated at pH 1. The spectrophotometric analysis of river water reveals that fulvic acid is predominant in suspended particles as well as in filtered samples. The concentration of dissolved humic and fulvic acids is approximately ten times that of suspended particles.     

Effect of pH, temperature, conductivity and sediment size on thorium and radium activities along Jucar River (Spain)

A study is presented on the distribution of thorium and radium isotopes in sediments, suspended matter and water collected along Jucar river (East of Spain), using low-level α-spectrometry. The first aim of this work is to study the thorium and radium activity in water, sediment and suspended matter and their dependence on pH, temperature, conductivity and sediment sizes along Jucar river. The analysis of activity variation with these parameters will provide information about the dynamics of these radionuclides in rivers. The values obtained for the distribution factors between suspended matter and water (K _d ) are also discussed.     

Surface water preparation procedure for chromatographic determination of polycyclic aromatic hydrocarbons and polychlorinated biphenyls

A new sample preparation procedure for the analysis of polycyclic aromatic hydrocarbons (PAHs) and polychlorinated biphenyls (PCBs) in water containing suspended particulate matter (SPM) has been developed. A specially designed filtration vessel coupled directly to an SPE cartridge was used for this purpose. SPM separation and analyte isolation/concentration were carried out in a single step. Both the SPE cartridge and the suspended matter collected on the filter were solvent extracted, and analyte recoveries were determined. Analyte recoveries from the filtrate ranged from 64 to 100% of the spiked amount for PAHs with the highest aqueous solubilities, and did not exceed 20% for those with the lowest solubilities. Total recoveries of PAHs from surface water containing 21 mg l(-1) SPM ranged from 65 to 121%. PCB recoveries from the particulate matter reached over 10% of the spiked amount, while those from the filtrate ranged from 20 to 57%. Total PCBs recoveries ranged from 34 to 69%.     

Application of Non-Destructive X-Ray Fluorescence Spectrometry to the Analysis of Suspended Matter in Sea Water

Abstract

In the framework of remote sensing studies concerning coastal transport of pollution in the Northern Adriatic Sea, a method has been developed for the quantitative determination of sulphur, iron, titanium, calcium, phosphorus, silicon, aluminium, magnesium in suspended matter of sea water.

The suspended material was collected by filtering on millipore membrane filters with pore width of 0.45 μ and directly analysed by X-ray spectroscopy. For calibration dried solution and particulate standard samples were used. Limits of sensitivity and precision of the method are reported.

Correlations between the concentration of these elements and the total suspended matter/chlorophyll are discussed.

The aim is to study the geochemical composition of particulate matter and its variations within the geographical site of the sea basin and the seasonal conditions. The approach is to consider aluminium and the other elements normalized on Al. On the basis of a matrix correlation analyses of some sets of data chosen in the restricted area for investigation, some hypothesis on superficial distribution of clay, carbonate, iron hydrous oxides and other mineral detrites, are taken into account. The results confirm the complex situation existing in the offshore area of the Venice lagoon from a geochemical point of view.

The suspended matter seem to be argillaceous in the Southern part of the investigated area and semi-argillaceous with hydrous oxides and carbonates in the Northern part which is influenced by the Piave river.     

Comparison of GC/MSD and GC/AED for the determination of organotin compounds in the environment

Summary Methods are described for the analysis of environmental samples like water, sediment and suspended matter for the determination of all organotin compounds (OTs) that are currently used as biocides: tributyltin (TBT), triphenyltin (TPT), tricyclohexyltin (TCT) and fenbutatin oxide (FBTO). In water also five degradation products (di and mono substituted analogs) can be determined. Alkylation using a Grignard reagent was used to obtain OT derivatives amenable to gas chromatography (GC). Both methylation and pentylation have been employed for derivatization prior to GC analysis. The present results show that derivatization efficiencies for TPT, TCT and FBTO at trace levels are higher using methylation than pentylation. Detection limits for each type of sample matrix were determined using GC/Mass Selective Detection (GC/MSD) and GC/Atomic Emission Detection (AED). In sediment and suspended matter only tri-substituted OTs (i.e. the parent compounds) could be determined. Detection limits ranged from 0.2 to 10 ng/g dry weight. FBTO, not previously detected in environmental samples, was found at levels of 4 and 11 ng/g in a suspended matter sample and a sediment sample, respectively. In water the OTs and their degradation products were determined at levels of 1–10 ng/l (as tin) using 200 ml water samples.     

