Preparation method and testing method of mineral capability verification sample

Abstract

The present application relates to the technical field of mineral detection, and particularly provides a preparation method and a detection method of a mineral proficiency verification sample. The method comprises the following steps: determining target element types and content ranges to be detected in mineral proficiency verification, screening and determining mineral raw materials used in the proficiency verification, grinding and mixing, performing initial detection of uniformity, determining data results and method applicability by using a specific formula, and then verifying the accuracy of the detection data and the reliability of the proficiency verification results by using F test, t test and the like.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of mineral detection, and particularly relates to a preparation method and a detection method of a mineral proficiency testing sample. BACKGROUND

[0002] Proficiency testing refers to an activity for evaluating the proficiency of participants according to pre-prepared rules, and is usually performed through inter-laboratory comparison to show the reliability of the measurement results of a laboratory.

[0003] A proficiency testing sample refers to a detection sample specially used for proficiency testing activities. The sample is prepared by a proficiency testing provider and distributed to each participating laboratory, and the participating laboratory detects the sample according to the daily detection process without knowing or partially knowing the sample, and returns the result to the organizer. The detection technology and reliability of the participating detection laboratory are evaluated through the proficiency testing sample. The consistency of the proficiency testing sample in time and space is crucial for the proficiency testing activities using inter-laboratory comparison. When implementing the proficiency testing plan, the organizer should ensure that the unsatisfactory results in the proficiency testing are not attributed to the variability between or among the samples. Therefore, the proficiency testing sample must be effectively prepared and detected. A scientific and reasonable preparation method and a qualified detection method of the mineral proficiency testing sample are prerequisites for ensuring the smooth implementation of the proficiency testing plan.

[0004] At present, there is a lack of a relatively scientific and effective preparation and detection scheme for the proficiency testing sample of the mineral. SUMMARY

[0005] Therefore, it is necessary to provide a preparation method and a detection method of a mineral proficiency testing sample.

[0006] The present application adopts the following technical scheme:

[0007] The present application provides a preparation method of a mineral proficiency testing sample, which comprises the following steps: determining the target element type and the content range to be detected in the mineral proficiency testing; screening mineral raw materials meeting the requirements of the target element type and the content range; drying the mineral raw materials to a constant weight, cooling, and obtaining dried mineral materials; grinding the dried mineral materials to ensure that the particle sizes meet the requirement that 98% is less than 200 mesh (0.074 mm), and obtaining ground mineral materials; uniformly mixing all the ground mineral materials, and obtaining the mineral proficiency testing sample. Preferably, a ball mill or a rod mill is used to grind the dried mineral materials, and a V-shaped mixer or a three-dimensional mixer is used to uniformly mix the ground mineral materials.

[0008] The application further provides a testing method for a mineral proficiency testing sample, comprising the following steps: preparing the mineral proficiency testing sample according to the preparation method; performing initial homogeneity testing on the mineral proficiency testing sample, performing F testing on the detection result of the initial homogeneity testing by using a single-factor variance method, and preliminarily judging whether the homogeneity meets the requirement that a statistical value (F) is less than a critical value (F alpha); if the initial homogeneity testing meets the preset requirement, performing secondary homogeneity testing, which comprises determining the suitability of an analysis method, and the determination formula is as follows:

[0009]

[0010] In the formula, n represents the number of detections, S represents the standard deviation of the detection result, and r represents the repeatability limit of the national standard method.

[0011] If the determination result of the suitability of the analysis method meets the preset requirement, performing detection result analysis on the detection sequence and the processing sequence, and judging whether the requirement is met; if the determination result of the suitability of the analysis method does not meet the preset requirement, discarding the obtained analysis result and replacing the analysis method; if the analysis result of the detection sequence or the processing sequence does not meet the preset requirement, judging that the mineral proficiency testing sample is unqualified; if the analysis result of the detection sequence or the processing sequence meets the preset requirement, determining that the secondary homogeneity testing is qualified; if the secondary homogeneity testing meets the preset requirement, performing stability testing, and judging whether the stability meets the preset requirement; if the stability testing does not meet the preset requirement, judging that the mineral proficiency testing sample is unqualified.

[0012] If the stability testing meets the preset requirement, performing re-detection on the sample, and analyzing and judging whether the stability of the sample can cover the entire proficiency testing period by using a t test method; if the verification meets the requirement, determining that the mineral proficiency testing sample is qualified, otherwise, determining that the mineral proficiency testing sample is unqualified.

