52 results about "Perchloric acid" patented technology

This invention discloses a method for dissolving NiCrPSi nickel alloy samples for ICP-OES detection, comprising the following steps: mixing the NiCrPSi nickel alloy sample to be tested with hydrochloric acid aqueous solution, concentrated nitric acid, and hydrofluoric acid aqueous solution, digesting at 120-140℃ for 1.5-2.5h, and then evaporating the solution to dryness at 220-260℃; then adding nitric acid aqueous solution and heating until the solid is completely dissolved, and then diluting with water to obtain the NiCrPSi nickel alloy test solution. The dissolution method of this invention can completely dissolve NiCrPSi nickel alloy powder without elemental loss, providing an accurate sample solution for ICP-OES detection; and it eliminates the need for specialized equipment such as microwave digesters or electrothermal digesters, as well as special reagents such as perchloric acid and tartaric acid, using only conventional acid reagents and general experimental equipment, thus reducing costs, simplifying operation, and enhancing versatility.

A quantitative detection method of thallium content in converter graphite ball, steps include: 1) the pretreatment of converter graphite ball; 2) the preparation of standard solution series; 3) the detection of thallium content in converter graphite ball.The application finds that the suitable pretreatment method of converter graphite ball is carbon removal by burning, and then high-chloric acid and dilute nitric acid are used to dissolve salt, by which the converter graphite ball can be completely dissolved, thereby the stability of quantitative determination of thallium content in converter graphite ball is improved, the pretreatment method is simple, fast and operable; the method is suitable for the quantitative detection of thallium content in converter graphite ball with thallium content not less than 0.0062 μg / L, the recovery rate of thallium is as high as 99.1%, the analysis accuracy is high, the detection lower limit is as low as ppb level, the sensitivity is high, and the method has the advantages of simple operation, simple analysis condition and low labor intensity.Therefore, the application has significant economic benefits and the advantages of simplicity and economy.

This invention discloses a method for determining the arsenic content in ores, belonging to the field of ore element detection technology, comprising the following steps: (1) weighing the ore sample, adding hydrochloric acid-nitric acid mixed acid for acid hydrolysis, then adding hydrofluoric acid and perchloric acid for auxiliary digestion, evaporating to near dryness, and dissolving the residue with hydrochloric acid; (2) adding a thiourea-ascorbic acid-citric acid mixed reducing masking agent to reduce and mask interfering ions; (3) using an atomic fluorescence spectrometer to determine the fluorescence intensity of arsenic in the sample solution, and calculating the arsenic content according to the standard curve. This method achieves accurate and stable determination of arsenic in various ores such as phosphate rock and iron ore by optimizing sample pretreatment conditions, improving the reduction system and matrix interference suppression strategy.

This invention provides a method for the simultaneous and rapid detection of four oxidative stress-related biomarkers and its application. The detection method includes: (S1) pretreatment of samples using a protein precipitation extract to simultaneously extract four target compounds: 8-hydroxydeoxyguanosine, 8-isoprostaglandin F2β, 8-isoprostaglandin F2α, and acetyllysine, and preparing a test solution; the protein precipitation extract is a methanol-acetonitrile-perchloric acid mixed solution containing formic acid, wherein the volume ratio of methanol, acetonitrile, and perchloric acid is (8-10):(8-10):(0.5-1), and the volume concentration of formic acid is 0.1-0.5%; (S2) detection of the test solution and standard solution using liquid chromatography-tandem mass spectrometry, and matrix calibration using an internal standard method; plotting a standard curve with the peak area ratio of the target compound to the internal standard as the ordinate and the concentration as the abscissa; and calculating the concentration of the target compound in the test solution based on the standard curve.

The application discloses a kind of nitrogen-rich oxygen three-component high-energy density materials and synthesis method thereof.By introducing high-energy or low-sense energetic anion and cation to regulate neutral compound performance is the most direct and effective way to alleviate the contradiction between energy and stability of energetic material,can fundamentally realize the dual promotion of energy and stability.Nitrogen-rich compound 4,5-diamino-3-aminomethyl-1,2,4-triazole is used as substrate,ionization reaction is carried out with perchloric acid,then hydroxylamine ion is introduced by intermolecular force,obtains nitrogen-rich oxygen three-component high-energy density material.The synthesis method has the characteristics of easy-to-obtain raw materials,operation is simple,high safety,high yield and the like.

