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PubMed2005

Stage change in binding of pyrene to selected humic substances under different ionic strengths.

Influence of ionic strength (I) on the pyrene binding constant (Koc) in six different humic substance (HS) solutions, three soil humic acids, one freshwater humic acid, one freshwater fulvic acid, and one freshwater natural organic matter was investigated by fluorescence quenching technique. Specific two-stage changes of Koc with increasing ionic strength were only observed in three soil humic acid solutions with varying to different extents. Two primary governing factors for the differences of these HS systems are binding potential and the abundance of acidic functional groups (carboxyl and phenolic) of HS. Experimental results demonstrated that within the ionic strength range studied in the present research, ionic strength had a major effect on molecular size of HS and brought about change of Koc. The salting-out effect did not. The change in molecular size was caused by the associations between cations and acidic groups of HS. Using pyrene as a probe, we also investigated the interaction of cation and dissolved HS and found relatively slow kinetics (at least 5 d), leading us to believe that the special cation-HS kinetics may influence the results of geochemical studies involving the measurement of ionic strength effect.

Adsorption↗

PubMed2002

Characterization of humic substances present in landfill leachates with different landfill ages and its implications.

Humic and fulvic acids extracted from landfill leachates were characterized using elemental analysis and various spectroscopic methods. Molecular size distribution of the humic substances (HS) was also determined using batch ultrafiltration technique and permeation coefficient model. The element analysis and spectral features obtained from UV/visible, IR, and 1H and 13C NMR showed that the aromatic character in the leachate HS was relatively lower than that of commercial humic acid (Aldrich Co.), and higher in the HS of older landfill leachate. Fluorescence spectra indicated that humic acids had a relatively higher content of condensed aromatic compounds than the fulvic acids obtained from the same sources, and the spectrum of commercial humic acid showed that aromatic compounds may be present in a much more condensed and complex form. Molecular size distribution data revealed that the leachate humic acids contained a higher percentage of smaller molecules of < 10,000 D, compared with that of the commercial humic acid (45 approximately 49% vs. 33%), and molecular size of the leachate HS had a tendency to increase as landfill age increased. These results indicate that the HS from landfill leachates were in an early stage of humification, and the degree of humification increased as the landfilling age increased, which implies important information on various related researches, such as interactions of HA with pollutants in terrestrial environments, and optimization of leachate treatment processes with respect to landfill age.

Benzopyrans↗

PubMed2000

A comparative characterization of dissolved organic matter by means of original aqueous samples and isolated humic substances.

The aim of our study is to test the use of less time-consuming spectroscopic methods applied on original water samples in order to obtain information about DOM composition without any sample preparation. These results were directly compared with results from a conventional isolation and characterization procedure of dissolved humic substances (fulvic acids--FA) isolated from the same water sample. FAs were characterized by UV-, fluorescence-, FTIR spectroscopy and elemental composition. UV absorbance and fluorescence behavior of FAs and original water samples follow the same pattern. A lower UV absorbance and a lower humification index (derived from the synchronous fluorescence spectra) of about 15% is typical for water samples compared to the FAs. We computed linear relationships between properties of the original water sample (UV-, synchronous fluorescence spectra) and the isolated FA (IR absorption, C/N ratio). The application of synchronous fluorescence and UV spectroscopy of aqueous samples has been proved to result in similar information about DOM composition as the characterization of isolated humic substances concerning the content of aromatic structures and the degree of humification.

Adsorption↗

PubMedDate not supplied

In situ speciation studies of copper-humic substances in a contaminated soil during electrokinetic remediation.

Speciation of copper-humic substances (HS) in the electrokinetic remediation (EKR) of a contaminated soil was studied by in situ extended X-ray absorption fine structure (EXAFS) and X-ray absorption near edge structure (XANES) spectroscopies. The least-square fits of the XANES spectra suggested that the main Cu species in the contaminated soil were Cu-HS (50%), CuCO(3) (28%), Cu(2)O (11%), and CuO (11%). The Cu-HS in the contaminated soil possessed equatorial and axial Cu-O bond distances of 1.94 and 2.17 A with coordination numbers (CNs) of 3.6 and 1.4, respectively. In the EKR process, the axial Cu-O bond distance in the Cu-HS complexes was increased by 0.15 A, which might be due to a ligand exchange of the Cu-HS with H(2)O molecules in the electrolyte. After 180 min of EKR, about 50% of the Cu-HS complexes (or 24% of total Cu) in the soil were dissolved and formed [Cu(H(2)O)(6)](2+) in the electrolyte, 71% (or 17% of total Cu in the soil) of which were migrated to the cathode under the electric field (5 V/cm). This work exemplifies the use of in situ EXAFS and XANES spectroscopies for speciation studies of Cu chelated with HS in the contaminated soil during EKR.

