Stabilization treatment method and stability test method for mineral standard material

Abstract

The present application relates to the technical field of detection analysis, and particularly relates to a mineral standard substance stabilization treatment method and a stability test method. The mineral standard substance stabilization treatment method comprises crushing, aging, drying to constant weight and homogenization treatment on the mineral standard substance raw material, and then performing sealing after sub-packaging. The mineral standard substance stability test method comprises obtaining the standard substance stabilized mineral material, performing short-term stability and / or long-term stability detection on the standard substance stabilized mineral material, performing analysis and test by using a linear fitting method, and determining the stability of the standard substance content in the mineral material. The present application first provides a mineral component analysis standard substance stabilization treatment method, can fully guarantee the long-term stability and the opening bottle stability of the standard substance mineral material product, and the standard substance value will not have significant changes within at least 5 years.

Description

Technical Field

[0001] This invention relates to the field of detection and analysis technology, specifically to a method for stabilizing mineral standard materials and a method for testing their stability. Background Technology

[0002] A reference material (RM) is a substance or material with one or more sufficiently homogeneous characteristic values ​​that have been determined. Its values ​​possess accuracy, homogeneity, and stability. Stability refers to the ability of a reference material to maintain its characteristic values ​​within a specified range under specified environmental conditions and time. The stability of prepared mineral reference materials is easily altered by physical factors, chemical factors, time effects, and storage environment, leading to changes in their characteristic values ​​and rendering them unusable as measuring instruments.

[0003] The stability of mineral reference materials plays a crucial role in ensuring data accuracy and traceability, supporting quality control and certification systems, reducing long-term research costs, promoting long-term verification of scientific discoveries, and preventing the transmission of systematic errors. It also affects the reliability of scientific research, the quality control of industrial production, and the traceability of international standards. Summary of the Invention

[0004] Therefore, it is necessary to provide a method for stabilizing mineral standard materials and a method for testing their stability.

[0005] This invention provides a simple, feasible, and effective method for stabilizing mineral composition analysis standard references, thereby improving their stability and offering a scientific and reasonable testing method for stability testing.

[0006] The present invention adopts the following technical solution:

[0007] This invention provides a method for stabilizing mineral standard materials, comprising the following steps: obtaining mineral standard material raw materials and pretreatment;

[0008] The mineral material is pretreated by aging. The aging process involves gradient control of temperature, humidity, light intensity, light duration, wind speed, and treatment time to obtain aged mineral material. The aged mineral material is dried to constant weight and ground to obtain homogenized mineral material. The homogenized mineral material is then packaged and sealed to obtain standard substance stabilized mineral material.

[0009] In some embodiments, the aging process includes at least four stages of gradient-controlled process parameter conditions:

[0010] The first stage of process parameters are: temperature 25℃~35℃, humidity 70~85%, light intensity 70000~100000Lx, light duration 14~15h, wind speed 2~3, and treatment duration 3~4 months.

[0011] Second stage process parameters: temperature 2 ℃~27 ℃, humidity 55~75%, light intensity 50000~70000Lx, light duration 9~12 h, wind speed 3~4, treatment duration 3~4 months;

[0012] The process parameters for the third stage are: temperature -30℃ to -10℃, humidity 50% to 70%, light intensity 30,000 to 50,000 Lx, light duration 8 to 9 hours, wind speed 3 to 4, and treatment time 3 to 4 months.

[0013] The fourth stage process parameters are: temperature -4℃~15℃, humidity 40~60%, light intensity 60000~80000 Lx, light duration 11~13 h, wind speed 4~5, and treatment time 3~4 months.

[0014] Preferably, the aging process includes at least four stages of gradient-controlled process parameters:

[0015] The first stage of process parameters are: temperature 30 ℃, humidity 80%, light intensity 90000 Lx, light duration 14 h, wind speed level 2, and treatment duration 3 months.

[0016] Second stage process parameters: temperature 20 ℃, humidity 65%, light intensity 60000 Lx, light duration 10 h, wind speed level 3, treatment duration 3 months.

