A method for rapid initial determination of total rock re content of geological samples

Abstract

The application provides a kind of geological sample whole rock Re content fast preliminary measurement method, comprising: step one, collecting geological samples and carrying out superfine crushing;Step two, prepare the Re standard powder material same as the lithology of the geological sample;Step three, the geological sample after superfine crushing and the Re standard powder material are pressed respectively to prepare Re sample target and Re standard target;Step four, according to the Re standard target, the whole rock Re content fast preliminary determination of the Re sample target is carried out by laser in-situ analysis method.Using the preliminary measurement method, the whole preliminary measurement process only needs one hour, compared with the process of Re content preliminary measurement in the prior art which needs 5 days, the test time is saved, and the test analysis efficiency is improved;No chemical reagent is used in the whole whole rock Re content preliminary measurement process, cost is saved, and the best ratio test requirement of Re diluent is completely met, which provides a basis for the accurate measurement of whole rock Re content.

Description

Technical Field

[0001] This invention belongs to the field of preliminary determination of Re content, specifically relating to a rapid preliminary determination method for whole-rock Re content in geological samples. Background Technology

[0002] Currently, accurate determination of Re content in geological samples at the ppb-ppt level mainly employs isotope dilution combined with thermal ionization mass spectrometry or multiple receiver mass spectrometry (ID-NTIMS / ID-MC-ICP-MS). This process typically involves weighing the sample and then dissolving it in a Carius tube.

[0003] It takes two days to reach room temperature and open the tubes; from distilling to separate the interfering element Os, to enriching and purifying Re via anion exchange or acetone extraction, and preparing for instrumentation, another two days are needed; finally, instrumentation testing takes one day. One experimental procedure takes five days. However, to obtain accurate Re content results, two procedures are generally required: the first is mainly used for initial Re content determination to identify the optimal Re diluent ratio; the second is used for precise determination to obtain the accurate Re content. Thus, from initial dilution to obtaining accurate results, the entire process takes 10 days. Furthermore, the entire experimental process consumes a large amount of chemical reagents and equipment, resulting in high experimental costs.

[0004] In summary, existing methods for preliminary determination of Re content in geological samples suffer from problems such as complex analytical procedures, long testing cycles, and high testing costs, which cannot meet the testing needs of large batches of samples.

[0005] To address the aforementioned issues, it is necessary to propose a well-designed and effective method for rapid preliminary determination of Re content in whole-rock geological samples. Summary of the Invention

[0006] The present invention aims to solve at least one of the technical problems existing in the prior art, and to provide a rapid preliminary determination method for whole-rock Re content in geological samples.

[0007] This invention provides a rapid preliminary determination method for whole-rock Re content in geological samples, the method comprising:

[0008] Step 1: Collect geological samples and perform ultrafine grinding;

[0009] Step 2: Prepare Re standard powder material with the same lithology as the geological sample;

[0010] Step 3: The ultrafine pulverized geological sample and the Re standard powder are respectively compressed into tablets to prepare Re sample targets and Re standard targets;

[0011] Step 4: Based on the Re standard target, use laser in-situ analysis to rapidly and preliminarily determine the whole-rock Re content of the Re sample target.

[0012] Optionally, in step three, a sample powder pressing device for micro-area in-situ analysis is used to press the ultrafine pulverized geological sample and the Re standard powder material into tablets respectively; wherein,

[0013] The tableting device includes a base, a fixing ring, a splicing plate, a pressing column, an insert rod, a plastic ring, and a polyethylene powder filler.

[0014] The splicing plate consists of multiple pieces, all of which can be slidably connected to the upper surface of the base. The fixing ring can be slidably connected to the outer side wall of the base, and each splicing plate has a first limiting surface.

[0015] During tableting, multiple splicing plates slide and splice on the base, and multiple first limiting surfaces combine to form a groove. The fixing ring is sleeved on the outer periphery of the spliced ​​multiple splicing plates. The insertion rod passes through the fixing ring and is inserted into the base. The pressure column is inserted into the groove.

[0016] The plastic ring is disposed in the groove and is used to place geological sample powder. The polyethylene powder filler is used to fill the groove to cover the geological sample powder inside the plastic ring and the outside of the plastic ring.