[0013] In some embodiments, the method steps of the initial homogeneity testing are as follows: laying the mineral proficiency testing sample flat, uniformly dividing the sample into N regions, numbering each region from left to right and from top to bottom as region 1 to region N, respectively taking sufficient quality samples from the upper part, the middle part and the lower part of each region into three sample bags, completing sampling, and numbering the initial testing samples in the order of 1-1, 1-2, 1-3,..., N-1, N-2, N-3 according to the region number;

[0014] If N is even and N is greater than or equal to 3, the initial testing sample target element content is detected in the following order under the same conditions: 1-1—2-1—3-1—4-1—5-1,..., —N-1.

[0015] N-2,..., —5-2—4-2—3-2—2-2—1-2.

[0016] 1-1—2-1—3-1—4-1—5-1···—N-1;

[0017] If N is odd and N>=3, the detection is carried out in the same condition according to the following order:

[0018] 1-1—2-1—3-1—4-1—5-1···—N-1;

[0019] N-2···—5-2—4-2—3-2—2-2—1-2;

[0020] 1-1—2-1—3-1—4-1—5-1···—N-1;

[0021] In some embodiments, the uniformity double-check sampling method comprises: sub-packaging the samples qualified in the uniformity preliminary check, a total of X units are sub-packaged, and the sub-packaging order is numbered 1-X; Y units are randomly taken out and the numbers 1-Y are recorded, and sampling and detection are carried out again according to the sampling method and detection order of the uniformity preliminary check.

[0022] In some embodiments, the corresponding relationship between the number Y of extracted units and the total number X of units is: if X<=100, Y takes Max (3, 10%X); if 100X<=200, Y>=11; if 200X<=500, Y>=15; if 500X<=1000, Y>=25; and if X>=1000, Y=30.

[0023] In some embodiments, the stability test comprises: respectively carrying out 7-day simulation experiments on the samples under the condition of shaking, taking samples on the 0th day, the 1st day, the 3rd day and the 7th day, and analyzing and testing the detection results by using the linear fitting method to determine whether the transportation condition affects the detection results.

[0024] In some embodiments, the linear fitting method is used for analysis to determine whether the detection order and the processing order affect the detection results; and the single factor variance method (F test) is used for analysis to determine whether the uniformity of the sub-packaged samples meets the requirements.

[0025] Compared with the prior art, the core advantages and beneficial effects of the present application are:

[0026] The mineral capacity verification sample preparation method of the present application is prepared by screening mineral raw materials, calculating the proportion, drying, grinding, weighing, and mixing, especially by meeting the requirement that 98% of the particle size is less than 200 mesh (0.074 mm), which ensures the consistency of the samples in time and space as a whole, and can meet the requirements of different capacity verification plans for the types of mineral capacity verification samples, the types and contents of elements contained.

[0027] This invention explores a formula for determining the applicability of analytical methods used in homogeneity testing for mineral proficiency testing. This formula can relatively scientifically and quickly eliminate interference from analytical methods in homogeneity testing. It also combines one-way variance method (F-test) and linear fitting method to eliminate the influence of testing order and processing order on the test results. In the sample stability testing process, not only is the t-test used to determine whether the sample stability can cover the entire proficiency testing program cycle, but the linear fitting method is also used to eliminate the influence of the transportation process on sample stability. Through simultaneous stability and classical stability studies, the accuracy of mineral proficiency testing sample test results and the reliability of proficiency testing results are comprehensively guaranteed. Attached Figure Description

[0028] Figure 1 This is a trend analysis chart of Au, Ag, and Cu content in the gold concentrate proficiency testing sample from Example 1.

[0029] Figure 2 This is a production trend analysis chart of Au, Ag, and Cu content in the gold concentrate capability verification sample of Example 1.

[0030] Figure 3 This is a trend analysis chart of Au, Ag, and Pb content in the lead concentrate proficiency testing sample from Example 2.

[0031] Figure 4 This is a production trend analysis chart of Au, Ag, and Pb content in the lead concentrate capability verification sample from Example 2.

[0032] Figure 5 A graph showing the processing trend of Cu content in the copper concentrate capability verification samples for comparative analysis. Detailed Implementation

[0033] 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.

[0034] In this invention, the standards for detecting the content of target elements in mineral materials are as follows:

[0035] The gold element (Au) content detection method is fire assaying gravimetric method (GB / T7739.1-2019 "Gold concentrate chemical analysis method Part 1 Determination of gold and silver content"), the test material is prepared by batching and melting to obtain a lead button containing noble metals and a brittle molten slag. Gold and silver are separated from the lead button by ash blowing to obtain a gold-silver alloy. After the alloy is separated by nitric acid, the gold content is measured by gravimetric method.

