Aqueous Acid Research Articles

Transient Covalent Polymers through Carbodiimide-Driven Assembly.

Biochemical systems make use of out-of-equilibrium polymers generated under kinetic control. Inspired by these systems, many abiotic supramolecular polymers driven by chemical fuel reactions have been reported. Conversely, polymers based on transient covalent bonds have received little attention, even though they have the potential to complement supramolecular systems by generating transient structures based on stronger bonds and by offering a straightforward tuning of reaction kinetics. In this study, we show that simple aqueous dicarboxylic acids give poly(anhydrides) when treated with the carbodiimide EDC. Transient covalent polymers with molecular weights exceeding 15,000 are generated which then decompose over the course of hours to weeks. Disassembly kinetics can be controlled using simple substituent effects in the monomer design. The impact of solvent polarity, carbodiimide concentration, temperature, pyridine concentration, and monomer concentration on polymer properties and lifetimes has been investigated. The results reveal substantial control over polymer assembly and disassembly kinetics, highlighting the potential for fine-tuned kinetic control in nonequilibrium polymerization systems.

The influence of dissolved molecular oxygen on the corrosion of metals in aqueous acid solutions. Review

The influence of dissolved molecular oxygen on the corrosion of metals in aqueous acid solutions. Review

Field evaluations of biodegradable boric acid hydrogel baits for the control of Argentine ants: Promising results in vineyards and citrus orchards

Argentine ants are a major pest in California. In this study, a biodegradable calcium alginate hydrogel with an aqueous boric acid bait was tested against Argentine ant populations in a citrus orchard and a vineyard. A new continuous method was developed to produce large quantities of hydrogel bait for the field test. Foraging activity levels of ants were compared between baited and untreated zones. For both study sites, four to five monthly bait applications throughout summer provided a greater than 80% reduction in ant activity. Based on spatial analyses by distance indices, the baited areas were characterized by gaps (areas with lower ant counts) and the untreated control zones were characterized by patches (areas with higher ant counts). This indicated area-wide suppression of Argentine ants. For the citrus orchard, post-baiting panel trap monitoring showed reductions of both ants and Asian citrus psyllid in the baited zone compared to the control. For the vineyard, mid-season soil analyses indicated that the impact of boric acid baiting on soil boron concentration was negligible. In sum, the calcium alginate hydrogel bait with boric acid as an active ingredient may provide a promising solution for Argentine ant baiting.

Uptake and coordination behaviour of uranyl on functionalised silica

The safe decommissioning of nuclear reactors is a complex process, requiring a range of technological options for it to be done effectively. It has become more important in recent years, with the substantial number of reactors entering the decommissioning phase. This paper details the use of functionalised silica for the recovery of uranium from aqueous hydrochloric acid solutions, a potential agent for the treatment of steel reactor components during nuclear reactor decommissioning. Silica functionalised with either phosphonic acid, bistriazine, or bistriazinylbipyridine ligands was shown to extract uranium, with the commercially available phosphonic acid functionality being the most effective. Extractions of 100 % were observed at [H+] ≤ 0.24 M, further the phosphonic acid functionality also had the highest loading capacity. Increasing [H+] has a suppressive effect on uranyl recovery, which was more pronounced for the in-house synthesized silica, and was attributed to protonation of the extracting moiety. Extended x-ray absorption fine structure spectroscopy was also used to determine the uranium coordination environments on the functionalised silica, and gain insights into the extraction mechanism. The uranyl cation was bound by two phosphonic acid groups, two bis-triazine groups, and one bistriazinylbipyridine group, respectively on each respective extractant. Uranyl was found to be penta-coordinate in the equatorial plane for all systems, with oxygen and/or chloride always present in the first coordination sphere. Evaluation of the mechanism indicated that uranyl must be loading onto the phosphonic acid functionality via multiple mechanisms, to both the phosphonic acid and silica related surface groups, although preferential binding of uranyl to the phosphonic acid groups was observed.