[0017] Optionally, the tableting device further includes:

[0018] The base has a vertical sliding groove on its side wall. The fixing ring includes a ring body and a vertical slider. The vertical slider is provided on the inner side wall of the ring body. The ring body is sleeved on the base, and the vertical slider is slidably connected in the vertical sliding groove.

[0019] Optionally, the tableting device further includes:

[0020] The top wall of the base is provided with multiple horizontal sliding grooves. Each splicing plate includes a plate body and a first horizontal slider. The first horizontal slider is provided on one side of the plate body. When pressing the plate, the first horizontal slider is slidably connected in the horizontal sliding groove. The end face inside the plate body is the first limiting surface.

[0021] The splicing plate also includes a second horizontal slider, which is provided on the other side of the plate body. When the sample after pressing is taken out, the second horizontal slider can be slidably connected in the horizontal groove.

[0022] Optionally, in step four, the preliminary determination of whole-rock Re content of the Re sample target using laser in-situ analysis based on the Re standard target to obtain preliminary whole-rock Re content data of the geological sample includes:

[0023] Under the same laser and mass spectrometry experimental conditions, laser spot ablation was used to sequentially perform laser spot analysis on the Re standard target and the Re sample target, respectively.

[0024] The preliminary whole-rock Re content of the geological sample is obtained according to the following formula;

[0025] C2 = (A2 / A1) × C1,

[0026] Wherein, C2 represents the preliminary whole-rock Re content of the geological sample, C1 represents the whole-rock Re content of the Re standard powder material, A1 represents the measurement count of the Re standard target, and A2 represents the measurement count of the Re sample target.

[0027] Optionally, the laser spot size is 70μm to 80μm, and the dot dwell time is 0.4s to 0.5s.

[0028] Optionally, preparing Re standard powder material with the same lithology as the geological sample includes:

[0029] Collect alternative standard materials with the same lithology as the geological samples;

[0030] The candidate standard substances are subjected to ultrafine pulverization;

[0031] The crushed candidate standard substances were dispensed into multiple wide-mouth bottles and mixed evenly.

[0032] Optionally, the alternative standard material may be ground to a fineness of less than 200 mesh.

[0033] Optionally, after completing the dispensing of the candidate standard substances, the method further includes:

[0034] The homogeneity, stability, and normality of the setpoint data of the candidate standard substances were tested respectively.

[0035] Optionally, the collection of geological samples and ultrafine grinding includes:

[0036] Collect the geological samples and clean them with deionized water;

[0037] The geological sample was ultra-finely ground and pulverized using a ball mill to a mesh size below 200. The ultra-finely ground and pulverized geological sample was then mixed evenly to increase the uniformity of the sample.

[0038] This invention presents a rapid preliminary determination method for whole-rock Re content in geological samples. It innovatively proposes preparing Re sample targets and Re standard targets through pelleting, and then using laser in-situ analysis based on the Re standard targets to rapidly determine the whole-rock Re content of the Re sample targets. From the preparation of the Re sample targets to the rapid preliminary determination of whole-rock Re content based on the Re standard targets using laser in-situ analysis, the entire preliminary determination process takes only one hour, compared to the five days required by existing technologies. This significantly saves testing time and improves testing and analysis efficiency. Furthermore, the entire process of whole-rock Re content determination in geological samples does not use chemical reagents, saving costs and fully meeting the requirements of obtaining the optimal Re diluent ratio test quickly and cheaply, providing a foundation for accurate determination of whole-rock Re content. This whole-rock Re content preliminary determination process can also be used for rapid screening of Re resources in large batches of geological samples. Attached Figure Description

[0039] Figure 1 This is a flowchart illustrating a rapid preliminary determination method for whole-rock Re content in geological samples according to an embodiment of the present invention.

[0040] Figure 2 This is a perspective view of a sample powder tableting device for in-situ analysis of micro-area provided in another embodiment of the present invention.

[0041] Figure 3 This is a top view of a sample powder tableting device for in-situ analysis of micro-area provided in another embodiment of the present invention.

