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PubMed2001

Transformation of dissolved organic matter during ozonation: effects on trihalomethane formation potential.

Transformation of dissolved organic matter (DOM) during ozonation results in a higher reduction in trihalomethane formation potential (THMFP) relative to dissolved organic carbon (DOC). This study was conducted to determine the effect of DOM transformation after ozonation on THM formation and to elucidate the difference in THMFP and DOC removal. Changes in DOC, THMFP, reactivities of the hydrophilic and hydrophobic DOC, and phenolic-OH were determined to explain the difference in THMFP and DOC removal after ozonation. Higher reduction in THMFP (24-46%) relative to DOC (10-16%) was obtained and was attributed to the following: transformation of DOM from a more reactive hydrophobic DOC (microg THM produced per mg organic carbon) to a less reactive hydrophilic DOC and to the decrease in the reactivities of both the hydrophobic and hydrophilic DOC after ozonation. The results also showed decrease in phenolic-OH indicating the oxidation of some reactive sites like resorcinol or meta-dihydroxy benzene ring structures, which are prone to chlorine substitution, consequently decreasing the reactivity of the organic carbon to form THM. These changes in DOM led to a significant decrease in THMFP with no remarkable removal in DOC.

Disinfection↗

PubMed2002

Investigations on the binding mechanism of the herbicide simazine to dissolved organic matter in leachates of compost.

14C-labelled simazine was composted together with biowaste on a pilot (m3) scale. The herbicide was quickly bound to the compost matrix. By aqueous extraction of 29 and 200 days old compost (equivalent to thermophilic and mesophilic phase of composting) only 4.2% and 3.1% respectively of the radioactivity in the compost samples could be extracted with water. Analysis of the extracts using high-performance size exclusion chromatography (HPSEC) revealed that the dissolved organic matter (DOM) had molecular weights ranging between 2 and 28 kDa. The amount of DOM-associated radioactivity increased from 53% (day 29) to 65% (day 200) of total extractable radioactivity. The type of binding of the 14C-labelled residues and the DOM was elucidated by silylation of humic matter and subsequent HPSEC. The data demonstrated that besides polar metabolites also intact simazine was bound to the DOM. A distinct shift from rather weak interactions to strong covalent linkages of simazine and its metabolites with increasing age of the compost was observed. The results showed that only low amounts of free simazine and its degradates can be extracted with water. We concluded that the shift towards stable covalent linkages is equivalent to a detoxification of the contaminant in aged compost. Consequently, the use of the analysed compost in its mature stage should not pose an environmental risk to the groundwater or the subsoil.

Carbon Radioisotopes↗

PubMed1999

An experimental design to probe the interactions of dissolved organic matter and xenobiotics: bioavailability of pyrene and 2,2',5,5'-tetrachlorobiphenyl to Daphnia magna.

Experiments were conducted to probe the interactions between natural dissolved organic matter (DOM) and two xenobiotics, and to determine how DOM influences their bioavailability. The experimental set-up, using dialysis bags, was designed to expose test organisms to the same constant concentration of free dissolved chemical, while increasing the concentration of the bound-to-DOM fraction. Daphnia magna S. were exposed to pyrene or 2,2',5,5'-tetrachlorobiphenyl in the presence of 0, 1, 2, 5, 10 or 20 mg L(-1) of a reference riverine humic acid (Suwannee River Humic Acid). The physico-chemical parameters were well constrained in the microcosm, demonstrating its potential usefulness. However bioaccumulation by D. magna showed important variability between replicate treatments, sufficient to mask any trends as a function of DOM concentration. The organic-carbon-normalised partition coefficients (K(OC)) ranged from 52000 to 92000 L kg(-1) for pyrene and from 8200 to 89000 L kg(-1) for 2,2',5,5'-tetrachlorobiphenyl, with a marked "concentration effect" for the latter compound.

Animals↗

PubMed2002

The importance of organic matter distribution and extract soil:solution ratio on the desorption of heavy metals from soils.

