Sulfamic Acid Research Articles

Optical studies of fluorescein dye doped sulphamic acid single crystal

Fluorsceine, a dye used in lasers and non-linear optics have been studied for its interaction with crystal matrix (Sulphamic acid). Present study reveals the effect of fluorescein dye on sulphamic acid single crystals that are grown by slow evaporation solution technique at room temperature. Cell Parameters and crystal structure of pure sulphamic and 0.1 mol % fluorescein dye doped crystals is confirmed by Single Crystal XRD. The crystal structure is found to be orthorhombic and space group Pbca. Slight increase is noticed in cell parameters. Vibrational bands are assigned by FTIR and Raman spectroscopy. UV–Vis spectroscopy is also studied to find out band gap energy which is found to increase from 5.13 eV to 5.2 eV due to dye doping in crystal. Decrease in cutoff wavelength confirms that the synthesized crystals are permissible material for electro-optic application.

Eco-friendly and efficient sulfamic acid functionalized MIL-53 (Al) nanocomposite for removal of hazardous pollutants from wastewater and catalytic synthesis of 3,4-dihydropyrimidinone pharmacological moiety

This study proposed the facile synthesis of sulfamic acid functionalized MIL-53 (Al) (SA@MIL-53(Al)) nanocomposite for dual-functional pollutant removal and catalytic synthesis. The composite was synthesized through a facile, straightforward, and one-step solvothermal process. Furthermore, different analysis techniques like XRD, SEM, XPS, FT-IR, and TGA were applied to examine the prepared composites' structure properties, confirming the successful preparation of functionalized frameworks. Several factors, including the initial concentration of pollutants, adsorbent dosage, pH, and pHpzc, have been established to optimize the suitable parameters for adsorption. 25 wt.% SA@MIL-53(Al) has the greatest adsorption capacities of 146.5, 97.7, and 35.5 mg g−1 for removing MB, CR dyes, and Pb (II), respectively. The rate-limiting steps were also discussed, and the experimental adsorption measurements obeyed the Langmuir and the pseudo-second-order kinetic models. Moreover, the fabricated composites were used as catalysts to produce 3,4-dihydropyrimidinone (3,4-DHP). 50 wt.% SA@MIL-53(Al) demonstrated the highest efficiency, nearly 92.0 %, with great durability and stability.

Cellulose modification using sulfamic acid for adsorption of methylene blue and lead ions

Cellulose modification using sulfamic acid for adsorption of methylene blue and lead ions

Synthesis and Reduction Processes of Silver Nanowires in a Silver(I) Sulfamate-Poly (Vinylpyrrolidone) Hydrothermal System.

Silver (Ag) nanowires, as an important one-dimensional (1D) nanomaterial, have garnered wide attention, owing to their applications in electronics, optoelectronics, sensors, and other fields. In this study, an alternative hydrothermal route was developed to synthesize Ag nanowires via modified reduction of Ag+. Silver sulfamate plays an important role in the formation of Ag nanowires via controlled release of free Ag+. Results of controlled experiments and characterizations such as UV-vis spectroscopy, FTIR, XPS, and 1H NMR revealed that sulfamic acid does not function as a reductant, supporting by the generation of free Ag+ instead of Ag nanostructures in hydrothermally treated silver sulfamate solution. The initial reduction of Ag+ was induced by the combination of poly (vinylpyrrolidone) (PVP) end group and degradation products. This phenomenon was supported by abundant free Ag+ in the mixed preheated silver sulfamatic and preheated PVP aqueous solutions, indicating a second and distinct Ag+ autocatalytic reduction. Thus, the roles of different reagents and Ag+ reduction must be studied for nanomaterial syntheses.

