Phosphate Precipitation Research Articles

Ultra-Short Laser-Assisted Micro-Structure Formations on Mg/Zn Double-Doped Calcium Phosphate Ceramics for Enhanced Antimicrobial Activity.

Bacterial infection is one of the most common and harmful medical issues following the implantation of materials and devices in the body leading to antibiotic resistance of diverse bacterial strains. In this work, a novel approach is presented combining adopted laser-based patterning method in addition to doping (Mg and Zn) metal ions to prepare calcium phosphate ceramic substrate, applicable in medicine, with enhanced surface antimicrobial characteristics. The preparation of tablets containing Mg (8.44 mol%) and Zn (2.63 mol%) β-tricalcium phosphate involved biomimetic precipitation of amorphous calcium phosphate in media of simulated body fluid enriched with Mg2+ and Zn2+ ions as well as the presence of valine as an organic additive, followed by step-wise calcination up to 1000 °C. The results from laser processing showed formation of deeper patterns with increased surface roughness (from 4.9 µm to 9.4 µm) as laser power and velocity increase, keeping constant the hatch sizes of 50 µm. The textured surfaces consist of peaks and valleys arrangement that change the morphology of Escherichia coli cells and decrease of cell viability. Our study reveals the possibilities of the application of ultra-short laser radiation as a potential alternative therapy for controlling the antimicrobial effect of the ceramic surface.

Precipitation of Lithium Phosphate from Cathode Materials of Spent Lithium-Ion Battery by Hydrometallurgy Process

Spent lithium-ion batteries (LIBs) have significantly increased due to the high consumption of LIBs for automobile applications; therefore, the recovery of valuable materials to use as the second resource can bring economic benefits and reduce an environmental impact. This study investigated the production of lithium phosphate (Li3PO4), which can be used as a starting material for the synthesis of LIBs, from spent LiNixMnyCozO2 (NMC) cathodes. The experimental procedure started with discharging, dismantling the battery, and removing the aluminum foil, followed by the leaching of cathode material before precipitating the lithium phosphate from the solution. In the leaching stage, the parameters to optimize the process were studied. The results showed that the lithium leaching efficiency could be achieved at 96.10% using 2 M H2SO4, 8 vol.% H2O2, 40 g/L pulp density, and 4 hrs at 70°C. The final precipitate product of 98.98% purity of Li3PO4 was recovered from the solution using Na2HPO4 under the experimental condition.

Leaching of phosphorus from phosphate tailings and extraction of calcium phosphates: Toward comprehensive utilization of tailing resources

Phosphate tailing is an extremely fine by-product during phosphate ore flotation. Due to the large quantities and relatively higher P2O5 content, the phosphate tailings have been considered as a potential P resource, compared to other P-bearing wastes. Besides, phosphate tailings also contain a large amount of available components, such as Ca, Mg, and Si. To explore a low-cost and efficient process for the utilization of phosphate tailings, the hydrochloric acid leaching-precipitation method was employed to recover phosphorus. The P in phosphate tailings can be selectively dissolved into leaching liquor, followed by the precipitation of calcium phosphates from the leaching liquor through pH adjustment. The results showed that P was predominantly concentrated in fluorapatite and its dissolution ratio increased with the decrease in pH. At pH 1.0, the P dissolution efficiency from phosphate tailings reached 96.3%, along with the majority of Mg and Ca. However, Si was hardly dissolved. It demonstrated that almost all the fluorapatite and dolomite were dissolved while the quartz was difficult to dissolve. Dolomite was more preferentially dissolved than fluorapatite. Increasing temperature contributed to the dissolution of dolomite while suppressing fluorapatite dissolution. The residue containing 87.9% SiO2 (quartz) and only 0.25% P2O5 has the potential as a building material. As the pH increased to 7.0, the collected precipitate consisted of 34.18% P2O5 and 56.10% CaO, which can serve as a source of a slow-released phosphate fertilizer. The highly efficient utilization of phosphate tailings was achieved via this process.