The application discloses an anti-migration ferrocenyl hyperbranched polymer burning rate catalyst, a preparation method thereof and application thereof. The ferrocenyl hyperbranched polymer is prepared by one-pot method through amidation reaction with 1,1'-ferrocene dicarboxylic acid and tri(2-aminoethyl)amine as monomers. The ferrocenyl hyperbranched polymer has high anti-migration performance in a composite solid propellant and can reduce the thermal decomposition temperature of ammonium perchlorate.

A method for simultaneous rapid detection of heavy metals in farmland soil and fertilizer includes the following steps: (1) unified sample pretreatment; (2) compound extraction solution; (3) dual-mode quantitative detection; and (4) dual-coefficient result correction. The detection method of this invention is applicable to both soil and fertilizer, and the same detection process is used for farmland soil and fertilizer, simplifying operation and reducing costs; it does not require perchloric acid or hydrofluoric acid, nor does it require high-temperature digestion, thus eliminating the need for a strong acid high-temperature digestion system and improving detection safety; the detection is completed within 40 minutes, which is more efficient than the national standard method; dual-mode detection + dual-coefficient correction eliminates the interference of fertilizer organic matter and soil matrix on the detection results, with a relative error of ≤5.0%, which is highly consistent with the national standard method; it does not require large instruments and is suitable for use by grassroots agricultural technology stations, fertilizer companies, and planting bases; it fully complies with the national standards for heavy metal limits in soil and fertilizer, achieving rapid, accurate, and stable quantitative detection of heavy metals, and can be directly used for qualification judgment.

This invention belongs to the technical field of battery material analysis, and discloses a sample digestion method for determining the titanium content in carbon-coated lithium iron phosphate and a method for determining the titanium content therein. The sample digestion method provided by this invention uses concentrated sulfuric acid, perchloric acid, and ammonium sulfate as the first digestion reagents. The carbon-degradation-oxidation-decomposition of carbon-coated lithium iron phosphate is achieved at a high temperature of 200℃~350℃. Concentrated hydrochloric acid is used as the second digestion reagent to achieve complexation-stabilization of titanium ions, thereby achieving complete digestion of carbon-coated lithium iron phosphate. This yields a clear, transparent digestion solution with stable titanium ions, which can be directly used for quantitative analysis of titanium. This method has the advantages of simple operation, short processing time, and high processing efficiency, and has excellent application prospects for accurate and industrialized batch detection of titanium content in this complex matrix battery material, carbon-coated lithium iron phosphate.

This invention provides a method for the synergistic catalytic thermal decomposition of ammonium perchlorate (AP) based on metal fuels. The method employs a pre-prepared composite metal fuel (C / M), where C is a low-melting-point fuel metal (such as Al, B, etc.) and M is a highly catalytically active metal (such as Ni, Cu, etc.). By uniformly mixing the above fuel with AP in a specific ratio, during heating, the fuel not only provides the heat of reaction as a high-energy fuel, but also, the transition metals and their potentially in-situ generated metal derivatives within it, work synergistically with the low-melting-point metal component to significantly reduce the high-temperature decomposition temperature of AP, greatly increase its decomposition reaction rate, and lower its apparent activation energy. The method described in this invention is simple, has significant catalytic efficiency, and good safety, showing promising application prospects in solid propellant formulations and providing effective technical support for improving propellant combustion performance.

The application discloses a method for determining silicon dioxide in serpentine, which comprises the following steps: decomposing a sample with a mixed solvent, extracting with hydrochloric acid, dehydrating with perchloric acid to separate silicon dioxide from other metal ions, filtering, burning, and weighing to a constant amount, so as to determine the content of silicon dioxide. The method provides accurate data for the content of silicon dioxide in serpentine and fills the blank of determining the content of silicon dioxide in serpentine.