DIFFERENT APPROACHES TO AGAROSE SULFATION WITH SULFAMIC ACID

Sulfated polysaccharides are important promising biologically active substances with anticoagulant properties. Biological activity is affected by the method of preparation, as well as the type of the polysaccharide and its molecular structure. In this work, we have considered various methods for the synthesis of promising anticoagulants – polysaccharide sulfates using the example of obtaining agarose sulfate. We compared various sulfating agents: chlorosulfonic acid, sulfamic acid, with various activators, and a deep eutectic solvent mixture of sulfamic acid with urea (in the melt). It has been shown that when urea is used as an activator of the process of sulfation of agarose with sulfamic acid in 1,4-dioxane, agarose sulfate with a high sulfur content (up to 14.5 wt%) is formed, which is close to the use of chlorosulfonic acid as a sulfating agent (with the production of agarose sulfate with 15.0 wt% sulfur). The use of solid catalysts in the process of sulfation of agarose with sulfamic acid leads to the production of agarose sulfate with a sulfur content of up to 14.1 wt% (for a catalyst based on the oxidized carbonaceous material Sibunit-4®). Sulfation of agarose in a deep eutectic solvent – a mixture of sulfamic acid with urea – leads to the production of agarose sulfate with a sulfur content of up to 13.7 wt%. The resulting agarose sulfates were characterized by FTIR spectroscopy, X-ray diffraction, elemental analysis, atomic force microscopy and DFT.

Preparation of stable polyvinyl alcohol/polyurea hydrogel using oligomeric compounds containing urea-bonded

The aim of this research is the production of a biocompatible hydrogel film with high stability; the polymer should absorb enough water, and its structure should be preserved in water for a long time and not disintegrate. Polyvinyl alcohol (PVA) was chosen as the main polymeric base of the desired hydrogel. Oligomeric compounds with urea bonded containing active groups at two chain ends can react with the hydroxyl groups of the polymer and play the role of a cross-linker. Urea linkage oligomers (ULO) were prepared by reacting 2 mol of sulfamic acid, 3 mol of phosphorus, and 8 mol of urea in a molten state. The amount of PVA was kept constant, while the amount of ULO was different, the prepolymer solution was mold-dried at ambient temperature and subjected to a heat press. The gel behavior and characterization of the polymer films were investigated by FT-IR, NMR, SEM, ion chromatography, and XRD analyses, the data on the tensile strength and antibacterial properties of the samples are also reported. The production of a hybrid composite consisting of PVA and polyurea under the heat press has been confirmed; the ammonium phosphate, sulfate, nitrate, and melamine powder were produced in the layer of polymer structure. This innovative hybrid polymer with a network of urea bonds can be a favorable option for skin treatment applications due to the specific characteristic of urea known as keratolytic.

Thiocarbamoyl sulfamic acid‐derived mesoporous silica: a comprehensive study on selective adsorption of cobalt and lithium from spent lithium‐ion batteries

AbstractBACKGROUNDThe recycling of spent lithium‐ion batteries (LIBs) is crucial for resource conservation and environmental sustainability, particularly due to the valuable metals they contain, such as cobalt and lithium. This study focuses on developing an ion‐exchange method for cobalt recovery from waste LIB solutions, using a mesoporous silica derivative of carbamoyl sulfamic acid (PST‐SA) as the adsorbent.RESULTSThe batch method for adsorption experiments identified the most effective conditions: a pH of 8, 0.08 g PST‐SA, and a shaking time of 60 min, at room temperature. These experiments demonstrated a remarkable cobalt uptake capacity of 270.70 mg g−1, highlighting PST‐SA's exceptional adsorption capabilities. Additionally, thermodynamic studies revealed the adsorption process to be both endothermic and spontaneous, enhancing our understanding of its chemically reactive mechanisms.CONCLUSIONSThe practical application of PST‐SA, particularly when processing spent LIBs, showcases its real‐world utility. The efficient separation of cobaltous oxalate and lithium phosphate into pure forms emphasizes PST‐SA's potential in recycling and resource recovery. Given its cost‐effectiveness and strong adsorption capacity, PST‐SA stands out as an excellent solution for the removal of Co(II) from discarded LIBs, promoting sustainable material recovery practices. © 2024 Society of Chemical Industry (SCI).

Preparation of Co-Ni-Ce/TiC alloy coatings by double-pulse under a sulfamic acid system and a process mechanism study.