Synergetic effect on fouling alleviating of membrane distillation in urine resource recovery by thermally activated peroxydisulfate pretreatment

Given that the spontaneous precipitation of minerals caused by urea hydrolysis and abundant organic compounds, membrane fouling became a major obstacle for urine recovery by membrane distillation (MD). Herein, this study developed a combined system (TAP-MD) by integrating thermally activated peroxydisulfate (TAP) and MD process to inhibit membrane fouling and improve separation efficiency. Based on the TAP-MD system, the separation performance was improved significantly, improving nutrient recovery efficiency and quality of reclaimed water. More than 80% of water could be recovered from urine, and about 94.13% of total ammonia nitrogen (TAN), 99.02% of total nitrogen (TN), 100% of total phosphate (TP), and 100% of K+ were rejected. The mechanism for alleviating urine-induced fouling was systematically and intensively studied. With TAP pretreatment, the TAN concentration of pretreated urine was kept at a low level steadily and the pH was at neutral or weakly acidic. Hence, inorganic scaling represented by carbonate and phosphate precipitates were significantly inhibited by creating unfavorable solvent environment for crystallization with TAP pretreatment. Additionally, aromatic proteins were found as the main organic foulants. According to the secondary structure of protein, the proteins were degraded by the cleavage of peptide bonds by TAP pretreatment. Meanwhile, the hydrophilicity of protein increased, which reduced the hydrophobic interaction of protein and membrane surface and thus alleviated protein-induced membrane fouling. This study revealed the inorganic and organic foulants in urine that caused membrane fouling and demonstrated the mechanism of membrane fouling alleviation by TAP-MD system. The experimental results will be instrumental in better understanding the mechanisms of membrane fouling induced by urine and optimize MD process for resource recovery from urine.

Corrosion behavior, mechanical properties, and in-vitro biocompatibility of cast Mg–3Zn–xSi biodegradable alloys for bone regeneration

In this research, Mg–3Zn–xSi (x = 0, 0.1, 0.3, and 0.6 wt%) biodegradable alloys were produced by simple stir casting method, their microstructure and phase changes were evaluated using X-ray diffraction (XRD), optical microscope (OM) and scanning electron microscope coupled with energy dispersive x-ray analysis (SEM–EDS). Potentiodynamic polarization was conducted to measure the alloys’ corrosion behavior in simulated body fluid (SBF). Tensile strength test and in-vitro biocompatibility evaluation regarding MTT cytotoxicity, ALP osseointegration assay and MG-63 cell growth pattern were conducted. Electrochemical investigations showed that Mg–3Zn alloys enclosing Si attained degradation rates suitable for structural support until bone healing, while the Mg–3Zn alloy without Si had a corrosion rate of 0.128 mm/year which is much lower than the required value. None of the inspected alloys exhibited a significant cytotoxic effect, meanwhile, Mg–Zn base alloy and the alloy with 0.3 wt% Si demonstrated the highest ALP level. The optimum cell growth pattern was demonstrated for Mg–Zn base alloy and the alloy with 0.1 wt% Si. Evidence of calcium phosphate precipitation was observed in the four investigated Mg–3Zn alloys. Therefore, based on the fore mentioned results, Mg–3Zn–xSi alloys were suggested as viable biodegradable materials due to their compatible degradation rates, proved cytocompatibility, high cell viability and excellent osseointegration potential.

Apatite-coated outer layer eggshell membrane: A novel osteoinductive biohybrid composite for guided bone/tissue regeneration