[0042] Figure 4 This is a side view of a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0043] Figure 5 This is a cross-sectional view of a sample powder tableting device for in-situ analysis of micro-area provided in another embodiment of the present invention.

[0044] Figure 6 The first perspective view of a base for a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0045] Figure 7 This is a second perspective view of a base for a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0046] Figure 8 This is a perspective view of a fixing ring for a sample powder tableting device for in-situ analysis of micro-area, provided in another embodiment of the present invention.

[0047] Figure 9This is a first perspective view of a splicing plate for a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0048] Figure 10 This is a second perspective view of a splicing plate for a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0049] Figure 11 This is a perspective view of a pressing column for a sample powder pressing device for in-situ micro-area analysis, provided in another embodiment of the present invention.

[0050] Figure 12 This is a perspective view of a plunger for a sample powder tableting device for in-situ micro-area analysis, provided in another embodiment of the present invention. Detailed Implementation

[0051] To enable those skilled in the art to better understand the technical solution of the present invention, the present invention will be further described in detail below with reference to the accompanying drawings and specific embodiments.

[0052] like Figure 1 As shown, this invention proposes a rapid preliminary determination method for whole-rock Re content in geological samples, the method comprising:

[0053] Step 1: Collect geological samples and perform ultrafine grinding.

[0054] Specifically, first, the geological samples are collected and cleaned with deionized water;

[0055] Secondly, the geological samples were ultra-finely ground and pulverized using a ball mill to a mesh size of less than 200. The ultra-finely ground and pulverized geological samples were then mixed evenly to increase the uniformity of the samples.

[0056] Step 2: Prepare Re standard powder material with the same lithology as the geological sample.

[0057] First, select alternative standard materials with the same lithology as the geological samples.

[0058] Specifically, if the geological sample is limestone, the candidate standard material is also collected from limestone to ensure that the lithology of the candidate standard material is consistent with that of the collected geological sample. In this embodiment, Re standard materials were developed from Permian limestone and Sinian black shale from the Dongchuanling area of ​​Guangde, Anhui Province, and two types of Re analytical standard materials for carbonate and silicate black rock formations were developed respectively.

[0059] Next, the candidate standard substances are subjected to ultrafine pulverization.

[0060] Specifically, the collected candidate standard substances are cleaned with deionized water, then ultra-finely ground to less than 200 mesh and mixed evenly.

[0061] Next, the pulverized candidate standard material is dispensed into multiple wide-mouth bottles and mixed evenly.

[0062] Specifically, the pulverized candidate standard material was dispensed into 100 2L wide-mouth plastic bottles, 10g per bottle. After dispensing, the bottles were shaken by hand to ensure thorough mixing. Each bottle was numbered for sampling to test homogeneity and stability.

[0063] Finally, the homogeneity, stability, and normality of the setpoint data of the candidate standard substances were tested.

[0064] Specifically, 12 bottles of limestone and 12 bottles of black shale candidate standard materials were selected, with 0.5g of each sample weighed. After dissolution, chemical separation, enrichment and purification, the homogeneity, stability and normality of the fixed value data were tested in sequence.

[0065] The mean value (AV1) of the limestone candidate standard material was 6.473 ppb, the inter-bottle standard deviation (s1) was 0.144, the total standard deviation within the bottle (s2) was 0.117, and the RSD (%, 2s, n=15) was 0.02. The mean value (AV1) of the black shale candidate standard material was 26.39, the inter-bottle standard deviation (s1) was 0.55, the total standard deviation within the bottle (s2) was 0.332, and the RSD (%, 2s, n=15) was 0.02. The results indicate that the homogeneity of the two black rock series candidate standard materials is good. Stability testing showed that the deviation of the test results over a 6-month interval did not exceed the standard deviation of the variance itself, and was consistent with the total mean value obtained from the fixed-value analysis, indicating good sample stability. The Shapiro-Wilk method was used to test the normality of all raw measurement data, determining the Re standard value for limestone reference material to be 6.473 ppb with an uncertainty of 0.016; and the Re standard value for black shale reference material to be 26.71 ppb with an uncertainty of 0.07. Through collaborative value determination research with the Institute of Geology and Geophysics, Chinese Academy of Sciences, the Re standard value for limestone reference material was determined to be 6.413 ppb with an uncertainty of 0.387; and the Re standard value for black shale reference material to be 25.85 ppb with an uncertainty of 0.27. The obtained results are consistent with those presented in this paper within the uncertainty range.