To enhance the protective ability of copper crystallizers and extend their service life, this study explores the use of double pulse co-deposition under a sulfamic acid system to create protective coatings such as Co-Ni. The hardness test and friction wear analysis compare Co-Ni, Co-Ni-Ce, and Co-Ni-Ce/TiC coatings, revealing that the Co-Ni-Ce/TiC coating exhibits the most outstanding protective performance. SEM and XRD techniques are employed to characterize the three protective coatings, demonstrating that the incorporation of rare-earth cerium and nanoparticles improves the coating morphology and modifies their crystalline phase structure. Furthermore, cyclic voltammetry tests on the plating solutions of the three protective coatings indicate that the addition of Ce3+ and nanoparticles influences the deposition potentials. The deposition of Co2+ and Ni2+ follows a two-step, two-electron process, while the deposition of Ce3+ follows a one-step, three-electron process. It is observed that the deposition of all three ions is irreversible. To gain further insights into the nucleation mechanism of Ce3+, a chronoamperometry test is conducted, revealing that the nucleation of Ce3+ is a transient process controlled by diffusion.

Coupled Stable Isotope Tracing and Sulfamic Acid Reduction (SIT-SAR) Method to Determine the Ammonia and Nitrite Oxidation Rates in Water and Sediments.

Herein, a method was developed to measure the ammonia oxidation rate (Ra) and the nitrite oxidation rate (Rn) of water and sediment samples using a coupled stable isotope tracing and sulfamic acid reduction (SIT-SAR) method. 15NH4+ was used as a tracer to determine the ammonia oxidation rates (Ra) by calculating the concentrations of produced 15NO2- and 15NO3- during incubation, while 15NO2- was used as a tracer to determine the nitrite oxidation rates (Rn) by calculating the increase of 15NO3- during incubation. 15NO2- was chemically reduced to 29N2 with 15 mmol·L-1 sulfamic acid (SA). 15NO3- was first reduced to 15NO2- with a zinc-cadmium reducing agent, and then 15NO2- was subsequently reduced to 29N2 with SA. The produced 29N2 was measured by a membrane inlet mass spectrometer (MIMS). Under optimized experimental conditions, this method provides a sensitive (detection limit: 0.5 μmol·L-1) and precise (relative standard deviation: 4.80% for 15NO2-, 3.82% for 15NO3-) approach to quantify the concentrations of 15NO2- (0.5-150 μmol·L-1) and 15NO3- (0.5-120 μmol·L-1) in water and sediment samples over a wide range of salinities (0-30‰) with excellent calibration curves (R2 ≥ 0.999). This method was a successful application to estuarine water and sediments along the salinity gradient. Overall, the SIT-SAR method provided a rapid, accurate, and cost-effective means to determine Ra and Rn simultaneously.

Observation of the Water-HNSO2 Complex.

Sulfamic acid (NH2SO3H, SFA) is supposed to play an important role in aerosol new particle formation (NPF) in the atmosphere, and its formation mainly arises from the SO3-NH3 reaction system in which weakly bonded donor-acceptor complexes such as SO3···NH3 and isomeric HNSO2···H2O have been proposed as the key intermediates. In this study, we reveal the first spectroscopic observation of HNSO2···H2O in two forms in a solid Ar matrix at 10 K. The major form consists of two intermolecular H bonds by forming a six-membered ring structure with a calculated dissociation energy of 7.6 kcal mol-1 at the CCSD(T)-F12a/aug-cc-pVTZ level of theory. The less stable form resembles SO3···H2O in containing a pure chalcogen bond (S···O) with a dissociation energy of 7.2 kcal mol-1. The characterization of HNSO2···H2O with matrix-isolation IR spectroscopy is supported by D- and 18O-isotope labeling and quantum chemical calculations.