Quantification and analyses of seven tyrosine kinase inhibitors targeting hepatocellular carcinoma in human plasma by QuEChERS and UPLC-MS/MS

Tyrosine kinase inhibitors (TKIs) are commonly used to treat various cancers. Literature suggests that the blood concentration of TKIs strongly correlates with their efficacy and adverse effects. Therefore, establishing a Therapeutic Drug Monitoring (TDM) methodology for TKI drugs is crucial to improving their clinical efficacy and minimizing the treatment-related adverse effects. However, quantifying their concentrations in the plasma using existing methods to avoid potential toxicity is challenging. Herein, seven TKIs, namely sorafenib tosylate, axitinib, erlotinib, cediranib, brivanib, linifanib, and golvatinib, were successfully analyzed in human plasma by following a quick, easy, cheap, effective, rugged, and safe (QuEChERS) pretreatment method combined with ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Briefly, biological samples were extracted using 1 mL of methanol, followed by the sequential addition of 250 mg of anhydrous magnesium sulfate and 25 mg of N-propylethylenediamine (PSA) for salinization and purification by adsorption, respectively. In this study, dovitinib was used as the internal standard. The seven TKIs were detected by the gradient elution method for 4 min in the positive ion electrospray mode. The mobile phase comprised methanol (phase A) and 0.1 % aqueous formic acid solution (phase B) on the Agilent Zorbax RRHD Stablebond Aq, (2.1 × 50 mm; 1.8 μm). Brivanib, linifanib, axitinib, sorafenib tosylate, and golvatinib exhibited good linearity in the range of 5–500 ng/mL, and erlotinib and cediranib exhibited good linearity in the range of 10–1000 ng/mL, with linear correlation coefficients (R2) ≥ 0.99. The limits of detection and quantification were 0.60–0.18 ng/mL and 5–10 ng/mL, respectively. The intraday and interday accuracy values ranged from −6.12 % to 7.31 %, with a precision (RSD) of ≤ 10.57 %. The method was rapid, accurate, specific, simple, reproducible, and suitable for the quantitative determination of the seven TKIs in human plasma.

Laser‐Induced Nucleation of Acetaminophen through the Addition of Insoluble Impurities and Acidic Polymers

AbstractThis study investigates the crystallization of acetaminophen (ACET) in ultrapure water and a 10 wt.% aqueous polyacrylic acid (PAA) solution using non‐photochemical laser‐induced nucleation (NPLIN) for the first time. Using a 532 nm nanosecond laser, two distinct crystal morphologies—rhombic and tetragonal plate‐like—are formed in both solvents after adding impurities. Notably, the PAA solution showed a reduced number of crystals and slower growth rates compared to ultrapure water, suggesting that the acidic polymer modulates crystal growth. Interestingly, crystals are not induced by the laser without impurities. However, impurities like copper phthalocyanine (CuPc) or boron carbide (CB4) enabled successful NPLIN, with CB4 showing higher nucleation efficiency than CuPc. The study also explores how laser power affects nucleation probability and identifies potential laser energy thresholds. Experimental data on ACET crystal sizes over time are fitted to derived equations, which accurately represented trends and predicted results. The nanoparticle heating mechanism and the role of acidic polymers in affecting nucleation probability and growth rate are discussed, along with potential mechanisms for changes in crystal morphology.

Different formation pathways of nitrogen-containing organic compounds in aerosols and fog water in northern China

Abstract. While aqueous-phase processing is known to contribute to the formation of nitrogen-containing organic compounds (NOCs), the specific pathways involved remain poorly understood. In this study, we aimed to characterize the NOCs present in both pre-fog aerosols and fog water collected at a suburban site in northern China. Fourier-transform ion cyclotron resonance mass spectrometry was utilized to analyze the molecular composition of NOCs in both negative and positive modes of electrospray ionization (ESI− and ESI+). In both pre-fog aerosols and fog water samples, NOCs constituted a significant portion, accounting for over 60 % of all assigned formulas in ESI− and more than 80 % in ESI+. By comparing the molecular composition of NOCs originating from biomass burning, coal combustion, and vehicle emissions, we identified that 72.3 % of NOCs in pre-fog aerosols were attributed to primary anthropogenic sources (pNOCs), while the remaining NOCs were categorized as secondary NOCs formed within the aerosols (saNOCs). Unique NOCs found in fog water were classified as secondary NOCs formed within the fog water (sfNOCs). Through a comprehensive “precursor–product pair” screening involving 39 reaction pathways, we observed that the nitration reaction, the amine pathway, and the intramolecular N-heterocycle pathway of NH3 addition reactions contributed 43.6 %, 22.1 %, and 11.6 % of saNOCs, respectively. In contrast, these pathways contributed 26.8 %, 28.4 %, and 29.7 % of sfNOCs, respectively. This disparity in formation pathways is likely influenced by the diverse precursors, the aqueous acidity, and the gas-phase species partitioning. Correspondingly, saNOCs were found to contain a higher abundance of carbohydrate-like and highly oxygenated compounds with two nitrogen atoms compared to pNOCs. Conversely, sfNOCs exhibited a higher content of lipid-like compounds with fewer oxygen atoms. These results underscore the distinct secondary processes contributing to the diversity of NOCs in aerosols and fog water, which may lead to their different climate effects.