[0017] Phase 3: Temperature -20℃, humidity 60%, light intensity 40000 Lx, light duration 8 h, wind speed level 3, treatment duration 3 months;

[0018] Phase 4: Temperature 10℃, humidity 50%, light intensity 70000 Lx, light duration 11 h, wind speed level 4, treatment duration 3 months.

[0019] In some embodiments, the mineral standard material raw material, such as copper concentrate or gold ore, is preferably aged for a total period of 15-18 months.

[0020] Preferably, the pretreatment includes preliminary crushing using a jaw crusher.

[0021] Preferably, the drying temperature of the aged mineral material is 100~105 ℃.

[0022] Preferably, the sealing process includes: vacuum sealing the dispensed homogenized mineral material, observing for one week for no air leakage, and then transferring it to a plastic bottle for aluminum foil heat sealing.

[0023] This invention also provides a method for testing the stability of mineral standard materials, comprising: obtaining stabilized mineral material according to a mineral standard material stabilization treatment method; performing short-term and / or long-term stability tests on the stabilized mineral material, wherein the stability test data are obtained by parallel testing 2 to 4 times, using a linear fitting method y= β 1X+ β 0 was analyzed and tested, based on To determine the stability of the content of the standard substance.

[0024] In some embodiments, the short-term stability test includes a high-temperature test, a low-temperature test, and / or a shock test.

[0025] In some embodiments, the long-term stability test includes testing the stability of the standard substance content in the standard substance stabilized mineral material after opening and removing the packaging, under normal storage conditions.

[0026] Compared with the prior art, the beneficial effects of the present invention are:

[0027] The mineral standard material stabilization method of this invention involves fully aging the mineral raw materials. Almost all sulfides in the minerals, such as pyrrhotite (FexS), chalcopyrite (CuFeS2), galena (PbS), and sphalerite (ZnS), undergo varying degrees of oxidation. Oxides of variable-valence metal elements are also easily further oxidized. Residual beneficiation reagents, such as xanthate, blackening agent, sulfiding agent, and foaming agent, may undergo slow oxidation reactions upon long-term exposure, leading to changes in the content of the target components. This invention, through at least one year of gradient aging with temperature, humidity, light, and wind speed, allows the components in the mineral raw materials to fully react, thereby stabilizing the content of the standard material.

[0028] The stabilization treatment method for mineral composition analysis standard substances of the present invention employs vacuum sealing and aluminum foil heat sealing technology for double protection when dispensing the prepared mineral composition analysis standard substances into the smallest packaging unit, so as to protect the sample from external interference to the greatest extent and fully guarantee the stability of the standard substance product.

[0029] The present invention provides a method for testing the stability of mineral composition analysis standard materials. This method uses a simultaneous research method to test short-term stability and a classical research method to test long-term stability and open-bottle stability, confirming that the stability of the stabilized mineral standard materials meets the requirements. Detailed Implementation

[0030] This invention essentially provides a method for stabilizing mineral composition analysis standard materials, comprising the following steps: obtaining mineral standard material raw materials; processing the raw materials using a jaw crusher and / or a rod mill to obtain pretreated mineral materials; aging the pretreated mineral materials, wherein the aging process involves gradient control of temperature, humidity, light intensity, light duration, wind speed, and processing time to obtain aged mineral materials; drying the aged mineral materials in an oven to constant weight, and grinding them uniformly to obtain homogenized mineral materials; packaging the homogenized mineral materials, and vacuum sealing the samples with aluminum foil to obtain stabilized standard material mineral materials.

[0031] In the embodiments of the present invention, the aging process preferably includes at least four stages of process parameters controlled by gradient:

[0032] The first stage of the process parameters are: temperature 25℃~35℃, humidity 70~85%, light intensity 70,000~100,000 Lx, light duration 14~15 h, wind speed 2~3, and treatment time 3~4 months. This can be achieved through open-air treatment in the Northeast summer (June to August) environment, or by using artificial environmental simulation conditions.

[0033] The second-stage process parameters are: temperature 2℃~27℃, humidity 55~75%, light intensity 50000~70000 Lx, light duration 9~12 h, wind speed 3~4, and treatment duration 3~4 months. This can be achieved through open-air treatment in the autumn environment of Northeast China (September to November), or by using artificial environmental simulation conditions.

