Rapid initial measurement method for total rock Re content of geological sample

Abstract

The invention provides a rapid initial measurement method for the total rock Re content of a geological sample. The rapid initial measurement method comprises the following steps: step 1, collecting the geological sample and carrying out ultrafine crushing; step 2, preparing a Re standard powder substance with the same lithology as the geological sample; step 3, respectively tabletting the geological sample and the Re standard powder substance which are subjected to superfine grinding so as to prepare a Re sample target and a Re standard target; and 4, according to the Re standard target, carrying out rapid preliminary determination on the total rock Re content of the Re sample target by adopting a laser in-situ analysis method. By the adoption of the initial testing method, the whole initial testing process only needs one hour, and compared with the prior art that the Re content initial testing process needs five days, the testing time is saved, and the testing analysis efficiency is improved; no chemical reagent is used in the whole total rock Re content initial measurement process, the cost is saved, the test requirement for obtaining the Re diluent optimal ratio quickly and cheaply is completely met, and a basis is provided for accurate measurement of the total rock Re content.

Description

Technical Field

[0001] The invention belongs to the technical field of Re content initial measurement, and particularly relates to a method for rapid initial measurement of Re content in whole-rock geological samples. Background Art

[0002] Currently, accurate determination of Re content in geological samples at the ppb-ppt level is mainly achieved by isotope dilution combined with thermal ionization mass spectrometry or multi-collector mass spectrometry (ID-NTIMS / ID-MC-ICP-MS), which generally involves the following steps: sample weighing, sample dissolution in a Carius tube, and sample reduction.

[0003] It takes two days to open the tube and reach room temperature; two days to prepare for the test, from separating the interfering element Os by distillation to enriching and purifying Re through anion exchange or acetone extraction; and finally one day for on-machine testing. A single experimental process takes five days. However, obtaining an accurate result for Re content generally requires two steps: the first experimental step is mainly used for preliminary measurement of Re content to determine the optimal Re diluent ratio; the second experimental step is used for fine measurement to obtain the precise Re content. From the initial measurement and diluent addition to the fine measurement and obtaining an accurate result, a total of 10 days is required. Furthermore, the entire experimental process consumes a large amount of chemical reagents and laboratory equipment, making the experimental testing costly.

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

[0005] In view of the above problems, it is necessary to propose a method for rapid initial determination of Re content in whole rock of geological samples that is reasonably designed and can effectively solve the above problems. Summary of the Invention

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

[0007] The present invention provides a method for rapid initial determination of Re content in whole-rock geological samples, the method comprising:

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

[0009] Step 2: preparing a Re standard powder material having the same lithology as the geological sample;

[0010] Step 3: tableting the ultrafinely crushed geological sample and the Re standard powder material to prepare a Re sample target and a Re standard target;

[0011] Step 4: Using the laser in-situ analysis method based on the Re standard target, a rapid preliminary determination of the whole-rock Re content of the Re sample target is performed.

[0012] Optionally, in step 3, a powder tabletting device for micro-area in-situ analysis of samples is used to tablet the ultrafinely crushed geological sample and the Re standard powder material respectively; wherein,

[0013] The tablet pressing device includes a base, a fixing ring, a splicing plate, a pressing column, an inserting rod, a plastic ring and a polyethylene powder filling body;

[0014] There are multiple splicing plates, each of which is slidably connected to the upper surface of the base, the fixing ring is slidably connected to the outer side wall of the base, and each of the splicing plates has a first limiting surface;

[0015] During sheet pressing, the plurality of splicing plates are slidably spliced ​​on the base and the plurality of first limiting surfaces are combined to form a groove, the fixing ring is sleeved on the outer peripheral side of the plurality of spliced ​​splicing plates, the insertion rod passes through the fixing ring and is inserted into the base, and the pressure column is inserted into the groove;

[0016] The plastic ring is arranged in the groove, and is used to place geological sample powder. The polyethylene powder filling body is used to fill the groove to cover the geological sample powder in the plastic ring and the outside of the plastic ring.

[0017] Optionally, the tablet pressing device further comprises:

[0018] A vertical sliding groove is provided on the side wall of the base. The fixed ring includes a ring body and a vertical sliding block. The vertical sliding block is provided on the inner side wall of the ring body. The ring body is sleeved on the base. The vertical sliding block can be slidably connected in the vertical sliding groove.