The application relates to a sample pretreatment method for pyrite element analysis. First, a pretreatment agent is prepared: carboxymethyl chitosan is activated on the surface through NHS / EDC, and then reacts with phosphoethanolamine to obtain the pretreatment agent; secondly, a pyrite sample is crushed into particles, and is fully ground into powder together with NaOH, NaNO3 and the pretreatment agent; then, the temperature is increased to 180-250 DEG C and then to 350-450 DEG C for heat preservation; the sintered solid is transferred into a beaker, hot nitric acid solution is added, ultrasonic is used to dissolve the solid, and after cooling, filtration is carried out into a volumetric flask, and dilute nitric acid is used for constant volume to obtain a sample to be tested. The treatment method avoids the use of a large amount of concentrated acid and perchloric acid, the reagent consumption is small, and the method is environment-friendly; the treated sample is determined by an ICP-MS instrument and the like, and the recovery rate can be ensured to be above 95%; compared with a standard value, the RSD value is not more than 5%, and the accuracy is good.

This invention provides a kit for the simultaneous detection of nine flavor nucleotides in livestock and poultry products. The flavor nucleotides are cytidine monophosphate, uridine monophosphate, guanylic acid, inosine monophosphate, adenosine monophosphate, hypoxanthine, inosine, adenosine diphosphate, and adenosine triphosphate. The kit includes: a high-concentration extraction reagent, a standard curve solution, a high-concentration phosphate buffer solution, pH adjustment solution A, and pH adjustment solution B. The high-concentration extraction reagent is perchloric acid; the standard curve solution is a mixed solution of the nine flavor nucleotides; the high-concentration phosphate buffer solution is a solution of potassium dihydrogen phosphate and dipotassium hydrogen phosphate; pH adjustment solution A is sodium hydroxide; and pH adjustment solution B is phosphate. This invention also provides a method for the simultaneous detection of the nine flavor nucleotides using the above kit. This invention enables the simultaneous determination of the content of nine flavor nucleotides in livestock and poultry products. The method is simple, rapid, accurate, and sensitive, and can be used for batch determination, showing good prospects for practical application.

This utility model discloses a screening device for ammonium perchlorate crystal particles, relating to the field of sorting technology. The device includes a discharge box, with a crystal particle screening box slidably connected inside. A particle screening structure is located on the crystal particle screening box. The particle screening structure includes two stepper motors, two rotating shafts, and two cross-shaped screen plates. Both rotating shafts are rotatably connected inside the crystal particle screening box. The two cross-shaped screen plates work alternately. When large particles accumulate on one screen plate, the stepper motor drives its rotation, transferring the large particles to the arc-shaped screen plate. The other screen plate immediately takes over the screening work, ensuring uninterrupted screening. Combined with the vibration of the crystal particle screening box, qualified particles can quickly pass through the screen plates, effectively avoiding the problem of low screening efficiency caused by material accumulation and further increasing the screening volume per unit time.

This invention relates to the field of graphene and discloses a method for preparing highly dispersible graphene oxide with a high monolayer ratio at low temperatures. The method includes: S1: ball milling a mixture of graphite and activated carbon; S2: immersing the graphite / activated carbon mixture in an acidic solution containing hypochlorous acid and / or hypochlorite under light irradiation for a pre-oxidation reaction to exfoliate the graphite into a monodisperse state; S3: oxidizing the product of reaction S2 in a concentrated sulfuric acid / perchloric acid mixed acid system; S4: diluting the product of reaction S3 with water and then introducing a ferrous salt for a reduction reaction; and finally, separating and washing to obtain a graphene oxide dispersion. This invention can prepare highly dispersible graphene oxide with a high monolayer ratio under low temperature and mild conditions. Furthermore, during the preparation process, this invention utilizes the synergistic effect of activated carbon and chloride ions to fully disrupt the large π bonds of the conjugated aromatic domains in graphite, thereby increasing the flexibility of the graphene sheets and reducing viscosity.

This invention discloses an NPTTz-based anionic energetic complex, prepared by a volatilization method using 6-(4-nitro-1H-pyrazole-1-yl)-[1,2,4]triazolo[4,3-b][1,2,4,5]tetraazine and metal nitrates as raw materials. The NPTTz-based anionic energetic complex of this invention exhibits a detonation response upon laser irradiation, demonstrating good safety and detonation performance. It can be used as a laser-initiated detonator or as a component of explosives and propellants. Furthermore, the NPTTz-based anionic energetic complex of this invention exhibits good catalytic activity and can be used as an ammonium perchlorate catalyst, showing promising application prospects in the field of high-energy insensitive energetic materials.