[0066] This embodiment provides a Re standard powder material for Re component analysis of geological samples, filling the gap in domestic Re standard materials, providing a solid guarantee for the accuracy and reliability of Re content analysis results, and meeting my country's needs for the development and utilization of rhenium resources.

[0067] Step 3: The ultrafine pulverized geological sample and the Re standard powder are pressed into tablets to prepare Re sample targets and Re standard targets, respectively.

[0068] Conventional tableting devices, due to the structure of the pressing mold, require a second reverse pressing after sample compression to remove the tablet, resulting in low efficiency and wasted time and manpower. Furthermore, because rock sample powders are difficult to bind, conventional tableting equipment often requires insufficient pressure to effectively compress the sample into tablets. This introduces additional chemical interference, leads to loose powder sample compression, uneven powder sample surfaces, and issues such as mineral effects and particle effects.

[0069] In response to this, such as Figures 2 to 12 As shown, in this embodiment, a sample powder pressing device for in-situ micro-area analysis is used to press ultrafine pulverized geological samples and Re standard powder materials into tablets to prepare Re sample targets and Re standard targets, respectively. In this embodiment, the preparation of Re sample targets is used as an example for explanation; the process of preparing Re standard targets is the same as that of preparing Re sample targets.

[0070] like Figures 2 to 12 As shown, the present invention provides a sample powder pressing device for in-situ analysis of micro-area, comprising a base 1, a fixing ring 2, a splicing plate 3, a pressing column 4, an insert rod 5, a plastic ring 6, and a polyethylene powder filler 7.

[0071] There are multiple splicing panels 3, and all splicing panels 3 can be slidably connected to the upper surface of the base 1. The fixing ring 2 can be slidably connected to the outer side wall of the base 1. Each splicing panel 3 has a first limiting surface 311.

[0072] During tablet pressing, multiple splicing plates 3 slide and splice on the base 1, and multiple first limiting surfaces 311 combine to form a groove. The fixing ring 2 is sleeved on the outer periphery of the multiple splicing plates 3 after splicing. The insertion rod 5 passes through the fixing ring 2 and is inserted into the base 1. The pressure column 4 is inserted into the groove.

[0073] A plastic ring 6 is disposed in the groove. The plastic ring 6 is used to place geological sample powder. A polyethylene powder filler 7 is used to fill the groove to cover the top and outside of the plastic ring 6.

[0074] In the above embodiment, it should be noted that the base 1 is cylindrical, the fixing ring 2 is annular, and the splicing plate 3 is fan-shaped. When the geological sample powder needs to be pressed into tablets, multiple splicing plates 3 slide and splice on the base 1 to form a cylindrical structure in the shape of an annular ring. The first limiting surfaces 311 of the multiple splicing plates 3 combine to form a circular groove. Then, the fixing ring 2 slides upward until the upper end surface of the fixing ring 2 is flush with the upper end surface of the splicing plate 3. At this time, a part of the fixing ring 2 is sleeved on the base 1 and fixed. Another part of ring 2 is fitted onto a cylindrical structure formed by splicing multiple splicing plates 3. Then, the fixing ring 2 is fixed to the base 1 by the insert rod 5. The fixing ring 2 realizes the limiting of multiple splicing plates 3. When tableting is required, the plastic ring 6 is placed in the groove, the geological sample powder is poured into the plastic ring 6, and the groove is filled with polyethylene powder filler 7 to cover the geological sample powder inside the plastic ring 6 and the outside of the plastic ring 6. Then, the pressing column 4 is inserted into the groove, and then the tableting machine is used to press the pressing column 4 to form a tablet.