[0019] Optionally, the tablet pressing device further comprises:

[0020] The top wall of the base is provided with a plurality of transverse sliding grooves, and each of the splicing plates includes a plate body and a first transverse sliding block. The first transverse sliding block is provided on one side of the plate body. When pressing the plate, the first transverse sliding block is slidably connected in the transverse sliding groove in a one-to-one correspondence, and the inner end surface of the plate body is a first limiting surface;

[0021] The splicing plate further comprises a second transverse sliding block, and the second transverse sliding block is provided on the other side of the plate body. When the sample after tableting is taken out, the second transverse sliding block can be slidably connected in the transverse sliding groove.

[0022] Optionally, in step 4, performing a preliminary whole-rock Re content determination on the Re sample target using a laser in-situ analysis method 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 point ablation was used to perform laser point 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 beam used is 70 μm to 80 μm, and the dot dwell time is 0.4 s to 0.5 s.

[0028] Optionally, preparing a Re standard powder material having the same lithology as the geological sample comprises:

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

[0030] Ultrafinely grinding the candidate standard substance;

[0031] The crushed candidate standard substances are divided into a plurality of wide-mouth bottles and mixed evenly.

[0032] Optionally, the candidate standard material is ground to less than 200 mesh.

[0033] Optionally, after completing the packaging of the candidate standard substance, the method further comprises:

[0034] The candidate standard substances were tested for homogeneity, stability and normality of fixed value data.

[0035] Optionally, collecting geological samples and performing ultrafine grinding includes:

[0036] Collecting the geological sample and washing it with deionized water;

[0037] The geological samples are ultrafinely ground and pulverized using a ball mill to grind the geological samples to below 200 meshes, and the ultrafinely ground and pulverized geological samples are mixed evenly to increase the homogeneity of the samples.

[0038] The method for rapid preliminary determination of Re content in whole rock of geological samples of the present invention creatively proposes preparing Re sample targets and Re standard targets by tabletting, and adopting laser in-situ analysis method to conduct rapid preliminary determination of Re content in whole rock of Re sample targets based on Re standard targets. From preparation of Re sample targets to rapid preliminary determination of Re content in whole rock of Re sample targets by laser in-situ analysis method based on Re standard targets, the entire preliminary determination process only takes one hour, while the process of preliminary determination of Re content in the prior art requires 5 days, which greatly saves test time and improves test and analysis efficiency. Moreover, no chemical reagents are used in the entire preliminary determination of Re content in whole rock of geological samples, which saves costs and fully meets the test requirements of obtaining the optimal Re diluent ratio "quickly" and "cheaply", providing a basis for precise determination of Re content in whole rock. The process of preliminary determination of Re content in whole rock can also be used for rapid screening of Re resources in large quantities of geological samples. BRIEF DESCRIPTION OF THE DRAWINGS

[0039] Figure 1 The figure is a flow chart of a method for rapid initial determination of Re content in whole rock of geological samples according to one embodiment of the present invention.

[0040] Figure 2 This is a three-dimensional diagram of a powder tabletting device for micro-area in-situ analysis of samples provided by another embodiment of the present invention.

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

[0042] Figure 4 A side view of a powder tabletting device for in-situ analysis of samples in micro areas provided in another embodiment of the present invention.

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

[0044] Figure 6 This is a first perspective view of a base of a powder tabletting device for micro-area in-situ analysis of samples provided by another embodiment of the present invention.

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

[0046] Figure 8 A three-dimensional diagram of a fixing ring of a powder tabletting device for micro-area in-situ analysis of samples provided in another embodiment of the present invention.

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

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

[0049] Figure 11 This is a three-dimensional diagram of a pressing column of a powder tabletting device for micro-area in-situ analysis of samples provided in another embodiment of the present invention.

[0050] Figure 12 This is a three-dimensional diagram of an insertion rod of a powder tabletting device for micro-area in-situ analysis of samples provided in another embodiment of the present invention. DETAILED DESCRIPTION

[0051] In order to enable those skilled in the art to better understand the technical solution of the present invention, the present invention is further described in detail below with reference to the accompanying drawings and specific implementation methods.

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

[0053] Step 1: Collect geological samples and grind them into ultrafine powder.

[0054] Specifically, first, the geological sample is collected and cleaned with deionized water;

[0055] Secondly, the geological samples are ultra-finely ground and pulverized using a ball mill, the geological samples are ground to below 200 mesh, and the ultra-finely ground and pulverized geological samples are mixed evenly to increase the homogeneity of the samples.