Hybrid biomimetic materials aim to replicate the organic-inorganic constructs of mineralized tissues. During eggshell formation, the outer surface of the eggshell membrane (ESM) promotes calcium carbonate nucleation, while the inner one prevents mineralization toward the egg white and yolk. In the current study, the outer surface of the ESM acted as a heteronucleant in calcium phosphate precipitation by the vapor diffusion sitting drop method, while the inner one remained unmineralized. The aim was to fabricate a 2D biomaterial with dual functions, osteoinductive on one side and protective against cell invasion on the other side. The microstructural, physicochemical, morphological, and mechanical properties of the mineralized ESM were characterized by XRD, TGA, XPS, FTIR/Raman, HR-SEM, and mechanical testing techniques. The cytocompatibility and osteoinductive ability were assessed by biological assays of cell viability, proliferation, and osteogenic differentiation on human mesenchymal stromal cells (hMSCs). Results indicate that the outer surface of the ESM induces the heterogeneous precipitation of carbonate-apatite phase depicting biomimetic features. In addition, the apatite/ESM shows a much higher cytocompatibility than the pristine ESM and promotes the osteogenic differentiation of hMSCs more efficiently. Overall, the apatite/ESM composite exhibits compositional, crystalline, mechanical, and biological properties that resemble those of mineralized tissues, rendering it an approachable and novel material especially useful in guided tissue/bone regeneration.

Impacts of Modified Fly Ash on Soil Available Lead and Copper and Their Accumulation by Ryegrass

Fly ash (FA) is promising for environmental remediation, but how to modify the FA with high remediation efficiency through an environmentally friendly and low-cost modification method is scare. A modified FA (MFA) was prepared through a one-step hydrothermal modification with Ca(OH)2 and KH2PO4. Results indicated that irregular agglomerates occurred on the surface of the MFA and that the specific surface area increased by 1.94 times compared to that of FA. Compared to FA, glassy compositions in MFA were destroyed and amorphous Si/Al and alkaline aluminosilicate gels were formed. The soil application of 0.2–0.6% MFA significantly increased soil pH by 0.23–0.86 units compared to FA and decreased available lead (Pb) and copper (Cu) by 25–97.1% and 13.5–75%, respectively. MFA significantly decreased exchangeable Pb and Cu by 12.5–32% and 11.4–35.2%, respectively, compared to FA. This may be due to the high pH and specific surface area of MFA, which promoted to the formation of amorphous Si/Al, metal–phosphate precipitation, and complexation with functional groups. In addition, MFA slightly increased the biomass of shoots and roots and decreased the uptake of Pb and Cu by ryegrass. This study provides a new modification method for the utilization of FA in the heavy metal-contaminated soils.

Research on square wave pulsed electrochemical phosphate recovery technology by Pt graphene foam metal electrode

Currently, using electrochemical precipitation techniques for phosphate removal and recovery in hydroxyapatite (HAP) or calcium phosphate (CaP) form is widely used, while the high energy consumption of electrochemical precipitation is a major obstacle to its application. In this study, a square wave pulsed electrochemical phosphate precipitation method was developed, which achieved phosphate pollution control and phosphate resource recovery and reuse at the same time. The square wave pulsed electrochemical phosphate recovery system was constructed and a Pt-rGO/CuF electrode was synthesized and evaluated. This result indicated that the Pt-rGO/CuF electrode had the highest electrocatalytic activity, the better electrical conductivity, and the smallest electron transport barrier. Under optimal operation conditions, the phosphate removal efficiency and specific energy consumption of Pt-rGO/CuF were 64.2% and 21.49 kWh kg−1, respectively. The Pt-rGO/CuF electrode demonstrated the best electrochemical precipitation reaction performance. The Pt-rGO/CuF electrode was applied to multiple types of actual wastewater, and the results showed that it has better application prospects in both low (7.75 mg L−1) and high (66 mg L−1) phosphate concentration wastewater, the phosphate removal efficiency was 75.5% and 59.1%, respectively. Compared with traditional chemical precipitation, the electrochemical precipitation method saved $2.88 per kg P and $57.57 per kg P, respectively.