[0036] The silver element (Ag) content detection method is flame atomic absorption spectrometry (GB / T7739.2-2019 "Gold concentrate chemical analysis method Part 2 Determination of silver content Flame atomic absorption spectrometry"), the test material is decomposed by hydrochloric acid, nitric acid and perchloric acid. In a dilute hydrochloric acid medium, the absorbance value of silver is measured at a wavelength of 328.1 nm on a flame atomic absorption spectrometer with an air-acetylene flame. The silver content is calculated according to the standard curve method.

[0037] The copper element (Cu) content detection method is flame atomic absorption spectrometry (GB / T7739.4-2021 "Gold concentrate chemical analysis method Part 4 Determination of copper content"), the test material is decomposed by hydrochloric acid, nitric acid and perchloric acid. In a dilute hydrochloric acid medium, the absorbance value of copper is measured at a wavelength of 324.7 nm on a flame atomic absorption spectrometer with an air-acetylene flame. The copper content is calculated according to the standard curve method.

[0038] The lead element (Pb) content detection method is EDTA titration method (GB / T8152.1-2006 "Lead concentrate chemical analysis method Determination of lead content Acid dissolution-EDTA titration method"), the test material is dissolved with nitric acid, sulfuric acid and bromine water, and treated with hydrobromic acid to remove arsenic, antimony and tin. Lead is separated from other interfering elements by lead sulfate precipitation, and the precipitate is dissolved in ammonium acetate solution. Lead is titrated in EDTA titration solution with dimethyl phenol orange as the indicator.

[0039] The zinc element (Zn) content detection method is precipitation separation-EDTA titration method (GB / T8151.1-2012 "Zinc concentrate chemical analysis method Part 1 Determination of zinc content Precipitation separation-EDTA titration method"), the test material is dissolved with hydrochloric acid, nitric acid and sulfuric acid, and the coexisting elements such as iron, manganese and lead are separated by precipitation. A small amount of interfering elements is masked by adding a masking agent to the filtrate. In a pH 5-6 acetic acid-sodium acetate buffer solution, dimethyl phenol orange is used as the indicator, and EDTA standard titration solution is used for titration. The measured result is the combined amount of zinc and cadmium, and the cadmium amount is deducted to obtain the zinc amount.

[0040] The following examples are provided for illustration.

[0041] Example 1

[0042] The present embodiment provides a preparation method and testing method for gold concentrate proficiency testing samples, comprising the following steps:

[0043] S1, determine the target element type and content range to be detected for gold concentrate capacity verification.

[0044] Gold element (Au) content: 40-50 g / t; silver element (Ag) content: 100-200 g / t; copper element (Cu) content: <2%.

[0045] S2, screen mineral raw materials that meet the target element type and content range requirements.

[0046] After investigation, there is a gold concentrate raw material on the market that meets the target element type and content range requirements: gold content is about 44 g / t, silver content is about 130 g / t, and copper content is about 0.6%.

[0047] S3, determine the rough amount of mineral raw materials required for gold concentrate capacity verification.

[0048] Determine about 10 kg of gold concentrate raw material that meets the target element type and content range requirements.

[0049] S4, prepare the gold concentrate capacity verification sample.

[0050] Dry the gold concentrate raw material at 100°C until the weight is constant (take out and weigh every 1 hour until the weight no longer changes), and then cool it in a dryer to obtain the dried mineral material. Grind the dried mineral material in a rod mill to ensure that the particle size meets the requirement of 98% less than 200 mesh, and then obtain the ground mineral material. Further mix the ground mineral material in a three-dimensional mixer to obtain the ground and mixed gold concentrate sample.

[0051] S5, perform initial inspection of the uniformity of the ground and mixed gold concentrate sample.

[0052] Place the ground and mixed gold concentrate sample on a plastic film and evenly divide it into 6 areas (m). Number each area from left to right and top to bottom as 1-6, and then take enough mass of the ground and mixed gold concentrate sample from the surface, middle and lower layers of each area, respectively, and number them as 1-3. Place them in 3 sample bags, and detect them in the order of 1-1 (area number 1 + upper layer number 1), 1-2, 1-3, 2-1··· 6-3 (area number 6 + lower layer number 3).

[0053] Under the same conditions, detect the Au, Ag and Cu contents in the following sample taking order:

[0054] 1-1—2-1—3-1—4-1—5-1—6-1;

[0055] 6-2—5-2—4-2—3-2—2-2—1-2;

[0056] 1-3—3-3—5-3—2-3—4-3—6-3.