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

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

[0058] Specifically, if the geological sample is limestone, limestone is also sampled as the candidate standard material to ensure that the lithology of the candidate standard material is consistent with that of the collected geological sample. In this embodiment, the Re standard material development work was carried out using Permian limestone from the Dongchuanling area of ​​Guangde, Anhui Province, and Sinian black shale from the Kunyang Phosphate Mine. Two black rock series Re analysis standard materials, carbonate and silicate, were developed, respectively.

[0059] Secondly, the candidate standard substance is ultrafinely ground.

[0060] Specifically, the collected candidate standard substances were cleaned with deionized water, ultrafinely ground to less than 200 mesh, and mixed evenly.

[0061] Next, the crushed candidate standard substances are divided into a plurality of wide-mouth bottles and mixed evenly.

[0062] Specifically, the crushed candidate standard substance was dispensed into 100 2L plastic jars, with 10g of the substance per jar. After filling, the jars were shaken by hand to ensure uniform mixing. Each jar was numbered for sampling for homogeneity and stability testing.

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

[0064] Specifically, 12 bottles of limestone and 12 bottles of black shale alternative standard materials were respectively extracted, 0.5 g of each was weighed, and after sample dissolution, chemical separation, enrichment and purification, the uniformity, stability and normality of the fixed value data were tested in turn.

[0065] The inter-bottle average (AV1) of the limestone candidate standard material was 6.473 ppb, the inter-bottle standard deviation (s1) was 0.144, the total standard deviation (s2) within the bottle was 0.117, and the RSD (%, 2s, n=15) was 0.02. The inter-bottle average (AV1) of the black shale candidate standard material was 26.39, the inter-bottle standard deviation (s1) was 0.55, the total standard deviation (s2) within the bottle was 0.332, and the RSD (%, 2s, n=15) was 0.02. These results demonstrate good uniformity for both black rock candidate standard materials. Stability testing revealed that the deviations in test results six months apart did not exceed the standard deviation of the variance itself and were consistent with the total average 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, and the Re values ​​of the limestone reference material were determined to be 6.473 ppb with an uncertainty of 0.016; the Re values ​​of the black shale reference material were 26.71 ppb with an uncertainty of 0.07. Collaborative value determination research conducted by the Institute of Geology and Geophysics, Chinese Academy of Sciences, yielded the Re values ​​of the limestone reference material to be 6.413 ppb with an uncertainty of 0.387; and the Re values ​​of the black shale reference material to be 25.85 ppb with an uncertainty of 0.27. These results are consistent with those reported in this paper within the uncertainty range.

[0066] In this embodiment, a Re standard powder material for Re component analysis of geological samples is provided, which fills the gap in domestic Re standard materials, provides a solid guarantee for the accuracy and reliability of Re content analysis results, and meets my country's demand for the development and utilization of rhenium resources.

[0067] Step 3: The ultrafinely crushed geological sample and the Re standard powder material are respectively tableted to prepare a Re sample target and a Re standard target.

[0068] Conventional tableting devices require a second, reverse pressing operation to remove the sample after pressing due to structural issues with the pressing mold. This is inefficient, time-consuming, and labor-intensive. Furthermore, because rock sample powders are not easily bonded, conventional tableting equipment has too low a pressure, often requiring the addition of a binder to effectively form tablets. This introduces additional chemical interference, loosely pressing the powder sample, uneven surfaces, and the presence of mineral and particle effects.

[0069] In response to this, Figures 2 to 12 As shown, in this embodiment, a sample powder tableting apparatus for micro-area in-situ analysis is used to tablet ultrafinely pulverized geological samples and Re standard powder materials to prepare Re sample targets and Re standard targets, respectively. In this embodiment, the preparation of the Re sample target is used as an example for illustration; the process for preparing the Re standard target is the same as that for preparing the Re sample target.

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

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

[0072] When pressing the sheets, multiple splicing plates 3 are slid and spliced ​​on the base 1 and multiple first limiting surfaces 311 are combined to form a groove. The fixing ring 2 is sleeved on the outer peripheral side of the multiple splicing plates 3 after splicing. The insertion rod 5 passes through the fixing ring 2 and is inserted on the base 1, and the pressure column 4 is inserted in the groove.

