CN110987570A - Pretreatment system for total organic carbon test - Google Patents

Pretreatment system for total organic carbon test Download PDF

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Publication number
CN110987570A
CN110987570A CN201911402465.9A CN201911402465A CN110987570A CN 110987570 A CN110987570 A CN 110987570A CN 201911402465 A CN201911402465 A CN 201911402465A CN 110987570 A CN110987570 A CN 110987570A
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sample
liquid
liquid injection
reaction
organic carbon
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Inventor
许智超
张小涛
黄春华
徐学敏
秦婧
杨佳佳
栗敏
沈斌
汪双清
孙玮琳
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NATIONAL Research CENTER OF GEOANALYSIS
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NATIONAL Research CENTER OF GEOANALYSIS
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Priority to CN201911402465.9A priority Critical patent/CN110987570A/en
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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/34Purifying; Cleaning
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00Sampling; Preparing specimens for investigation
    • G01N1/28Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/44Sample treatment involving radiation, e.g. heat

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  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical & Material Sciences (AREA)
  • Analytical Chemistry (AREA)
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  • General Physics & Mathematics (AREA)
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  • Molecular Biology (AREA)
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  • Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)

Abstract

The invention relates to the technical field of oil-gas exploration and hydrocarbon source rock testing, and provides a pretreatment system for testing total organic carbon, which comprises: the reaction device comprises a sample disc, the sample disc is connected to a first rotating shaft, a plurality of sample sites are arranged on the sample disc in an annular mode, and the sample sites are used for containing reaction containers; the liquid adding device comprises a liquid injection assembly, an acid injection passage and a water injection passage, wherein the liquid injection assembly is provided with a liquid injection head, the liquid injection head is connected with the acid injection passage and the water injection passage, and the liquid injection head moves to the sample grade and is aligned to the reaction container. According to the pretreatment system for testing the total organic carbon, the sample bits are distributed in a ring shape, and when the area is the same, the number of the sample bits is increased, the single batch processing amount is improved, and the testing efficiency is improved.

Description

Pretreatment system for total organic carbon test
Technical Field
The invention relates to the technical field of oil-gas exploration and hydrocarbon source rock testing, in particular to a pretreatment system for testing total organic carbon.
Background
The Total Organic Carbon (TOC) content is a primary index for measuring the abundance of organic matters in the rock and is one of necessary basic items for potential evaluation of the hydrocarbon source rock. The basis for determining the TOC content in China is GB/T19145-2003 'determination of total organic carbon in sedimentary rock', and the standard test principle is that after inorganic carbon in a sample is removed by dilute hydrochloric acid, the sample is placed in high-temperature oxygen flow to be fully combusted to generate CO2And detecting by an infrared detector to finally give the content of the total organic carbon. The process of removing inorganic carbon with dilute hydrochloric acid is also called as sample pretreatment, and is divided into steps of sample dissolving, sample washing, sample drying and the like.
In the existing pretreatment device, a plurality of sample grades are arranged on a sample disc for containing samples, the sample disc is rectangular, the sample grades are sequentially arranged along the length and the width direction of the sample disc, the number of sample sites which are linearly arranged is limited under the condition that the area of the sample disc is fixed, and further the number of samples tested on one sample disc is limited, namely, the single batch processing capacity is limited, so that the testing efficiency is influenced. In addition, in the conventional pretreatment apparatus, the number of liquid transfer lines is the same as the number of rows of sample stages, the number of liquid transfer lines required is large, and the number of detectors is also large, so that the apparatus structure is complicated and the cost is high.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides a pretreatment system for testing total organic carbon, wherein the sample bits are distributed in a ring shape, and when the sample bits have the same area, the number of the sample bits is increased, the single batch processing capacity is improved, and the testing efficiency is improved.
The pretreatment system for the total organic carbon test according to the embodiment of the first aspect of the invention comprises:
the reaction device comprises a sample disc, the sample disc is connected to a first rotating shaft, a plurality of sample sites are arranged on the sample disc in an annular mode, and the sample sites are used for containing reaction containers;
the liquid adding device comprises a liquid injection assembly, an acid injection passage and a water injection passage, wherein the liquid injection assembly is provided with a liquid injection head, the liquid injection head is connected with the acid injection passage and the water injection passage, and the liquid injection head moves to the sample grade and is aligned to the reaction container.