The lability (mobility and bioavailability) of metals varies significantly with soil properties for similar total soil metal concentrations. We studied desorption of Cu, Ni and Zn, from 15 diverse, unamended soils. These studies included evaluation of the effects of soil:solution extraction ratio and the roles of soil properties on metal desorption. Dcsorption was examined for each metal by computing distribution coefficients (Kd) for each metal in each soil where Kd = [M]soil/[M]solution, Results from soil:solution ratio studies demonstrated that Kd values for the metals tended to increase with increasing soil:solution ratio. This result also held true for distribution of soil organic matter (SOM). Because the soil:solution ratio has a significant effect on measured metal distributions, we selected a high soil:solution ratio to more closely approach natural soil conditions. Copper showed strong affinity to operationally defined dissolved organic matter (DOM). In this study, DOM was operationally defined based on the total organic carbon (TOC) content in 0.45-microm or 0.22-microm filtrates of the extracts. The Kd of Cu correlated linearly (r2 = 0.91) with the Kd of organic matter (Kd-om) where the Kd-om is equal to SOM as measured by Walkley-Black wet combustion and converted to total carbon (TC) by a factor of 0.59. These values representing solid phase TC were then divided by soluble organic carbon as measured by TOC analysis (DOM). The conversion factor of 0.59 was employed in order to construct Kd-om values based on solid phase carbon and solution phase carbon. SOM plays a significant role in the fate of Cu in soil systems. Soil-solution distribution of Ni and Zn, as well as the activity of free Cu2+, were closely related to SOM, but not to DOM. Kd values for Ni, Zn and free Cu2+ in a particular soil were divided by the SOM content in the same soil. This normalization of the Kd values for Ni, Zn, and free Cu2+ to the SOM content resulted in significant improvements in the linear relationships between non-normalized Kd values and soil pH. The semi-empirical normalized regression equations can be used to predict the solubility of Ni and Zn and the activity of free Cu2+ as a function of pH.

Absorption↗

PubMed2002

Dissolved organic matter, aluminium and iron interactions: precipitation induced by metal/carbon ratio, pH and competition.

To better understand the precipitation behaviour of dissolved organic matter induced by interactions with metals, a systematic titration experiment was conducted mimicking the soil solution conditions in an acidic, sandy soil. The variables of interest included the type of metal species (Al, Fe), the redox state [Fe(II), Fe(III)], the pH (3.5, 4.0, 4.5), the metal to organic carbon (M/C) ratio and the competition between Al and Fe. Precipitation of DOM-Al appeared to be strongly correlated with M/C ratio and the pH. For Fe(II) only little precipitation occurred, while the strongest flocculation degree was found after addition of Fe(III). In contrast to Al, hardly any correlation between DOM-Fe precipitation and pH was observed. Both reduction and oxidation of Fe was found and exhibited a strong effect on the precipitated amounts of DOM and Fe. In competition, Al determined the precipitation behaviour at lower M/C ratios (<0.10), while at higher M/C ratios Fe determined the flocculation. Below a M/C ratio of 0.06 Al was the dominant metal in the precipitates, especially at lower pH levels, while the opposite trend was found at M/C ratios above 0.06. Overall, Fe(III) gave the strongest flocculation, although Al influenced the impact of Fe(III) interactions with DOM in relation to pH and M/C ratio.

Journal Article↗

PubMed2004

Soil mobility of sewage sludge-derived dissolved organic matter, copper, nickel and zinc.

A soil (sandy loam) column leaching study aimed to determine the extent of mobility and co-mobility of Cu, Ni, Zn and dissolved organic matter (DOM) released from a surface-application (equivalent to 50 t ds ha(-1) of anaerobically-digested sewage sludge. Leaching of DOM through the soil column was found to be almost un-retarded. Decidedly similar behaviour was exhibited by Ni suggesting that it migrated as organic complexes. Whilst Cu was also found to be leached, significant retardation was evident. However, the importance of DOM in promoting the mobility of both Cu and Ni was evidenced by their lack of mobility when added to the soil column as inorganic forms. The presence of DOM did not prevent Zn from becoming completely adsorbed by the soil solid phase. In relation to WHO drinking water guidelines, only Ni concentrations showed potential environmental significance, due to the relatively poor retention of Ni by the sludge solid phase.