[0057] The homogeneity preliminary test results were analyzed by single factor variance method (F test), and the content tests of Au, Ag and Cu were shown in the following tables:

[0058] Table 1 Statistics and results analysis of Au homogeneity preliminary test data of mixed grinding gold concentrate samples

[0059]

[0060] Table 2 Statistics and test results of Ag homogeneity preliminary test data of mixed grinding gold concentrate samples

[0061]

[0062] Table 3 Statistics and test results of Cu homogeneity preliminary test data of mixed grinding gold concentrate samples

[0063]

[0064] The mixed grinding gold concentrate samples that passed the homogeneity preliminary test were divided into 80 bags and numbered as 01-80. 8 bags were randomly taken out and numbered as 1-8. Each bag of sample was tested in parallel for 3 times. The measurement data was analyzed by linear fitting method to determine whether the test sequence and processing sequence affected the test results. Then, single factor variance method (F test) was used for analysis to determine whether the homogeneity of the divided samples met the requirements. The sampling sequence number and sample number were shown in the following table:

[0065] Table 4 Sampling sequence number and sample number of gold concentrate samples

[0066]

[0067] The test sequence numbers of the 8 gold concentrate samples were: 1-2-3-4-5-6-7-8, 8-7-6-5-4-3-2-1, 1-3-5-7-2-4-6-8. A total of 24 test records were recorded as test sequence numbers 1 to 24 (see the following table). The test results were shown in the following table:

[0068] Table 5 Test sequence number and test results of gold concentrate samples

[0069]

[0070] The following determination formula was used to confirm the applicability of the detection and analysis method:

[0071]

[0072] In the formula: S—standard deviation of test data;

[0073] n—number of tests;

[0074] r - repeatability limit of national standard method.

[0075] The calculation results are shown in the following table:

[0076] Table 6 Determination results of the applicability of each element detection method in gold concentrate samples

[0077]

[0078] Further, the linear fitting method is used to determine whether the detection order and processing order have a significant impact on the detection analysis results, and the F test is used to determine whether the uniformity of the sub-packaged samples meets the requirements.

[0079] According to the detection order number, the detection results are analyzed, and the analysis results are shown in the following table: Figure 1 and the following table:

[0080] Table 7 Trend analysis of Au, Ag, and Cu in gold concentrate samples

[0081]

[0082] According to the correspondence between the extracted sample number and the original sample number, the detection results are reordered in the order of the original number from small to large, and then the detection results are analyzed according to the production order. The analysis results are shown in the following table:

[0083] Table 8 Trend analysis of Au, Ag, and Cu in gold concentrate samples

[0084]

[0085] Based on the confirmation that the detection order and production order have no significant impact on the detection results, the F test method is used to analyze the detection data to determine whether the uniformity is qualified. The analysis results are shown in the following table:

[0086] Table 9 Uniformity test of gold in gold concentrate samples

[0087]

[0088] Table 10 Uniformity test of silver in gold concentrate samples

[0089]

[0090] Table 11 Uniformity test of copper in gold concentrate samples

[0091]

[0092] After the homogeneity test is passed, the stability test is performed on the sample. In order to test the stability of the sample under transportation conditions, the sample that has passed the homogeneity test is subjected to a 7-day simulation experiment under shaking conditions, and samples are taken at four time points of 0 days, 1 day, 3 days and 7 days. The samples are respectively extracted for detection, and the detection data is analyzed by linear fitting method to determine whether the transportation conditions affect the detection results. After all the participants in the proficiency testing return the detection data, the remaining sample is detected again, and the measurement data is analyzed by t-test method to determine whether the stability of the sample can cover the entire proficiency testing period. The detection results of the gold concentrate sample after shaking experiment and data analysis are shown in the following table:

[0093] Table 12 Data analysis of gold in gold concentrate sample after shaking experiment

[0094]

[0095] Table 13 Data analysis of silver in gold concentrate sample after shaking experiment

[0096]

[0097] Table 14 Data analysis of copper in gold concentrate sample after shaking experiment

[0098]

[0099] After the detection data of all the participants in the proficiency testing is returned, the prepared proficiency testing sample is detected again and compared with the detection data before the sample is sent. The detection data and comparison results are shown in the following table:

[0100] Table 15 Data analysis of gold in gold concentrate sample for stability test

[0101]

[0102] Table 16 Data analysis of silver in gold concentrate sample for stability test

[0103]

[0104] Table 17 Data analysis of copper in gold concentrate sample for stability test

[0105]

[0106] Example 2

[0107] The embodiment provides a preparation method and a test method of a lead concentrate proficiency testing sample, which comprises the following steps:

[0108] S1, determining the target element type and content range to be detected in the lead concentrate proficiency testing.

[0109] The content of gold element (Au) is 2-5 g / t; the content of silver element (Ag) is 500-1000 g / t; and the content of lead element (Pb) is >60%.