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

[0074] In the above embodiment, it should be noted that the shape of the base 1 is cylindrical, the shape of the fixing ring 2 is annular, and the shape of the splicing plate 3 is fan-shaped. When the geological sample powder needs to be tableted, multiple splicing plates 3 are slid and spliced ​​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 are combined to form a circular groove. Then the fixing ring 2 is slid 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. The other part of the ring 2 is sleeved on a cylindrical structure formed by splicing multiple splicing plates 3 into a circular ring shape, and then the fixed ring 2 is fixed to the base 1 by the insertion rod 5, and the multiple splicing plates 3 are limited by the fixed ring 2; when tableting is required, the plastic ring 6 is placed in the groove, and the geological sample powder is poured into the plastic ring 6, and the polyethylene powder filling body 7 is filled into the groove to cover the geological sample powder in the plastic ring 6 and the outside of the plastic ring 6, and then the pressing column 4 is inserted into the groove, and then the tablet press is used to press the pressing column 4 for tableting.

[0075] After the geological sample powder is pressed into a Re sample target, first pull out the pressure column 4 from the groove, then pull out the insertion rod 5 from the base 1, then slide the fixing ring 2 downward until the fixing ring 2 is completely separated from the splicing plate 3, then slide and withdraw the multiple splicing plates 3 on the base 1, and then take out the Re sample target 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 the sample pressing. At the same time, since the plastic ring 6 has a certain degree of deformability, when the polyethylene powder filling body covers the top of the geological sample powder and the outside of the plastic sealing ring 6 and is pressurized, the ring wall of the plastic ring 6 also applies pressure to the surrounding side of the geological sample powder to make the geological sample powder better into sheets.

[0076] Optional, such as Figures 2 to 12 As shown, in some embodiments, a vertical slide groove 14 is provided on the side wall of the base 1, 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 can be slidably connected in the vertical slide groove 14.

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

[0078] The beneficial effects of the above optional embodiments are: reliable sliding of the fixing ring 2 relative to the base 1 is achieved through the coordinated arrangement of the vertical slide groove 14 and the vertical slider 23, and reliable positioning of the fixing ring 2 can be achieved through the arrangement of the fifth limiting surface 16 abutting against the upper end surface of the vertical slider 23, thereby ensuring the reliability of the fixing ring 2 in limiting and fixing the multiple splicing plates 3.

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

[0080] The splicing plate 3 further includes a second transverse slide block 33 . The second transverse slide block 33 is provided on the other side of the plate body 31 . When the pressed sample 6 is taken out, the second transverse slide block 33 is slidably connected in the transverse slide groove 15 in a one-to-one correspondence.

[0081] The cross-sectional shapes of the transverse sliding groove 15 , the first transverse sliding block 32 , and the second transverse sliding block 33 are all convex.

[0082] The plurality of transverse sliding grooves 15 are distributed in a circular array.

[0083] The end surface of the first transverse sliding block 32 close to the first limiting surface 311 is a third limiting surface 321 , and the end surface of the second transverse sliding block 33 close to the first limiting surface 311 is a fourth limiting surface 331 ;

[0084] The distance between the third limiting surface 321 and the first limiting surface 311 is smaller 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, 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 the tableting operation is carried out, the second limiting surface 12 and the third limiting surface 321 abut against each other; when the sample 6 after tableting needs to be removed, the other splicing plates 3 are removed, and a splicing plate 3 is used to be slidably connected to the horizontal sliding groove 15 through the corresponding second horizontal sliding block 33, and the second sliding block 33 is slid to drive the first limiting surface 311 of the plate body 31 to move, and the first limiting surface 311 moves to push the sample 6 after tableting to separate it from the base 1, thereby ensuring the integrity of the sample 6 after tableting after separation from the base 1, and increasing the convenience of separating the sample 6 from the base 1.

[0087] The beneficial effect of the above optional embodiment is that by setting the distance between the third limiting surface 321 and the first limiting surface 311 to be smaller than the distance between the fourth limiting surface 331 and the first limiting surface 311, the integrity of the sample 6 after being separated 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 portion 41 and a positioning ring 42 , and a positioning ring 42 is provided at one end of the column portion 41 ; when working, the column portion 41 is inserted into the groove.

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

[0090] The beneficial effect of the above optional embodiment is that the setting of the positioning ring 42 can realize the setting of the tablet press shaft centering, 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, a slot 13 is formed on the side wall of the base 1 , and a plug hole 22 is formed on the side wall of the ring body 21 . The insertion rod 5 passes through the plug hole 22 and is inserted into the slot 13 .