According to an embodiment of the present invention, the liquid injection assembly further comprises a guide rail connected to the second rotation shaft, and the guide rail is slidably connected to the CO2The detector and the liquid injection head, the guide rail drives the CO2The detector and the liquid injection head rotate to the upper part of the reaction vessel, and CO is discharged2The detector and/or the injection head are/is slidably adjusted to be aligned with the reaction vessel.
According to one embodiment of the present invention, the pouring head includes a first pouring port connected to the acid pouring passage and a second pouring port connected to the water pouring passage.
According to one embodiment of the invention, the liquid injection assemblies are uniformly distributed on the periphery of the reaction device.
According to one embodiment of the invention, the sample stage is arranged to form a plurality of concentric rings, and the reaction apparatus further comprises a heating element having a ring shape, the heating element being disposed between two of the concentric rings.
According to an embodiment of the present invention, the reaction device further includes a filtrate tank, a filtrate chamber is formed in the filtrate tank, the filtrate tank is fixedly connected to the sample tray, the sample tray is provided with a through hole, the through hole communicates the filtrate tank with the sample cavity in the reaction container, and the filtrate tank is communicated with a liquid discharge device.
According to one embodiment of the invention, a negative pressure component is further connected to the filtrate tank, and the reaction device further comprises a first sealing component which closes an opening above the reaction device.
According to one embodiment of the present invention, a fixing groove is formed at the sample position, a separate sample compartment is formed in the fixing groove, the first sealing member is provided at an upper opening of the fixing groove, and the reaction container is provided in the fixing groove.
According to one embodiment of the invention, the sample tray is formed with a connected sample compartment thereon; a flow guide surface gradually decreasing towards the center direction along the periphery of the sample disc is formed in the sample bin;
the first sealing component is sealed above the reaction container, and the reaction container is communicated with the sample bin and the filtrate bin;
the reaction device is also connected with a liquid supply assembly, and the liquid supply assembly is communicated with the sample bin and supplies liquid to the sample bin.
According to one embodiment of the invention, the negative pressure assembly comprises a negative pressure pipeline connected to the filtrate tank, wherein the negative pressure pipeline is a flexible pipeline or a movable sleeve; the liquid drainage device comprises a liquid drainage pipeline connected with the filtrate tank, and the liquid drainage pipeline is a flexible pipeline or a movable sleeve.
According to an embodiment of the invention, further comprising a placeholder container for filling with the sample level empty.
One or more technical solutions in the embodiments of the present invention have at least one of the following technical effects:
in the embodiment of the invention, the sample sites on the sample tray are annularly distributed, so that the reaction vessels on the sample tray are annularly distributed, the number of the reaction vessels which can be accommodated on the sample tray with the same area is increased, the single batch processing capacity is increased, and the test effect is improved; and, the sample dish is rotatory to carry out the liquid feeding with the notes liquid subassembly cooperation of liquid feeding device, simplifies the structure of annotating the liquid subassembly, and annotates the volume of liquid subassembly and reduce, only need set one on the notes liquid subassembly and annotate the liquid head, annotates liquid head quantity and reduce, and the pipeline structure is simplified, further simplifies the structure of annotating the liquid subassembly, reduce cost.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic structural diagram of an embodiment of a pre-processing system for total organic carbon testing provided by an embodiment of the present invention;
FIG. 2 is an enlarged partial schematic view of the structure of FIG. 1 in phantom;
FIG. 3 is a schematic structural diagram of another embodiment of a pretreatment system for total organic carbon testing according to an embodiment of the present invention;
FIG. 4 is an enlarged partial schematic view of the structure in the dashed box of FIG. 3;
FIG. 5 is a schematic diagram of a top view of a pretreatment system for total organic carbon testing according to an embodiment of the present invention;
reference numerals:
1: a reaction device; 11: a sample tray; 111: fixing grooves; 112: a liquid inlet; 113: a liquid level detector; 114: a liquid outlet; 12: a first rotating shaft; 13: a filtrate tank; 14: a heating member; 15: a first seal assembly; 151: a first gasket; 152: pressing a plate; 153: a locking member; 16: a second seal assembly; 17: a temperature control panel; 18: a communicating groove; 19: a drainage rod;
2: a reaction vessel; 21: a sample chamber;
3: a liquid adding device; 31: a liquid injection assembly; 311: a liquid injection head; 3111: a first liquid injection port; 3112: a second liquid injection port; 3113: CO 22A detector; 312: a guide rail; 313: a second rotating shaft; 32: an acid injection passage; 321: an acid reagent bottle; 322: a first syringe pump; 323: a first valve body; 33: a water injection passage; 331: a water reagent bottle; 332: a second syringe pump; 333: a second valve body; 34: a reset groove;
41: a negative pressure pipeline; 42: a pressure control panel;
5: a liquid discharge device; 51: a filtrate collection tank; 52: an ion detector; 54: a pump body; 55: a lifting assembly; 56: a drainage line;
6: a third seal.
