Method for measuring content of metal zinc in high-purity zinc powder

Abstract

The invention provides a method for measuring the content of metal zinc in high-purity zinc powder, which comprises the following steps: under set reaction conditions, carrying out chemical reaction on the high-purity zinc powder and an acid solution to generate hydrogen; the ratio of the amount of substance of the high-purity zinc powder to the amount of substance of hydrogen ions in the acid solution is (1: 2)-(1: 4); measuring the volume of hydrogen generated by the chemical reaction in a gas measuring device at the temperature of 15-30 DEG C; and obtaining the content of metal zinc in the high-purity zinc powder according to the hydrogen volume. According to the embodiment of the invention, the amount-of-substance ratio of the reactants and the reaction temperature are accurately controlled, and the hydrogen volume is accurately measured by utilizing the gas measuring device, so that the accuracy and the high efficiency of measuring the content of the metal zinc in the high-purity zinc powder are ensured.

Description

Technical Field

[0001] The present application relates to the technical field of metal content determination, and in particular to a method for determining the content of metallic zinc in high-purity zinc powder. Background Art

[0002] High-purity zinc powder is a widely used metal powder material with important applications in the fields of metallurgy, chemical industry, medicine, food and electronics. Currently, the preparation methods of high-purity zinc powder mainly include atomization and evaporation-condensation. The atomization method uses airflow or hydraulic jets for atomization, but it has problems such as high energy consumption, low recovery rate, and uneven particle size. The evaporation-condensation method produces zinc powder by condensing after heating zinc ingots for evaporation, but uneven temperature control can easily lead to oxidation of zinc powder, reducing purity, and making it difficult to meet application scenarios with high purity requirements, such as semiconductor doping. Therefore, accurately determining the content of metallic zinc in high-purity zinc powder is of great significance for optimizing the preparation process, improving production efficiency, and expanding the scope of application.

[0003] The national standard GB / T6890-2012, "High-Purity Zinc Powder," specifies that metallic zinc content is a key indicator for determining the grade of high-purity zinc powder and provides a determination method: Under a carbon dioxide atmosphere, metallic zinc reacts with ferric sulfate (using a copper salt as a catalyst) to produce ferrous sulfate, which is then titrated with a standard potassium permanganate solution to indirectly calculate the metallic zinc content. However, this method presents numerous challenges: it requires the preparation of carbon dioxide gas, making it difficult to maintain a completely inert environment during operation, it uses corrosive reagents, and the presence of other metallic elements in the high-purity zinc powder can bias the result upward, requiring correction. Furthermore, while differential scanning calorimetry is rapid, simple, and minimizes interference, it is expensive, resulting in high analytical costs. Summary of the Invention

[0004] The present application provides a method for determining the metallic zinc content in high-purity zinc powder to solve the following technical problem: how to improve the accuracy and efficiency of determining the metallic zinc content in high-purity zinc powder.

[0005] In a first aspect, the present invention provides a method for determining the content of metallic zinc in high-purity zinc powder, comprising:

[0006] Under set reaction conditions, high-purity zinc powder and an acidic solution are chemically reacted to generate hydrogen; the ratio of the amount of the high-purity zinc powder to the amount of hydrogen ions in the acidic solution is 1:2 to 1:4;

[0007] measuring the volume of hydrogen produced by the chemical reaction in a gas measuring device at a temperature of 15°C to 30°C;

[0008] The content of metallic zinc in the high-purity zinc powder is obtained according to the volume of the hydrogen gas.

[0009] Optionally, the parameters of the chemical reaction include: temperature of 15° C. to 30° C., and time of 5 minutes to 40 minutes.

[0010] Optionally, the chemical reaction is carried out under stirring conditions, and the stirring speed is 50 r / min to 100 r / min.

[0011] Optionally, the purity of the high-purity zinc powder is not less than 99%; and / or,

[0012] The particle size range of the high-purity zinc powder is 100 mesh to 325 mesh.

[0013] Optionally, the molar concentration of the acidic solution is 4 mol / L to 8 mol / L.

[0014] Optionally, the pH value of the acidic solution ranges from 1 to 3.

[0015] Optionally, the ratio of the mass of the high-purity zinc powder to the volume of the acidic solution is 0.008 g / mL to 0.012 g / mL.

[0016] Optionally, the acidic solution includes at least one of the following: hydrochloric acid solution and sulfuric acid solution.