[0110] S2, screening of mineral raw materials and crude dosage meeting the requirements of target element types and content range.

[0111] It is found that the commercially available single lead concentrate raw materials cannot meet the requirements of target element types and content range, and it is necessary to use commercially available lead concentrate raw materials and high-grade gold concentrate raw materials for preparation:

[0112] The commercially available lead concentrate raw materials have a gold content of about 0.8 g / t, a silver content of about 800 g / t, and a lead content of about 67%.

[0113] The commercially available high-grade gold concentrate raw materials have a gold content of about 450 g / t, a silver content of about 300 g / t, and a lead content of about 8%.

[0114] It is determined that about 10 kg of mineral raw materials are required for the capacity verification of gold concentrate, and the dosage ratio of the mineral raw materials meeting the requirements of target element types and content range is calculated: about 9 kg of lead concentrate raw materials and about 1 kg of high-grade gold concentrate raw materials.

[0115] S3, preparation of lead concentrate capacity verification sample.

[0116] The commercially available lead concentrate raw materials and high-grade gold concentrate raw materials are respectively dried to constant weight at 100°C (removed every 1 hour for weighing until the weight no longer changes), and then naturally cooled in a dryer to obtain dried mineral materials. The dried mineral materials are respectively ground in a rod mill to ensure that the particle size meets the requirement of 98% less than 200 mesh to obtain ground mineral materials. The commercially available lead concentrate ground mineral materials and high-grade gold concentrate ground mineral materials are weighed according to a mass ratio of 9:1, and then fully mixed in a three-dimensional mixer to obtain the ground and mixed lead concentrate sample.

[0117] The ground and mixed lead concentrate sample is subjected to initial homogeneity test: the ground and mixed lead concentrate sample is evenly divided into 6 areas on a plastic film, each area is numbered 1-6 in order from left to right and from top to bottom, and then enough quality of ground mineral material sample is taken from the upper, middle and lower layers of each area respectively, and numbered 1-3, and then placed in 3 sample bags, and numbered in order of 1-1, 1-2, 1-3, 2-1 to 6-3. Under the same conditions, Au, Ag and Pb content detection is carried out in the same detection order as in the above example.

[0118] The results of Au, Ag and Pb content test and initial homogeneity test are analyzed by single factor variance method (F test) as shown in the following table:

[0119] Table 18 Statistical data and test results of initial homogeneity test of gold in lead concentrate sample

[0120]

[0121] Table 19 Statistics and test results of initial homogeneity test data of silver in lead concentrate samples

[0122]

[0123] Table 20 Statistics and test results of initial homogeneity test data of lead in lead concentrate samples

[0124]

[0125] On the basis of passing the initial homogeneity test, the samples were divided into 80 bags, numbered 1-80 according to the order of division. Eight bags were randomly selected by the random number list method, and numbered 1-8, and each sample was tested three times. The sampling sequence number and sample number are shown in the following table:

[0126] Table 21 Sampling sequence number and sample number of lead concentrate samples

[0127]

[0128] The eight lead concentrate samples were tested according to the above method, and the test sequence number and test results are shown in the following table:

[0129] Table 22 Test sequence number and test results of lead concentrate samples

[0130]

[0131] The following determination formula was used to confirm the applicability of the test method:

[0132] In the formula: S—standard deviation of test data; n—number of tests; r—repeatability limit of national standard method.

[0133] The calculation results are shown in the following table:

[0134] Table 23 Determination results of test method applicability of each element in lead concentrate samples

[0135]

[0136] The measurement data was analyzed by linear fitting method to determine whether the test sequence and processing sequence affected the test results; single factor variance method (F test) was used for analysis to determine whether the homogeneity of the divided samples met the requirements. The test results were analyzed according to the test sequence number, and the analysis results are shown in the following table:

[0137] Table 24 Analysis of test trend of gold in lead concentrate samples

[0138]

[0139] According to the correspondence between the extracted sample number and the original sample number, the detection results are reordered in ascending order of the original number, and the detection results are analyzed according to the production order. The analysis results are shown in the following table:

[0140] Table 25 Production trend analysis of gold in lead concentrate samples

[0141]

[0142] On the basis of confirming that the detection order and the production order have no significant effect on the detection results, the detection data is analyzed by F-test method to judge whether the uniformity is qualified. The analysis results are shown in the following table:

[0143] Table 26 Uniformity test of gold in lead concentrate samples

[0144]

[0145] Table 27 Uniformity test of silver in lead concentrate samples

[0146]

[0147] Table 28 Uniformity test of lead in lead concentrate samples

[0148]

[0149] After the uniformity test is qualified, the stability test of the sample is carried out. In order to test the stability of the sample under transportation conditions, the sample is subjected to 7-day simulation experiment under shaking condition, and the sample is detected on the 0th day, 1st day, 3rd day and 7th day. The detection data is analyzed by linear fitting method to judge whether the transportation condition affects the detection results.

