Cluster isotope sample gas injection device, use method and preparation device

Abstract

The invention discloses a cluster isotope sample gas sampling device, a use method and a preparation device. A connecting channel is formed in the center of an inner disc; the outer disc is rotationally sleeved outside the inner disc; wherein a plurality of mutually isolated sample cabins are formed in the outer disc; a sample introduction channel is formed in the inner disc; a connecting hole is formed in one side, close to the inner disc, of the sample bin; one end of the sampling channel is communicated with the connecting channel, and the other end is communicated with the connecting hole of the inner disc; and the top of the connecting channel is lower than the connecting hole of the sample bin. According to the invention, the sample positions are separately separated, and only one sample introduction channel is arranged, so that high independence among all samples is ensured, and sample powder mixed dyeing caused by continuous high-strength vacuumizing of the samples in a standing state is prevented. By adopting the rotatable sample bin and using a single sample injection channel, continuous sample injection can be ensured, and only one sample is allowed to enter a reaction system for reaction during each sample injection.

Description

Technical Field

[0001] The present invention belongs to the technical field of gas preparation devices, and in particular relates to a cluster isotope sample gas injection device, a use method and a preparation device. Background Art

[0002] Cluster isotopes are isotopologues containing two or more heavy isotopes (rare isotopes). These isotopologues possess unique physical and chemical properties that distinguish them from conventional stable isotopes. Currently, carbonate growth temperatures and paleofluid δ18O values ​​recovered using cluster isotopes of carbonates have been widely applied in paleoclimate reconstruction, paleoaltitude reconstruction, and carbonate diagenesis. Existing linear sample chambers are suitable for single or small sample reactions. However, in actual research, convincing data from large sample reactions is generally required. In existing cluster isotope gas preparation devices, the sample injection system consists of a rectangular glass tube, a sample tube, and an electric push rod. The sample tube is placed inside a sealed rectangular glass tube. The electric push rod is fixed to the outside of the glass tube by a bracket. The push rod and the sample tube are connected by an arc-shaped magnet through the push rod's rotatable front swing head. During the experiment, the electric push rod is controlled by a remote control to move back and forth, thereby moving the sample tube to achieve the desired injection effect. In this design, the glass tubes containing the samples are interconnected, with no partitions between the individual sample locations. The vacuum required throughout the experiment is achieved by pumping the sample through the tube. During this process, airflow can cause powder on top of the sample to move within the tube, potentially contaminating the sample.

[0003] Patent publication number CN106092691B, titled "Online Sample Preparation Device for Hydrogen Isotopes in Solid Hydrogen-Containing Samples," involves feeding a sample package wrapped in a tin capsule into a redox tube via a solid autosampler to perform an online redox reaction on the hydrogen-containing solid sample. The resulting gas is separated by a chromatographic column and then enters a flow divider. It then enters a gas isotope mass spectrometer to measure the hydrogen isotope ratio in the sample, completing online hydrogen isotope testing of the solid hydrogen-containing sample. While this patent application can prepare isotope sample gas, it cannot perform continuous experiments on multiple samples. Summary of the Invention

[0004] To overcome the aforementioned problems in the prior art, the present invention provides a cluster isotope sample gas injection device, method of use, and preparation apparatus. This device isolates the sample locations and provides a single injection channel, ensuring high independence between samples and preventing contamination of sample powders caused by continuous high-intensity vacuuming while the samples are stationary. By employing a rotatable sample chamber and a single injection channel, only one sample is allowed to enter the reaction system for reaction at a time.

[0005] To achieve the above object, the technical solution adopted by the present invention is:

[0006] A cluster isotope sample gas injection device, comprising:

[0007] An inner plate, wherein a connecting passage is provided in the center of the inner plate;

[0008] An outer disk, the outer disk being rotatably sleeved on the outer side of the inner disk;

[0009] In which, the outer disk is provided with a plurality of sample chambers isolated from each other; the inner disk is provided with an injection channel; a connecting hole is provided on the side of the sample chamber close to the inner disk; one end of the injection channel is connected to the connecting channel, and the other end is connected to the connecting hole of the inner disk; the top height of the connecting channel is lower than the height of the connecting hole of the sample chamber.

[0010] Optionally, the number of the sample bins is 10 to 12.

[0011] Optionally, both the inner plate and the outer plate are funnel-shaped.

[0012] Optionally, the sample chambers are equidistantly arranged along the circumference of the outer disk.

[0013] Optionally, the diameter of the sample chamber is 10 mm to 15 mm.

[0014] Optionally, the diameter of the injection channel is 10 mm.

[0015] Optionally, the angle between the injection channel and the horizontal plane is 60°.

[0016] The method for using the cluster isotope sample gas injection device comprises the following steps:

[0017] Place all samples in the sample chamber;

[0018] Rotate the outer disk to connect the sample chamber with the injection channel;

[0019] After the reaction of the previous sample is completed, rotate the outer disk to connect the other sample chamber to the injection channel.

[0020] A preparation device comprises the cluster isotope sample gas injection device and a reaction container, wherein the reaction container is arranged below the connecting channel.