[0017] Optionally, the gas measuring device includes a burette, a level bottle and a reaction bottle, the burette is connected to the reaction bottle, and the level bottle is used to adjust the air pressure in the burette; the accuracy of the gas measuring device is not less than 0.01 mL.

[0018] Optionally, the calculation formula for obtaining the mass fraction of metallic zinc in the high-purity zinc powder based on the volume of hydrogen is as follows:

[0019]

[0020] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0021] The above technical solution provided by the embodiment of the present application has the following advantages compared with the prior art:

[0022] The present invention provides a method for determining the content of metallic zinc in high-purity zinc powder. First, from the perspective of chemical reaction principle, zinc reacts with acid to generate hydrogen, and the reaction equation is Zn+2H + =Zn 2+ +H2↑. By controlling the molar ratio of high-purity zinc powder to hydrogen ions in the acidic solution to a value of 1:2 to 1:4, the reaction proceeds fully without incomplete reaction or side reactions caused by excess acid or zinc. This precise control of the molar ratio ensures complete zinc reaction, and the volume of hydrogen generated maintains a strict stoichiometric relationship with the amount of zinc, providing a theoretical basis for accurately determining the metallic zinc content. Secondly, by conducting the reaction and gas volume measurement within a temperature range of 15°C to 30°C, the effects of excessively high or low temperatures on the reaction rate and gas volume measurement are avoided. Excessively high temperatures can cause gas expansion, resulting in an inflated measurement result; excessively low temperatures can slow the reaction rate and affect measurement efficiency. This temperature range ensures both smooth reaction progress and accurate gas volume measurement. Finally, a gas measurement device is used to accurately measure the volume of hydrogen generated. Because the volume of hydrogen and the amount of zinc have a clear stoichiometric relationship, precise hydrogen volume measurement allows for accurate calculation of the metallic zinc content in the high-purity zinc powder. This method is not only easy to operate, but also can obtain results quickly, thus improving the efficiency of the measurement.

[0023] In summary, the embodiments of the present application ensure the accuracy and efficiency of the determination of the metallic zinc content in high-purity zinc powder by precisely controlling the molar ratio of the reactants and the reaction temperature and accurately measuring the hydrogen volume using a gas measuring device. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] The accompanying drawings, which are incorporated in and constitute a part of this specification, illustrate embodiments consistent with the present application and, together with the description, serve to explain the principles of the present application.

[0025] In order to more clearly illustrate the technical solutions in the embodiments of the present application or the prior art, the following summarizes the drawings necessary for the embodiments or the description of the prior art. Obviously, for professionals in this field, other relevant drawings can be derived based on these drawings without creative efforts.

[0026] Figure 1 This is a flow chart of a method for determining the content of metallic zinc in high-purity zinc powder provided in an embodiment of the present application. DETAILED DESCRIPTION

[0027] To more clearly illustrate the purpose, technical solutions, and advantages of the embodiments of the present application, the technical solutions of the embodiments are described in detail below with reference to the accompanying drawings. Please note that the embodiments described herein are merely illustrative and do not represent all possible implementation paths. All other embodiments obtained by persons of ordinary skill in the art based on the embodiments of the present application without creative effort are within the scope of protection of this application.

[0028] The ranges described herein, regardless of numerical values or ratios, include all subranges and individual numerical values therein. For example, when referring to '1 to 6' or '1-6', it means including any subrange from 1 to 6 (such as 1 to 3, 2 to 5) and all individual numbers (1, 2, 3, 4, 5, 6). Unless otherwise specified, the terms "include", "comprising", etc. used herein mean "including but not limited to"; relational terms such as "first" and "second" are only used to distinguish different entities or operations and do not imply an actual sequence or association relationship; "and / or" means that multiple situations can exist alone or simultaneously; expressions such as "at least one", "multiple", and "at least one" all refer to any combination of corresponding objects, including a combination of single or multiple objects. The proportional relationships involved in the text, such as mass ratios, molar ratios, etc., should be understood as the corresponding relationship between the first and second terms of the proportional formula in the order of description. The raw materials, reagents, instruments, and equipment used in this article can all be purchased on the market or prepared by existing methods.

[0029] Figure 1 This is a flow chart of a method for determining the content of metallic zinc in high-purity zinc powder provided in an embodiment of the present application.