[0150] After all the participants of the ability verification return the detection data, the remaining sample is detected again, and the measurement data is analyzed by t-test method to judge whether the stability of the sample can cover the whole ability verification period.

[0151] The detection results and data analysis of the lead concentrate sample after shaking experiment are shown in the following table:

[0152] Table 29 Data analysis of gold in lead concentrate samples after shaking experiment

[0153]

[0154] Table 30 Data analysis of silver in lead concentrate samples after shaking experiment

[0155]

[0156] Table 31 Analysis of the data of the shaking experiment of lead in the lead concentrate sample

[0157]

[0158] After the detection data of all the participants in the proficiency testing were returned, the prepared proficiency testing samples were detected again and compared with the detection data before the samples were sent, and the detection data and comparison results are shown in the following table:

[0159] Table 32 Analysis of the stability test data of gold in the lead concentrate sample

[0160]

[0161] Table 33 Analysis of the stability test data of silver in the lead concentrate sample

[0162]

[0163] Table 34 Analysis of the stability test data of lead in the lead concentrate sample

[0164]

[0165] From the above data, it can be seen that the uniformity and stability of the proficiency testing samples prepared by the detection and analysis method are good, and the proficiency testing sample qualification determination method is scientific and applicable.

[0166] Comparative Example 1

[0167] The present comparison provides a preparation method and a test method for a copper concentrate proficiency testing sample, and the difference between the preparation method steps of the present comparison and those of Example 1 is only that:

[0168] S1, determine the target elements to be detected in the copper concentrate proficiency testing: copper element (Cu) content of 10-20%.

[0169] S2, screen mineral raw materials meeting the requirements of target element types and content ranges.

[0170] After investigation, there is a copper concentrate raw material on the market: the copper content is about 19%.

[0171] The uniformity preliminary test results are analyzed by single factor variance method (F test), and the content of Cu is determined by flame atomic absorption spectrometry, and the results and analysis are shown in the following table:

[0172] Table 35 Data statistics and test results of the uniformity preliminary test of copper in the copper concentrate sample

[0173]

[0174] According to the above table data, a conclusion that the sample is not uniform will be given, but this conclusion is an incorrect conclusion given without determining the applicability of the detection method, and the reasons are as follows:

[0175] Using the decision formula The above data were analyzed.

[0176] The results are shown in the following table:

[0177] Table 36 Determination method judgment results of copper concentrate sample

[0178]

[0179] As can be seen from the above table, the detection method used is not suitable for uniformity test, that is, the conclusion that the uniformity test is unqualified may not be due to the insufficient uniformity of the sample itself, but due to the insufficient precision of the detection method, and the sample should be retested for uniformity using a suitable detection method.

[0180] Comparative Example 2

[0181] The present comparison provides a preparation method and a test method for a zinc concentrate proficiency testing sample, comprising the following steps:

[0182] S1, determining the target element types and content ranges to be detected for zinc concentrate proficiency testing.

[0183] The content of lead element (Pb) is 5-10%, and the content of zinc element (Zn) is 40-50%.

[0184] S2, screening mineral raw materials meeting the requirements of target element types and content ranges, and determining the coarse amount thereof.

[0185] It is found that there is a zinc concentrate raw material on the market: the lead content is about 6%, and the zinc content is about 43%. It is determined that about 10 kg of zinc concentrate raw material meeting the requirements of target element types and content ranges.

[0186] S3, preparing a gold concentrate proficiency testing sample.

[0187] The zinc concentrate raw material is dried at 100°C until constant weight, and then naturally cooled in a desiccator to obtain a dried mineral material. The dried mineral material is ground in a rod mill, and then taken out after 2 hours of grinding according to conventional experience to obtain a ground mineral material. The ground mineral material is further mixed in a three-dimensional mixer to obtain a ground and mixed zinc concentrate sample.

[0188] The ground and mixed zinc concentrate sample is subjected to initial uniformity test: the ground and mixed zinc concentrate sample is evenly divided into 6 regions on a plastic film, each region is numbered 1-6 in order from left to right and from top to bottom, and then sufficient quality of the ground mineral material sample is taken from the upper, middle and lower parts of each region, respectively, and numbered 1-3, and then placed in 3 sample bags. The ground mineral material sample in each small region is numbered in the order of 1-1, 1-2, 1-3, 2-1 to 6-3.