[0092] In the above optional embodiment, it should be noted that the number of slots 13 and sockets 22 is at least two, at least two slide grooves 13 are distributed in a circular array on the side wall of the base 1, and at least two sockets 22 are distributed in a circular array on the side wall of the ring body 21, and the sockets 22 and slots 13 are coaxially arranged in a one-to-one correspondence.

[0093] The beneficial effect of the above optional embodiment is that the fixing ring 2 is reliably fixed during operation by the coordinated arrangement of the inserting rod 5 , the slot 13 and the inserting 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] Pull grooves 53 are formed on both sides of the pull block 51 .

[0096] The beneficial effect of the above optional embodiment is that the arrangement of the pull block 51 and the pull groove 53 ensures the convenience of inserting and removing the insertion rod 5.

[0097] In this embodiment, a micro-area in-situ analysis sample powder tableting device is used to tablet ultrafinely crushed geological samples and Re standard powder materials to prepare Re sample targets and Re standard targets, respectively, without adding a binder, and the geological sample powder is pressed more compactly, thereby improving the sensitivity of in-situ analysis element testing; efficiency is improved, and the splicing plate is set to move backward after tableting, and the sample tablet is taken out of the groove from the side, without the need for secondary reverse pressing to take out the sample tablet, further improving efficiency; at the same time, the surface of the pressed powder tablet is flat, avoiding problems such as mineral effect and particle effect, and has overall representativeness; in addition, the device places a plastic ring in the groove, then sets the geological sample powder in the plastic ring, and then fills the groove with a polyethylene powder filling body to cover the top and outside of the plastic ring, and then presses it by a tableting device, so as to set plastic rings of different sizes to press stable tablet-formed geological sample powders of different sizes, which can be suitable for the sample bin sizes of different analytical instruments and can be directly sent to the sample analysis room of the analytical instrument.

[0098] Step 4: Using the laser in-situ analysis method based on the Re standard target, a rapid preliminary determination of the whole-rock Re content of the Re sample target is performed.

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

[0100] The Re content of the whole rock was preliminarily determined by LA-MC-ICP-MS. The black rock samples were all subjected to laser point ablation mode with an energy of 5.3 J cm -2 , frequency 8 Hz, background acquisition 20 s, analysis 50 s, rinse 30 s.

[0101] Under the same laser and mass spectrometry experimental conditions, laser point ablation was used to perform laser point 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 was obtained according to the following formula:

[0103] C2=(A2 / A1)×C1,

[0104] Among them, C2 represents the preliminary whole-rock Re content of the black rock 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 spot size used is 70 μm to 80 μm, and the dot dwell time is 0.4 s to 0.5 s. Preferably, in this embodiment, the laser spot size used is 80 μm, and the dot dwell time is 0.5 s.

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

[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 measurement results for the high-Re shale (GRe-1) (7375±420.05 ppb) agree with the reference result (7529.07±56.25 ppb) within the acceptable range, with a relative error of 2.09%. The laser in-situ measurement results for the low-Re shale (DRe-1) are 121±8.84 ppb, slightly higher than the reference result of 91.89±0.6788 ppb, with a relative error of 24.06%. The analysis reveals 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%, far higher than the other samples (all around 1%), indicating a significant matrix effect. The relative errors of the test results for three mudstone samples (16BZ-17, 16BZ-19, and 16BZ-98) with Re contents in the units, tens, and hundreds of ppb range, respectively, compared to the standard results were all less than 20%, at 9.4%, 10.7%, and 17.65%, respectively. Sample 16BZ-98, despite containing only 1.4 ppb of Re, still exhibited a relative error of less than 20%, strongly demonstrating that the S100 method for rapid and accurate Re content determination in black rock series is also applicable to black shale samples with ultra-low Re contents.

[0110] The method for rapid preliminary determination of Re content in whole rock of geological samples of the present invention creatively proposes preparing Re sample targets and Re standard targets by tabletting, and adopting laser in-situ analysis method to conduct rapid preliminary determination of Re content in whole rock of Re sample targets based on Re standard targets. From preparation of Re sample targets to rapid preliminary determination of Re content in whole rock of Re sample targets by laser in-situ analysis method based on Re standard targets, the entire preliminary determination process only takes one hour, while the process of preliminary determination of Re content in the prior art requires 5 days, which greatly saves test time and improves test and analysis efficiency. Moreover, no chemical reagents are used in the entire preliminary determination of Re content in whole rock of geological samples, which saves costs and fully meets the test requirements of obtaining the optimal Re diluent ratio "quickly" and "cheaply", providing a basis for precise determination of Re content in whole rock. The process of preliminary determination of Re content in whole rock can also be used for rapid screening of Re resources in large quantities of geological samples.