Copper↗

PubMed2004

Evidence for the interaction of technetium colloids with humic substances by X-ray absorption spectroscopy.

Spectroscopic extended X-ray absorption fine structure (EXAFS) evidence was obtained on the chemical environment of 99Tc(IV) atoms formed upon introduction of TcO4- into four types of laboratory-scale synthetic and natural systems which mimic in situ natural reducing conditions in humic-rich geochemical environments: (a) magnetite/pyrite in synthetic groundwater in the absence of humic substances (HSs), (b) magnetite/pyrite in natural Gorleben groundwater in the presence of HSs, (c) Boom clay sediment mixed with synthetic groundwater, and (d) Gorleben sand mixed with natural Gorleben groundwater. The investigated systems obey to pH 8-9 conditions, and all measured samples show similar EXAFS spectra for Tc, which could be fitted by a hydrated TcO2 x xH2O phase. The results are interpreted as follows: upon introduction of high concentrations (millimolar to micromolar) of TcO4-to chemically reducing environments, small Tc(IV) oxidic polymers are formed, which either may aggregate into larger units (colloids) and finally precipitate or may interact in their polymeric form with (dissolved and immobile) humic substances. This latter type of interaction--Tc(IV) colloid sorption onto HSs--differs significantly from the generally accepted metal--humate complexation and therefore offers new views on the possible reaction pathways of metals and radionuclides in humic-rich environments.

Aluminum Silicates↗

PubMed2004

Oxygen uptake during mineralization of humic substances from Infernão Lagoon (São Paulo, Brazil).

Assays were carried out to evaluate the dissolved oxygen uptake resulting from mineralization of humic substances (fulvic acid (FA) and humic acid (HA)) from different sources: sediment, dissolved organic matter (DOM) of 120-day decomposed aquatic macrophyte (Scirpus cubensis and Cabomba piauhyensis), and lagoon DOM. The experiments were also aimed at estimating the oxygen uptake coefficient of the mineralization. About 20-30 mg of substrate were added to 1.1 liters of water from Infernão Lagoon (21 degrees 33' to 21 degrees 37'S; 47 degrees 45' to 47 degrees 51'W). The solutions were aerated and the dissolved oxygen (DO) was monitored during 40 days. Dissolved organic carbon (DOC) and particulate organic carbon (POC) were estimated after 80 days of the experiment. Anaerobic processes were avoided by aerating the solutions. The results were fitted to a first-order kinetics model, from which the uptake of oxygen parameters was obtained. Oxygen consumption (OC) ranged from 4.24 mg L(-1) (HA--S. cubensis) to 33.76 mg L(-1) (FA--sediment). The highest deoxygenation coefficient (kD) was observed during mineralization of FA--DOM (0.299 day(-1)), followed in decreasing order by FA--S. cubensis, HA--sediment, HA--S. cubensis, FA --sediment, and FA--C. piauhyensis (0.282; 0.255; 0.178; 0.130, and 0.123 day(-1), respectively). The carbon analyses indicated that the FA and HA samples at the end of the experiment presented a decay that varied from 15.23% to 42.35% and that the FA and HA conversions into POC were relatively low (from 0.76% to 3.94%).

Biodegradation, Environmental↗

PubMed2001

Specific association of 36Cl with low molecular weight humic substances in soils.