[0034] The third stage process parameters are: temperature -30℃ to -10℃, humidity 50% to 70%, light intensity 30,000 to 50,000 Lx, light duration 8 to 9 hours, wind speed 3 to 4, and treatment duration 3 to 4 months. It can be carried out in the open air in the winter environment of Northeast China (December to February) or it can be achieved by artificial environmental simulation conditions.

[0035] The fourth stage process parameters are: temperature -4℃ to 15℃, humidity 40% to 60%, light intensity 60,000 to 80,000 Lx, light duration 11 to 13 hours, wind speed 4 to 5, and treatment duration 3 to 4 months. This can be achieved through open-air treatment in the Northeast spring (March to May) environment, or by using artificial environmental simulation conditions.

[0036] This invention also provides a method for testing the stability of stabilized mineral reference materials, including: testing its short-term stability through simultaneous research methods following high-temperature experiments, low-temperature experiments, and / or shock experiments; and testing its long-term stability through classical research methods following long-term storage under conventional storage conditions. The mineral composition analysis reference material is a repeatable sample reference material. Its open-bottle stability is tested using classical research methods that examine the stability of characteristic values ​​after opening the packaging. The effectiveness of the mineral reference material stabilization treatment method is confirmed based on the test results.

[0037] The test data were analyzed and verified using a linear fitting method, with X representing time and y representing the content of the target element in the mineral, and fitted into a straight line.

[0038] The specific formula algorithm and result analysis process are as follows:

[0039] y = β1X + β0;

[0040] Where y refers to the content of the target element in the mineral, β1 refers to the slope of the fitted line, X refers to the time of the stability study, and β0 refers to the intercept of the fitted line.

[0041] Standard deviation of the line s:

[0042] ;

[0043] Slope uncertainty s(β1):

[0044] ;

[0045] Among them, t 0.95，n-2 The number of t-factors with n-2 degrees of freedom and 95% confidence probability can be obtained from the t-distribution numerical table.

[0046] The criterion |β1|≤t can be used. 0.95,n-2 The stability of mineral standard materials was analyzed by ×s(β1) to confirm the effect of stabilization treatment.

[0047] like This indicates that the content of the target element in the mineral has not changed significantly, and the mineral raw material stabilization treatment method is effective.

[0048] like This indicates that the content of the target element in the mineral has changed significantly, and the stabilization treatment method for the mineral raw material is ineffective.

[0049] The present invention will be further described in detail below with reference to specific embodiments, so that those skilled in the art can more clearly understand the present invention. The following embodiments are only used to illustrate the present invention, and are not intended to limit the scope of the present invention. Based on the specific embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the protection scope of the present invention. In the embodiments of the present invention, unless otherwise specified, all raw material components are commercially available products well known to those skilled in the art; in the embodiments of the present invention, unless specifically specified, the technical means used are conventional means well known to those skilled in the art.

[0050] Example 1: Stabilization and Detection Methods for Standard Reference Materials for Copper Concentrate Composition Analysis

[0051] Example 1-1

[0052] This embodiment provides a method for stabilizing standard reference materials for copper concentrate composition analysis, including the following steps:

[0053] S1, Purchasing mineral raw materials for preparing mineral standard substances.

[0054] Purchase 500 kg of copper concentrate, with a particle size of approximately 0.150 mm (100 mesh) and a copper content of approximately 19%.

[0055] S2, Preprocessing

[0056] In Changchun City, Jilin Province, purchased mineral raw materials are processed using jaw crushers and rod mills to obtain pre-treated mineral materials. (Some raw materials exhibit agglomeration and require preliminary crushing; if there is no agglomeration, this crushing step can be omitted.)

[0057] S3, Aging

[0058] In Changchun, Jilin Province, crushed mineral raw materials were spread out on waterproof tarpaulins and air-dried in the open air for 15 months, from June 2013 to August 2014.

[0059] The parameters for the first phase of summer (June to August 2013) are: temperature 25℃~35℃, humidity 70~85%, light intensity 70000~100000 Lx, sunshine duration 14~15 h, wind speed level 2~3, and duration 3 months.