[0021] Optionally, the reaction container is a conical flask.

[0022] Compared with the prior art, the present invention has the following beneficial effects:

[0023] The present invention separates the sample positions individually and only provides one injection channel, which has the characteristics of high independence and low probability of influence between each sample. The present invention transforms the linear sample bin into a funnel-shaped circular rotating sample bin with a low middle interior and high surroundings, which ensures the high independence between each sample and prevents sample powder from being mixed due to continuous high-intensity vacuuming when the sample is in a static state. Furthermore, the present invention improves the original multiple injection channels and uses a single injection channel to ensure that only one sample is allowed to enter the reaction system for reaction each time. Different from the traditional linear moving injection method, the method of the present invention adopts a rotary moving injection method. Each time injection is required, the turntable is rotated to connect the sample position and the injection channel, while the other sample positions are still in a completely independent sample position space, which can improve the accuracy of injection.

[0024] Existing devices use unstable curved magnets, resulting in uncontrolled forward and backward movement of the sample tubes driven by an electric push rod. This prevents samples from being dropped properly or results in multiple samples falling simultaneously into the acid bath. This device effectively addresses this issue by combining a rotating sample tray with a single sample inlet channel. To ensure the sample tubes fit within the quartz glass tubes, the diameter of existing sample tubes is smaller than the quartz glass tubes, resulting in ineffective isolation between samples within the tubes and a high risk of contamination. This device's sample tray utilizes independent sample positions, effectively resolving this issue. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] The drawings described herein are for illustrative purposes only and are not intended to limit the scope of the present invention in any way. In addition, the shapes and proportional dimensions of the components in the drawings are only schematic and are used to help understand the present invention, and are not intended to specifically limit the shapes and proportional dimensions of the components of the present invention. In the drawings:

[0026] Figure 1 It is a schematic diagram of the structure of the present invention;

[0027] Figure 2 This is a schematic diagram of an embodiment of the present invention;

[0028] Among them, 1. Inner plate; 2. Outer plate; 3. Injection channel; 4. Sample chamber; 5. Connecting channel; 6. Reaction vessel, 101-glass tube, 102-U-shaped cold trap, 103-GC column trap, 104-mass spectrometer. DETAILED DESCRIPTION

[0029] In order to enable those skilled in the art to better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings of the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts should fall within the scope of protection of the present invention.

[0030] It should be noted that when an element is referred to as being "disposed on" another element, it may be directly on the other element or there may be an element centered thereon. When an element is referred to as being "connected to" another element, it may be directly connected to the other element or there may be an element centered thereon. The terms "vertical," "horizontal," "left," "right," and similar expressions used herein are for illustrative purposes only and do not represent the only embodiments.

[0031] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the art to which this invention pertains. The terms used herein in the specification of the present invention are for the purpose of describing specific embodiments only and are not intended to limit the present invention. The term "and / or" as used herein includes any and all combinations of one or more of the associated listed items.

[0032] The present invention will be described in detail below with reference to the accompanying drawings.

[0033] like Figure 1 As shown, a cluster isotope sample gas injection device of the present invention includes an inner disk 1 and an outer disk 2.

[0034] A connecting channel 5 is provided in the center of the inner plate 1 , and the connecting channel 5 is perpendicular to the plate surface of the inner plate 1 .

[0035] The outer disk 2 is rotatably mounted on the outer surface of the inner disk 1. The outer disk 2 is provided with a plurality of mutually isolated sample compartments 4. Specifically, the sample compartments 4 are equidistantly spaced along the circumference of the outer disk 2. The number of sample compartments 4 ranges from 10 to 12. The diameter of each sample compartment 4 ranges from 10 mm to 15 mm.

[0036] The inner disk 1 has an injection channel 3 formed inside, and a connecting hole is formed on the side of the sample chamber 4 near the inner disk 1. One end of the injection channel 3 is connected to the connecting channel 5, and the other end is connected to the connecting hole of the inner disk 1. Specifically, the diameter of the injection channel 3 is 10 mm.

[0037] The top of the connecting channel 5 is lower than the height of the connecting hole of the sample chamber 4. Both the inner plate 1 and the outer plate 2 are funnel-shaped with a lower center and higher edges. Specifically, the injection channel 3 is angled at 60° with the horizontal plane to ensure that the sample to be tested slides into the injection channel 3 under gravity during each injection and smoothly enters the reaction system for sample gas preparation reaction.

[0038] A reaction container 6 is provided below the connecting channel 5, and the reaction container 6 is communicated with the connecting channel 5. Optionally, the reaction container 6 is a conical flask or a wide-mouth bottle.

[0039] A cluster isotope sample gas injection device of the present invention, when used, comprises the following steps:

[0040] Place all samples in the sample chamber 4;

[0041] Rotate the outer disk 2 to connect the sample chamber 4 with the injection channel 3;

[0042] After the reaction of the previous sample is completed, the outer disk 2 is rotated to connect another sample chamber 4 with the injection channel 3.