Detailed Description
The embodiments of the present invention will be described in further detail with reference to the drawings and examples. The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
In the description of the embodiments of the present invention, it should be noted that the terms "center", "longitudinal", "lateral", "upper", "lower", "front", "rear", "left", "right", "vertical", "horizontal", "top", "bottom", "inner", "outer", and the like indicate orientations or positional relationships based on those shown in the drawings, and are only for convenience in describing the embodiments of the present invention and simplifying the description, but do not indicate or imply that the referred devices or elements must have a specific orientation, be constructed in a specific orientation, and be operated, and thus, should not be construed as limiting the embodiments of the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the embodiments of the present invention, it should be noted that, unless explicitly stated or limited otherwise, the terms "connected" and "connected" are to be interpreted broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; may be directly connected or indirectly connected through an intermediate. Specific meanings of the above terms in the embodiments of the present invention can be understood in specific cases by those of ordinary skill in the art.
In embodiments of the invention, unless expressly stated or limited otherwise, the first feature "on" or "under" the second feature may be directly contacting the first and second features or indirectly contacting the first and second features through intervening media. Also, a first feature "on," "over," and "above" a second feature may be directly or diagonally above the second feature, or may simply indicate that the first feature is at a higher level than the second feature. A first feature being "under," "below," and "beneath" a second feature may be directly under or obliquely under the first feature, or may simply mean that the first feature is at a lesser elevation than the second feature.
In the description herein, references to the description of the term "one embodiment," "some embodiments," "an example," "a specific example," or "some examples," etc., mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of an embodiment of the invention. In this specification, the schematic representations of the terms used above are not necessarily intended to refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples. Furthermore, various embodiments or examples and features of different embodiments or examples described in this specification can be combined and combined by one skilled in the art without contradiction.
Referring to fig. 1 to 5, an embodiment of the present invention provides a pretreatment system for testing total organic carbon, including: the reaction device 1 comprises a sample disc 11, the sample disc 11 is connected to a first rotating shaft 12, a plurality of sample positions are arranged on the sample disc 11, the sample positions are arranged in a ring shape, and the sample positions are used for containing the reaction containers 2; the liquid adding device 3 comprises a liquid injecting assembly 31, an acid injecting passage 32 and a water injecting passage 33, wherein a liquid injecting head 311 is arranged on the liquid injecting assembly 31, the liquid injecting head 311 is connected with the acid injecting passage 32 and the water injecting passage 33, and the liquid injecting head 311 moves to a sample grade and is aligned with the reaction container 2.
The rock sample is reacted in the reaction vessel 2 and the liquid adding device 3 provides the liquid required for the reaction. The acid injection passage 32 adds acid to the reaction vessel 2 through the injection head 311, and the inorganic carbon in the rock sample meets the acid reagent to form CO2Gas is discharged (i.e. sample dissolution), the water injection passage 33 injects water into the reaction vessel 2 through the injection head 311, and the acid reagent remaining in the rock sample reaction is washed and flushed out, thereby realizing the pretreatment of the detection of the total organic carbon in the rock sample.
Wherein the sample sites are arranged in a ring, i.e. the reaction vessels 2 are arranged in a ring on the sample plate 11. The "ring" is generally a circular ring, wherein the circular ring can be a whole circular ring, a semicircular ring, a fan-shaped ring and the like in various shapes. The "annular" may be another annular such as an elliptical ring. The sample positions are arranged on the sample tray 11 to form a plurality of rings, and when the sample positions are arranged to form a plurality of rings, the rings are concentric rings, so that liquid adding operation is facilitated. Compared with the sample positions arranged in a straight line, the sample trays 11 with the same area have more sample positions which can be accommodated by the annular arrangement, so that the single batch processing capacity is improved, and the processing efficiency and the testing efficiency are improved. In general, the outline of the sample tray 11 is shaped to conform to the outline of the sample site array.