[0060] The parameters for the second phase of autumn (September to November 2013) are: temperature 2℃~27℃, humidity 55~75%, light intensity 50000~70000 Lx, sunshine duration 9~12 h, wind speed 3~4, and duration 3 months.

[0061] The parameters for the third stage of winter (December 2013 to February 2014) are: temperature -30℃ to -10℃, humidity 50 to 70%, light intensity 30,000 to 50,000 Lx, sunshine duration 8 to 9 hours, wind speed 3 to 4, and duration 3 months.

[0062] The parameters for the fourth stage, spring (March to May 2014): temperature -4℃ to 15℃, humidity 40% to 60%, light intensity 60,000 to 80,000 Lx, sunshine duration 11 to 13 hours, wind speed 4 to 5, duration 3 months.

[0063] The parameters for the fifth stage of summer (June to August 2013) are: temperature 25℃~35℃, humidity 70~85%, light intensity 70000~100000 Lx, sunshine duration 14~15 h, wind speed level 2~3, duration 3 months.

[0064] During the drying process, cover the raw materials with waterproof tarpaulins during rainy or snowy weather to prevent them from getting wet. When the temperature is high and there is plenty of sunshine, turn the mineral raw materials regularly to ensure that they have full contact with air and sunlight, thus aging the mineral materials.

[0065] S4, grind evenly

[0066] The aged mineral material is ground to a particle size of less than 200 mesh, dried at 100℃ to constant weight, cooled to room temperature, and then homogenized using grinding equipment to obtain homogenized mineral material that passes the homogenization test.

[0067] S5, repackaging and sealing

[0068] The homogenized mineral material that passed the homogenization test was divided into the smallest packaging unit (50g / unit). Each unit of raw material was vacuum sealed. After sealing, it was observed for one week to ensure that there was no air leakage. Then, the sealed raw material was transferred to a plastic bottle and the plastic bottle was heat-sealed with aluminum foil to obtain the standard substance stabilized mineral material.

[0069] This embodiment also tests the storage stability (short-term stability and long-term stability) of the standard material stabilized mineral material for the standard material copper element. First, the short-term stability is tested by synchronous stability study under repeatable measurement conditions, that is, the stability of the sample under transportation conditions. The extreme conditions of transportation are fully simulated. High temperature experiment, low temperature experiment and shock experiment are carried out on the sample respectively. After the sample is tested for different durations, the test is carried out simultaneously.

[0070] In this embodiment, the method for detecting the target copper content is the iodometric method (GB / T3884.1-2012): the sample is decomposed by hydrochloric acid, nitric acid, and bromine; the pH of the solution is adjusted to 3.0-4.0 with an acetic acid-ammonium acetate solution; iron is masked with ammonium bifluoride; potassium iodide is added to react with divalent copper ions; the precipitated iodine is titrated with a standard sodium thiosulfate solution using starch as an indicator. The copper content is calculated based on the volume of standard sodium thiosulfate solution consumed.

[0071] (1) Short-term stability - high temperature test

[0072] Eight units of samples were randomly selected and numbered 1 to 8, and placed in a 60℃ constant temperature chamber. Samples 1 and 2 were removed on day 0, samples 3 and 4 on day 1, samples 5 and 6 on day 3, and samples 7 and 8 on day 7. Samples 1 to 8 were then tested simultaneously, with each unit tested twice in parallel (e.g., samples 1 and 2 were tested twice each, resulting in four data points, which were recorded as 1, 2, 3, and 4 in the table; the same data recording method was used for other samples). The test data were analyzed using linear fitting. The high-temperature experimental test data and results analysis are shown in Table 1 below.

[0073] Table 1. High-Temperature Experimental Data and Results Analysis of Copper in Copper Concentrate Samples

[0074]

[0075] (2) Short-term stability – Low temperature test

[0076] Eight units of samples were randomly selected and numbered 1 to 8. They were placed in a freezer at -20°C. Samples 1 and 2 were taken out on day 0, samples 3 and 4 on day 1, samples 5 and 6 on day 3, and samples 7 and 8 on day 7. Samples 1 to 8 were then tested simultaneously. Each unit of sample was tested twice in parallel (the test data for every two samples were recorded in the same way as above). The test data were analyzed and verified using the linear fitting method.