[0030] See Figure 1 The present invention provides a method for determining the content of metallic zinc in high-purity zinc powder, comprising:

[0031] Under set reaction conditions, high-purity zinc powder and an acidic solution are chemically reacted to generate hydrogen; the ratio of the amount of the high-purity zinc powder to the amount of hydrogen ions in the acidic solution is 1:2 to 1:4;

[0032] measuring the volume of hydrogen produced by the chemical reaction in a gas measuring device at a temperature of 15°C to 30°C;

[0033] The content of metallic zinc in the high-purity zinc powder is obtained according to the volume of the hydrogen gas.

[0034] High-purity zinc powder: refers to zinc powder with extremely high zinc content, usually used for high-precision chemical analysis and industrial applications. Its high purity and extremely low impurity content can ensure the accuracy of chemical reactions and product performance. Acidic solution: refers to a solution containing hydrogen ions (H +) solution, which is usually highly acidic (pH less than 7). Hydrogen ions are the key factor in the reaction of zinc powder and can undergo a replacement reaction with zinc to produce hydrogen gas.

[0035] This method is based on the chemical reaction between zinc powder and acidic solution. The reaction equation is: Zn+2H + →Zn 2+ +H2↑; According to stoichiometric relations, 1 mole of zinc reacts with 2 moles of hydrogen ions to produce 1 mole of hydrogen gas. This reaction is a typical metal-acid replacement reaction. Zinc, as an active metal, displaces hydrogen ions from the acid, producing hydrogen gas. By measuring the volume of hydrogen gas produced and combining it with stoichiometric relations, the metallic zinc content in the zinc powder can be calculated. The ratio of the amount of zinc powder to the amount of hydrogen ions in the acid solution is 1:2 to 1:4. This ratio has been experimentally verified to ensure sufficient reaction time while avoiding excessive or insufficient acid. Insufficient acid will result in an incomplete reaction, leading to a low result. Excessive acid may introduce impurities or affect reaction stability. The reaction is carried out at a temperature of 15°C to 30°C. This temperature range ensures reaction activity while avoiding excessively high temperatures that could lead to excessive reaction activity or side reactions. The accuracy of the gas measurement device must be no less than 0.01 mL, as the accuracy of hydrogen gas volume measurement directly affects the accuracy of zinc content calculation. High-precision gas measurement devices can ensure the reliability of measurement results, thereby improving the accuracy of zinc content determination.

[0036] Applications: High-purity zinc powder is often used as the negative electrode material for zinc batteries. Accurately measuring the zinc content can optimize battery performance, increasing energy density and cycle life. In chemical production, high-purity zinc powder is used to produce high-purity zinc compounds. Determining zinc content using this method ensures the purity of raw materials, thereby improving product quality. In the electronics industry, high-purity zinc powder is used to manufacture electronic components. Accurately measuring zinc content can optimize production processes and ensure the performance and reliability of electronic components. Exemplarily, the ratio of the amount of the high-purity zinc powder to the amount of hydrogen ion in the acidic solution can be: 1:2, 1:2.2, 1:2.4, 1:2.6, 1:2.8, 1:3, 1:3.2, 1:3.4, 1:3.6, 1:3.8, 1:4, etc.; the reaction temperature can be: 15°C, 16°C, 17°C, 18°C, 19°C, 20°C, 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C, 30°C, etc.

[0037] In some embodiments, the parameters of the chemical reaction include: a temperature of 15° C. to 30° C., a time of 5 minutes to 40 minutes; and / or,

[0038] The chemical reaction is carried out under stirring conditions, and the stirring speed is 50 r / min to 100 r / min.

[0039] Stirring speed: refers to the speed of the stirring device, measured in revolutions per minute (r / min). The stirring speed affects the degree of mixing between the reactants and the reaction rate.