The sample plate 11 is fixedly connected with a first rotating shaft 12, the first rotating shaft 12 can be driven by a structure which provides rotating power through a motor, a motor and the like, and the driving structure of the motor and the like can be fixed on the ground or other fixed structures (such as a shell) to ensure that the sample plate 11 stably rotates.
The treatment process comprises the following steps: the pouring head 311 of the liquid adding device 3 is moved above the sample tray 11, and the pouring head 311 is moved above the reaction vessel 2 of one of the sample grades (hereinafter referred to as the first sample grade), the pouring head 311 is aligned with the reaction vessel 2 and acid is poured therein; after the acid injection is completed, the first rotating shaft 12 is driven to rotate by external force, the first rotating shaft 12 drives the sample disc 11 to rotate, the sample disc 11 rotates until the injection head 311 corresponds to the second sample grade (the second sample grade is adjacent to the first sample grade in general), the injection head 311 injects acid into the reaction container 2 of the second sample grade, and after the acid injection is completed, the sample disc 11 continues to rotate until all the samples in the reaction containers 2 on the ring where the first sample grade is located complete the acid injection operation. When the sample sites are arranged to form a plurality of rings, and the acid injection operation is completed for one ring, the liquid adding device 3 moves to adjust the liquid injection head 311 to correspond to the reaction vessel 2 on the other ring, and the above operation is repeated until the acid injection operation for the reaction vessel 2 on the entire sample plate 11 is completed. When the removal of the inorganic carbon in the rock sample in the reaction vessel 2 is completed, the acid injection operation is completed, and then the water injection operation is performed by repeating the above-described steps.
It should be noted that, when there is no sample to be tested in a sample stage adjacent to the first sample stage, the second sample stage is located on the same ring as the first sample stage and close to the first sample stage, and therefore, the first sample stage and the second sample stage are not limited to adjacent positions.
Combining the above-mentioned processing procedure can know, liquid filling device 3 can only set up one and annotate liquid head 311, can accomplish the notes liquid operation, for the mode that sets up a plurality of notes liquid heads 311 on current liquid filling device 3, has simplified liquid filling device 3's structure, reduces spare part, has reduced manufacturing cost simultaneously.
The reaction vessel 2 is generally a crucible, has good acid resistance and heat resistance, and is suitable for the total organic carbon test of rock samples. The reaction vessel 2 may employ a pre-calcination-treated TOC-dedicated crucible.
In this embodiment, the sample levels are distributed annularly on the sample tray 11 to increase the number of sample levels, improve the single batch processing capacity, and further improve the processing efficiency; meanwhile, the sample plate 11 can rotate, and the sample plate 11 rotates, so that the liquid adding device 3 can be kept at a set position, and the structure of the liquid adding device 3 is simplified; moreover, the liquid adding device 3 may be provided with only one liquid pouring head 311, thereby further simplifying the structure of the liquid adding device 3.
The liquid adding device 3 will be further described below with reference to fig. 1 to 5, taking as an example a case where a plurality of sample stages are arranged to form a plurality of concentric rings.
In another embodiment, the liquid injection assembly 31 further comprises a guide rail 312, the guide rail 312 is connected to the second rotating shaft 313, the liquid injection head 311 is slidably connected to the guide rail 312, the guide rail 312 drives the liquid injection head 311 to rotate above the reaction vessel 2, and the liquid injection head 311 is slidably adjusted to be aligned with the reaction vessel 2. The guide rail 312 can be rotated to the upper part of the reaction vessel 2, then the position of the liquid injection head 311 on the guide rail 312 is adjusted in a sliding way, and the liquid injection head 311 is aligned to the reaction vessel 2 through the cooperation of the rotation adjustment and the sliding adjustment, so that the operation is simple and convenient, and the adjustment accuracy is high.
The second rotating shaft 313 can also be driven by a structure with a rotation driving function, such as a motor, a motor and the like, and the driving structure, such as the motor and the like, is fixed on the ground or on the shell of the device, so that the structure is simple and the fixation is stable.