[0077] The detection data and test results of the low-temperature experiment are shown in Table 2 below.

[0078] Table 2. Analysis of Low-Temperature Experimental Data of Copper in Copper Concentrate Samples

[0079]

[0080] (3) Short-term stability - shock test

[0081] Eight units of samples were randomly selected and numbered 1 to 8. They were placed on a shaker. Samples 1 and 2 were taken out on day 0, samples 3 and 4 were taken out on day 1, samples 5 and 6 were taken out on day 3, and samples 7 and 8 were taken out on day 7. Samples 1 to 8 were then tested simultaneously. Each unit of sample was tested twice in parallel (the test data of every two samples was recorded in the same way as above). The test data were analyzed and verified using the linear fitting method. The test data and test results are shown in Table 3 below.

[0082] Table 3 Analysis of shock test data of copper in copper concentrate samples

[0083]

[0084] (4) Long-term stability – under normal storage conditions

[0085] The long-term stability, i.e. the stability of the samples under normal storage conditions, was tested using classical stability study methods. According to the principle of "dense first, sparse later", two units of samples were randomly selected for testing in years 0, 0.5, 1, 2, 5 and 10 respectively. Each unit of sample was tested twice in parallel (the test data of each pair of samples was recorded in the same way as above). The test data were analyzed and tested using the linear fitting method.

[0086] The test data and results are shown in Table 4.

[0087] Table 4. Analysis of long-term stability data of copper in copper concentrate samples

[0088]

[0089] As shown in the table above, the stabilized samples exhibit good long-term stability, with no significant changes in their values ​​over at least 10 years.

[0090] (5) Long-term stability – stability after opening

[0091] Classical stability study methods were used to test the stability after opening the bottle, that is, the stability of the sample under normal storage conditions after the packaging is removed. A unit mineral standard material is generally used up within six months to one year. In order to fully examine its stability after opening the bottle, it was monitored for 5 years, and the same opened sample was tested in year 0, year 1, year 2, year 3, year 4 and year 5.

[0092] The test was performed in parallel four times (each sample was tested four times in parallel, and the results were recorded as 1, 2, 3, and 4 in the table). The test data were analyzed and tested using the linear fitting method. The test data and test results are shown in Table 5 below.

[0093] Table 5. Analysis of the open-bottle stability data of copper in copper concentrate samples

[0094]

[0095] As shown in the table above, the stabilized samples exhibit good stability after opening, and the values ​​will not change significantly within at least 5 years.

[0096] Comparative Example 1-1

[0097] This experimental example also provides a control experiment on the stabilization treatment of copper concentrate analytical standard materials, which did not employ an aging process and included the following steps:

[0098] S1, Purchase mineral raw materials for preparing mineral standard substances: 300 kg of copper concentrate.

[0099] S2, Preprocessing

[0100] In Changchun, Jilin Province, the purchased mineral raw materials are initially crushed using a jaw crusher.

[0101] S3, grind evenly

[0102] The aged mineral material was ground to a particle size of less than 200 mesh, dried at 100℃ to constant weight, cooled to room temperature, and homogenized to obtain homogenized mineral material that passed the homogenization test.

[0103] S4, Packaging and Sealing

[0104] The homogenized and qualified mineral material is divided into the smallest packaging unit, 50g / unit. Each unit of material is vacuum sealed. After sealing, it is observed for one week to ensure that there is no air leakage. Then, the sealed material is transferred to plastic bottles and sealed with aluminum foil. The processed mineral material is then obtained.

[0105] The stability after opening was tested using classical stability study methods, i.e., the stability of the sample after removing the packaging under normal storage conditions. The samples were monitored for 5 weeks, with tests performed on the same opened package at weeks 0, 1, 2, 3, 4, and 5.

[0106] The test was performed in parallel four times (each sample was tested four times in parallel, and the results were recorded as 1, 2, 3, and 4 in the table). The test data were analyzed and tested using the linear fitting method. The test data and test results are shown in Table 6.

[0107] Table 6. Analysis of Opening Stability Data of Copper in Copper Concentrate Samples

[0108]

[0109] In this embodiment, the product was treated with mineral standard material that had not undergone "aging" treatment, and the stability of the target copper element could not meet the requirements.