Growth, characterization, and anti-bacterial activity of l-methionine supplemented with sulphamic acid single crystals

Abstract Sulphamic acid (SA) crystals supplemented with l-methionine (LM) were grown at moderate temperatures using a slow evaporation procedure. The powder XRD pattern showed that LM supplemented with SA (LMSA) crystals have an orthorhombic crystal structure. The FTIR studies confirmed the presence of various vibrational modes. Using a UV-Vis spectrometer, the transmittance of LMSA in the UV and visible range was observed, and the band gap of the LMSA was also calculated. The hardness value of LMSA was higher compared to that of pure SA. Photoluminescence emission studies of LMSA pointed out emissions at 491 and 542 nm, which were attributed to the transition from the 5D4 state to 7F6 and 7F5 ground, respectively. LMSA crystals were effective in killing pathogenic bacteria, according to the studies on their anti-bacterial activity.

Deprotonated sulfamic acid and its homodimers: Does sulfamic acid adopt zwitterion during cluster growth?

We present a joint experimental and computational study on the geometric and electronic structures of deprotonated sulfamic acid (SA) clusters [(SA)n–H]− (n = 1, 2) employing negative ion photoelectron spectroscopy and high-level ab initio calculations. The photoelectron spectra provide the vertical/adiabatic detachment energy (VDE/ADE) of the sulfamate anion (SM−) H2N●SO3− at 4.85 ± 0.05 and 4.58 ± 0.08 eV, respectively, and the VDE and ADE of the SM−●SA dimer at 6.41 ± 0.05 and 5.87 ± 0.08 eV, respectively. The significantly increased electron binding energies of the dimer confirm the enhanced electronic stability upon the addition of one SA molecule. The CCSD(T)-predicted VDEs/ADEs agree excellently with the experimental data, confirming the identified structures as the most stable ones. Two types of dimer isomers possessing different hydrogen bonding (HB) motifs are identified, corresponding to SM− binding to a zwitterionic SA (SM−●SAz) and a canonical SA (SM−●SAc), respectively. Two N–H⋯O HBs and one superior O–H⋯O HB are formed in the lowest-lying SM−●SAc, while SM−●SAz has three moderate N–H⋯O HBs, with the former being 4.71 kcal/mol more stable. Further theoretical analyses reveal that the binding strength advantage of SM−●SAc over SM−●SAz arises from its significant contributions of orbital interactions between fragments, illustrating that sulfamate strongly interacts with its parent SA acid and preferably chooses the canonical SA in the subsequent cluster formations. Given the prominent presence of SA, this study provides the first evidence that the canonical dimer model of sulfamic acid should exist as a superior configuration during cluster growth.

Inhibitory effects of 1-butylpyridin-1-ium bromide in 0.1 M sulphamic acid for mild steel

ABSTRACT In recent years, there has been a consistent development in the introduction of novel corrosion inhibitors due to their potential to reduce the dissolution of metal surfaces under various corrosive environments. The current study investigates the inhibitory effect of the surfactant 1-butylpyridin-1-ium bromide (BPB) on mild steel (MS) in 0.1 M sulphamic acid. The electrochemical impedance spectroscopy (EIS) and potentiodynamic polarisation (PDP) studies were used to analyse the inhibition investigations. In addition, atomic force microscopy (AFM), scanning electron microscopy (SEM) and contact angle (CA) measurements were also used to analyse the inhibition investigations. The PDP studies showed a maximum inhibition efficiency of 63.3% at 400 ppm concentration, demonstrating the inhibitor’s efficacy. The investigated compound was found to comply with the Temkin adsorption isotherm with an R 2 value of 0.99954. The results of PDP tests firmly suggest that the inhibitor is of mixed type. ΔG ads values of −9.659 kJ mol−1 suggested that the inhibitor adhered to the metal surface by physical adsorption. Based on the findings it appears that the molecules adhere to the surface of MS forming partial hydrophobic films that act as a barrier for the metal surface.