Adsorption↗

PubMed2003

Effects of local pressure and vibration on muscle pain from eccentric exercise and hypertonic saline.

In human subjects the triceps surae of one leg was exercised eccentrically by asking subjects to walk backwards on an inclined treadmill. Before the exercise controlled local pressure, applied to the muscle with an electromagnet, produced mild soreness, which was reduced when the pressure was combined with vibration. When delayed-onset muscle soreness (DOMS) had set in, 24-48 h after the exercise, vibration increased pain from local pressure. Vibrating at different frequencies suggested 80 Hz as the optimal frequency. During 2-h testing post-exercise, evidence of a change in character of the effects of vibration was first detected at 6 h. It persisted up to 72 h post-exercise. When muscle pain was generated in an unexercised triceps by injection of hypertonic (5%) saline, controlled local pressure applied to the sore area increased pain levels by 32% while pressure plus vibration reduced this to 11%. In a subject with DOMS, local pressure again increased pain from saline by 32% but combining it with vibration increased pain further by an additional 20%. The effect of vibration on DOMS could be abolished with a large nerve fibre block applied to the sciatic nerve. It is concluded that the vibration effects are the result of stimulation of large-diameter mechanoreceptive afferents in the muscle which, it is speculated, play a role in generating DOMS.

Analysis of Variance↗

PubMed2002

Immobilizing humic acid in a sol-gel matrix: a new tool to study humic-contaminants sorption interactions.

Humic substances originated from aquatic, soil, or sediment environments are mixtures of humic compounds with various characteristics. Sorption interactions with isolated, well defined humic fractions can be studied either in an aqueous phase ("dissolved humic substances"), or in a solid-phase, by coating mineral particles with the humic materials, or simply by working with humic acid particles (powder) at low pH to minimize dissolution. Each attitude, by definition, can be studied by different experimental techniques and has a different meaning for understanding natural environmental processes. In this study, a new tool for studying sorption interactions is presented. Sol-gel was used as an inert matrix to immobilize (entrap) various humic acids (HAs), and then used to study the interactions of several polycyclic aromatic hydrocarbons (PAHs) with the entrapped HA. Linear and nonlinear sorption coefficients were highly correlated with contaminant hydrophobicity. Sorption of pyrene to immobilized HA was in the order of soil HA > Aldrich HA approximately = peat HA. It was concluded that the entrapped HAs retained their original properties in the gel matrix and were accessible to the external contaminant through the pore network. Additionally, binding coefficients of pyreneto dissolved humic substances and to dissolved organic matter (DOM) were determined from the reduction in pyrene sorption to immobilized HA in the presence of dissolved humic material or DOM in solution. Binding coefficients of pyrene were in the order of the following: dissolved Aldrich HA > dissolved peat fulvic acid (FA) > DOM derived from mature compost > DOM derived from fresh compost.

Adsorption↗

PubMed2002

Reactions of hydroxyl radical with humic substances: bleaching, mineralization, and production of bioavailable carbon substrates.