[0110] Example 2: Stabilization and Detection Methods for Standard Reference Materials for Gold Ore Composition Analysis

[0111] Example 2-1

[0112] This experimental example provides a method for stabilizing standard reference materials for gold ore composition analysis, including the following steps:

[0113] S1, Purchasing mineral raw materials for preparing mineral standard substances.

[0114] Gold ore: 500kg of raw ore, with a gold content of approximately 2.6g / t.

[0115] S2, Preprocessing

[0116] In Changchun, Jilin Province, purchased mineral raw materials are initially crushed using a jaw crusher to obtain pre-treated mineral materials.

[0117] S3, Aging

[0118] In Changchun City, Jilin Province, the crushed mineral raw materials were spread out on waterproof tarpaulins and air-dried in the open air for 15 months, from June 2013 to August 2014. For specific gradient control parameters during the aging process, please refer to Example 1-1.

[0119] During the drying process, cover the raw materials with waterproof tarpaulins during rainy or snowy weather to prevent them from getting wet. When the temperature is high and there is plenty of sunshine, turn the mineral raw materials regularly to ensure that they have full contact with air and sunlight, thus obtaining weathered mineral materials.

[0120] S4, grind evenly

[0121] The weathered mineral material was ground to a particle size of less than 200 mesh, dried at 100℃ to constant weight, cooled to room temperature, and homogenized to obtain homogenized mineral material that passed the homogenization test.

[0122] S5, repackaging and sealing

[0123] The homogenized mineral material that passed the homogenization test was divided into the smallest packaging unit (500g / unit). Each unit of raw material was vacuum sealed. After sealing, it was observed for one week to ensure that there was no air leakage. Then, the sealed raw material was transferred to a plastic bottle and the plastic bottle was heat-sealed with aluminum foil to obtain the standard substance stabilized mineral material.

[0124] This embodiment further tests the short-term and long-term stability of the stabilized mineral material. The test methods and steps are the same as those in Example 1-1, which test the high temperature experiment, low temperature experiment, shock experiment, long-term stability under normal storage conditions, and long-term stability of the opened sample under normal storage conditions.

[0125] In this embodiment, the method for testing the content of the target gold element (Au) is the fire assay gravimetric method (GB / T20899.1-2019).

[0126] The sample was prepared and melted to obtain lead buckles containing precious metals of appropriate quality and brittle slag. Gold and silver were separated from the lead buckles by ash blowing to obtain gold-silver granules. After gold separation with nitric acid, the gold content of the granules was determined by gravimetric method.

[0127] (1) Short-term stability - high temperature test

[0128] Eight units of samples were randomly selected and numbered 1 to 8. They were placed in a constant temperature chamber at 60℃. Samples 1 and 2 were removed on day 0, samples 3 and 4 on day 1, samples 5 and 6 on day 3, and samples 7 and 8 on day 7. Samples 1 to 8 were then tested simultaneously. Each unit of sample was tested twice in parallel (for example, samples 1 and 2 were tested twice in parallel, resulting in four results, which were recorded as 1, 2, 3, and 4 in the table; the same method was used to record the data for other samples). The test data were analyzed and verified using the linear fitting method.

[0129] The statistical results of the high-temperature experiment are shown in Table 7 below.

[0130] Table 7. High-Temperature Experimental Data Analysis of Gold in Gold Ore Samples

[0131]

[0132] (2) Short-term stability – Low temperature test

[0133] Eight units of samples were randomly selected and numbered 1 to 8. They were placed in a freezer at -20°C. Samples 1 and 2 were taken out on day 0, samples 3 and 4 on day 1, samples 5 and 6 on day 3, and samples 7 and 8 on day 7. Samples 1 to 8 were then tested simultaneously. Each unit of sample was tested twice in parallel (the test data for every two samples were recorded in the same way as above). The test data were analyzed and verified using the linear fitting method.

[0134] The statistical results of the low-temperature experiment are shown in Table 8 below.