[0075] After the geological sample powder is pressed into a Re sample target, firstly, the pressure column 4 is pulled out of the groove, then the insertion rod 5 is pulled out of the base 1, and then the fixing ring 2 is slid downwards until it is completely detached from the splicing plate 3. Then, multiple splicing plates 3 are slid off the base 1, and finally, the Re sample target is removed from the side. By placing the sample on the plastic ring 6, the shape and size of the geological sample powder can be fixed during pressing. Simultaneously, because the plastic ring 6 has a certain degree of deformability, when pressure is applied after covering the top of the geological sample powder and the outside of the sealing ring 6 with polyethylene powder filler, the ring wall of the plastic ring 6 also applies pressure to the periphery of the geological sample powder, thus better forming the geological sample powder into sheets.

[0076] Optional, such as Figures 2 to 12 As shown, in some embodiments, the side wall of the base 1 is provided with a vertical sliding groove 14, and the fixing ring 2 includes a ring body 21 and a vertical slider 23. The inner side wall of the ring body 21 is provided with a vertical slider 23. The ring body 21 is sleeved on the base 1, and the vertical slider 23 is slidably connected in the vertical sliding groove 14.

[0077] In the above optional embodiments, it should be noted that there are multiple vertical sliding grooves 14, which are distributed in a circular array on the outer periphery of the base 1. The number of vertical sliders 23 is equal to that of the vertical sliding grooves 14, and the multiple vertical sliders 23 are slidably connected in the vertical sliding grooves 14 in a one-to-one correspondence. The cross-sectional shape of the vertical sliding groove 14 and the cross-sectional shape of the vertical slider 23 are both "convex" shaped. The top end face of the vertical sliding groove 14 is the fifth limiting surface 16. When the tablet pressing operation is performed, the fifth limiting surface 16 abuts against the upper end face of the vertical slider 23.

[0078] The advantages of the above optional embodiments are as follows: the cooperation between the vertical sliding groove 14 and the vertical slider 23 enables the fixed ring 2 to slide reliably relative to the base 1, and the fifth limiting surface 16 abuts against the upper end surface of the vertical slider 23 to reliably limit the fixed ring 2, thereby ensuring the reliability of the fixed ring 2 in limiting and fixing multiple splicing plates 3.

[0079] Optional, such as Figures 1 to 11 As shown, in some embodiments, the top wall of the base 1 is provided with multiple horizontal sliding grooves 15, and each splicing plate 3 includes a plate body 31 and a first horizontal slider 32. The first horizontal slider 32 is provided on one side of the plate body 31. When pressing the plate, the first horizontal slider 32 is slidably connected in the horizontal sliding groove 15 in a one-to-one correspondence. The end face of the inner side of the plate body 31 is the first limiting surface 311.

[0080] The splicing plate 3 also includes a second horizontal slider 33. The second horizontal slider 33 is provided on the other side of the plate body 31. When the sample 6 after pressing is taken out, the second horizontal slider 33 is slidably connected in the horizontal sliding groove 15.

[0081] The cross-sectional shape of the horizontal slide groove 15, the cross-sectional shape of the first horizontal slider 32, and the cross-sectional shape of the second horizontal slider 33 are all "convex" shaped.

[0082] Multiple transverse sliding grooves 15 are distributed in a circular array.

[0083] The end face of the first horizontal slider 32 that is close to the first limiting surface 311 is the third limiting surface 321, and the end face of the second horizontal slider 33 that is close to the first limiting surface 311 is the fourth limiting surface 331.

[0084] The distance between the third limiting surface 321 and the first limiting surface 311 is less than the distance between the fourth limiting surface 331 and the first limiting surface 311.

[0085] In the above optional embodiments, it should be noted that the inner end face of the transverse sliding groove 15 is the second limiting surface 12, and the first limiting surface 311, the second limiting surface 12, the third limiting surface 321 and the fourth limiting surface 331 are all arc surfaces, and the arcs of the second limiting surface 12, the third limiting surface 321 and the fourth limiting surface 331 have the same center.