[0040] The temperature and time of chemical reactions are key factors affecting the reaction rate and completeness of the reaction. Within the temperature range of 15°C to 30°C, the reaction rate is moderate, which can ensure the completeness of the reaction. The reaction time is controlled within 5 minutes to 40 minutes, which not only ensures the full progress of the reaction, but also avoids increased energy consumption or side reactions caused by too long a time. Stirring can accelerate the mixing of zinc powder and acidic solution and increase the reaction rate. The stirring speed is 50r / min to 100r / min. This speed range can ensure that the reactants are fully mixed, while avoiding the generation of bubbles or splashing of reactants caused by too fast stirring. By stirring, the situation of local concentration being too high or too low can be reduced, thereby improving the accuracy of the measurement. Exemplary:

[0041] The temperature of the chemical reaction can be: 15°C, 16°C, 17°C, 18°C, 19°C, 20°C, 21°C, 22°C, 23°C, 24°C, 25°C, 26°C, 27°C, 28°C, 29°C, 30°C, etc.; the time of the chemical reaction can be: 5 minutes, 10 minutes, 15 minutes, 20 minutes, 25 minutes, 30 minutes, 35 minutes, 40 minutes, etc.; the stirring speed of the chemical reaction can be: 50r / min, 55r / min, 60r / min, 65r / min, 70r / min, 80r / min, 90r / min, 100r / min, etc.

[0042] In some embodiments, the purity of the high-purity zinc powder is not less than 99%; and / or,

[0043] The particle size range of the high-purity zinc powder is 100 mesh to 325 mesh.

[0044] Purity: This refers to the mass percentage of the target component in a substance. High-purity zinc powder has a purity of at least 99%, meaning the zinc content is at least 99% by mass. Particle size range: This refers to the size range of the particles, typically expressed in mesh size. The larger the mesh size, the finer the particles.

[0045] The higher the purity of high-purity zinc powder, the fewer impurities, and the more accurate the measurement results. Impurities may affect the reactivity of zinc powder, resulting in incomplete reaction or side reactions, thereby affecting the measurement results. The purity of high-purity zinc powder is not less than 99%, which can ensure the accuracy and reliability of the reaction. The particle size range of zinc powder affects its contact area with the acidic solution. The finer the particle size, the larger the specific surface area and the faster the reaction rate. At the same time, fine-particle zinc powder is easier to disperse and can improve the uniformity of the reaction. The particle size range is 100 mesh to 325 mesh, which can not only ensure the full progress of the reaction, but also avoid the problem of agglomeration or flying caused by overly fine particles. Exemplary:

[0046] The purity of high-purity zinc powder can be: 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9%, 100%, etc.; the particle size of high-purity zinc powder can be: 100 mesh, 125 mesh, 150 mesh, 175 mesh, 200 mesh, 225 mesh, 250 mesh, 275 mesh, 300 mesh, 325 mesh, etc.

[0047] In some embodiments, the molar concentration of the acidic solution is 4 mol / L to 8 mol / L; and / or,

[0048] The pH value of the acidic solution ranges from 1 to 3.

[0049] The molar concentration of the acidic solution affects the reaction rate and completeness of the zinc powder. A higher molar concentration can provide more hydrogen ions and accelerate the reaction rate. However, too high a concentration may cause the reaction to be too violent, produce side reactions or affect the accuracy of the measurement. An acidic solution with a molar concentration of 4 mol / L to 8 mol / L can ensure that the reaction proceeds fully while avoiding the problems caused by too high a concentration. The pH value is an important parameter of the acidic solution and affects the reactivity of the zinc powder. A lower pH value (1 to 3) indicates that the solution is more acidic and can provide enough hydrogen ions to react with the zinc powder. A pH value that is too low may cause the solution to be too corrosive and affect the service life of the reaction device; a pH value that is too high may cause the reaction rate to be too slow and affect the efficiency of the measurement. The molar concentration and pH value of the acidic solution jointly affect the chemical equilibrium of the reaction. Appropriate molar concentration and pH value can ensure that the reaction proceeds in the direction of generating hydrogen while avoiding the occurrence of other side reactions. Exemplary:

[0050] The molar concentration of the acidic solution can be: 4mol / L, 4.5mol / L, 5mol / L, 5.5mol / L, 6mol / L, 6.5mol / L, 7mol / L, 7.5mol / L, 8mol / L, etc.; the pH value of the acidic solution can be: pH 1, pH 1.5, pH 2, pH2.5, pH 3, etc.

[0051] In some embodiments, the ratio of the mass of the high-purity zinc powder to the volume of the acidic solution is 0.008 g / mL to 0.012 g / mL.

[0052] Mass to volume ratio: refers to the mass of zinc powder in unit volume of solution.