Soils initially contaminated with 36Cl in the chloride form were subjected to solid-liquid extractions using a variety of reagents including deionised water and 1 M sodium hydroxide (NaOH). 1 M NaOH was found to result in the greatest recovery of 36Cl from the soils, a result which provided initial evidence that radioactive chlorine became attached to humic substances present naturally within the soils. Deionised water and 1 M NaOH extracts were subjected to analysis involving separation by gel filtration chromatography (GFC). It was found that 36Cl in 1 M NaOH extracts associated preferentially with low molecular weight (LMW) fractions of humic substances whereas, in deionised water extracts, 36Cl appeared to be present exclusively in the chloride form. Previous literature evidence, mainly from highly organic forest soils, suggests that conversion of stable chlorine from chloride to organic forms can occur as a result of biological action. The present paper also presents good evidence for the specific attachment of stable chlorine (37Cl) to a LMW humic fraction, again demonstrated using GFC separation. Current risk assessments of the deep geological disposal of solid radioactive wastes containing 36Cl typically assume a very low degree of sorption based on the notion that the predominant environmental species of radiochlorine is chloride. This paper concludes with a brief discussion on the implications of organochlorine formation in the biosphere for assessment of the radiological impact of deep geological disposal of solid radioactive wastes.

Adsorption↗

PubMed2006

Multielement characterization of metal-humic substances complexation by size exclusion chromatography, asymmetrical flow field-flow fractionation, ultrafiltration and inductively coupled plasma-mass spectrometry detection: a comparative approach.

The use of three different separation techniques, ultrafiltration (UF), high performance size exclusion chromatography (HPSEC) and asymmetrical flow field-flow fractionation (AsFlFFF), for the characterization of a compost leachate is described. The possible interaction of about 30 elements with different size fractions of humic substances (HS) has been investigated coupling these separation techniques with UV-vis absorption spectrophotometry and inductively coupled plasma-mass spectrometry (ICP-MS) as detection techniques. The organic matter is constituted by a polydisperse mixture of humic substances ranging from low molecular weights (around 1kDa) to significantly larger entities. Elements can be classified into three main groups with regard to their interaction with HS. The first group is constituted by primarily the monovalent alkaline metal ions and anionic species like B, W, Mo, As existing as oxyanions all being not significantly associated to HS. The second group consists of elements that are at least partly associated to a smaller HS size fraction (such as Ni, Cu, Cr and Co). A third group of mainly tri- and tetravalent metal ions like Al, Fe, the lanthanides, Sn and Th are rather associated to larger-sized HS fractions. The three separation techniques provide a fairly consistent size classification for most of the metal ions, even though slight disagreements were observed. The number-average molecular weight (Mn), the weight-average molecular weight (Mw) and the polydispersity (rho) parameters have been calculated both from AsFlFFF and HPSEC experiments and compared for HS and some metal-HS species. Differences in values can be partly explained by an overloading effect observed in the AsFlFFF experiments induced by electrostatic repulsion effects in the low ionic strength, high pH carrier solution. Size information obtained from ultrafiltration is not as resolved as for the other methods. Molecular weight cut-offs (MWCO) of the individual filter membranes refer to globular proteins and molecular weight information may therefore, deviate from that given by the other methods after calibration with polystyrene sulfonate (PSS) standards.

Chromatography, Gel↗

PubMed2005

Coagulation of humic substances and dissolved organic matter with a ferric salt: an electron energy loss spectroscopy investigation.

Transmission electron microscopy (TEM) coupled with electron energy loss spectroscopy (EELS) and energy dispersive X-ray spectroscopy (EDXS) was used to investigate the coagulation of natural organic matter with a ferric salt. Jar-test experiments were first conducted with a reconstituted water containing either synthetic or natural extracts of humic substances, and then with a raw water from Moselle River (France). The characterization of the freeze-dried coagulated sediment by EELS in the 250-450 eV range, showed that Fe-coagulant species predominantly associate with the carboxylic groups of organic matter, and that this interaction is accompanied by a release of previously complexed calcium ions. The variation of Fe/C elemental ratio with iron concentration provides insightful information into the coagulation mechanism of humic substances. At acid pH, Fe/C remains close to 3 over the whole range of iron concentrations investigated, while a much lower atomic ratio is expected from the value of optimal coagulant dosage. This suggests that a charge neutralization/complexation mechanism is responsible for the removal of humic colloids, the aggregates being formed with both iron-coagulated and proton-neutralized organic compounds. At pH 8, the decrease in Fe/C around optimal coagulant concentration is interpreted as a bridging of stretched humic macromolecules by Fe-hydrolyzed species. Aggregation would then result from a competition between reconformation of humic chains around coagulant species and collision of destabilized humic material. EELS also enabled a fingerpriting of natural organic substances contained in the iron-coagulated surface water, N/C elemental analyses revealing that humic colloids are removed prior to proteinic compounds.