[0086] When tableting is performed, the second limiting surface 12 and the third limiting surface 321 abut against each other. When it is necessary to remove the tableted sample 6, the other splicing plates 3 are removed. A splicing plate 3 is slidably connected to the horizontal sliding groove 15 through the corresponding second horizontal slider 33. The second sliding block 33 is slid, which drives the first limiting surface 311 of the plate body 31 to move. The movement of the first limiting surface 311 pushes the tableted sample 6 to separate it from the base 1, thereby ensuring the integrity of the tableted sample 6 after separation from the base 1 and increasing the convenience of separating the sample 6 from the base 1.

[0087] The beneficial effects of the above optional embodiments are as follows: by setting the distance between the third limiting surface 321 and the first limiting surface 311 to be less than the distance between the fourth limiting surface 331 and the first limiting surface 311, the integrity of the sample 6 after separation from the base 1 after tableting is ensured, and the convenience of separating the sample 6 from the base 1 is increased.

[0088] Optional, such as Figures 2 to 12 As shown, in some embodiments, the pressure column 4 includes a column body 41 and a positioning ring 42, with the positioning ring 42 provided at one end of the column body 41; during operation, the column body 41 is inserted into the groove.

[0089] In the above optional embodiments, it should be noted that the positioning ring 42 is an annular cylindrical structure, and the cylindrical part 41 and the positioning ring 42 are integrally formed.

[0090] The advantages of the above optional embodiments are as follows: the positioning ring 42 can realize the centering of the tablet press shaft, realize the reliable fixation of the mold during tableting, and thus ensure the reliability of powder tableting.

[0091] Optional, such as Figures 2 to 12 As shown, in some embodiments, the side wall of the base 1 is provided with a slot 13, and the side wall of the ring body 21 is provided with a socket 22. The plug rod 5 passes through the socket 22 and is inserted into the slot 13.

[0092] In the above optional embodiments, it should be noted that there are at least two slots 13 and at least two sockets 22. At least two slots 13 are arranged in a circumferential array on the side wall of the base 1, and at least two sockets 22 are arranged in a circumferential array on the side wall of the ring body 21. The sockets 22 and slots 13 are arranged coaxially in a one-to-one correspondence.

[0093] The advantages of the above optional embodiments are that the fixing ring 2 is reliably fixed during operation by means of the cooperation of the insertion rod 5, the slot 13 and the insertion hole 22.

[0094] Optional, such as Figures 2 to 12As shown, in some embodiments, the insertion rod 5 includes a pull block 51 and a rod body 52. ​​During operation, one end of the rod body 52 passes through the insertion hole 22 and is inserted into the slot 13, and the other end of the rod body 52 is provided with a pull block 51.

[0095] Both sides of the pull block 51 are provided with pull grooves 53.

[0096] The advantages of the above optional embodiments are that the arrangement of the pull block 51 and the pull groove 53 ensures the convenience of inserting and pulling out the plug 5.

[0097] In this embodiment, a sample powder pressing device for micro-area in-situ analysis is used to press ultrafine pulverized geological samples and Re standard powder into tablets to prepare Re sample targets and Re standard targets, respectively. This achieves the goal of pressing geological sample powder more compactly without the need for binders, thereby improving the sensitivity of in-situ elemental analysis. It also improves efficiency by using a splicing plate that allows the tablet to be removed from the groove from the side after pressing, eliminating the need for secondary reverse pressing. Furthermore, the pressed powder tablets have a smooth surface, avoiding mineral effects and particle effects, and possessing overall representativeness. In addition, this device places a plastic ring in the groove, then places the geological sample powder on the plastic ring, and then fills the groove with polyethylene powder to cover the top and outside of the plastic ring before pressing. This allows for the use of plastic rings of different sizes to press stable, pressable geological sample powders of different sizes, suitable for different sample chamber sizes of analytical instruments, and enabling direct delivery into the sample analysis chamber of the analytical instrument.

[0098] Step 4: Based on the Re standard target, use laser in-situ analysis to rapidly and preliminarily determine the whole-rock Re content of the Re sample target.

[0099] In this embodiment, the specific process of step S140 is as follows:

[0100] The whole-rock Re content of Re samples was preliminarily determined using LA-MC-ICP-MS. All samples from the black rock series were analyzed using laser point ablation mode at an energy of 5.3 J / cm². -2 Frequency 8Hz, background acquisition 20s, analysis 50s, rinsing 30s.