[0053] The ratio of the mass of zinc powder to the volume of the acidic solution affects the extent of the reaction. A suitable ratio can ensure the complete reaction while avoiding excessive zinc powder or acidic solution. If there is an excess of zinc powder, the reaction will not be complete, resulting in a low measurement result; if there is an excess of acidic solution, other impurities may be introduced or the stability of the reaction may be affected. According to the stoichiometric relationship, the zinc powder and the hydrogen ions in the acidic solution need to react in a certain ratio. By optimizing the volume ratio of zinc powder to acidic solution, the completeness of the reaction can be ensured, thereby improving the accuracy of the measurement. For example:

[0054] The volume ratio of high-purity zinc powder mass to acidic solution can be 0.0080 g / mL, 0.010 g / mL, 0.0090 g / mL, 0.0085 g / mL, 0.012 g / mL, 0.0095 g / mL, 0.011 g / mL, etc.

[0055] In some embodiments, the acidic solution includes at least one of the following: a hydrochloric acid solution and a sulfuric acid solution.

[0056] Different acidic solutions have varying effects on the reaction rate and completeness of zinc powder. Hydrochloric acid and sulfuric acid are strong acids, providing sufficient hydrogen ions to react with zinc powder. Hydrochloric acid's milder reaction makes it suitable for high-precision chemical analysis, while sulfuric acid's faster reaction rate makes it suitable for large-scale production.

[0057] In some embodiments, the gas measuring device includes a burette, a level bottle and a reaction bottle, the burette is connected to the reaction bottle, and the level bottle is used to adjust the gas pressure in the burette; the accuracy of the gas measuring device is not less than 0.01 mL.

[0058] Burette: A device used to measure gas volume, typically read on a scale. Level: A device used to regulate air pressure within a burette, balancing the pressure by adjusting the liquid level. Reaction flask: A container used for chemical reactions, typically connected to a burette to collect the gases produced. Accuracy: Refers to the accuracy of the measurement results.

[0059] The gas measuring device consists of a burette, a level bottle, and a reaction bottle. The burette is used to measure the volume of hydrogen generated by the reaction, the level bottle is used to adjust the air pressure within the burette, and the reaction bottle is used to carry out the chemical reaction and collect the generated gas. By accurately measuring the volume of hydrogen, the metallic zinc content in the zinc powder can be indirectly calculated. The level bottle balances the air pressure within the burette by adjusting the liquid level, ensuring that the gas volume measurement is not affected by changes in air pressure. Changes in air pressure can affect the gas volume measurement results, so adjusting the level bottle can improve measurement accuracy. The accuracy of the gas measuring device is no less than 0.01mL. This is because the accuracy of hydrogen volume measurement directly affects the accuracy of zinc content calculation. A high-precision gas measuring device can ensure the reliability of measurement results, thereby improving the accuracy of zinc content determination.

[0060] In some embodiments, the calculation formula for obtaining the mass fraction of metallic zinc in the high-purity zinc powder based on the volume of hydrogen is as follows: wherein: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the weighed mass of the high-purity zinc powder, in grams (g); K is the conversion coefficient of hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0061] Mercury barometer reading (P1): refers to the air pressure value read by the barometer, in kilopascals (kPa). Barometer reading temperature correction value (P2): refers to the value corrected for the barometer reading based on temperature, in kilopascals (kPa). Saturated vapor pressure of water (P3): the maximum pressure of water vapor at a certain temperature, in kilopascals (kPa). Initial volume reading (V0) and endpoint volume reading (V1) of the gas measuring device: refers to the gas volume readings before and after the reaction, in milliliters (mL). Conversion factor for hydrogen to metallic zinc (K): a factor calculated based on the stoichiometric relationship. Thermodynamic temperature constant (273): a constant used to convert Celsius temperature to thermodynamic temperature.

[0062] This formula takes into account the thermodynamic properties of the gas, including the effects of air pressure, temperature, and water vapor pressure. Thermodynamic corrections ensure that the hydrogen volume measurement accurately reflects the amount of hydrogen produced by the reaction. The conversion factor K in the formula is calculated based on the stoichiometric relationship to ensure that the hydrogen volume can be accurately converted to the mass fraction of zinc. By accurately measuring the hydrogen volume and combining corrections for air pressure, temperature, and water vapor pressure, an accurate zinc content can be obtained. This formula reduces measurement errors by correcting for the effects of air pressure, temperature, and water vapor pressure. For example, changes in temperature can cause the gas volume to expand or contract. By correcting for the effects of temperature, the accuracy of the measurement results can be improved.

