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A thermodynamic Gibbs energy minimization (GEM) solid solution-aqueous solution (SSAS) equilibrium model was used to determine the solubility of Zn from calcium silicate hydrate (CSH) phases doped with 0, 0.1, 1, 5, and 10% Zn at a unity (Ca+Zn)/Si molar ratio. Both the stoichiometry and standard molar Gibbs energy (G(o)298) of the Zn-bearing end-member in the ideal ternary Zn-bearing calcium silicate hydrate (CZSH) solid solution were determined by a "dual-thermodynamic" (GEM-DT) estimation technique. The SSAS model reproduces a complex sequence of reactions suggested to occur in a long-term weathering scenario of cementitious waste forms at subsurface repository conditions. The GEM model of CZSH leaching at several Zn loadings and solid/water (s/w) ratios in a C02-free system showed that, upon complete dissolution of portlandite and calcium zincate phases at decreasing s/w < 0.01 mol x kg(H2O)(-1), the total dissolved concentrations Si(aq), Ca(aq), and Zn(aq) are controlled by a CZSH solid solution of changing composition, with a trough-like Znaq drop by 2-3 orders of magnitude. Carbonation was simulated in another GEM model run series by CO2 titration of the system with initial s/w approximately 0.9 mol/kg(H2O). Formation of (Ca,Zn)-CO3 nonideal solid solution was predicted already at early reaction stage in the presence of both portlandite and calcium zincate hydrate phases. Upon their disappearance, pH, Zn(aq), C(aq), and fCO2 were predicted to change due to the incongruent dissolution of two concurrent CZSH-I and CZSH-II solid solutions, until the total re-partitioning of Ca and Zn into a carbonate solid solution coexisting with amorphous silica at fCO2 > 0.1 bar. Along this solid-phase transition, dissolved Zn(aq) concentrations follow a highly nonlinear trend. The model results predict that at low to moderate Zn loading (< or = 1% per mole Si), CZSH-type compounds can efficiently immobilize Zn in the near field of a cement-stabilized waste repository.
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PMID:Aqueous solubility diagrams for cementitious waste stabilization systems. 4. A carbonation model for Zn-doped calcium silicate hydrate by Gibbs energy minimization. 1214 69

It is generally assumed that phosphate (Pi) effluxes from proximal tubule cells by passive diffusion across the basolateral (BL) membrane. We explored the mechanism of BL Pi efflux in proximal tubule-like OK cells grown on permeable filters and then loaded with 32P. BL efflux of 32P was significantly stimulated (P < 0.05) by exposing the BL side of the monolayer to 12.5 mM Pi, to 10 mM citrate, or by acid-loading the cells, and was inhibited by exposure to 0.05 mM Pi or 25 mM HCO3; by contrast, BL exposure to high (8.4) pH, 40 mM K+, 140 mM Na gluconate (replacing NaCl), 10 mM lactate, 10 mM succinate, or 10 mM glutamate did not affect BL 32P efflux. These data are consistent with BL Pi efflux from proximal tubule-like cells occurring, in part, via an electro-neutral sodium-sensitive anion transporter capable of exchanging two moles of intracellular acidic H2PO4- for each mole of extracellular basic HPO4= or for citrate.
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PMID:Basolateral phosphate transport in renal proximal-tubule-like OK cells. 1219 5

Pure goethite particles in the nanometer size range (from approximately 200 to approximately 80 nm) with an elongated shape (axial ratio from approximately 5 to approximately 8) useful as iron precursors for magnetic recording have been prepared by oxidation of the suspensions resulting from the addition of sodium carbonate to Fe(II) sulfate aqueous solutions under a restrictive set of experimental conditions (Fe(II) concentration, carbonate/Fe(II) mole ratio, temperature, and air flow rate). In all cases, the goethite particles were formed by a dissolution-recrystallization mechanism through an intermediate green-rust phase. The particle size was determined by the carbonate/Fe(II) ratio (which controls the formation pH), the FeSO(4) concentration, and the air flow rate. The smallest particles (length 80 nm) were obtained for a high carbonate/Fe(II) mole ratio (>/=3), a low Fe(II) concentration (0.075 mol dm(-3)), and an air flow rate of 2 dm(3) min(-1). The goethite particles were also characterized by the electron diffraction and high-resolution TEM finding that they were monocrystalline, having the crystalline c axis parallel to the longest particle dimension.
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PMID:Uniform nanosized goethite particles obtained by aerial oxidation in the FeSO4-Na2CO3 system. 1270 28