[0101] Under the same laser and mass spectrometry experimental conditions, laser spot ablation was used to sequentially perform laser spot analysis on the Re standard target and the Re sample target, respectively.

[0102] The preliminary whole-rock Re content of the black rock series sample is obtained according to the following formula;

[0103] C2 = (A2 / A1) × C1,

[0104] Wherein, C2 represents the preliminary whole-rock Re content of the black rock series sample, C1 represents the whole-rock Re content of the Re standard powder material, A1 represents the measurement count of the Re standard target, and A2 represents the measurement count of the Re sample target.

[0105] The laser beam used has a beam size of 70μm to 80μm, and the dot dwell time is 0.4s to 0.5s. Preferably, in this embodiment, the laser beam used has a beam size of 80μm, and the dot dwell time is 0.5s.

[0106] As shown in Table 1, preliminary whole-rock Re content data of the black rock series samples were obtained by using laser in-situ analysis based on the Re standard target to determine the whole-rock Re content of the Re sample target.

[0107] Table 1. Preliminary whole-rock Re content data analysis results of black shale and mudstone samples.

[0108]

[0109] Table 1 shows that the laser in-situ test results of high Re content shale (GRe-1) (7375±420.05 ppb) are consistent with the standard result (7529.07±56.25 ppb) within the error range, with a relative error of 2.09%, which is within a controllable range. The laser in-situ test result of low Re content shale (DRe-1) is 121±8.84 ppb, which is larger than the standard result of 91.89±0.6788 ppb, with a relative error of 24.06%. The analysis results show that the SiO2 content of the DRe-1 sample is only 40%, the lowest among all samples, while its CaO content is close to 15%, much higher than the other samples (all around 1%). Therefore, the matrix effect has a significant impact on it. The relative errors between the test results and the standard results for three mudstone samples (16BZ-17, 16BZ-19, and 16BZ-98) with Re contents in the single, double, and hundreds ppb ranges were all less than 20%, specifically 9.4%, 10.7%, and 17.65%, respectively. Sample 16BZ-98 had a Re content of only 1.4 ppb, yet the relative error was still less than 20%, strongly demonstrating that the rapid and accurate Re content determination method S100 for this black rock formation is also applicable to black shale samples with ultra-low Re content.

[0110] This invention presents a rapid preliminary determination method for whole-rock Re content in geological samples. It innovatively proposes preparing Re sample targets and Re standard targets through pelleting, and then using laser in-situ analysis based on the Re standard targets to rapidly determine the whole-rock Re content of the Re sample targets. From the preparation of the Re sample targets to the rapid preliminary determination of whole-rock Re content based on the Re standard targets using laser in-situ analysis, the entire preliminary determination process takes only one hour, compared to the five days required by existing technologies. This significantly saves testing time and improves testing and analysis efficiency. Furthermore, the entire process of whole-rock Re content determination in geological samples does not use chemical reagents, saving costs and fully meeting the requirements of obtaining the optimal Re diluent ratio test quickly and cheaply, providing a foundation for accurate determination of whole-rock Re content. This whole-rock Re content preliminary determination process can also be used for rapid screening of Re resources in large batches of geological samples.

[0111] It is understood that the above embodiments are merely exemplary implementations used to illustrate the principles of the present invention, and the present invention is not limited thereto. For those skilled in the art, various modifications and improvements can be made without departing from the spirit and essence of the present invention, and these modifications and improvements are also considered to be within the scope of protection of the present invention.