[0063] The present application will be further described below in conjunction with specific examples. It should be understood that these examples are intended to illustrate the present application only and are not intended to limit the scope of the present application. The experimental methods in the following examples where specific conditions are not specified are generally measured according to industry standards. If there are no corresponding industry standards, then the methods are carried out according to general international standards, conventional conditions, or the conditions recommended by the manufacturer.

[0064] Example 1

[0065] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 1#) is carried out according to the following steps:

[0066] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0067] Weigh 0.2452 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0068] Place the weighing tube in the conical flask and tighten the stopper.

[0069] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel all air from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 99.10 mL). At this time, the ambient temperature (t) is 20°C and the atmospheric pressure (P1) is 100.39 kPa.

[0070] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 5.85 mL). At this time, the ambient temperature (t) is 20°C and the atmospheric pressure (P1) is 100.39 kPa.

[0071] When the ambient temperature is t = 20 ° C and the atmospheric pressure is P1 = 100.39 kPa, the corresponding barometer reading temperature revision value P2 = 0.326 kPa and the saturated vapor pressure of water P3 = 2.332 kPa is checked.

[0072] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0073] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0074] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 99.17%.

[0075] Example 2

[0076] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 1#) is carried out according to the following steps:

[0077] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0078] Weigh 0.2441 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0079] Place the weighing tube in the conical flask and tighten the stopper.

[0080] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel as much air as possible from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 99.00 mL). At this time, the ambient temperature (t) is 22°C and the atmospheric pressure (P1) is 100.10 kPa.

[0081] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 4.90 mL). At this time, the ambient temperature is t = 22°C and the atmospheric pressure is P1 = 100.10 kPa.

[0082] When the ambient temperature is t = 22°C and the atmospheric pressure is P1 = 100.10 kPa, the corresponding barometer reading temperature revision value P2 = 0.358 kPa and the saturated vapor pressure of water P3 = 2.637 kPa are checked.

[0083] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0084] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0085] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 99.21%.

[0086] Example 3

[0087] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 1#) is carried out according to the following steps:

[0088] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0089] Weigh 0.2415 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0090] Place the weighing tube in the conical flask and tighten the stopper.

[0091] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel all air from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 98.80 mL). At this time, the ambient temperature (t) is 23°C and the atmospheric pressure (P1) is 100.00 kPa.

[0092] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 5.15 mL). At this time, the ambient temperature is t = 23°C and the atmospheric pressure is P1 = 100.00 kPa.

[0093] When the ambient temperature is t = 23 ° C and the atmospheric pressure is P1 = 100.00 kPa, the corresponding barometer reading temperature revision value P2 = 0.374 kPa and the saturated vapor pressure of water P3 = 2.802 kPa is checked.

[0094] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0095] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0096] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 99.17%.

[0097] Example 4

[0098] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 1#) is carried out according to the following steps:

[0099] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0100] Weigh 0.2432 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0101] Place the weighing tube in the conical flask and tighten the stopper.

[0102] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel all air from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 98.80 mL). At this time, the ambient temperature (t) is 24°C and the atmospheric pressure (P1) is 99.85 kPa.

[0103] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Continue shaking every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 3.80 mL). At this time, the ambient temperature (t) is 24°C, and the atmospheric pressure (P1) is 99.85 kPa.

[0104] When the ambient temperature is t = 24 ° C and the atmospheric pressure is P1 = 99.85 kPa, the corresponding barometer reading temperature revision value P2 = 0.390 kPa and the saturated vapor pressure of water P3 = 2.976 kPa are checked.

[0105] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0106] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0107] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 99.21%.

[0108] Example 5

[0109] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 1#) is carried out according to the following steps:

[0110] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0111] Weigh 0.2402 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0112] Place the weighing tube in the conical flask and tighten the stopper.

[0113] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel all air from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 98.00 mL). At this time, the ambient temperature (t) is 26°C and the atmospheric pressure (P1) is 99.70 kPa.

[0114] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 3.00 mL). At this time, the ambient temperature (t) is 26°C and the atmospheric pressure (P1) is 99.70 kPa.

[0115] When the ambient temperature is t = 26 ° C and the atmospheric pressure is P1 = 99.70 kPa, the corresponding barometer reading temperature revision value P2 = 0.423 kPa and the saturated vapor pressure of water P3 = 3.353 kPa is checked.