Colloids↗

PubMed2001

Alkaline hydrolysis of humic substances--spectroscopic and chromatographic investigations.

To find out more on the structure of humic substances (HS), isolated dissolved organic carbon (DOC) samples from a brown water lake and a wastewater effluent were fractionated and subjected to alkaline hydrolysis. UV/Vis and fluorescence spectroscopy, as well as size-exclusion chromatography with on-line detection of UV absorption, fluorescence and DOC concentration were used to investigate the structural changes caused by the hydrolysis reaction. Following hydrolysis, the fluorescence intensity increased considerably despite a decrease in the UV absorption. The UV absorption and the DOC data from the SEC experiments revealed a strong shift to smaller molecular sizes after hydrolysis. The spectra of the hydrolysed samples, as well as the size-exclusion chromatograms, were compared to spectra of hydroxybenzoic acids and hydroxycinnamic acids. From this comparison, it can be concluded that the hydrolysis products have a structure similar to these organic acids.

Absorption↗

PubMed2006

[The effects of the humic substances on Azoreduction by Shewanella spp].

Under anaerobic conditions, Shewanella cinicaD14(T), Shewanella baltica and Shewane-lla putrefaciens are capable of high-rate azoreduction and humus reduction. The results indicated that at low concentration ( <2 mmol/L) AQS was a accelerator for bacterial azoreduction. However, when the concentration of AQS was more than 5 mmol/L a strong inhibition was occurred. On the other hand, the concentration of AQDS as high as 12 mmol/L the inhibition of azoreduction was still not exhibited, but the effect of acceleration was gradually decreased with the concentration of AQDS increasing (1 mmol/L to 12 mmol/L). 6 azo dyes (Table 1) were tested, all of which had a similar results. These results indicated that the humic substances were not only as a redox mediator during the azoreduction, but also as the competitor for electron from respiration chain. Because the humic substances could be act as the terminal electron acceptor for bacterial anaerobic respiration. AQS and AQDS exhibiting different behaviour on the azoreduction were determined by their standard redox potentials.

Anaerobiosis↗

PubMed2001

Quantification and prediction of the detoxifying properties of humic substances related to their chemical binding to polycyclic aromatic hydrocarbons.

Effects of 27 different humic materials on the toxicity of polycyclic aromatic hydrocarbons (PAH) were studied for crustacean Daphnia magna. Sources included isolated humic acids, fulvic acids, and their combination from soil, peat, and freshwater. The PAH used were pyrene, fluoranthene, and anthracene. The observed reduction in toxicity of PAH in the presence of humic substances (HS) was shown to be a result of the detoxification effect caused by the chemical binding of PAH to HS and of the direct effect of HS on D. magna. An approach was developed to quantify the detoxifying impact of humic materials related to their chemical binding to PAH with a use of the "constant of detoxification" or "toxicological partition coefficient" K(oc)D. The latter was proposed to determine by fitting the experimental relationships of the detoxification effect versus concentration of HS. The obtained K(oc)D values were well tracked by the corresponding partition coefficients determined by the fluorescence quenching technique (K(oc)fq): K(oc)D=b x K(oc)fq, b (mean+/-Cl, n=26, P=95%)=2.6+/-0.3, 4.6+/-0.6, and 6.0+/-1.4 for pyrene, fluoranthene, and anthracene, respectively. The predictive relationships between the structure and detoxifying properties of humic materials in relation to PAH were developed. It was shown that the magnitude of the K(oc)D values correlated closely with the aromaticity of humic materials characterized with the 13C NMR descriptors (sigma(C)Ar, sigma(C)Ar/sigma(C)Alk) and atomic H/C ratio. The obtained relationships showed the highest detoxifying potential of the humic materials enriched with aromatics and allowed a conclusion on the chemical binding as the governing mechanism of the mitigating action of HS on the toxicity of PAH.