Quantitation of thiorphan in human plasma using LC-MS/MS and its application to a bioequivalence study

Racecadotril, an anti-secretory medication, has been used as an adjuvant in an oral rehydration therapy for children experiencing severe diarrhea. Racecadotril is quickly converted to thiorphan, an active metabolite, after oral treatment, which mediates all subsequent activities. An efficient and rapid liquid chromatography-tandem mass spectrometry method was developed and fully validated to measure thiorphan in human plasma, using thiorphan-d7 as an internal standard. The extraction method used was protein precipitation while chromatographic separation was achieved using InertSil CN-3 (50 × 2.1 mm, 5 µm column). The assay was linear over the concentration range of 1–200 ng/ml with correlation coefficients of ≥0.9991. The intra- and inter-day precisions were less than 10.0 % for all concentrations investigated. 0.02 % aqueous formic acid and methanol (30:70 v: v) were used as mobile phases, with an analysis time of less than 1 min. This method proved stable under several conditions. The developed method worked well in a three-period pharmacokinetic bioequivalence study after a single oral administration of 100 mg racecadotril to 15 healthy Jordanian volunteers under fasting conditions.

Experimental study of hollow fiber membrane contactor process using aqueous amino acid salt-based absorbents for efficient CO2 capture

Gas–liquid membrane contactors are a promising alternative to packed columns that suffer from channeling, bubble formation, and flooding problems. In this study, potassium serinate + piperazine (PSZ) and potassium alaninate + piperazine (PAZ), which are amino acid salts with good CO2 absorption performances and high surface tensions, are investigated to determine the effects of the operating parameters on the CO2 removal efficiency, CO2 absorption flux, CO2 loading, and overall mass-transfer coefficient in the membrane contactor process. The experimental results demonstrate that the 2.5 M PSZ and 2.5 M PAZ absorbents outperform 2.5 M monoethanolamine (MEA) under various operating conditions, including the gas flow rate, liquid flow rate, CO2 concentration, and CO2-loaded absorbent. Based on these results, an expression for predicting the CO2 loading from the pH is proposed. The amount of cross-over confirmed that amino acids with high surface tension have better resistance to membrane wetting than 2.5 M MEA. In addition, empirical correlation expressions were established from the results of several operating parameters. The absolute average deviation (AAD) values were 6.50 %, 2.95 %, and 4.71 % for 2.5 M MEA, 2.5 M PSZ, and 2.5 M PAZ, respectively, suggesting good agreement between the theoretical and experimental results.

Fully upgrade bamboo biomass into three multifunctional products through biphasic γ-valerolactone and aqueous phosphoric acid pretreatment

In this manuscript, three components of lignocellulosic biomass were obtained by deconstructing bamboo with γ-valerolactone-H2O biphasic system, and the delignification rate of 80.92 % was achieved at 120 °C for 90 min. Lignin nanospheres with diameters ranging from 75 nm to 2 um could be customized by varying the self-assembly rate. Furthermore, the lignin nanospheres-poly(vinyl alcohol) film was prepared by cross-linking lignin nanospheres and poly(vinyl alcohol), which can obtain 90 % ultraviolet absorption capacity, while the light transmittance in non-ultraviolet band was almost unchanged. At the same time, due to the strong hydrogen formation between lignin nanospheres and poly(vinyl alcohol) bond network, the tensile properties of the composite film were also improved by 30 %. Besides, the high specific surface area of biomass-derived porous biochar (2056 m2/g) can be obtained after carbonization of solid residues at 850 °C for 2 h, which was almost 8 times the specific surface area of the direct biomass carbonization due to the removal of lignin and hemicellulose. biomass-derived porous biochar can be used as an adsorbent, with a CO2 capture capacity of 4.5 mmol g−1 at normal temperature (25 °C, 1 bar). The filtrate after the reaction contained a large amount of hemicellulose oligomers, which can be reacted with dichloromethane at 170 °C for 1 h to obtain the furfural yield of 74 %. In summary, the proposed biorefinery scheme achieves a full-component upgrade of lignocellulose and can be further applied in various downstream fields.