Claims

1. A pelleting device for rapid preliminary determination of Re content in whole-rock geological samples, characterized in that, Includes base, fixing ring, splicing plate, pressure column, insertion rod, plastic ring and polyethylene powder filler; The splicing plate consists of multiple pieces, all of which can be slidably connected to the upper surface of the base. The fixing ring can be slidably connected to the outer side wall of the base, and each splicing plate has a first limiting surface. During tableting, multiple splicing plates slide and splice on the base, and multiple first limiting surfaces combine to form a groove. The fixing ring is sleeved on the outer periphery of the spliced ​​multiple splicing plates. The insertion rod passes through the fixing ring and is inserted into the base. The pressure column is inserted into the groove. The plastic ring is disposed in the groove, and the plastic ring is used to hold rock powder. The polyethylene powder filler is used to fill the groove to cover the rock powder inside the plastic ring and the outer side of the plastic ring; wherein, The base has a vertical sliding groove on its side wall. The fixing ring includes a ring body and a vertical slider. The vertical slider is provided on the inner side wall of the ring body. The ring body is sleeved on the base. The vertical slider is slidably connected in the vertical sliding groove. The top wall of the base is provided with multiple horizontal sliding grooves. Each splicing plate includes a plate body and a first horizontal slider. The first horizontal slider is provided on one side of the plate body. When pressing the plate, the first horizontal slider is slidably connected in the horizontal sliding groove. The end face inside the plate body is the first limiting surface. The splicing plate also includes a second horizontal slider. The second horizontal slider is provided on the other side of the plate body. When the sample after pressing is taken out, the second horizontal slider can be slidably connected in the horizontal sliding groove. The pressure column includes a column body and a positioning ring, with the positioning ring provided at one end of the column body; during operation, the column body is inserted into the groove. The base has a slot on its side wall, and the ring body has a hole on its side wall. The rod passes through the hole and is inserted into the slot. The insertion rod includes a pull block and a rod body. During operation, one end of the rod body passes through the insertion hole and is inserted into the slot. The other end of the rod body is provided with the pull block, and both sides of the pull block are provided with pull grooves. The cross-sectional shape of the horizontal sliding groove, the cross-sectional shape of the first horizontal sliding block, and the cross-sectional shape of the second horizontal sliding block are all "convex" shaped.

2. A rapid preliminary determination method for Re content in whole-rock geological samples, characterized in that, The pelleting device for rapid preliminary determination of whole-rock Re content in geological samples as described in claim 1 is used; wherein the method includes: Step 1: Collect geological samples and perform ultrafine grinding; Step 2: Prepare Re standard powder material with the same lithology as the geological sample; Step 3: The ultrafine pulverized geological sample and the Re standard powder are pressed into tablets using the tablet pressing device to prepare Re sample targets and Re standard targets, respectively. Step 4: Based on the Re standard target, use laser in-situ analysis to rapidly and preliminarily determine the whole-rock Re content of the Re sample target.

3. The method according to claim 2, characterized in that, In step four, the preliminary whole-rock Re content of the Re sample target is determined using laser in-situ analysis based on the Re standard target, resulting in preliminary whole-rock Re content data for the geological sample, including: Under the same laser and mass spectrometry experimental conditions, laser spot ablation was used to sequentially perform laser spot analysis on the Re standard target and the Re sample target, respectively. The preliminary whole-rock Re content of the geological sample is obtained according to the following formula; C2 = (A2 / A1) × C1, Wherein, C2 represents the preliminary whole-rock Re content of the geological sample, C1 represents the whole-rock Re content of the Re standard powder material, A1 represents the measurement count of the Re standard target, and A2 represents the measurement count of the Re sample target.

4. The method according to claim 3, characterized in that, The laser spot size used is 70 μm to 80 μm, and the dwell time of the dots is 0.4 s to 0.5 s.

5. The method according to claim 2, characterized in that, Preparation of Re standard powder material with the same lithology as the geological sample includes: Collect alternative standard materials with the same lithology as the geological samples; The candidate standard substances are subjected to ultrafine pulverization; The crushed candidate standard substances were dispensed into multiple wide-mouth bottles and mixed evenly.

6. The method according to claim 5, characterized in that, The candidate standard material is ground to a fineness of less than 200 mesh.

7. The method according to claim 5, characterized in that, After completing the dispensing of the candidate standard substances, the method further includes: The homogeneity, stability, and normality of the setpoint data of the candidate standard substances were tested respectively.

8. The method according to claim 2, characterized in that, The collection and ultrafine grinding of geological samples includes: Collect the geological samples and clean them with deionized water; The geological sample was ultra-finely ground and pulverized using a ball mill to a mesh size below 200. The ultra-finely ground and pulverized geological sample was then mixed evenly to increase the uniformity of the sample.

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