Animals↗

PubMed2001

Description of characteristics of humic substances from different waste materials.

Humic acids (HAs) extracted from different organic wastes have been characterised by chemical methods. The chemical properties of HAs showed differences depending on the source from which they were obtained. The C content in HAs from organic wastes (41.1-63.2%) fluctuated around the C value in soil HA with the exception of composted bark and tobacco dust. Compared with soil HA, the N contents of HAs from sewage sludge and brewery sludge were found much higher than the others. E4:E6 ratios for HAs in organic wastes were generally greater than that for soil HA, which indicated a low degree of condensation and humification. The carboxyl and phenolic-OH group contents ranged 0.51-2.23 and 11.1-20.7 meq g(-1), respectively. High values of carboxyl and phenolic-OH contents indicated that these materials were still within early stages of humification.

Fruit↗

PubMed2003

Electrophoretic assembly of naturally occurring humic substances as thin films.

Polydisperse humic acid thin films on optically transparent electrodes (OTEs) have been prepared by electrophoretic deposition from a solution of Suwanee River humic acid (SHA) in ethanol/acetonitrile. The thickness of the film and the rate of deposition of SHA are dependent on the applied voltage and the concentration of the solution. Tapping-mode atomic force microscopy (TM-AFM) confirms the assembly of SHA aggregates on the electrode surface. The ability of these thin films to incorporate redox-active species such as ferrocene from solution is demonstrated by cyclic voltammetry experiments. A linear dependence of the peak current for the oxidation of ferrocene as a function of scan rate indicates that the ferrocene is incorporated into the humic membrane.

Electrochemistry↗

PubMed2005

Effect of humic substance photodegradation on bacterial growth and respiration in lake water.

This study addresses how humic substance (HS) chemical composition and photoreactivity affect bacterial growth, respiration, and growth efficiency (BGE) in lake water. Aqueous solutions of HSs from diverse aquatic environments representing different dissolved organic matter sources (autochthonous and allochthonous) were exposed to artificial solar UV radiation. These solutions were added to lake water passed through a 0.7-microm-pore-size filter (containing grazer-free lake bacteria) followed by dark incubation for 5, 43, and 65 h. For the 5-h incubation, several irradiated HSs inhibited bacterial carbon production (BCP) and this inhibition was highly correlated with H2O2 photoproduction. The H2O2 decayed in the dark, and after 43 h, nearly all irradiated HSs enhanced BCP (average 39% increase relative to nonirradiated controls, standard error = 7.5%, n = 16). UV exposure of HSs also increased bacterial respiration (by approximately 18%, standard error = 5%, n = 4), but less than BCP, resulting in an average increase in BGE of 32% (standard error = 10%, n = 4). Photoenhancement of BCP did not correlate to HS bulk properties (i.e., elemental and chemical composition). However, when the photoenhancement of BCP was normalized to absorbance, several trends with HS origin and extraction method emerged. Absorbance-normalized hydrophilic acid and humic acid samples showed greater enhancement of BCP than hydrophobic acid and fulvic acid samples. Furthermore, absorbance-normalized autochthonous samples showed approximately 10-fold greater enhancement of BCP than allochthonous-dominated samples, indicating that the former are more efficient photoproducers of biological substrates.

Bacteria↗

PubMed2005

Photosensitized degradation of bisphenol A involving reactive oxygen species in the presence of humic substances.

The photodegradation of endocrine disrupter bisphenol A (BPA) in the presence of natural humic substances (HS) under simulated solar irradiation was studied. BPA underwent slow direct photolysis in neutral pure water, but rapid photosensitized degradation in four kinds of HS, following pseudo-first-order reaction. Reactive oxygen species (ROS) formed from HS were determined, including OH, (1)O(2) and H(2)O(2). The enhancement of BPA degradation by adding Fe(III) was primarily attributed to the oxidation of OH produced from photo-Fenton-like reaction. And the joint effects of HS and nitrate ions coexisting on BPA degradation appeared to depend on respective concentration levels. The effects of dissolved oxygen suggested that the energy transfer between excited state of SRFA and NOFA likely occurred, while the abstraction of phenolic hydrogen atom to reactive triplet state of NOHA possibly took place. Based on the structural analyses of main intermediates and degradation products of BPA detected by GC-MS, the possible photodegradation pathways were proposed, involving the alky cleavage, alkyl oxidation and OH addition. This study gave a better understanding for the photochemical transformation of BPA induced by ROS generated from natural water composition under sunlight irradiation.