In this study, we examine the role of the hydroxyl (OH*) radical as a mechanism for the photodecomposition of chromophoric dissolved organic matter (CDOM) in sunlit surface waters. Using gamma-radiolysis of water, OH* was generated in solutions of standard humic substances in quantities comparable to those produced on time scales of days in sunlit surface waters. The second-order rate coefficients of OH* reaction with Suwannee River fulvic (SRFA; 2.7 x 10(4) s(-1) (mg of C/L)(-1)) and humic acids (SRHA; 1.9 x 10(4) s(-1) (mg of C/L)(-1)) are comparable to those observed for DOM in natural water samples and DOM isolates from other sources but decrease slightly with increasing OH* doses. OH* reactions with humic substances produced dissolved inorganic carbon (DIC) with a high efficiency of approximately 0.3 mol of CO2/mol of OH*. This efficiency stayed approximately constant from early phases of oxidation until complete mineralization of the DOM. Production rates of low molecular weight (LMW) acids including acetic, formic, malonic, and oxalic acids by reaction of SRFA and SRHA with OH* were measured using HPLC. Ratios of production rates of these acids to rates of DIC production for SRHA and for SRFA were similar to those observed upon photolysis of natural water samples. Bioassays indicated that OH* reactions with humic substances do not result in measurable formation of bioavailable carbon substrates other than the LMW acids. Bleaching of humic chromophores by OH* was relatively slow. Our results indicate that OH* reactions with humic substances are not likely to contribute significantly to observed rates of DOM photomineralization and LMW acid production in sunlit waters. They are also not likely to be a significant mechanism of photobleaching except in waters with very high OH* photoformation rates.

Biological Availability↗

PubMed2002

Mercury(II) sorption to two Florida Everglades peats: evidence for strong and weak binding and competition by dissolved organic matter released from the peat.

The binding of mercury(II) to two peats from Florida Everglades sites with different rates of mercury methylation was measured at pH 6.0 and 0.01 M ionic strength. The mercury(II) sorption isotherms, measured over a total mercury(II) range of 10(-7.4) to 10(-3.7) M, showed the competition for mercury(II) between the peat and dissolved organic matter released from the peat and the existence of strong and weak binding sites for mercury(II). Binding was portrayed by a model accounting for strong and weak sites on both the peat and the released DOM. The conditional binding constants (for which the ligand concentration was set as the concentration of reduced sulfur in the organic matter as measured by X-ray absorption near-edge structure spectroscopy) determined for the strong sites on the two peats were similar (Kpeat,s = 10(21.8 +/- 0.1) and 10(22.0 +/- 0.1) M-1), but less than those determined for the DOM strong sites (Kdom,s = 10(22.8 +/- 0.1) and 10(23.2 +/- 0.1) M-1), resulting in mercury(II) binding by the DOM at low mercury(II) concentrations. The magnitude of the strong site binding constant is indicative of mercury(II) interaction with organic thiol functional groups. The conditional binding constants determined for the weak peat sites (Kpeat,w = 10(11.5 +/- 0.1) and 10(11.8 +/- 0.1) M-1) and weak DOM sites (Kdom,w = 10(8.7 +/- 3.0) and 10(7.3 +/- 4.5) M-1) were indicative of mercury(II) interaction with carboxyl and phenol functional groups.

Adsorption↗

PubMed2002

Fouling of microfiltration and ultrafiltration membranes by natural waters.

Membrane filtration (microfiltration and ultrafiltration) has become an accepted process for drinking water treatment, but membrane fouling remains a significant problem. The objective of this study was to systematically investigate the mechanisms and components in natural waters that contribute to fouling. Natural waters from five sources were filtered in a benchtop filtration system. A sequential filtration process was used in most experiments. The first filtration steps removed specific components from the water, and the latter filtration steps investigated membrane fouling by the remaining components. Particulate matter (larger than 0.45 microm) was relatively unimportant in fouling as compared to dissolved matter. Very small colloids, ranging from about 3-20 nm in diameter, appeared to be important membrane foulants based on this experimental protocol. The colloidal foulants included both inorganic and organic matter, but the greatest fraction of material was organic. When the colloidal fraction of material was removed, the remaining dissolved organic matter (DOM), which was smaller than about 3 nm and included about 85-90% of the total DOM, caused very little fouling. Thus, although other studies have identified DOM as a major foulant during filtration of natural waters, this work shows that a small fraction of DOM may be responsible for fouling. Adsorption was demonstrated to be an important mechanism for fouling by colloids.