Spontaneous Precipitation of Phosphates in Artificial Urine: Effect of Magnesium, Calcium, pH and Supersaturation

AbstractUrinary stone disease affects a significant portion of the global population, with calcium phosphate and magnesium phosphate calculi being among the most prevalent types. In this study, we have grown crystals of DCPD and MAP using supersaturated artificial urine, which was prepared by mixing two equal volumes of solutions A and B. The aim of this investigation was to contribute to the understanding of the effect of Calcium or Magnesium concentration, supersaturation and pH on the crystallization of phosphate stones in artificial urine and the characterization of the precipitated phase. The initial molar ratio of Ca/P and Mg/P solutions was varied in the range of 0.0 to 0.35, while the solution pH was maintained between 6.0 and 8.0. The analysis of the crystals that precipitated using FT‐IR spectroscopy and X‐Ray diffraction techniques revealed that DCPD was obtained at acidic pH (6.0 and 6.5). MAP was obtained at basic pH (7.5 and 8.0). A mixture of DCPD and MAP was formed at neutral pH. The calculated supersaturation values of MAP, OCP, HAP and TCP increased with increase in pH. At lower (pH=5), the order of increasing stability is OCP<HAP<TCP<MAP<DCPD. For higher (pH=10), the order of increasing stability is DCPD<MAP<TCP<OCP<HAP.

Controllable Synthesis of Hemoglobin-Metal Phosphate Organic-Inorganic Hybrid Nanoflowers and Their Applications in Biocatalysis.

In recent years, organic-inorganic hybrid nanoflower technology has become an effective method for enzyme immobilization. Here, seven hierarchical flower-like hemoglobin-phosphate organic-inorganic hybrid nanomaterials (Hb-M3(PO4)2·nH2O HNFs) were synthesized through an improved universal one-pot wet-chemical method, with Ca2+, Mn2+, Fe2+, Co2+, Ni2+, Cu2+ and Zn2+ as inorganic components. In this synthesis process, the metal cations are successively involved in the coordination reaction with Hb and the metathesis reaction to generate phosphate precipitation. The coordination ability of metal cations and the generation rate of phosphate precipitations were evaluated, then the progress of the two chemical reactions was controlled synchronously by adjusting the phosphate buffer (PB) concentration, and finally a flower-like structure conducive to substrate diffusion and transport was obtained. Due to the conformational transformation of hemoglobin and the abundant Cu2+/Fe3+ active sites, the hemoglobin-Cu3(PO4)2·3H2O nanoflowers have extremely high catalytic activity, which is ∼14 times that of Hb. Importantly, this method is suitable for the monometallic-ionic, polymetallic-ionic and polyvalent metal-ion nanoflowers, which broadens the chemical composition and structural diversity of nanoflowers.

Formation of Fluorapatite in the Equilibrium System CaO–P2O5–HF–H2O at 298 K in a Nitrogen Atmosphere

The process of biomineralization of apatite in nature has been studied by scientists from various fields of science for more than a century. Unlike the volcanogenic, hydrothermal, and other types of igneous apatites, the genesis of which is entirely clear, the formation of phosphate ores of marine sedimentary origin is still debatable. Since phosphate concentrations in water bodies are too low for the spontaneous precipitation of solid phosphates, the study of different ways for their concentration is of particular interest. In this work, phase equilibria in the system CaO–P2O5–HF–H2O at 298 K, involving fluorapatite formation, have been studied. Fluorapatite is known to be the most common phosphate mineral and the main source of phosphorus on Earth, playing an important role in the mineralization process of dental tissues in vertebrates. The equilibrium in the system defined above was studied at a low mass fraction of the liquid phase components, i.e., in conditions close to natural. It has been shown that the compounds of variable composition with the fluorapatite structure containing HPO42− ions were formed in the acid region of this system. These compounds are formed at pH ≤ 7.0 and have invariant points with monetite, CaHPO4, and fluorite, CaF2. Stoichiometric fluorapatite was formed at the lowest concentrations of the liquid phase components in a neutral and weakly alkaline medium and had an invariant point with Ca(OH)2. The composition of the resulting equilibrium solid phases was found to be dependent on the Ca/P ratio of the initial components and pH of the equilibrium liquid phase. Fluorite CaF2 was present in each sample obtained in this study.