Benzhydryl Compounds↗

PubMed2002

Trichloroethylene adsorption by activated carbon preloaded with humic substances: effects of solution chemistry.

Trichloroethylene (TCE) adsorption by activated carbon previously loaded ("preloaded") with humic substances was found to decrease with increasing concentrations of monovalent ions (NaCl), calcium (until solubility was exceeded), or dissolved oxygen in the preloading solution. For a given percentage of organic carbon removal during humic acid loading, greater reductions in TCE adsorption occurred with increasing monovalent ion concentration and calcium concentration at constant ionic strength. However, this effect was related primarily to the amount of humic material adsorbed--the reduction in TCE adsorption was independent of the ionic composition of the preloading solution when compared at similar humic acid loading. Experiments were performed which showed that calcium ions can associate with humic material after the humic has been adsorbed, which subsequently reduces TCE uptake, but this effect does not dominate when calcium is present during humic loading. At sufficiently high calcium concentrations (approaching solubility), aggregation or co-precipitation of humic acid mitigated the effects of preloading. In contrast to the effects of ionic composition, the presence of dissolved oxygen did fundamentally change the mechanism by which organic macromolecules compete with TCE. TCE uptake was lower when preloading by poly(maleic acid) (PMA) occurred in the presence of dissolved oxygen, even when the amount loaded was the same. One explanation invokes a coupling mechanism promoted by the carbon surface, which results in either additional blockage of TCE sorption sites, additional site competition, or both. In all experiments, the effects of preloading were consistent with those reported previously, which have been interpreted as a loss of high-energy sites available to TCE, causing a significant reduction in the site-energy heterogeneity, and reduced uptake in the low concentration region.

Adsorption↗

PubMed2006

Effect of humic substance on thermal treatment of chromium(VI)-containing latosol soil.

Latosol soils contaminated with chromium(VI) [Cr(VI)], which is hazardous, can be recycled as raw materials for porcelain and construction sectors if a proper thermal stabilization process is implemented. This study investigates how thermal treatment affects Cr behavior during the sintering of latosol and deorganic latosol samples; both samples are artificially contaminated with CrO3. Approaches including X-ray absorption spectroscopy, scanning electron microscopy, N2-based Brunauer Emmett Teller surface analyzer, thermogravimetric analyzer/differential scanning calorimeter, and the toxicity characteristic leaching procedure promulgated by Taiwan Environmental Protection Administration are used in this study. After drying the Cr(VI)-contaminated latosol (i.e., containing 37,120 mg of Cr/kg sample) at 105 degrees C, approximately 80% of the doped CrO3 is chemically reduced to Cr(OH)3 by a humic substance naturally existing in the soil. In contrast, in the organics-free CrO3-contaminated latosol dried at 105 degrees C, only 9% of the doped CrO3 is reduced to Cr(OH)3. Heating the samples at 500 and 1100 degrees C transforms hazardous Cr(VI) into Cr(III) that is negligibly toxic; Cr2O3, which is insoluble, is detected as the most abundant Cr species. Moreover, formation of Cr2SiOs, which is suggested to relate to low Cr leaching, is only detected in the sample heated at 1100 degrees C. Surface morphology, surface area, and thermogravimetric analyzer/differential scanning calorimeter results demonstrate that thermal treatment at 1100 degrees C can incur considerable soil sintering/ melting if the humic substance in the soil has been heated off previously. Finally, Cr concentrations in the toxicity characteristic leaching procedure leachates collected from the samples thermally treated at 1100 degrees C for 4 hr are < or =0.21 mg of Cr L(-1) that are much less than the Taiwan Environmental Protection Administration regulatory limit (<5 mg of Cr L(-1)); consequently, these two samples are nonhazardous, and they have the potential for resource recycling. Conversely, Cr concentrations in the leachates from all 500 degrees C and 105 degrees C samples are in the 25.6-1279 mg L(-1) range.

Calorimetry, Differential Scanning↗