Adsorption↗

PubMed2003

Photoformation of low-molecular-weight organic acids from brown water dissolved organic matter.

This work describes the effects of simulated solar UV light on the bulk properties of dissolved organic matter (DOM) of bog lake water and on the formation of low-molecular-weight organic acids (LMWOAs). By means of size-exclusion chromatography it was shown that the more hydrophilic moieties of the DOM were preferentially photodegraded while the more hydrophobic ones remained relatively unaffected or were even formed. The combined photochemical-biological degradation proved to be more important than the pure photochemical mineralization. Formic, acetic, pyruvic, oxalic, malonic, and succinic acids were identified as important degradation products. Their contribution to the dissolved organic carbon increased from 0.31% before to 6.4% after 24 h irradiation. About 33% of the bioavailable photoproducts of DOM were comprised of these LMWOAs. The influence of nitrate on the formation of carboxylic acids could not be observed in the investigated system. Kinetic experiments indicated that degradation of LMWOAs occurred simultaneously during irradiation experiments, alpha-oxygen-substituted LMWOAs being more amenable to these processes. Dissolved iron acted as a catalyst of DOM photodegradation and LMWOA photoformation. Copper played an antagonistic role in the irradiation experiments, reducing the formation of formic, acetic, and malonic acids while increasing the formation of oxalic acid.

Acetic Acid↗

PubMed2004

Physical and kinetic speciation of copper and zinc in three geochemically contrasting marine estuaries.

The physical and kinetic speciation of Cu and Zn in three impacted marine estuaries was examined. Contrasts in sources of metal-binding ligands, solution chemistry, and hydrologic forcing between and withinthethree study systems (Cape Fear River Estuary, North Carolina; Norfolk-Hampton Roads-Elizabeth River, Virginia; San Diego Bay, California) were exploited to enhance our understanding of Cu and Zn speciation. Trace metal-optimized tangential-flow ultrafiltration at 1 kDa nominal molecular weight limit (NMWL) was used to fractionate <0.4 microm species into colloidal and "dissolved" pools. Colloidal species of dissolved organic matter (DOM) and copper were significant and often the dominant pools in each of the three study systems. Characteristic colloidal fractions of both DOM and Cu ranged from near 70% of <0.4 microm concentrations in Cape Fear to 50% in San Diego Bay. Colloidal Cu and DOM were strongly coupled, and variability in observed <0.4 microm Cu concentrations was closely related to the concentrations of colloidal-associated metal. Colloidal fractions were much smaller for Zn than that of Cu; ranging from 10-30% in Cape Fear to less than 5% in San Diego Bay, and no relationship to DOM was observed. Kinetic separations on Chelex resin revealed the presence of large nonlabile pools of Cu in each of the study systems, with the highest fractions (70-100%) in Cape Fear and Norfolk and lowest (30-50%) in San Diego Bay. A close relationship was observed between colloidal and nonlabile Cu species, implying slow reactivity of colloidal-bound Cu. The fraction of filterable Zn labile to Chelex averaged 97%, 85%, and 60% in San Diego, Norfolk, and Cape Fear, respectively. Anthropogenic Zn appeared almost exclusively in the <1 kDa fraction, while anthropogenic Cu was distributed between dissolved and colloidal pools. Copper particle-partition coefficients (Kd) followed the trend: San Diego >> Norfolk > Cape Fear and were inversely correlated with DOC concentrations. Colloid-based partition coefficients were significantly greater, in many cases an order of magnitude greater, than particle-based partition coefficients. The partitioning data suggest the presence of metal-enriched bacterial-derived exudates and/or discrete metal phases in colloidal-sized particles in impacted regions of these estuaries. The strong relationships observed between Cu and DOC indicate that Cu partitioning behavior over a range of estuarine environments may be modeled effectively with a limited set of coefficients. Our measurements of metal lability and size distribution imply that the fraction of <0.4 microm Zn that is likely to be bioavailable is greater than that for Cu, especially in impacted regions of the study systems.