Microwave-Assisted Production of 5-Hydroxymethylfurfural from Fructose Using Sulfamic Acid as a Green Catalyst

The development of safe-by-design synthesis of valuable chemicals from biomass derivatives is a key step towards sustainable chemical transformations in both academia and industry. 5-Hydroxymethylfurfural (5-HMF) is a biomass derivative chemical of high commercial interest due to its wide range of chemical and biofuel applications. In this scenario, the present work contributes to a methodology for producing 5-hydroxymethylfurfural (5-HMF) through fructose dehydration reaction under microwave irradiation. The proposed protocol uses a simple sodium chloride–saturated aqueous-i-PrOH biphasic system and catalysis of sulfamic acid, a low-cost solid Brønsted–Lowry inorganic acid, which presents pivotal features of a sustainable catalyst. A 23 full factorial design was applied to achieve the highest conversion and 5-HMF yield, allowing the identification of the main factors involved in the process. Under the optimized conditions, fructose at the concentration of 120 g L−1 was converted with 91.15 ± 6.98% after 20 min at 180 °C, using 10 mol% of catalyst. 5-HMF was produced in 80.34 ± 8.41% yield and 73.20 ± 8.23% selectivity. Thus, the present contribution discloses a new optimized methodology for converting the biomass derivative fructose to 5-hydroxymethylfurfural (5-HMF).

Eco-Friendly Piper cubeba Official Extract Corrosion Inhibition of C-Steel in 1 M Sulfamic Acid.

This work offers a high-performing, environmentally friendly corrosion inhibitor for carbon steel in 1 M sulfamic acid (H2NSO3H). Potentiodynamic polarization and electrochemical impedance spectroscopy were used to evaluate the anticorrosion properties of Pipper cubeba official extract (P.cubebaOE) for carbon steel in 1 M H2NSO3H at 25 to 45 °C. At a temperature of 45 °C, the P.cubebaOE reached a maximum corrosion inhibition efficiency of 96%. P.cubebaOE was also subjected to Fourier transform infrared spectroscopy in order to ascertain its primary chemical composition. Additionally, the behavior of P.cubebaOE in terms of corrosion inhibition on carbon steel was examined at the microscopic level using scanning electron microscopy. The findings demonstrate that P.cubebaOE's adsorption type on carbon steel conforms to the Langmuir adsorption isotherm model. Based on the adsorption isotherm model, the free energy was estimated to be approximately -20.0 kJ/mol, suggesting that P.cubebaOE is physically adsorbing on the surface of carbon steel. The results of the density functional theory and molecular dynamics simulations show that P.cubebaOE exhibits excellent inhibition performance on carbon steel in H2NSO3H solution and are consistent with the electrochemical experimental results. This work offers significant information on the development of environmentally friendly corrosion inhibitors for carbon steel.

New PFASs Identified in AFFF Impacted Groundwater by Passive Sampling and Nontarget Analysis.

Monitoring contamination from per- and polyfluoroalkyl substances (PFASs) in water systems impacted by aqueous film-forming foams (AFFFs) typically addresses a few known PFAS groups. Given the diversity of PFASs present in AFFFs, current analytical approaches do not comprehensively address the range of PFASs present in these systems. A suspect-screening and nontarget analysis (NTA) approach was developed and applied to identify novel PFASs in groundwater samples contaminated from historic AFFF use. A total of 88 PFASs were identified in both passive samplers and grab samples, and these were dominated by sulfonate derivatives and sulfonamide-derived precursors. Several ultrashort-chain (USC) PFASs (≤C3) were detected, 11 reported for the first time in Australian groundwater. Several transformation products were identified, including perfluoroalkane sulfonamides (FASAs) and perfluoroalkane sulfinates (PFASis). Two new PFASs were reported (((perfluorohexyl)sulfonyl)sulfamic acid; m/z 477.9068 and (E)-1,1,2,2,3,3,4,5,6,7,8,8,8-tridecafluorooct-6-ene-1-sulfonic acid; m/z 424.9482). This study highlights that several PFASs are overlooked using standard target analysis, and therefore, the potential risk from all PFASs present is likely to be underestimated.