This invention discloses a method for determining the content of metal oxides in cement, comprising: (1) sample pretreatment: adding hydrofluoric acid and perchloric acid to the sample to be tested, and performing a first digestion at 280-290℃ to obtain a first digestion product; adding perchloric acid to the first digestion product for a second digestion to obtain a second digestion product; adding nitric acid to the second digestion product for a third digestion to obtain a third digestion product; adjusting the volume of the third digestion product to obtain a digestion solution of the sample to be tested; (2) ICP-MS detection: using the internal standard calibration method of ICP-MS to detect the digestion solution of the sample to be tested to obtain the content of the target metal oxides in cement; this method significantly improves the problems of complex and variable interference factors, ionization and interatomic interference that exist in ICP-MS detection, and significantly improves the accuracy and stability of the detection results, making it suitable for large-scale application in cement quality detection.

The application provides a quantitative statistical method for sigma phase in austenitic heat-resistant steel, which comprises the following steps: firstly, wire cutting the sample according to the sample size requirement of an electron microscope; then, polishing and polishing the sample; after the polishing is completed, electrolytic polishing is performed on the sample; after the electrolytic polishing, the sample is cleaned and dried, and finally, image data acquisition is performed. The application has the advantages that an electrolytic polishing method suitable for EBSD characterization of austenitic heat-resistant steel with sigma phase precipitation is provided, in which the electrolyte is prepared by mixing perchloric acid with a purity of 70-72% and glacial acetic acid at a ratio of 1:3, and the electrolyte is placed in a thermostatic bath of ice water mixture for electrolytic polishing. It is found through experiments that the sigma phase does not dissolve and fall off when the sample is electrolytically polished under the condition, and the disadvantage that the sigma phase is prone to falling off and dissolving in traditional stainless steel electrolytic polishing is solved.

This invention provides a boron-based composite energetic material with sodium molybdate assembled with an oxidant and its preparation method. The material includes a boron matrix, an energetic oxidant assembled on the boron matrix, and sodium molybdate dispersed within the energetic oxidant. The boron matrix is ​​boron powder, mono-modified boron powder, or binary modified boron powder. The energetic oxidant is ammonium perchlorate, ammonium nitrate, or potassium perchlorate. The morphology of the boron-based composite energetic material is rough-surfaced spherical particles. The ignition delay time of the boron-based composite energetic material with sodium molybdate assembled with an oxidant prepared by spray drying is 37-30 ms, which is half that of boron powder or surface-modified boron powder; the oxidation peak temperature of this composite energetic material is 560-533℃, which is more than 100℃ lower than that of boron powder or surface-modified boron powder.

This invention discloses a high-energy, low-sensitivity energetic material based on a quaternary organic component and its synthesis method. The method uses 3-aminomethyl-4,5-diamino-1,2,4-triazole, dimethylamine, ammonium perchlorate, and perchloric acid as raw materials, and water as a solvent to prepare the target product [TATT][CH3NH2CH3][NH4](ClO4)7. The synthesis method of this invention is simple, uses readily available raw materials, is highly safe, has a mild reaction, and achieves a yield of up to 92%, enabling large-scale production of the product. This invention provides research ideas and experimental references for ensuring the supply of high explosives, explosive formulations, and pyrotechnics in wartime emergency situations.

This invention discloses a method for grain boundary display of high boron alloy steel, comprising the following steps: (1) Sample preparation: the sample to be tested is inlaid, ground, and polished to obtain a scratch-free mirror surface; (2) Initial grain boundary etching: the polished sample is immersed in an etching solution for 5-30 seconds; the etching solution is prepared from perchloric acid, citric acid, benzotriazole, sodium dodecylbenzenesulfonate, and deionized water; (3) the sample is quickly removed, rinsed with anhydrous ethanol, and dried; (4) Anodizing: the sample is used as the anode and placed in a 5%-10% chromic acid electrolyte for constant-voltage anodizing treatment; (5) after rinsing with deionized water, dehydrating with anhydrous ethanol, and drying, it is observed under a microscope. The method of this invention has the advantages of simple operation, good reproducibility, continuous and clear grain boundary display, and minimal damage to the matrix structure, providing a reliable technical means for the grain size assessment, microstructure analysis, and performance research of high boron alloy steel.