[0189] Under the same conditions, the Pb and Zn content detection was carried out in the following order of grinding mineral material sample sequence:

[0190] 1-1—2-1—3-1—4-1—5-1—6-1,

[0191] 6-2—5-2—4-2—3-2—2-2—1-2,

[0192] 1-3—3-3—5-3—2-3—4-3—6-3.

[0193] The homogeneity preliminary test result was analyzed by single factor variance method (F test), and the content test of Pb and Zn was shown in the following table:

[0194] Table 37 Statistics and test results of homogeneity preliminary test data of lead in zinc concentrate sample

[0195]

[0196] Table 38 Statistics and test results of homogeneity preliminary test data of zinc in zinc concentrate sample

[0197]

[0198] From the data in the above table, it can be seen that the sample homogeneity does not meet the requirements. After checking the grinding sample degree, it is found that the particle size is only 95% less than 200 mesh, which does not meet the requirement of at least 98% less than 200 mesh, thereby leading to the sample homogeneity failing to meet the requirements.

[0199] Comparative Example 3

[0200] The present comparison provides a preparation method and test method of copper concentrate capacity verification sample, which comprises the following steps:

[0201] S1, determining the target element to be detected in copper concentrate capacity verification: copper element (Cu) content 0.1-1.0%.

[0202] S2, screening mineral raw materials meeting the requirements of target element type and content range.

[0203] After checking, there is a kind of copper concentrate raw material on the market: the copper content is about 0.6%.

[0204] S3, determining the coarse amount of mineral raw materials required for copper concentrate capacity verification is about 10 kg.

[0205] Determine the gold concentrate raw material meeting the requirements of target element type and content range.

[0206] S4, preparing copper concentrate capacity verification sample.

[0207] The copper concentrate raw material is placed at 100°C and dried to constant weight (every 1 hour, take out and weigh until the weight no longer changes), and then placed in a dryer and naturally cooled to obtain a dried mineral material. The dried mineral material is placed in a rod mill for grinding to ensure that the particle size meets the requirement of 98% less than 200 mesh, and a ground mineral material is obtained. The ground mineral material is further mixed in a three-dimensional mixer to obtain a ground and mixed copper concentrate sample.

[0208] The ground and mixed copper concentrate sample is subjected to initial homogeneity testing. On the basis of passing the initial homogeneity testing, the sample is sub-packed, and 80 bags of copper concentrate samples are sub-packed, numbered 1-80 in sub-packing order, and 8 bags are randomly taken out according to the random number table method, and numbered 1-8, and each bag of sample is detected 3 times.

[0209] The detection order is: 1-2-3-4-5-6-7-8, 8-7-6-5-4-3-2-1, 1-3-5-7-2-4-6-8.

[0210] The measurement data is analyzed by single factor variance method (F test) to determine whether the homogeneity of the sub-packed sample meets the requirements. The sampling serial number and sample number of the copper concentrate sample are shown in the following table:

[0211] Table 39 Sampling serial number and sample number of copper concentrate sample

[0212]

[0213] The 8 copper concentrate samples taken out are detected according to the detection order, and the detection serial number and detection results are shown in the following table:

[0214] Table 40 Detection serial number and detection results of copper concentrate sample

[0215]

[0216] The detection data is analyzed by F test to determine whether the homogeneity of the sub-packed sample meets the requirements, and the analysis results are shown in the following table:

[0217] Table 41 Homogeneity test of copper in copper concentrate sample

[0218]

[0219] From the above table, it can be seen that the homogeneity of the copper concentrate proficiency testing sample meets the requirements. However, if only the F test result is used to determine that the sample meets the requirements, the subsequent determination process is continued, and then the sample is issued and the proficiency testing plan is implemented, which is easy to cause the detection data to be distorted, and the reasons are as follows:

[0220] After arranging the above data in ascending order according to the original number, the processing trend analysis is carried out, and the results are shown in the following table:

[0221] Table 42 Processing trend analysis of copper in copper concentrate samples

[0222]

[0223] From the above table, it can be seen that the copper concentrate proficiency testing sample values change significantly with the change of processing sequence, that is, there is a systematic error between different numbered samples, but only by F test cannot determine that there is a problem with sample uniformity, and in this case, the implementation of the proficiency testing plan will lead to the participants to appear due to sample problems The proficiency testing plan results are unqualified.

[0224] It should be pointed out here that the above examples are only limited to further illustrate and describe the technical solutions of the present application, and are not further limited to the technical solutions of the present application. The method of the present application is only a preferred embodiment, and is not used to limit the protection scope of the present application. Any modification, equivalent replacement, improvement, etc. within the spirit and principles of the present application shall be included in the protection scope of the present application.