California↗

PubMed2003

Leaching potential of persistent soil fumigant residues.

Persistent fumigant residues in soil resulting from agricultural pest-control practices may be released into water and leached to groundwater. In this study, the leaching potential of persistent soil fumigant residues was evaluated, and the effect of dissolved organic matter (DOM) and ammonium thiosulfate (ATS) amendment was investigated. A silt loam soil was incubated separately with the fumigants 1,3-dichloropropene (1,3-D), chloropicrin (CP), and methyl isothiocyanate (MITC) at 240-990 mg kg(-1) for 35 d, followed by 48 h of evaporation. The soil was packed into stainless steel columns (1.4 cm x 10 cm) and leached with water, 5 mM ATS, and DOM solution (DOC 250 mg L(-1)) by gravity. Residues of 1,3-D, CP, and MITC in the evaporated soil were 5.61, 11.38, and 1.83 mg kg(-1), respectively. Concentrations of 1,3-D, CP, and MITC in column effluents ranged from 0.05 to 0.73, 0.16 to 0.81, and 0.05 to 0.27 mg L(-1), respectively, when the soil was leached with 10 pore volumes of water. DOM did not promote the leaching of persistent fumigant residues, and ATS remarkably reduced the amount of 1,3-D and CP yet notably increased MITC recovered in the effluents. The results suggest that the leaching of persistent fumigant residues through soil to water is significant, and movement of fumigants in soil is not facilitated by DOM. Amending soil with ATS through irrigation is an effective method to remove persistent residues of halogenated fumigants. To reduce groundwater pollution risks posed by fumigation, persistent soil fumigant residues have to be considered.

Allyl Compounds↗

PubMed2003

Evaluation of Kd underestimation using solid phase microextraction.

Many important environmental pollutants are strongly adsorbing hydrophobic compounds. Because of their potential to adsorb to dissolved organic matter (DOM), their partition coefficient Kd may be underestimated by the conventional approach due to incomplete phase separation. In this study, solid-phase microextraction (SPME) was compared with liquid-liquid partition (LLP) for measuring Kd of bifenthrin and permethrin isomers on sediments. Due to its selective detection of the freely dissolved concentration, SPME gave Kd values 0.6-4.4-fold greater than those obtained by LLP in creek and field sediments and 3.6-21.7-fold greater in nursery runoff sediments. Underestimation by the conventional method was attributed to adsorption to DOM that was not excluded from the aqueous phase by centrifugation. The degree of underestimation was dependent on the source and amount of DOM and may be generally significant for compounds that have DOM adsorption coefficient (KDOM) > 10(4). This study provides evidence that the existing Kd values for many hydrophobic pollutants may be underestimated, and SPME may be a viable, efficacious tool for evaluating the underestimation.

Adsorption↗

PubMed2004

Preliminary study of lake dissolved organic matter in light of nanoscale supramolecular assembly.

Large-scale preparative high-performance size-exclusion chromatography (HPSEC) was performed to separate different molecular size fractions in milligram quantities from strongly colored dissolved organic matter (DOM) of a freshwater using a very mild conjugate acid-base pair (10 mM acetic acid-sodium acetate solution at pH 7.0 with an ionic strength of 6 x 10(-5)) as the mobile phase. The homogeneity-uniformity of different molecular size fractions in relation to their combined original mixture was verified by an analytical HPSEC system. In addition to molecular size distribution and basic spectroscopic characteristics, Fourier transform infrared spectroscopy was applied to specify structural features for different size fractions. The results demonstrate clearly that only a very small amount of conjugate organic acid-base pair is required to generate a powerful resolution for a DOM mixture, and very strong treatments with organic acids are not necessarily needed to reach a better SEC resolution. Most essential is the combined outcome of different HPSEC experiments and determined structural functionalities which indicate that almost all original DOM solutes are aggregated mixtures consisting of different associations possessing various molecular size ranges, which can be separated from their integrated whole as nearly homogeneous and uniform species. In summary, the present study strongly speaks for the need to direct the research of natural dissolved and colloidal organic carbon more strongly toward a nanoscale study of supramolecular assemblies. More precise knowledge about the primary, secondary, and tertiary structure of dissolved DOM constituents has its essential function, e.g., for environmental protection and utilization of surface waters.