Fabrication of nickel aluminate based electrochemical sensor for dopamine detection

Nickel aluminate nanoparticles (NiAl2O4 NPs) spinel structure is synthesized via a simple solution combustion method using aqueous nickel nitrate, aluminum nitrate and citric acid. The crystal structure and microstructure of the prepared NiAl2O4 NPs are confirmed by powder X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), Fourier transform infrared (FTIR) spectrum, scanning and transmission electron microscopy (SEM/TEM). The characterized NiAl2O4 NPs are applied on a glassy carbon electrode (GCE) to design electrochemical sensor for the detection of dopamine (DA) using cyclic voltammograms (CV) and differential pulse anodic stripping voltammograms. The proposed electrochemical sensor exhibits excellent sensing activity with a low detection limit of 1.78 μM and applicable for a wide linear concentration range of 10 μM–140 μM. Further, the proposed electrode exhibits well resolved differential pulse voltammogram for the dopamine in presence of interfering uric acid and ascorbic acid.

High energy supercapattery of polyaniline/cupric oxide/stannic oxide nanocomposite

The effects of different aqueous acid electrolytes in imparting different features of energy storage to the nanocomposite of PANI50 %: CuO41.7 %: SnO28.3 % (PCS) are studied with three different electrolytes 1 M H2SO4 (SA), 1 M H2SO4 + 1 M CH3SO3H (1:1) (SA + MSA) and acidified by-product (ABP). In the presence of SA, SA + MSA and ABP, the PCS produces, high energy density (E); high E & cyclic stability; and high E & rate capability, respectively. The maximum energy characters are achieved in the presence of SA + MSA. They are specific capacity (Q) of 301.6 C g−1, E of 50.26 W h kg−1 and power density (P) of 1.200 kW kg−1 at 1 A g−1. In the presence of SA + MSA the PCS nanocomposite exhibits 55.56 % retention of its initial Q up to 12500 cycles at 0.4 V s−1. This achieved high E is similar with E of Ni–Cd batteries. The use of by-product as electrolyte for supercapattery makes the process a green process.

Improved catalytic performance of Ru catalysts via CO2-assisted one-pot synthesis strategy for aqueous levulinic acid hydrogenation

Fabrication of metal/porous carbon catalysts with high catalytic activity and stability is highly desirable but challenging because the metal nanoparticles in these catalysts cannot have both high exposure and strong interaction with carbon support. Here, for the first time, a facile CO2-assisted one-pot pyrolysis (CAOP) strategy was developed to in situ liberate the inaccessible Ru sites without obviously affecting the size of Ru nanoparticles. The Ru@CN-700-80 prepared with the assistance of CO2 exhibits a remarkable improvement in catalytic activity for levulinic acid hydrogenation compared with that without CO2 during pyrolysis, giving a TOF of 28449 h−1 under mild conditions, which is superior to the reported Ru-based catalysts. Additionally, the Ru@CN-700-80 also demonstrates an excellent stability without activity loss after 10 cycles. We anticipate that this CAOP strategy addresses a crucial issue that currently plagues the design of metal/porous carbon catalyst with high catalytic performance applied in energy and environmental fields.

Investigation of electrostatic interactions in laponite-polyacrylic acid nanocomposites

Nanocomposites provides a unique opportunity to enhance thermal, mechanical, and waterproof resistance properties of polymer. The effectiveness of these enhancements typically depends on the optimal dispersion and interaction of nanofillers within the polymer matrix. The primary objective of this study is to provide direct chemical evidence for electrostatic interactions between Laponite nanofiller and polyacrylic acid. Samples were prepared by mixing Laponite dispersion and aqueous polyacrylic acid (PAA) that were adjusted to various pH conditions. We observed, an IR peak shift in the carbonyl peak of PAA and Si–O peak of Laponite to lower wave number in nanocomposite, with the maximum shift at pH 7. UV–Vis results also showed a hypsochromic shift in the carbonyl peak of PAA due to the interaction with Laponite. The extent of peak shift in IR, and UV–Vis region for the PAA-Laponite dispersion was found to be influenced by the molar mass of PAA used in the formulation of Laponite-PAA nanocomposite and pH of the medium. These results along with zeta potential measurements strongly suggest that electrostatic forces are in play between deprotonated PAA and the positively charged rim of Laponite in promoting electrostatic interactions between Laponite and PAA. The findings of the study can have a strong bearing on the design of next generation high performance coatings, sealants, and adhesives.