[0135] Table 8. Analysis of Low-Temperature Experimental Data of Gold in Gold Ore Samples

[0136]

[0137] (3) Short-term stability - shock test

[0138] Eight units of samples were randomly selected and numbered 1 to 8. They were placed on a shaker. Samples 1 and 2 were taken out on day 0, samples 3 and 4 were taken out on day 1, samples 5 and 6 were taken out on day 3, and samples 7 and 8 were taken out on day 7. Samples 1 to 8 were tested simultaneously. Each unit of sample was tested twice in parallel (the test data of every two samples was recorded in the same way as above). The test data were analyzed and verified using the linear fitting method.

[0139] The statistical results of the earthquake test are shown in Table 9 below.

[0140] Table 9. Analysis of shock test data for gold in gold ore samples.

[0141]

[0142] (4) Long-term stability – under normal storage conditions

[0143] The long-term stability, i.e. the stability of the samples under normal storage conditions, was tested using classical stability study methods. According to the principle of "dense first, sparse later", two units of samples were randomly selected for testing in years 0, 0.5, 1, 2, 5 and 10 respectively. Each unit of sample was tested twice in parallel (the test data of each pair of samples was recorded in the same way as above). The test data were analyzed and tested using the linear fitting method.

[0144] The statistical results of the long-term stability test are shown in Table 10 below.

[0145] Table 10 Analysis of long-term stability data of gold in gold ore samples

[0146]

[0147] (5) Long-term stability – stability after opening

[0148] Classical stability study methods were used to test the stability after opening the bottle, that is, the stability of the sample under normal storage conditions after the packaging is removed. A unit mineral standard material is generally used up within six months to one year. In order to fully examine its stability after opening the bottle, it was monitored for 5 years, and the same opened sample was tested in year 0, year 1, year 2, year 3, year 4 and year 5.

[0149] The test was performed in parallel four times (each sample was tested four times in parallel, and the results were recorded as 1, 2, 3, and 4 in the table). The test data were analyzed and verified using the linear fitting method. The statistical results of the long-term stability test after opening are shown in Table 11 below.

[0150] Table 11 Analysis of Opening Stability Data of Gold in Gold Ore Samples

[0151]

[0152] Comparative Example 2-1

[0153] This experimental example also provides a control experiment on the stabilization treatment method for gold ore analytical standard materials. In the control experiment, the open-air aging time was only one quarter, that is, from September to November 2023, without gradient aging treatment, including the following steps:

[0154] S1, Purchase mineral raw materials for preparing mineral standard substances: 500 kg of gold ore.

[0155] S2, Preprocessing

[0156] In Changchun, Jilin Province, purchased mineral raw materials are initially crushed using a jaw crusher to obtain pre-treated mineral materials.

[0157] S3, Aging

[0158] In Changchun, Jilin Province, the crushed mineral raw materials were spread out on waterproof tarpaulins and air-dried in the open air for a period of three months, from September to November 2023.

[0159] During the drying process, cover the raw materials with waterproof tarpaulins during rain or snow to prevent them from getting wet. When the temperature is high and there is plenty of sunshine, turn the mineral raw materials regularly to obtain weathered mineral materials.

[0160] S4, grind evenly

[0161] The weathered mineral material was ground to a particle size of less than 200 mesh, dried at 100℃ to constant weight, cooled to room temperature, and homogenized to obtain homogenized mineral material that passed the homogenization test.

[0162] S5, repackaging and sealing

[0163] The homogenized mineral material that passed the homogenization test was divided into the smallest packaging unit, 500g / unit. Each unit of raw material was vacuum sealed. After sealing, it was observed for one week to ensure that there was no air leakage. Then the sealed raw material was transferred to a plastic bottle and sealed with aluminum foil heat sealing to obtain the standard substance stabilized mineral material.

[0164] The stability after opening was tested using classical stability study methods, i.e., the stability of the sample after removing the packaging under normal storage conditions. The samples were monitored for 5 weeks, with tests performed on the same opened package at weeks 0, 1, 2, 3, 4, and 5.

[0165] The test was performed in parallel four times (each sample was tested four times in parallel, and the results were recorded as 1, 2, 3, and 4 in the table). The test data were analyzed and tested using the linear fitting method. The test data and test results are shown in Table 12.