The objective of this work was to synthesize and characterize a novel series of biodegradable cyclic carbonate polyester copolymers based on lactide and 5-methyl-5-benzyloxy-carbonyl-1,3-dioxan-2-one (MBC). Two compositions were selected for characterization. One copolymer was based on a racemic mixture of 1-lactide with 15.4 mole % MBC and the other was based on 1-lactide with 8.2 mole % MBC. These polymers contain carboxylic acid moieties along the backbone that may be used for tethering bioactive agents, forming ionic crosslinks or be reacted with vinyl containing monomers to allow free radical crosslinking. The initial materials evaluated have the carboxylic acid functionalities blocked with benzene. These polymers and the de-blocked versions may have potential applications for hard and soft tissue scaffolds, control drug delivery matrixes or a variety of other applications in medicine. The copolymer samples were pressed into 7.0-mm diameter disk using a KBr press. The disks were then sterilized using U.V radiation under a laminar flow hood. After sterilization, the copolymer disks were submerged in 2 ml of media and placed in a CO2 regulated incubator at 37 degrees C. A total of six groups per phase (n = 7 test tubes per group) were used in this study. Test tubes in groups I and III were plated with MRC-5 and subsequently treated with media alone (controls). Test tubes in groups II and IV were plated with MRC-5 and subsequently treated with media before being introduced to copolymer samples. Cell number, as well as, biochemical markers such as protein and malondialdehyde (MDA) were determined at the end of the 24, 48 and 72-hour time periods. Representative test tubes were subjected to an H&E staining procedure for microscopic morphological evaluation. The results of this evaluation suggest that the exposure of both copolymers produced a non-cytotoxic environment with the MRC-5 cell line. Although both copolymers are non-cytotoxic, the sample having the higher MBC content is the preferred composition based upon MDA levels and morphological evaluations.
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PMID:Evaluation of novel biodegradable cyclic carbonate polyester copolymers for cytocompatibility using MRC-5 cells. 1272 11

The primary method for standardizing or certifying an Mz+-ISE (Ion Selective Electrode for Mz+ where Mz+ = alkali or alkaline-earth cation) implies comparing the latter with the corresponding M-Amalgam electrode in the cell Pt/M-Amalgam/Mz+ Solution/Mz+ ISE/Pt, whose potential difference is obviously independent of Mz+ concentration. Assessment of the potential of the M-Amalgam electrode requires the precise determination of the mole fraction x of the M metal in amalgam, which is customarily performed by decomposing an M-Amalgam sample in excess HCl and titrating the HCl excess with standard NaOH solution. There arises the problem of choosing the correct end-point in pH-metric titrations of strong acids with carbonate-contaminated NaOH standard solutions, which is of frequent occurrence both in research and routine laboratory practice. This topic is either overlooked or insufficiently treated in textbooks: thus the interpretation of the above experimental pH-metric titration curves is often misled and the results may be affected by significant errors. Some recent misleading suggestions are here re-analyzed critically in order to focus correct, recommended methodological schemes.
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PMID:Problems in assessments of amalgam electrodes for standardising or certifying the corresponding ion selective electrodes. 1273 82

Fourier transform infrared spectroscopy was used to study the composition and microstructure of soluble complexes produced by different initial mole ratios of bovine serum albumin(BSA) and calcium hydroxyapatite [Ca10(OH)2(PO4)6] and calcium carbonate (CaCO3) in aqueous solution. The band shifts and intensity variations suggested that calcium complexes with multiple ligands such as BSA, apatite, carbonate as well as the hydrogen bond network formed in titled system. The interactions increased the solubility of Ca10 (OH)2(PO4)6 and CaCO3 and the composition of soluble complexes is nonstoichiometric. The results provided an ideal model to investigated biomineralization process.
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PMID:[Study on the formation mechanism of soluble complexes containing bovine serum albumin and calcium hydroxyapatite and calcium carbonate]. 1293 67