Aqueous phosphonic acid treatments of aluminium: Effect of oxide dissolution and re-oxidation on adsorbate formation

Functionalization of Aluminium surfaces by phosphonic acid (PA) treatments is of key industrial importance. This work discloses the effect of PA molecular design on the performance of aqueous PA surface treatments of Aluminium under acidic conditions. Comprehensive XPS and ToF-SIMS analyses show that the “final” nature of the PA adsorbate layer is not only governed by competing in-situ PA adsorption and oxide dissolution processes, but also by modifications of the transient state of the adsorbate layer during subsequent water rinsing in air. Low-soluble organo-metallic-phosphonic (OMP) deposits formed by complexation with Al3+ ions in solution are largely removed upon water-rinsing; only few physisorbed OMP complexes are converted trans-situ to a chemisorbed state. The in-situ oxide dissolution and ex-situ re-oxidation processes are suppressed with increasing steric size of the PA molecule. Moreover, intermolecular phenyl π-π interactions can act as a driving force to increase the surface density of the PA adsorbate layer in-situ, which also effectively suppresses in-situ oxide dissolution and ex-situ re-oxidation. The findings provide profound insights on how PA molecular designs can be tuned to tailor the chemistry and morphology of PA-adsorbate layers, which may contribute to advance surface treatment strategies of Al surfaces for a wealth of applications.

Facilitating the fabrication of diverse bio-based nanomaterials from bamboo using one-pot hydrated deep eutectic solvent pretreatment

The conversion of biomass feedstocks into bio-based nanomaterials was made easier with hydrated DES (HDES) pretreatment, which can boost the value-added applications of lignocellulosic biomass. In this study, two types of HDESs were initially prepared by 3-Chloro-2-hydroxypropyltrimethyl ammonium chloride (CHPTAC) with formic acid (FA) and acetic acid (AA), respectively. We achieved rapid conversion of bamboo feedstock into bio-based nanomaterials (including lignin nanoparticles, LNPs; lignin-containing cellulose nanofibers, LCNFs) through one-pot microwave-assisted HDES pretreatment coupled with robust nanofabrication strategies. The findings demonstrated that an impressive delignification ratio of 92.10 % and a cellulose retention ratio of 92.95 % were achieved under the optimal DES pretreatment conditions (120 °C, 20 min). The fractionated lignin fractions were effortlessly self-assembled into dispersed, uniformly shaped circular LNPs (<100 nm) using a novel proposed strategy, which was successfully applied to stabilizing oil-in-water (O/W) Pickering emulsions. To produce LCNFs, we conducted functionalization of cellulose-rich residue in aqueous citric acid followed by simple ultrasonic treatment. Compared to the control LCNF, the LCNF-based self-assembly films exhibited significantly improved mechanical properties and hydrophobicity (water contact angle 106.26°). In short, the proposed HDES pretreatment combined with robust nanofabrication strategies will broaden the fractionation and fabrication of bio-based nanomaterials, enhancing their potential in promising fields.

A simple and sensitive ultra-high performance liquid chromatography tandem mass spectrometry method for the quantitative analysis of VX-548 in monkey plasma: Method validation and application to pharmacokinetic study.

VX-548 is an orally active and highly selective NaV 1.8 inhibitor that is undergoing development for the treatment of acute pain. The aim of this study was to develop a liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the measurement of VX-548 in monkey plasma. VX-548 was extracted from the plasma using acetonitrile-mediated protein precipitation. The quantitative analysis was performed on a Thermo Vantage TSQ mass spectrometer with ibrutinib as an internal standard. Chromatography was performed on a Waters ACQUITY UPLC BEH C18 column with 0.1% aqueous formic acid and acetonitrile as mobile phase. The precursor-to-product ion transitions were m/z 474.2 > 165.0 and m/z 441.2 > 138.1 for VX-548 and internal standard, respectively. This developed method was successfully validated in the concentration range of 1-1000 ng/mL. The calibration curve showed excellent linearity with a correlation coefficient of >0.999. The precision expressed as relative standard deviation (RSD) was <8.4%, whereas the accuracy denoted as relative error (RE) ranged from -5.0% to 9.1%. The mean recovery was >84%. VX-548 was stable in monkey plasma after storage under certain conditions. The validated method was successfully applied to the pharmacokinetic study of VX-548 in monkey plasma after single oral (2 mg/kg) and intravenous (1 mg/kg) administrations.