Flow-through electrochemical organophosphorus degradation and phosphorus recovery: The essential role of chlorine radical

Phosphorus scarcity and the deleterious ecological impact of the release of organophosphorus pesticides have emerged as critical global issues. Previous research has shown the ability of electrochemistry to induce the precipitation of calcium phosphate from phosphorus-laden wastewater to recover the phosphorus. The current study presents a flow-through electrochemical system consisting of a column-shaped electrochemical reactor, a tubular stainless-steel (SS) cathode, and a titanium suboxides (TiSO) anode. This system simultaneously oxidizes tetrakis (hydroxymethyl) phosphonium sulfate (THPS) and recycles phosphates. The influence of current density, flow rate, and initial calcium ions concentration were examined under continuous flow operation. To enhance the electrochemical reactor's performance, we elevated the current density from 5 to 30 mA cm−2, which caused the phosphorus recovery efficiency to increase from 37% to 72% within 120 min, accompanied by an enhancement of the THPS mineralization efficiency from 57% to 90%. These improvements were likely due to the higher yield of reactive species chloride species (Cl•) formed at the TiSO anode and the higher local pH at the cathode. By investigating the formation of Cl• at the TiSO anode, we found that THPS mineralization exceeded 75% in the presence of NaCl at a current density of 20 mA cm−2. The demonstrated performance of the flow-through electrochemical system should enable the utilization of anodic oxidation-cathodic precipitation for the recovery of phosphorus from organophosphorus-contaminated wastewater.

Modulation of struvite composition in full-scale nutrient recovery system using source-separated urine.

Using urine collected from a public restroom at a highway rest stop in Northern California, a full-scale nutrient recovery system involving a two-part system consisting of urine distillation followed by the precipitation of struvite crystals was characterized. The study examined the effects of different operational parameters of the coupled ammonium distillation and struvite process (CADSP) on the composition of struvite crystals and the overall nutrient recovery rates. System inputs that were investigated included the feed:steam (F:S), alkalinity source, and urinary pH. Overall, the findings demonstrate that the composition of the struvite produced can be varied by adjusting the preceding distillation unit process. Low F:S distillation operations result in high ammonium distillation rates which coincided with increased formation of magnesium potassium phosphate (MPP) while higher F:S operations led to conditions favorable to magnesium ammonium phosphate (MAP) precipitation. Therefore, low energy distillation operations (high F:S) are more conducive to MAP formation and high phosphorus recovery rates while high energy operations (Iow F:S) are more conducive to MPP formation. Sodium-based alkalinity sources should also be avoided in instances of low ammonium concentrations in the struvite precipitation tank to minimize the co-precipitation of magnesium sodium phosphate (MSP) with MPP.

A new phosphate purification method for igneous weathering profiles.

The oxygen isotope composition of phosphate (δ18 OPO4 ) is widely employed for reconstructing paleotemperature and tracing biogeochemical phosphorus cycling. However, existing phosphate purification protocols do not work well for igneous rocks and igneous weathering profiles (IWPs). A reliable purification method is needed for measuring δ18 OPO4 in these materials. Our phosphate purification method includes two steps of cation exchange resin treatment separated by a step of calcium phosphate precipitation (R-Ca-R method). In addition, the silver phosphate precipitation in our procedure is featured by slow evaporation to crystallization until the appearance of ammonium nitrate or silver nitrate crystals. We evaluated our methods on weathered and pristine igneous rocks, phosphorite rocks, KH2 PO4 , and (NH4 )2 HPO4 solutions. Our purification method converted over 99.9% phosphate in solution to calcium phosphate, which can be easily decalcified by cation resin. The improved silver phosphate precipitation method produced high phosphate yields (97.1%-99.5%) and retained original δ18 OPO4 within analytical uncertainty (2σ = 0.6‰). We applied the purification and precipitation method on five igneous rocks and IWPs, and obtained δ18 OPO4 values ranging from 6.4‰ to 8.0‰. Duplicate phosphate extractions yielded δ18 OPO4 values differing by less than 0.3‰. We developed a new phosphate purification method that is applicable to phosphate extraction in igneous rocks and IWPs. We also proposed a reliable indicator for the termination of silver phosphate precipitation. Our method can achieve high phosphate yield and reproducible δ18 OPO4 value.