[0111] It will be understood that the above embodiments are merely exemplary embodiments for illustrating the principles of the present invention, and the present invention is not limited thereto. Those skilled in the art will appreciate that various modifications and improvements can be made without departing from the spirit and substance of the present invention, and such modifications and improvements are also considered to be within the scope of protection of the present invention.

Claims

1. A method for rapid initial determination of Re content in whole rock of geological samples, characterized in that: The method comprises: Step 1: Collect geological samples and perform ultrafine grinding; Step 2: preparing a Re standard powder material having the same lithology as the geological sample; Step 3: tableting the ultrafinely crushed geological sample and the Re standard powder material to prepare a Re sample target and a Re standard target; Step 4: Using the laser in-situ analysis method based on the Re standard target, a rapid preliminary determination of the whole-rock Re content of the Re sample target is performed.

2. The method according to claim 1, characterized in that In step 3, a powder tabletting device for micro-area in-situ analysis of samples is used to tablet the ultrafinely crushed geological sample and the Re standard powder material respectively; wherein, The tablet pressing device includes a base, a fixing ring, a splicing plate, a pressing column, an inserting rod, a plastic ring and a polyethylene powder filling body; There are multiple splicing plates, each of which is slidably connected to the upper surface of the base, the fixing ring is slidably connected to the outer side wall of the base, and each of the splicing plates has a first limiting surface; During sheet pressing, the plurality of splicing plates are slidably spliced ​​on the base and the plurality of first limiting surfaces are combined to form a groove, the fixing ring is sleeved on the outer peripheral side of the plurality of spliced ​​splicing plates, the insertion rod passes through the fixing ring and is inserted into the base, and the pressure column is inserted into the groove; The plastic ring is arranged in the groove, and is used to place geological sample powder. The polyethylene powder filling body is used to fill the groove to cover the geological sample powder in the plastic ring and the outside of the plastic ring.

3. The method according to claim 2, characterized in that The tablet pressing device also includes: A vertical sliding groove is provided on the side wall of the base. The fixed ring includes a ring body and a vertical sliding block. The vertical sliding block is provided on the inner side wall of the ring body. The ring body is sleeved on the base. The vertical sliding block can be slidably connected in the vertical sliding groove.

4. The method according to claim 3, characterized in that The tablet pressing device also includes: The top wall of the base is provided with a plurality of transverse sliding grooves, and each of the splicing plates includes a plate body and a first transverse sliding block. The first transverse sliding block is provided on one side of the plate body. When pressing the plate, the first transverse sliding block is slidably connected in the transverse sliding groove in a one-to-one correspondence, and the inner end surface of the plate body is a first limiting surface; The splicing plate further comprises a second transverse sliding block, and the second transverse sliding block is provided on the other side of the plate body. When the sample after tableting is taken out, the second transverse sliding block can be slidably connected in the transverse sliding groove.

5. The method according to any one of claims 1 to 3, characterized in that In step 4, the whole-rock Re content of the Re sample target is preliminarily determined using a laser in-situ analysis method based on the Re standard target to obtain preliminary whole-rock Re content data of the geological sample, including: Under the same laser and mass spectrometry experimental conditions, laser point ablation was used to perform laser point 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.

6. The method according to claim 5, characterized in that The laser spot beam used is 70μm to 80μm, and the dot dwell time is 0.4s to 0.5s.

7. The method according to any one of claims 1 to 3, characterized in that Preparation of Re standard powder material having the same lithology as the geological sample, comprising: Collect alternative reference materials with the same lithology as the geological samples; Ultrafinely grinding the candidate standard substance; The crushed candidate standard substances are divided into a plurality of wide-mouth bottles and mixed evenly.

8. The method according to claim 7, characterized in that The candidate standard material was ground to less than 200 mesh.

9. The method according to claim 7, characterized in that After completing the packaging of the candidate standard substances, the method further comprises: The candidate standard substances were tested for homogeneity, stability and normality of fixed value data.

10. The method according to any one of claims 1 to 3, characterized in that The collecting of geological samples and ultra-fine grinding includes: Collecting the geological sample and washing it with deionized water; The geological samples are ultrafinely ground and pulverized using a ball mill to grind the geological samples to below 200 meshes, and the ultrafinely ground and pulverized geological samples are mixed evenly to increase the homogeneity of the samples.

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