Sequential separation of uranium and plutonium in urine sample using UTEVA resin

This article describes the process of separating uranium (U) and plutonium (Pu) sequentially in urine samples through the use of UTEVA resin. The manuscript optimizes several parameters, including the concentration of nitric acid in the loading solution, the repeatability of results across the multiple uses of the column, and most significantly, implementation of distinctive eluting agents. These eluting agents encompass a combination of 0.002M sulfamic acid and 0.002M ascorbic acid in 2M HNO3, as well as 1.5M NH2OH, HCl (hydroxylamine hydrochloride) in 2M HCl, all aimed at enhancing recovery percentages. The selection of 0.002M sulfamic acid and 0.002M ascorbic acid in 2M HNO3 have been observed to be exceptionally effective in achieving higher radiochemical recoveries. The standardized methodology presented here is characterized by its swiftness and robustness, particularly when compared to the traditional ion exchange method and numerous other published works related to extraction chromatography materials. Radiochemical recoveries for spiked urine samples of 232U and 242Pu consistently fall within the range of 93%–100% and 71%–96%, demonstrating an average recovery percentage with a standard deviation of 96.2% ±2.4% and 82.4% ±10.1%, respectively.

3-(Sulfamic acid)-propyltriethoxysilane on biochar nanoparticles as a practical, biocompatible, recyclable and chemoselective nanocatalyst in organic reactions.

Recyclable and inexpensive catalysts, waste regeneration, use of available and safe solvents are important principles of green chemistry. Therefore, in this project, biochar nanoparticles (BNPs) were synthesized by the pyrolysis method from chicken manure. Then, 3-(sulfamic acid)-propyltriethoxysilane (SAPES) was immobilized on the surface of BNPs (SAPES@BNPs). The prepared catalyst (SAPES@BNPs) was used as a commercial, practical, biocompatible and reusable catalyst in the selective oxidation of sulfides to sulfoxides. Further, the catalytic application of SAPES@BNPs was explored in the multicomponent synthesis of tetrahydrobenzo[b]pyrans under mild and green conditions. BNPs were characterized using SEM, TGA and XRD techniques. SAPES@BNPs were characterized using SEM, FT-IR spectroscopy, WDX, EDS, TGA, and XRD techniques. Particle size distribution was obtained by histogram graph. SAPES@BNPs can be recovered and reused several times. The purity of the products was studied using NMR spectroscopy.

Azide-free cyclization reaction access to 4-aryl-NH-1,2,3-triazoles: P-toluenesulfonyl hydrazide and sulfamic acid as nitrogen sources.

An iodine-mediated cyclization has been developed to 4-aryl-NH-1,2,3-triazoles, with p-toluenesulfonyl hydrazide and sulfamic acid used as nitrogen sources. Sulfamic acid plays a crucial role in this reaction by both acting as a substrate and providing an acidic environment. This reaction offers a metal- and azide-free strategy to access NH-1,2,3-triazoles.

Synthesis of novel fatty acid 3,4-dihydropyrimidin-2-(1H)-one and antitumoral activity against breast and gastric cancer cells.

Monastrol is the best-known small compound from the dihydropyrimidinones/thiones (DHPMs) heterocycle family, a cell-permeable molecule recognized as an inhibitor of mitotic kinesin Eg5, that is over-expressed in tumor cells and is a very promising target for the development of new drugs for cancer. The lipophilic properties of the DHPMs have been demonstrated to be of pivotal importance in the design of new molecules. This work describes the synthesis and antitumoral activity of novel C5-substituted fatty-DHPMs against breast and gastric cancer cell lines. The compounds were synthesized via Biginelli multicomponent reaction from oleyl β-ketoester in good yields (40-72%) using a simple approach catalyzed by nontoxic and free-metal sulfamic acid. Among the compounds tested, the compound 10c, derived from 3-hydroxybenzaldehyde and urea, exhibited 77% cellular viability to normal cells (C2C12) and was selected to be evaluated against tumoral breast (MCF-7) and gastric (AGS) cell lines. The results obtained afforded an IC50 of breast cancer cells of 2.3 μM, qualifying the molecule as the most potent, and making it a promising compound for future experiments in vivo.