Lithium Extraction and Zeolite Synthesis via Mechanochemical Treatment of the Silicate Minerals Lepidolite, Spodumene, and Petalite

Lithium is in high demand: this is driven by current trends in e-mobility and results in increased global production and record prices for lithium ores and compounds. Pegmatite ores, in addition to brines, remain of particular interest because of their higher lithium content and lower geopolitical risks. In this work, we investigated lithium extraction via the mechanochemical treatment of the three most common lithium minerals: lepidolite, spodumene, and petalite. Indeed, we determine that the petalite crystal structure was much more suitable due to its less dense packing and the formation of cleavage planes along lithium sites, resulting in substantial lithium extraction of 84.9% and almost complete conversion to hydrosodalite after 120 min of ball milling in alkaline media. Further processing of the leach liquor includes desilication, the precipitation of lithium phosphate, and the conversion and crystallization of pure LiOH·H2O. Special attention was paid to a holistic approach entailing the generation of by-products, each of which has a specific intended application. The leaching residues were investigated by powder X-ray diffraction, Fourier transform infrared spectroscopy, N2 adsorption/desorption, and scanning electron microscopy. Moreover, hydrosodalite was found to have a high potential as an adsorbent for heavy metal ions which were studied separately using aqueous solutions containing Cu2+, Ni2+, Pb2+, and Zn2+.

Eco-friendly soil stabilization method using fish bone as cement material

The method of soil improvement by calcium phosphate precipitation is a novel, environmentally friendly, and non-toxic technique. Such technology provides advantages over ureolytic induced calcite precipitation (UICP), the most popular and widely used method in the field of geotechnical engineering. In this paper, an investigation of the consolidation of fine and coarse sand samples by enzyme induced calcium phosphate precipitation (EICPP) was carried out. Tuna bones were used as an alternative source of calcium and phosphorus ions, as one of the most popular fish species in Japan and the main source of food industry waste. Unconfined compressive strength (UCS) of the samples after 21 days of daily injection of the solution showed an increase in strength up to 6,05 MPa in fine and up to 4,3 MPa in coarse sand samples. X-ray powder diffraction (XRD), scanning electron microscope (SEM), and energy dispersive X-ray spectroscopy (SEM-EDS) analysis were performed to investigate the nature and type of deposition. Analyses confirmed that deposition is composed of brushite with needle-like crystals in the case of Toyoura sand and flower-like crystals in the case of Mikawa sand. SEM-EDS showed a presence of both, calcium, and phosphorus in the precipitate, indicating the presence of calcium phosphate compounds (CPCs). This study reveals that tuna bones are a rich source of calcium and phosphorus for EICPP, which results in a strengthening of silicate soil up to 3.4–6.05 MPa and is able to reduce ammonia emissions by 85.7 % - 97.5 % compared to UICP.

Solar distillation of human urine to recover non-potable water and metal phosphate mineral.

Human urine is a readily available nutrient source that can complement commercial fertilizer production, which relies on finite mineral resources and global supply chains. This study evaluated the effectiveness of a simplified solar distillation process for urine to recover phosphorus (P) and nitrogen for agricultural use and water for non-potable purposes. Synthetic fresh, synthetic hydrolyzed, real fresh, and real hydrolyzed urine were exposed to direct sunlight for 6 h in a simple distillation apparatus, which produced distillation bottoms and distillate. Metal phosphate precipitation in the distillation bottoms was evaluated to recover P. The non-potable water was recovered as distillate. Hydrolyzed urine recovered more metal phosphate solid in the distillation bottoms and had a higher conductivity in the distillate than fresh urine. Hydrolyzed urine also achieved greater distillate volume recovery than fresh urine. Hydrolyzed urine had a greater presence of UV-absorbing organics in the distillate than fresh urine and therefore produced a lower-quality product water. There was no significant correlation between the daily high air temperature and the volume of distillate recovered. This study provides a comprehensive data set on simplified solar distillation of human urine considering the fate of nutrients and water for different types of urine.