Concentration of elements in suspended matter discharges to Lerma River,Mexico

The S, K, Ca, Ti, V, Cr, Mn, Fe, Cu, Zn and Pb concentration and the elemental composition of particles in suspended matter from principal discharges to Lerma River, have been evaluated. The elemental concentration in suspended matter has been obtained by Energy Dispersive X-Ray Fluorescence Spectrometry. The elemental composition of particles has been obtained by means of Energy Dispersive X-Ray Spectrometry (EDS). The results show that K, Ca, Ti, Mn and Fe are mainly from natural origin in the Upper Course of the Lerma River (UCLR), where the principal contributions probably come from dragging of soils and sediments in the rainy season and Cr, Cu, Zn and Pb are mainly from anthropogenic origin where the principal contributions come from urban and industrial untreated discharge. The application of Energy Dispersive X-Ray Spectrometry plus Scanning Electron Microscopy is useful in the characterization of suspended matter in natural, anthropogenic and mixed water discharges.     

Chemical Analysis and Toxicity Tests of Organic Pollutants in Xi River Water and Suspended Sediment of Shenyang City

Abstract

In 1987, in a 10-day investigation, two kinds of raw water and their suspended sediment samples were successively collected from the upper and middle reaches of the Xi River. The water and the suspended sediment samples were prepared by filtration of the raw water through a 0.45 μm membrane. The pH values of the water samples were adjusted to neutral (pH 6.5), basic (pH 11.0) and acid (pH 2.0) and passed through three adsorption columns filled with GDX macroreticular resin (MRR). The organic pollutants were subsequently eluted from the columns with CH₂Cl₂. Suspended sediment samples were extracted with CH₂Cl₂ by Soxhlet extraction. Organic pollutants were separated on silica gel columns and analyzed by GC and GCMS and assayed for acute toxicity, Ames test response, and micronucleus test response. Over 200 organic pollutants in the river water and the suspended sediments were determined. More than 60 main pollutants were identified according to the results of the chemical analysis and toxicity tests.     

The use of ultrafiltration for the separation and fractionation of organic ligands in fresh waters

The effects of various experimental conditions on the results obtained by using membrane filtration for the separation and fractionation of organic matter in fresh waters (mainly fulvic and humic substances) are described. The technique used (washing or concentration) and the initial concentration of the organic matter to be filtered are the most critical factors. The technique is used for the fractionation of eight water samples, one sample of peat interstitial water, five water extracts of soil and four water samples obtained by decomposition of leaves. The results are compared. A comparison is also made with results cited in the literature.     

火力发电厂废水中悬浮物处理的影响因素探讨

对火力发电厂废水中悬浮物处理的影响因素如pH值、水温、接触介质、进水水质、混凝剂加入量等进行分析，对主要影响因素水温和混凝剂加入量进行了试验分析，制定出废水悬浮物处理的合理方案。     

Concentrations of aluminium, iron, and copper in water of some Shatskiye Lakes and specificity of their distribution among different forms of occurrence

The results of studies on the occurrence of aluminum, iron, and copper in water of Lyutsimir and Chernoe Bol’shoe Lakes belonging to the large group of Shatsk Lake system are discussed. Iron was shown to migrate mostly as suspended particles, and copper, as soluble species. The average annual fraction of suspended aluminum is about 40%. The ratio of suspended and dissolved aluminum depends not only on the concentration of suspended particles in water, but also on their nature. Anionic complexes predominate among soluble forms of the examined metals; their fractions in water of Lyutsimir and Chernoe Bol’shoe Lakes are on the average 86 and 70% (Al), 73 and 59% (Cu), and 60 and 47% (Fe). This is determined by the major contribution of humic substances to the total content of organic matter in water of both lakes and their participation in the complexation with metals. The metals compete for active centers in humic macroligands. Carbohydrates constitute the second important group of organic substances that participate in the complexation. Neutral complexes were found to consist mainly of iron compounds. Compounds with a molecular weight not exceeding 2.0 kDa predominate among anionic metal complexes.     

Influence of land development on heavy metal forms in the Bobrza River ecosystem (Świętokrzyskie Province,Poland)

Metals are perceived as pollutants but they are also natural substances found in the environment. The surface water environment is under the influence of continuing industrial pollution/effluents. Therefore it is necessary to determine various metal forms present in each component of the water ecosystem. The study presents analysis for Cd, Cu, Cr, Fe, Mn, Ni, Zn and Pb content in the Bobrza River bottom deposits and water. The analysis of water and sediment samples from the Bobrza River taken from the littoral zone at three sampling points: the riverhead, i.e. the natural environment; Białogon — the acidic environment; and Sitkówka-Nowiny — the alkaline environment, were analyzed. Sample quality indicators were defined with pH value, conductivity, heavy metal content for water and suspended matter samples. The metal forms in river sediment were also analyzed. The sediment samples were subjected to Tessier’s five-stage sequential extraction procedure assisted by microwave radiation. Analyte concentration in water samples and in the extracts was determined with the use of F-AAS and GF-AAS techniques. The results obtained reveal a relationship between land development, the degree of metal bonding with suspended matter and metal forms found in river sediments.