The present application relates to the technical field of metal sample preparation, and particularly relates to a detection method for a small-size dual-phase steel EBSD sample, which comprises the following steps: fixing the sample in a clamp; polishing the observation surface of the sample, mechanically polishing the polished observation surface, and cleaning the mechanically polished observation surface; placing the cleaned sample and the clamp in an electrolytic polishing device for electrolytic polishing, wherein: the electrolyte used is a mixed solution of 50%-70% perchloric acid, anhydrous ethanol and glycerol in a volume ratio of 1:6 to 8:1 to 3, the voltage is set to 20-25 V, the current density is 1.0-10.0 A / cm 2 , the polishing time is 10-25 s, and the electrolyte temperature is-20-5 DEG C; taking out the electrolytically polished sample from the clamp, cleaning the electrolytically polished observation surface, and obtaining the mirror surface observation surface for EBSD. The present application can improve the calibration rate during EBSD detection.

This invention provides a biological filter media ceramic particle for removing perchlorate from water and its preparation method. The preparation method of the biological filter media ceramic particle of this invention includes mixing the filter media ceramic particle with an iron modifier and performing a shaking treatment to obtain iron-modified biological filter media ceramic particle. The iron modifier impregnation of the biological filter media ceramic particle ensures sufficient contact between iron ions and the biological filter media ceramic particle, thereby loading the iron ions onto the biological filter media ceramic particle. The modified biological filter media ceramic particle can remove phosphorus, ammonia nitrogen, and COD, and also enhances the adsorption capacity of the biological filter media ceramic particle for perchlorate, which can significantly improve the removal efficiency of the biological filter media ceramic particle for perchlorate.

The application provides a kind of oxidant agglomerated multi-element boron-based composite energetic material and preparation method, and the multi-element boron-based composite energetic material is made of energetic oxidant, boron powder, metal element and metal oxide;The energetic oxidant is ammonium perchlorate, ammonium nitrate or potassium perchlorate.The metal oxide is titanium dioxide, bismuth oxide, vanadium oxide or molybdenum oxide.The metal element is molybdenum, magnesium or aluminum.The morphology of multi-element boron-based composite energetic material is rough surface spherical particle.In the application, the preparation method of one pot is used, and the energetic oxidant, boron powder, metal element particle and metal oxide particle are uniformly dispersed in water to form a solid-liquid mixed feed liquid, and the spray drying technology is used to prepare the spherical particle sample composed of numerous particles, which has the technical advantages of simple preparation, high efficiency, good repeatability and low cost.The multi-element boron-based composite energetic material has lower oxidation peak temperature and higher combustion heat value, and has very good application prospect.

The application provides an oxidant-assembled boron-based composite energetic material with high sphericity and a preparation method, comprising a boron matrix, and an energetic oxidant assembled on the boron matrix; the boron matrix is boron powder, monovalent modified boron powder or divalent modified boron powder; the monovalent modified boron powder is obtained by depositing metal oxide on the surface of boron powder by using an atomic layer deposition method; the divalent modified boron powder is obtained by depositing metal oxide and metal molybdenum on the surface of boron powder by using an atomic layer deposition method; the energetic oxidant is ammonium perchlorate, ammonium nitrate or potassium perchlorate; and the boron-based composite energetic material has a spherical particle shape. The composite energetic material prepared by using a spray drying technology has a short laser ignition delay time, excellent ignition and combustion performance, and has a very good application prospect. The application can simultaneously solve the problems of limited boron powder surface activity, nanoscale uniform composite of boron powder and energetic oxidant, and integrated solution of optimization of spheroidization morphology and improvement of process performance.

The utility model discloses an ammonium perchlorate vacuum crystallizer relates to vacuum crystallizer technical field, including the shell, the inside of shell is provided with the inner tank, and there is a gap between the inner tank and shell, and the outer surface of inner tank is provided with two spiral copper pipes vertically, and the bottom of shell is installed with the connecting frame, and one end of connecting frame is provided with the liquid tank, and the top of connecting frame extends to the inside of inner tank, and the extension end of connecting frame is provided with the overflow cylinder, and the outer surface of overflow cylinder is sleeved with the special section cylinder. The utility model discloses through being provided with a series of structures, can be more accurate control the heating or cooling rate and the final temperature of tank body to adapt to the different production process demand, and can promote the crystal to sink and grow down, and the crystal that sinks to the tank body bottom is in the relatively stationary environment, reduces the risk of collision breakage, avoids producing solution splashing and local over -concentration phenomenon, prevents the direct impact of solution to bottom crystal accumulation area.