[0116] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0117] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0118] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 99.20%.

[0119] Example 6

[0120] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 2#) is carried out according to the following steps:

[0121] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0122] Weigh 0.2468 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0123] Place the weighing tube in the conical flask and tighten the stopper.

[0124] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel as much air as possible from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 98.05 mL). At this time, the ambient temperature (t) is 26°C and the atmospheric pressure (P1) is 99.70 kPa.

[0125] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Continue shaking every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 1.10 mL). At this time, the ambient temperature is t = 26°C and the atmospheric pressure is P1 = 99.70 kPa.

[0126] When the ambient temperature is t = 26 ° C and the atmospheric pressure is P1 = 99.70 kPa, the corresponding barometer reading temperature revision value P2 = 0.423 kPa and the saturated vapor pressure of water P3 = 3.353 kPa is checked.

[0127] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0128] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0129] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 98.53%.

[0130] Example 7

[0131] Determine the content of metallic zinc in high-purity zinc powder using a gas meter. After the instrument has been leaked, the determination of metallic zinc in a certain high-purity zinc powder (numbered 3#) is carried out according to the following steps:

[0132] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0133] Weigh 0.2496 g of high-purity zinc powder into a weighing tube. The purity of the high-purity zinc powder is 99.5%, and the particle size is 100 mesh.

[0134] Place the weighing tube in the conical flask and tighten the stopper.

[0135] Turn the burette stopcock to connect the burette to the piston vent. Raise the level bottle to expel as much air as possible from the burette. Turn the burette stopcock to connect the burette to the reaction flask. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0 = 98.10 mL). At this time, the ambient temperature (t) is 26°C and the atmospheric pressure (P1) is 99.70 kPa.

[0136] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading (V1 = 1.30 mL). At this time, the ambient temperature (t) is 26°C and the atmospheric pressure (P1) is 99.70 kPa.

[0137] When the ambient temperature is t = 26 ° C and the atmospheric pressure is P1 = 99.70 kPa, the corresponding barometer reading temperature revision value P2 = 0.423 kPa and the saturated vapor pressure of water P3 = 3.353 kPa is checked.

[0138] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0139] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0140] According to the above formula, the metallic zinc content in the high-purity zinc powder is calculated to be 97.27%.

[0141] Example 8

[0142] Determine the content of metallic zinc in high-purity zinc powder using a gas meter after leak detection. The determination of metallic zinc in high-purity zinc powder (numbered 1#, 2#, 3#) is carried out according to the following steps:

[0143] Under the set reaction conditions, 25 mL of hydrochloric acid solution (6 mol / L) was added to the conical flask in advance.

[0144] 0.24 g to 0.25 g of high-purity zinc powder was weighed into a weighing tube. The purity of the high-purity zinc powder was 99.5% and the particle size was 100 mesh.

[0145] Place the weighing tube in the conical flask and tighten the stopper.

[0146] Turn the burette piston to connect the burette with the piston's vent. Raise the level bottle to expel as much air as possible from the burette. Turn the burette piston to connect the burette with the reaction bottle. Check the starting point every 5 minutes. If the starting point remains unchanged after two readings, record the starting point reading (V0) between 98mL and 99mL. At this time, the ambient temperature (t) is 24°C and the atmospheric pressure (P1) is 99.85kPa.

[0147] Gently shake the Erlenmeyer flask to tilt the weighing tube, allowing the sample and reaction solution to react. Shake the flask every 5 minutes until the liquid level in the burette stops falling. Raise the level bottle and check the endpoint every 5 minutes. If the endpoint remains unchanged after two readings, record the endpoint reading V1 between 4mL and 6mL. At this time, the ambient temperature t = 24°C and the atmospheric pressure P1 = 99.85kPa.

[0148] When the ambient temperature is t = 24 ° C and the atmospheric pressure is P1 = 99.85 kPa, the corresponding barometer reading temperature revision value P2 = 0.390 kPa and the saturated vapor pressure of water P3 = 2.976 kPa are checked.

[0149] Calculate the metallic zinc content in high-purity zinc powder according to the formula:

[0150] Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

[0151] The metallic zinc contents in the high-purity zinc powders (numbered 1#, 2#, and 3#) were calculated according to the above formula and are shown in Table 1.