Recovery of lactose from simulated delactosed whey permeate by a low-temperature crystallization process

Delactosed whey permeate is the mother liquor/by-product of lactose manufacture, but it still contains around 20 wt% lactose. The high mineral content, stickiness, and hygroscopic behavior prevent further recovery of lactose in the manufacturing process. Therefore, its use is currently limited to low-value applications such as cattle feed, and more often it is seen as waste. This study investigates a new separation technique operating at sub-zero conditions. At low temperature, precipitation of calcium phosphate is expected to be reduced and the lower solubility at sub-zero temperature makes it possible to recover a large portion of the lactose. We found that lactose could be crystallized at sub-zero conditions. The crystals had a tomahawk morphology and an average size of 23 and 31 µm. In the first 24 h, the amount of calcium phosphate precipitated was limited, whereas the lactose concentration was already close to saturation. The overall rate of crystallization was increased compared with the crystals recovered from a pure lactose solution. Mutarotation was rate limiting in the pure system but it did not limit the crystallization of lactose from delactosed whey permeate. This resulted in faster crystallization; after 24 h the yield was 85%.

THE INFLUENCE OF SODIUM CARBOXYMETHYL CELLULOSE ON THE SEDIMENTATION BEHAVIOUR OF NICKEL PHOSPHATE PRECIPITATE AT VARYING TEMPERATURES

The sedimentation data of nickel phosphate precipitate formed with or without a modifier - sodium carboxymethyl cellulose (Na-CMC) biopolymer were studied under controlled conditions of temperature. The main objective was to access the influence of Na-CMC and temperature on On-set Sedimentation Rate (OSR) and Sedimentation Volume Ratio (SVR) of nickel phosphate. Na-CMC at different concentrations (200ppm - 2000ppm) was mixed with constant volume of disodium hydrogen phosphate solution in a graduating measuring cylinder. On mixing the resulting solution with constant volume of nickel chloride solution, a precipitate was formed, stirred for 1 min and placed in the sedimentation measurement device - PreSed Meter. The settling of the precipitate was monitored and recorded at different temperatures (30oC, 40oC and 50oC). Blank sedimentation (0ppm Na-CMC) was also run at various temperatures by adding 10ml of deionized water (instead of 10ml of Na-CMC solution). A plot of precipitate displacement per settling time established a logarithmic curve which flattened with time. Regression analyses of OSR (0.71 ≤ R2 ≥ 0.94) and SVR (0.51 ≤ R2 ≥ 0.93) indicated the dependence of sedimentation on concentration of Na-CMC thus implying chemical interaction between the chemical species.

The Effect of Full-Scale Exchange of Ca2+ with Co2+ Ions on the Crystal Structure and Phase Composition of CaHPO4·2H2O

The influence of ionic substitution in the Ca1−xCoxHPO4·nH2O compound was studied systematically for the first time. Among the fascinating features of these biomaterials is that they can be easily tailored for specific applications, for example, as biocements and bioceramics. Different molar concentrations of Co(NO3)2·6H2O, Ca(NO3)2·4H2O, and NaH2PO4·2H2O compounds were employed in determining the starting solutions utilized in the present study. The experimental findings reveal that, when the Co/Ca molar ratio is below 0.67 (BCo4), Co doping (the partial substitution of Ca by Co) takes place in brushite as a monophase. However, in the Co/Ca 0.67–1.5 molar ratio range (BCo4–BCo6), biphasic Co3(PO4)2·8H2O/CaHPO4·2H2O crystals start to precipitate. Full Ca replacement by Co results in the precipitation of nanostructured monoclinic cobalt phosphate and orthorhombic ammonium cobalt phosphate hydrate. Subsequent X-ray photoelectron spectroscopy (XPS), powdered X-ray diffraction (XRD), Fourier-transform infrared spectroscopy (FTIR), and scanning electron microscopy (SEM) analyses, along with thermogravimetric analysis (TGA), confirmed that the starting solution ratio of Co/Ca had a significant influence on the material’s microstructure, while tuning this ratio ultimately tailored the desired properties of the material for the intended applications.