Chromatography, High Pressure Liquid↗

PubMed2005

Molecular characterization of biodegradable dissolved organic matter using bioreactors and [12C/13C] tetramethylammonium hydroxide thermochemolysis GC-MS.

Little is known about the molecular composition of the biodegradable fraction of dissolved organic matter (BDOM) in stream ecosystems. We combined plug-flow biofilm reactors, tetramethylammonium hydroxide (TMAH) thermochemolysis GC-MS, and 13C-labeled TMAH thermochemolysis GC-MS to study the molecular composition of BDOM from two stream ecosystems. TMAH products derived from fatty acids, lignin, and other aromatic molecules were quantified using an internal standard approach. We applied the 13C-TMAH thermochemolysis procedure to differentiate between compounds in dissolved organic matter (DOM) that had natural methoxyl groups from those that acquired methoxyl groups during the TMAH reaction. In Rio Tempisquito, a stream draining a tropical evergreen forest, and White Clay Creek, a stream draining a temperate deciduous woodlands, carbohydrates, fatty acids, and lignin contributed to the DOM and BDOM molecular composition. We observed 97 different peaks in the chromatograms of streamwater, with 57% of the peaks common to both streams. The DOM and BDOM pools from each site also contained a unique suite of compounds. Our combined use of TMAH and 13C-TMAH thermochemolysis revealed that heterotrophic bacteria can selectively degrade and demethylate different types of compounds in the lignin residues of DOM. This demonstration of bacterial demethylation of lignin, an abundant and refractory plant molecule, has potential implications for global carbon cycling.

Biodegradation, Environmental↗

PubMed2005

NMR spectroscopy study of freshwater humic material in light of supramolecular assembly.

The structural similarity-dissimilarity of several humic-type derivatives, separated from a strongly colored freshwater sample by different sorbing solid techniques, tangential-flow ultrafiltration (UF), and large-scale preparative high-performance size-exclusion chromatography (HPSEC), were in detail studied with one-dimensional liquid 1H and solid-state 13C nuclear magnetic resonance (NMR) spectroscopy, especially in light of the native humic-type dissolved organic matter (DOM-HM). The results support the applicability of functional cross-linked poly(vinylpyrrolidone) (PVP) or diethylaminoethyl-cellulose (DEAE) sorbents in concentrating representative integrated wholes of aquatic humic-type material along with a conventional nonionic XAD-8/DAX-8 (polymethyl methacrylates) technique. Apart from the fact that the acidification of the original humic water before a separation procedure seems not to be so destructive to the original structural composition of the DOM-HM as expected, the refinement of aquatic humic solutes, independent of the selected sorbing solid technique, will cause structural changes in the separated humic complexes in comparison with the situation predominating in the original starting material. Tangential-flow ultrafiltration (UF) proved an overpowering reliability to concentrate the aquatic DOM-HM. Most fundamental is the combined outcome of different HPSEC experiments and determined structural functionalities which indicate that almost all original DOM-HM solutes are aggregated mixtures consisting of structurally similar associations possessing various molecular size ranges, which can be separated from their integrated whole as nearly homogeneous and uniform species. This finding permits a reasonable starting point to go on working with more advanced multidimensional NMR techniques in resolving the uncertainty about supramolecular assembly of dissolved humic material. The tested conformity between the obtained molecular NMR descriptors and the corresponding previously collected FT-IR parameters was acceptable thus speaking for the fact that the less sensitive FT-IR spectroscopy can also provide valuable information on the structural and functional properties of heterogeneous humic-type mixtures.

Fresh Water↗