[0152] Table 1 Precision test table

[0153]

[0154] Based on the effect data of Examples 1 to 8 above, the following conclusions can be drawn:

[0155] 1. The metallic zinc content in high-purity zinc powder can be accurately measured using a gas meter. By correcting the barometer reading and taking into account the saturated vapor pressure of water under different ambient temperatures and atmospheric pressures, a more accurate metallic zinc content can be obtained.

[0156] 2. In Examples 1 to 5, the results of the determination of the metallic zinc content of the high-purity zinc powder (numbered 1#) were relatively stable, with an average value of 99.18%, a standard deviation of 0.041%, and a relative standard deviation (RSD) of 0.041%, indicating that the method has high precision.

[0157] 3. In Examples 6 and 7, the metallic zinc contents of the high-purity zinc powders (numbered 2# and 3#) were measured to be 98.56% and 97.21%, respectively, with standard deviations of 0.070% and 0.084%, and relative standard deviations (RSDs) of 0.071% and 0.086%, respectively. This indicates that while metallic zinc content may vary between batches of high-purity zinc powder, this method still provides relatively accurate measurement results.

[0158] 4. In Example 8, precision experiments conducted on high-purity zinc powders (numbered 1#, 2#, and 3#) further verified the reliability of this method. The average metallic zinc content in different batches of high-purity zinc powder was 99.18%, 98.56%, and 97.21%, respectively. The standard deviation and relative standard deviation (RSD) were all within acceptable ranges.

[0159] The foregoing is merely a list of specific embodiments of the present application, intended to enable those skilled in the art to understand or implement the present application. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present application. Therefore, the present application is not limited to the embodiments shown herein, but is intended to conform to the broadest scope consistent with the principles and novel features of the present application.

Claims

1. A method for determining the content of metallic zinc in high-purity zinc powder, comprising: Under set reaction conditions, high-purity zinc powder reacts chemically with acidic solution to generate hydrogen; The ratio of the amount of the high-purity zinc powder to the amount of the hydrogen ion in the acidic solution is 1:2 to 1:4; measuring the volume of hydrogen produced by the chemical reaction in a gas measuring device at a temperature of 15°C to 30°C; The content of metallic zinc in the high-purity zinc powder is obtained according to the volume of the hydrogen gas.

2. The measuring method according to claim 1, wherein The parameters of the chemical reaction include: temperature of 15° C. to 30° C., and time of 5 minutes to 40 minutes.

3. The measuring method according to claim 1, wherein The chemical reaction is carried out under stirring conditions, and the stirring speed is 50 r / min to 100 r / min.

4. The measuring method according to claim 1, wherein The purity of the high-purity zinc powder is not less than 99%; and / or, The particle size range of the high-purity zinc powder is 100 mesh to 325 mesh.

5. The measuring method according to claim 1, wherein The molar concentration of the acidic solution is 4 mol / L to 8 mol / L.

6. The measuring method according to claim 1, wherein The pH value of the acidic solution ranges from 1 to 3.

7. The measuring method according to claim 1, wherein The ratio of the mass of the high-purity zinc powder to the volume of the acidic solution is 0.008 g / mL to 0.012 g / mL.

8. The measuring method according to claim 1, wherein The acidic solution includes at least one of the following: hydrochloric acid solution and sulfuric acid solution.

9. The measuring method according to claim 1, wherein The gas measuring device includes a burette, a level bottle and a reaction bottle. The burette is connected to the reaction bottle, and the level bottle is used to adjust the air pressure in the burette. The accuracy of the gas measuring device is not less than 0.01 mL.

10. The measuring method according to claim 1, wherein The calculation formula for obtaining the mass fraction of metallic zinc in the high-purity zinc powder based on the volume of hydrogen is as follows: Where: P1 is the mercury barometer reading, in kilopascals (kPa); P2 is the temperature correction value of the barometer reading, in kilopascals (kPa); P3 is the saturated vapor pressure of water at the time of temperature measurement, in kilopascals (kPa); V0 is the initial volume reading of the gas measuring device, in milliliters (mL); V1 is the endpoint volume reading of the gas measuring device, in milliliters (mL); t is the temperature inside the gas measuring device during measurement, in degrees Celsius (°C); m is the mass of the weighed high-purity zinc powder, in grams (g); K is the conversion factor for converting hydrogen to metallic zinc, which is 0.007818; 273 is the thermodynamic temperature constant.

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