Claims

1. A method of testing a mineral capability verification sample, characterized by, Comprising the following steps: The homogeneity preliminary inspection is performed on the mineral proficiency testing sample, the detection result of the homogeneity preliminary inspection is subjected to F test by using single factor variance method, and whether the homogeneity meets the preset requirement is preliminarily judged; If the homogeneity preliminary inspection meets the preset requirement, the homogeneity secondary inspection is performed, the homogeneity secondary inspection comprises the analysis method applicability judgment, and the judgment formula is: In the formula, n represents the detection times, S represents the standard deviation of the detection result, and r represents the repeatability limit of the national standard method; If the analysis method applicability judgment result meets the preset requirement, the detection result analysis of the detection sequence and the processing sequence is performed, whether the requirement is met is judged, if the analysis method applicability judgment result does not meet the preset requirement, the obtained analysis result needs to be discarded and the analysis method is replaced; If the analysis result of the detection sequence or the processing sequence does not meet the preset requirement, it is judged that the mineral proficiency testing sample is unqualified; If the analysis result of the detection sequence or the processing sequence meets the preset requirement, it is judged that the homogeneity secondary inspection is qualified; The stability test is performed, whether the stability meets the preset requirement is judged; If the stability test does not meet the preset requirement, it is judged that the mineral proficiency testing sample is unqualified; If the stability test meets the preset requirement, the proficiency testing period review detection is performed on the sample, whether the stability of the sample can cover the whole proficiency testing period is analyzed and judged by using t test method, if the verification meets the requirement, it is judged that the mineral proficiency testing sample is qualified, otherwise, it is judged that the mineral proficiency testing sample is unqualified; The mineral proficiency testing sample is prepared according to the following steps: The target element type and the content range to be detected in the mineral proficiency testing are determined; The mineral raw materials meeting the target element type and the content range requirement are screened; The mineral raw materials are dried to constant weight, and then cooled to obtain dried mineral materials; The dried mineral materials are ground to ensure that the particle sizes meet the requirement that 98% is less than 200 mesh, and then the ground mineral materials are obtained; All the ground mineral materials are uniformly mixed to obtain the mineral proficiency testing sample; The detection result analysis of the detection sequence and the processing sequence is performed by using linear fitting method to judge whether the influence of the detection sequence and the processing sequence on the detection analysis result is significant. The stability test comprises: the sample is subjected to 7-day simulation experiment under the condition of shaking, the sample is taken and detected on the 0th day, the 1st day, the 3rd day and the 7th day, the detection result is analyzed and tested by using linear fitting method, and whether the transportation condition influences the detection result is judged.

2. The method of claim 1, wherein the mineral capacity verification sample is a sample of a mineral material. The dried mineral materials are ground by using a ball mill or a rod mill.

3. The testing method for mineral proficiency testing samples according to claim 1 or 2, characterized in that, The ground mineral materials are uniformly mixed by using a V-shaped mixer or a three-dimensional mixer.

4. The method of claim 1, wherein the mineral capacity verification sample is a mineral sample. The method steps of the homogeneity preliminary inspection are as follows: The mineral proficiency testing sample is laid flat and uniformly divided into N regions, each region is numbered from left to right and from top to bottom as region 1-N, then enough quality samples are taken from the surface layer, the middle layer and the lower layer of each region and respectively placed in three sample bags, and the preliminary inspection sample numbers are sequentially numbered as 1-1, 1-2, 1-3···N-1, N-2, N-3 according to the region numbers; If N is even and N is greater than or equal to 3, the target element content detection of the preliminary inspection sample is sequentially performed under the same condition as follows: 1-1—2-1···—N-1； N-2···2-2—1-2； 1-3—3-3···—(N-1)-3—2-3···—N-3; If N is odd and N≥3, the detection is carried out in the same condition according to the following order: 1-1—2-1···—N-1； N-2···—2-2—1-2； 1-3—3-3···—N-3—2-3····—(N-1)-3.

5. The testing method for mineral proficiency testing samples according to claim 4, characterized in that, The sampling method in the second detection of uniformity comprises: The samples qualified in the first detection of uniformity are sub-packed, and the total number of sub-packing is X units, numbered 1~X according to the sub-packing order; Y units are randomly taken out and numbered 1~Y, and then sampling and detection are carried out again according to the sampling method and detection order of the first detection of uniformity.

6. The method of claim 5, wherein the mineral capacity verification sample is a mineral sample. The corresponding relationship between the number of units Y and the total number of units X is: If X≤100, Y takes Max(3, 10%X); If 100X≤200, Y≥11; If 200X≤500, Y≥15; If 500X≤1000, Y≥25; If X≥1000, Y=30.

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