Analytical grade L-glutamic acid is chemically stable and has a C/N mole ratio of 5, which is close to that of many of natural biological materials, such as blood and animal tissue. Two L-glutamic acid reference materials with substantially different 13C and 15N abundances have been prepared for use as organic reference materials for C and N isotopic measurements. USGS40 is analytical grade L-glutamic acid and has a delta13C value of -26.24 per thousand relative to VPDB and a delta15N value of -4.52 per thousand relative to N2 in air. USGS41 was prepared by dissolving analytical grade L-glutamic acid with L-glutamic acid enriched in 13C and 15N. USGS41 has a delta13C value of +37.76 per thousand and a delta15N value of +47.57 per thousand. The delta13C and delta15N values of both materials were measured against the international reference materials NBS 19 calcium carbonate (delta13C=+1.95 per thousand ), L-SVEC lithium carbonate (delta13C=-46.48 per thousand ), IAEA-N-1 ammonium sulfate (delta15N=0.43 per thousand ), and USGS32 potassium nitrate (delta15N=180 per thousand ) by on-line combustion continuous-flow and off-line dual-inlet isotope-ratio mass spectrometry. Both USGS40 and USGS41 are isotopically homogeneous; reproducibility of delta13C is better than 0.13 per thousand, and that of delta15N is better than 0.13 per thousand in 100-microg amounts. These two isotopic reference materials can be used for (i) calibrating local laboratory reference materials, and (ii) quantifying drift with time, mass-dependent fractionations, and isotope-ratio-scale contraction in the isotopic analysis of various biological materials. Isotopic results presented in this paper yield a delta13C value for NBS 22 oil of -29.91 per thousand, in contrast to the commonly accepted value of -29.78 per thousand for which off-line blank corrections probably have not been quantified satisfactorily.
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PMID:Two new organic reference materials for delta13C and delta15N measurements and a new value for the delta13C of NBS 22 oil. 1460 17

Goethite is a representative iron oxide in natural environments due to its abundance and thermodynamic stability and may be responsible for many surface-mediated processes, including ion retention and mobility in aqueous settings. A large variability in morphologies and specific surface areas of goethite crystals exists but little work has been done to compare surface reactivity between them. The present work offers experimental evidence for the existence of an inverse relationship between sorption capacity for protons and carbonate ions and specific surface area of goethite for three synthetic goethite preparations spanning surface area differences by a factor of 2. An explanation for this was found by assuming a variable reactive site density between preparations in direct relationship to their sorption capacity based on congruency of carbonate sorption computed on a per-site basis. Previous evidence of maximum sorption capacities supports this explanation, and site density ratios between the goethites studied here were obtained. Triple layer surface complexation modeling was successful in describing adsorption data for all goethite preparations using equal stoichiometries. A new formulation of standard state for activities of surface species based on a 1.0 mole fraction of sites on the solid allowed transformation of the conventional molar concentration-based affinity constants to values based on site occupancy. In this fashion, by applying the appropriate site density ratios, a single set of affinity constant values was found that described accurately the adsorption data for all preparations.
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PMID:Variability in goethite surface site density: evidence from proton and carbonate sorption. 1464 28

Nine samples of Ca-deficient apatite (Ca-def Ap) were prepared from suspensions of CaHPO4 (monetite) at 90 degrees C by raising the pH from approximately 4 through release of NH3 produced by the hydrolysis of urea. Products were dried at 100 degrees C for 24h and studied by chemical analyses, X-ray powder diffraction (XRPD) (and Rietveld analysis of this data), Ca/P ratio determination (quantitative phase analysis of samples after heating to 900 degrees C from Rietveld analysis of XRPD data), scanning electron microscopy, He pycknometry, 1H and 31P MAS NMR spectrometry and Fourier transform infrared and Raman spectroscopy. All samples contained apatite, but three also contained monetite. Infrared and Raman spectroscopy confirmed the presence of HPO4(2-) and absence of carbonate ions in the six monetite-free samples. Mean results for the six samples were: a = 9.4320(40), c = 6.8751(31) A; unit cell formula from chemical analysis neglecting protonation of phosphate ion, Ca(9.303(50))(PO4)6(OH)(0.606(99)).1.97(12)H2O; theoretical density 3.10 g cm(-3); experimental density (mean for three samples) 3.15 g cm(-3); and Ca/P mole ratio from chemical analysis and phase analysis after heating to 900 degrees C, 1.550(8) and 1.550(2), respectively. An earlier assignment of a line at 6 ppm in the 1H NMR spectrum of similar samples to HPO4(2-) ions could not be confirmed; hence no information about the HPO4(2-) ion content could be derived, in disagreement with the previous NMR study. A shoulder at approximately 0.9 ppm relative to 85 wt% H3PO4 in the 31P NMR spectrum was assigned to HPO4(2-) ions. Occupancies from the Rietveld structure refinements indicated preferential loss of Ca from Ca2 sites compared with Ca1, but the loss was substantially smaller than expected from chemical analyses. It is suggested that imperfect modelling of the structure in the refinement, particularly disorder associated with the Ca2 site, resulted in errors in Ca2 occupancies. The P-O bonds were slightly shorter than those in stoichiometric hydroxyapatite, rather than longer as might be expected from protonation of phosphate tetrahedra. However, consideration of known acid phosphate structures indicated that it was unlikely that the increase in P-O lengths would be sufficient to be detected. The observed decrease was tentatively assigned to the presence of Ca2+ ion vacancies.
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PMID:Rietveld refinements and spectroscopic studies of the structure of Ca-deficient apatite. 1547 62