[0043] Example

[0044] The following combination Figure 1 and Figure 2 The specific embodiments of the present invention are further described.

[0045] In this embodiment, the number of the sample chambers 4 is 10, the diameter of the sample chambers 4 is 15 mm, the diameter of the connecting holes of the sample chambers 4 is 10 mm, and the sample chambers 4 are covered with screw-in glass covers.

[0046] The main process includes: reaction of carbonate and phosphoric acid to produce CO2 gas; CO2 purification to remove pollutants; cluster isotope measurement, using a mass spectrometer to measure CO2 to obtain the original signal intensity value; nonlinear correction, correcting the original △47 value to the absolute reference system, and correcting the acid fractionation coefficient to obtain the final result.

[0047] The sample in the glass tube 101 is subjected to a common acid bath through the device of the present invention, with a reaction time of 10 to 30 minutes, a temperature of 90°C, and a sample size of >1 mg. The entire sample is placed in the sample chamber 4, and the outer disk 2 is rotated to achieve the purpose of sampling.

[0048] Each time sampling is required, the outer disk 2 is manually rotated to the appropriate position so that the connecting hole of the sample chamber 4 is connected to the sampling channel 3. At this time, the sample to be tested enters the sampling channel 3 under gravity, while other samples remain in a completely independent and closed sample position space without being affected.

[0049] After the reaction of one sample is completed and the sample gas preparation is finished, the outer disk 2 continues to rotate and the above operation is repeated to allow the next sample to be tested to enter the reaction system to start preparing the next group of sample gases.

[0050] Before the gas is separated and purified by the GC column, a silver wire filling tube (single tube or multiple tubes to remove sulfur-containing pollutants) is used.

[0051] like Figure 2 As shown, water is removed using a -196°C liquid nitrogen U-trap 102. Remaining unrefrigerated gases are pumped away with N2 and O2 via a vacuum pump. Remaining contaminants, particularly chlorocarbons and hydrocarbons, are removed using a Porapak Q-GC column trap 103 (divinyl benzene polymer trap) filled with divinylbenzene polymer. Cooled in the U-trap 102 at temperatures between -10°C and -35°C, the target gas, CO2, passes through the GC column at a much higher rate than less volatile gases at these temperatures, allowing CO2 to pass through while impurity gases are retained. Finally, the CO2 is directly transferred to a mass spectrometer 104.

[0052] Unless otherwise specified, the device components involved in the above embodiments are all conventional device components, and the structural settings, working modes or control modes involved are all conventional settings, working modes or control modes in the art unless otherwise specified.

[0053] Finally, it should be noted that the above embodiments are only used to illustrate the technical solution of the present invention and are not limiting. Other modifications or equivalent substitutions made to the technical solution of the present invention by ordinary technicians in this field should be included in the scope of the claims of the present invention as long as they do not depart from the spirit and scope of the technical solution of the present invention.

Claims

1. A cluster isotope sample gas injection device, characterized in that: include: An inner plate (1), wherein a connecting passage (5) is provided at the center of the inner plate (1); An outer disk (2), the outer disk (2) being rotatably sleeved on the outside of the inner disk (1); The outer disk (2) is provided with a plurality of mutually isolated sample chambers (4); the inner disk (1) is provided with a sample injection channel (3); a connecting hole is provided on a side of the sample chamber (4) close to the inner disk (1); one end of the sample injection channel (3) is connected to the connecting channel (5), and the other end is connected to the connecting hole of the inner disk (1); the top height of the connecting channel (5) is lower than the height of the connecting hole of the sample chamber (4).

2. The cluster isotope sample gas injection device according to claim 1, characterized in that: The number of the sample chambers (4) is 10 to 12.

3. The cluster isotope sample gas injection device according to claim 1, characterized in that: The inner plate (1) and the outer plate (2) are both funnel-shaped.

4. The cluster isotope sample gas injection device according to claim 1, characterized in that: The sample chambers (4) are arranged at equal intervals along the circumferential direction of the outer disk (2).

5. The cluster isotope sample gas injection device according to claim 1, characterized in that: The diameter of the sample chamber (4) is 10 mm to 15 mm.

6. The cluster isotope sample gas injection device according to claim 1, characterized in that: The diameter of the injection channel (3) is 10 mm.

7. The cluster isotope sample gas injection device according to claim 1, characterized in that: The angle between the injection channel (3) and the horizontal plane is 60°.

8. The method for using the cluster isotope sample gas injection device according to any one of claims 1 to 7, characterized in that: The following steps are involved: Place all samples in the sample chamber (4); Rotate the outer disk (2) to connect the sample chamber (4) with the injection channel (3); After the reaction of the previous sample is completed, the outer disk (2) is rotated to connect another sample chamber (4) with the injection channel (3).

9. A preparation device, characterized in that: It comprises a cluster isotope sample gas injection device according to any one of claims 1 to 7 and a reaction container (6), wherein the reaction container (6) is arranged below the connecting channel (5).

10. A preparation device according to claim 9, characterized in that: The reaction container (6) is a conical flask.

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