Peptidomics- inspired discovery and activity evaluation of antioxidant peptides in multiple strains mixed fermentation of Porphyra yezoensis

This study investigated the production of antioxidant peptides from Porphyra yezoensis through fermentation with three strains of microorganisms: Lactiplantibacillus plantarum L13, Bacillus amyloliquefaciens MMB-02, and Saccharomyces cerevisiae A8. The crude peptides were extracted by aqueous acid precipitation and purified by Sephadex G-25 gel column to produce highly active antioxidant components with molecular weight of <4000 Da. The LC-MS/MS result revealed that the fermentation group contained more hydrophobic amino acids and oligopeptides, which were mainly originated from phycobiliproteins and algal blue proteins. Finally, the antioxidant activity of Porphyra yezoensis was determined with DPPH· and ABTS· scavenging rates of 54.87% and 57.39%, respectively. The ferric ion-reducing power (FRAP) and enzyme activities of SOD and CAT were significantly higher than those of the control group. This study provides a scientific foundation for the deep processing of striped seaweed and contributes to the theoretical understanding of synthetic antioxidant substitutes.

Evaluation of a low-cost staining method for improved visualization of sweet potato whitefly (Bemisia tabaci) eggs on multiple crop plant species

BackgroundThe sweet potato whitefly (Bemisia tabaci) is a globally important insect pest that damages crops through direct feeding and by transmitting viruses. Current B. tabaci management revolves around the use of insecticides, which are economically and environmentally costly. Host plant resistance is a sustainable option to reduce the impact of whiteflies, but progress in deploying resistance in crops has been slow. A major obstacle is the high cost and low throughput of screening plants for B. tabaci resistance. Oviposition rate is a popular metric for host plant resistance to B. tabaci because it does not require tracking insect development through the entire life cycle, but accurate quantification is still limited by difficulties in observing B. tabaci eggs, which are microscopic and translucent. The goal of our study was to improve quantification of B. tabaci eggs on several important crop species: cassava, cowpea, melon, sweet potato and tomato.ResultsWe tested a selective staining process originally developed for leafhopper eggs: submerging the leaves in McBryde’s stain (acetic acid, ethanol, 0.2% aqueous acid Fuchsin, water; 20:19:2:1) for three days, followed by clearing under heat and pressure for 15 min in clearing solution (LGW; lactic acid, glycerol, water; 17:20:23). With a less experienced individual counting the eggs, B. tabaci egg counts increased after staining across all five crops. With a more experienced counter, egg counts increased after staining on melons, tomatoes, and cowpeas. For all five crops, there was significantly greater agreement on egg counts across the two counting individuals after the staining process. The staining method worked particularly well on melon, where egg counts universally increased after staining for both counting individuals.ConclusionsSelective staining aids visualization of B. tabaci eggs across multiple crop plants, particularly species where leaf morphological features obscure eggs, such as melons and tomatoes. This method is broadly applicable to research questions requiring accurate quantification of B. tabaci eggs, including phenotyping for B. tabaci resistance.

A robust hydrothermal synthesis method of NH4Zr2(PO4)3, a precursor for HZr2(PO4)3 proton conductor

Hydrogen zirconium phosphate (HZP) is a ceramic material with the formula HZr2(PO4)3 that can potentially offer anhydrous protonic conductivity, with thermostability for the intrinsic protons up to 650 °C, and good chemical stability in aqueous environments or acid gases. Despite the attraction of these features for electrolyte applications, such as gas separation, fuel cells or electrolysers, work on this material remains in its infancy. A possible reason for this lack of attention may be related to the complexity to obtain the HZP material as a pure phase. For this reason, the current article examines a new hydrothermal synthesis method to produce the ammonium precursor, NH4Zr2(PO4)3, in its phase pure form, and consequently a refined overall route to produce the desired HZP target material. In the synthesis of the ammonium precursor, we underscore the precise control of reaction conditions that are necessary to obtain the pure NH4Zr2(PO4)3 material, both in its cubic and hexagonal structural polymorphs. For reaction times of 10 h, the cubic phase is obtained by employing a hydrothermal temperature of 150 °C and an aqueous ammonia volume of 2.1 mL, while the hexagonal phase is obtained for a hydrothermal temperature of 200 °C and an aqueous ammonia volume between 2.3 and 2.4 mL. Subsequently, we investigate the required conditions to convert hexagonal NH4Zr2(PO4)3 fully to hexagonal HZr2(PO4)3 via thermal treatment at 600 °C for 5 h, assessed by a combination of X-ray diffraction and infrared spectroscopy.In this way this article aims to open up further research on this interesting HZP material by documenting a robust route for its preparation.