[0166] Table 12 Analysis of Opening Stability Data of Gold in Gold Ore Samples

[0167]

[0168] In other words, mineral standard materials that have not undergone effective "aging" treatment cannot meet the stability requirements.

[0169] It should be noted that the above embodiments are only for further elaboration and explanation of the technical solution of the present invention, and are not intended to further limit the technical solution of the present invention. The method of the present invention is only a preferred embodiment and is not intended to limit the scope of protection of the present invention. Any modifications, equivalent substitutions, improvements, etc., made within the spirit and principles of the present invention should be included within the scope of protection of the present invention.

Claims

1. A method for stabilizing mineral standard materials, characterized in that, Includes the following steps: Obtaining raw materials for mineral standard reference materials; Preprocessing; The mineral material is pretreated by aging, and the aging process involves gradient control of temperature, humidity, light intensity, light duration, wind speed, and treatment time to obtain aged mineral material. The aged mineral material is dried to constant weight and then ground to obtain homogenized mineral material; The homogenized mineral material is packaged and sealed to obtain the standard substance stabilized mineral material. The aging process includes at least four stages of gradient control of process parameters: First-stage process parameters: temperature 25℃~35℃, humidity 70~85%, light intensity 70000~100000 Lx, light duration 14~15 h, wind speed 2~3, treatment duration 3~4 months; Second stage process parameters: temperature 2 ℃~27 ℃, humidity 55~75%, light intensity 50000~70000 Lx, light duration 9~12 h, wind speed 3~4, treatment duration 3~4 months; The third stage of process parameters are: temperature -30℃~-10℃, humidity 50~70%, light intensity 30000~50000 Lx, light duration 8~9 h, wind speed 3~4, and treatment time 3~4 months. The fourth stage process parameters are: temperature -4℃~15℃, humidity 40~60%, light intensity 60000~80000 Lx, light duration 11~13 h, wind speed 4~5, and treatment time 3~4 months.

2. The mineral standard material stabilization treatment method according to claim 1, characterized in that, The aging process includes at least four stages of gradient-controlled process parameters: First-stage process parameters: temperature 30 ℃, humidity 80%, light intensity 90000 Lx, light duration 14 h, wind speed level 2, treatment duration 3 months; Second-stage process parameters: temperature 20 ℃, humidity 65%, light intensity 60000 Lx, light duration 10 h, wind speed level 3, treatment duration 3 months. The third stage of process parameters are: temperature -20℃, humidity 60%, light intensity 40000 Lx, light duration 8 h, wind speed level 3, and treatment time 3 months. The fourth stage process parameters are: temperature 10℃, humidity 50%, light intensity 70000 Lx, light duration 11 h, wind speed level 4, and treatment time 3 months.

3. The method for stabilizing mineral standard materials according to claim 1 or 2, characterized in that, The raw materials for the mineral standard material are metallic ores or concentrates.

4. The method for stabilizing mineral standard materials according to claim 1 or 2, characterized in that, The pretreatment includes preliminary crushing using a jaw crusher.

5. The method for stabilizing mineral standard materials according to claim 1 or 2, characterized in that, The drying temperature of the aged mineral materials is 100~105℃.

6. The method for stabilizing mineral standard materials according to claim 1 or 2, characterized in that, The sealing process includes: vacuum sealing the packaged homogenized mineral material, observing for any leakage, and then transferring it to a plastic bottle for aluminum foil heat sealing.

7. A method for testing the stability of mineral standard references, characterized in that, include: The standard substance stabilized mineral material is obtained according to the method of any one of claims 1 to 6; The stabilized mineral materials of the standard substance were subjected to short-term and / or long-term stability tests. The stability test data were obtained by performing 2 to 4 parallel tests, using a linear fitting method y= β 1X+ β 0 was analyzed and tested, based on To determine the stability of the content of the standard substance.

8. The method for testing the stability of mineral standard materials according to claim 7, characterized in that, The short-term stability test includes high-temperature test, low-temperature test and / or shock test.

9. The method for testing the stability of mineral standard materials according to claim 7, characterized in that, The long-term stability test includes testing the stability of the standard substance content in the stabilized mineral material after opening and removing the packaging, under normal storage conditions.

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