Soil extraction of lead contaminated soil collected from sites near an abandoned battery recycling and secondary lead-smelting factory was investigated for potential use in decontaminating soil at the sites. A fractionation study was conducted to elucidate soil retention mechanism for Pb at the site. Three soil pits were selected from an area surrounding the factory based on level of Pb contamination. Soil samples were collected from each pit in two layers: surface soil and subsoil (0-15 cm and 15-30 cm). Soil physical analysis showed that the soil texture was sandy loam and sandy clay loam with clay content between 11-21%. Soil pH was strongly acid to moderately acid (pH 4.8-5.9). Pb levels in the surface soil were 1620 and 153 mg kg(-1) (air-dried basis) respectively for heavily and slightly contaminated soil. A reference soil site contained 15 mg kg(-1) of Pb. Partitioning studies indicated that more than 90% of total Pb in the soil existed in three primary fractions: exchangeable, carbonate, and Fe-Mn oxide. This suggested that Pb sources entering the soil from the Pb factory remained in relatively weakly bound forms, which are mobile and have potentially biological availability. Mobility of Pb as in the soil assessed by mobility factor (MF) was as high as 75% indicating a high potential of Pb remobilization. Due to high mobility, the Pb would be amendable to remediation or removal by soil extraction procedures. To determine if such weekly bound Pb could be easily removed, both soil washing (ex situ) and soil flushing (in situ) techniques were evaluated for potential Pb remediation procedure. Particle size separation of soil into coarse (2.0-0.25 mm), medium (0.25-0.15 mm), and fine size (<0.15 mm) was conducted before initiating soil washing for comparing Pb removal efficiency in these fractions with the indigenous soil fraction. Using EDTA (2:1 mole to Pb) as a washing solution up to 85-95% of Pb was removed under the optimum conditions (retention time = 60 min), and liquid to solid ratio (L/S) at 5:1 for coarse fraction and 10:1 for smaller fraction. Pb could be removed from contaminated soil using EDTA extraction; however, the efficiency was higher in the coarse texture soil fraction. As a result particle size separation is recommended before application of the soil washing procedure. For smaller soil particle size fraction a series of extraction was needed for obtaining an adequate extraction efficiency. Three solvents tested as flushing solution showed 85, 84, and 74% of Pb was removed by EDTA (2:1 mole to Pb), 1M HNO3, and 0.2 M ammonium citrate, respectively after flushing with 20 pore volumes. The capacity of the three flushing solutions to remove Pb from the contaminated soil were ranked in the order: EDTA approximately 1 M HNO3 > 0.2 N ammonium citrate. However, in highly contaminated soil all solvent extract required several Pb leaching cycles. The flushing process using 1 M HNO3 increased soil acidity to extreme acid conditions (pH 2.0) resulting in adverse effects to physicochemical properties of the treated soil. In general, results showed three factors influenced Pb removal by the extraction techniques: (i) initial Pb concentrations, (ii) Pb partitioning within soil, and (iii) particle size of soil matrix.
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PMID:Evaluation of extraction procedures for removing lead from contaminated soil. 1571 83


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