This utility model discloses a high-efficiency dissolving and stirring device for ammonium perchlorate, relating to the field of ammonium perchlorate production technology. The device includes an ammonium perchlorate stirring tank with a drive box mounted on its upper end; a drive assembly housed inside the drive box; and a stirring assembly housed inside the ammonium perchlorate stirring tank. During the dissolving and stirring process of ammonium perchlorate, some splashing ammonium perchlorate solution or powder is generated. A sealing disc seals the area between the ammonium perchlorate stirring tank and the drive box, effectively preventing these splashed materials from entering the drive box and preventing the ammonium perchlorate solution or powder from adhering to the gears and gear rings. Furthermore, the sealing disc, in conjunction with the turntable, improves the stability of the rotating shaft during its rotation and revolution, ensuring smooth rolling of the gears on the gear rings, maintaining stable operation of the entire stirring device, and improving production efficiency and product quality.

This application provides an electrolyte, a sodium metal battery cell, a battery device, and an electrical device. The sodium metal battery cell includes an electrolyte comprising an electrolyte salt, a non-fluorinated chain ether solvent, and a metal ion additive. The concentration of the electrolyte salt is 0.5 mol / L to 1.5 mol / L, and the concentration of the metal ion additive is greater than 0.0005 mol / L and less than 1.0 mol / L. The cations of the metal ion additive include alkali metal ions other than sodium or alkaline earth metal ions. The anions of the metal ion additive include one or more of sulfate, acetate, formate, phosphate, oxalate, borate, citrate, niobate, tetrafluoroborate, difluorooxaloborate, perchlorate, hexafluorophosphate, trifluoromethanesulfonate, iodate, bis(fluorosulfonyl)imide, arsenate, carbonate, or tantalate, thereby providing improved high-temperature storage performance.

The application belongs to the technical field of electromagnetic functional materials and conductive polymers, and particularly relates to a porous three-dimensional spherical PEDOT wave absorber as well as a preparation method and application thereof. The wave absorber is prepared through chemical oxidation polymerization reaction of the following raw materials: 3,4-ethylenedioxythiophene monomer, iron-based oxidizing agent and dopant. The application realizes, for the first time, systematic regulation of the amount of a single dopant on the morphology of PEDOT, and obtains an excellent wave absorption structure. Iron perchlorate has dual functions of oxidizing agent and dopant, can provide Fe 3+ ⁺ and ClO₄⁻ double-doping effects, and iron ions and their hydrolysis products can affect nucleation and growth kinetics in the polymerization process, thereby regulating the micro-morphology of PEDOT. The application realizes controllable preparation of PEDOT with different morphologies in one step by accurately changing the addition amount of iron perchlorate and the reaction temperature, significantly improves the conductivity of PEDOT, and further enhances the conductivity loss. The process is simple, stable, low in cost, green and environmentally friendly.

This invention discloses a polysaccharide esterified carbon dioxide / crude oil blending agent, its preparation method, and its application, relating to the technical field of carbon dioxide enhanced oil recovery (CEAR). The blending agent is an oligopolysaccharide esterified derivative or a mixture containing oligopolysaccharide esterified derivatives. The oligopolysaccharide molecule has one C12-18 long-chain ester group at one site and C2-C4 short-chain ester groups at the remaining sites. The blending agent is used to reduce the minimum miscibility pressure between crude oil and carbon dioxide. The preparation method involves using long-chain alkyl oligopolysaccharide esters and short-chain anhydrides as raw materials. Chain oligopolysaccharides are added to the reactor at a feed ratio of 1:3a+1, and cyclic oligopolysaccharides are added at a feed ratio of 1:3a-1. Copper perchlorate is used as a catalyst, and the reaction is carried out at 90-140℃ for 12-36 hours. After the reaction, the resulting product does not require purification to obtain the blending agent. The raw materials of this invention are readily available, the synthetic route is short, and the product can be used directly after the reaction without purification.