Further, the guide rail 312 is slidably connected to the CO2Detector 3113, guide 312 drives CO2The detector 3113 is rotated above the reaction vessel 2, CO2The detector 3113 is slidably adjusted to be aligned with the reaction vessel 2. Wherein, CO2The detector 3113 and the liquid injection head 311 may be adjusted simultaneously or independently.
Wherein, CO2The detector 3113 and/or the injector head 311 are slidably adjusted to be aligned with the reaction vessel 2, which can be understood as follows: when liquid injection is required, the liquid injection head 311 is aligned with the reaction vessel 2, and CO detection is required2When it is CO2Detector 3113 corresponding to vessel, CO2The detector 3113 and the liquid injection head 311 are independently aligned with the reaction vessel 2; alternatively, the injection liquid and CO2Detection is carried out simultaneously, CO2The detector 3113 is aligned with the reaction vessel 2 in synchronization with the liquid injection head 311.
In another embodiment, the pouring head 311 includes a first pouring port 3111 and a second pouring port 3112, the first pouring port 3111 is connected to the acid pouring passage 32, and the second pouring port 3112 is connected to the pouring passage 33. The first injection port 3111 communicates with the acid injection passage 32 and injects an acid reagent into the reaction vessel 2, and the second injection port 3112 communicates with the water injection passage 33 and injects distilled water into the reaction vessel 2.
Acid reagent and distilled water are carried through two passageways respectively and are got into reaction vessel 2, solve among the prior art problem that acid reagent and cleaner thoughtlessly annotated, avoid having remaining acid reagent in the pipeline because of the common pipeline leads to actually getting into the distilled water of rock sample, avoid increasing because of the inconsistent test error that leads to of same batch rock sample processing procedure, improved the stability of test data.
Further, the acid injection passage 32 includes an acid reagent bottle 321 and a first injection pump 322, the first injection pump 322 communicates with the acid reagent bottle 321 through a first valve 323, the first injection pump 322 further communicates with the first liquid injection port 3111 through a pipe, the water injection passage 33 includes a water reagent bottle 331 and a second injection pump 332, the second injection pump 332 communicates with the water reagent bottle 331 through a second valve 333, and the second injection pump 332 further communicates with the second liquid injection port 3112 through a pipe. In this embodiment, an acid reagent and distilled water are respectively contained in an acid reagent bottle 321 and a water reagent bottle 331 and are placed in a reagent tank together, the acid reagent bottle 321 is connected to a first valve body 323 and a first injection pump 322 in sequence through a hose, and the water reagent bottle 331 is connected to a second valve body 333 and a second injection pump 332 in sequence through a hose. In this embodiment, the first valve body 323 and the second valve body 333 both adopt six-way valves. The first injection pump 322 sucks the acid reagent through the six-way valve, switches the six-way valve and leads the acid reagent into the pipeline of the acid injection passage 32 carried by the guide rail 312 for concentration; the second injection pump 332 sucks distilled water through the six-way valve, switches the six-way valve, and concentrates the distilled water through the pipe line of the water injection passage 33 mounted on the guide rail 312. Thereby forming two completely independent liquid injection passages.
Further, liquid feeding device 3 still includes reset groove 34, and reset groove 34 is used for spacing annotating liquid subassembly 31, and the liquid feeding is accomplished the back, annotates liquid subassembly 31 and replies to reset groove 34 in, guarantees to annotate the stability of liquid subassembly 31.
In another embodiment, a plurality of liquid injection assemblies 31 are uniformly distributed on the periphery of the reaction device 1, and each liquid injection assembly 31 is connected with the acid injection passage 32 and the water injection passage 33. When the liquid injection assembly 31 is arranged, the sample tray 11 needs to rotate 360 degrees, and the liquid injection of the reaction container 2 can be completed in a circle, so that the time consumption is long, but the structure is simple and the structure cost is low. When the liquid injection assembly 31 is arranged two, the sample tray 11 rotates 180 degrees, so that the liquid injection of the reaction container 2 can be completed by one circle, the liquid injection time is shortened, and the treatment efficiency is improved. When annotating liquid subassembly 31 and setting up threely, three annotate liquid subassembly 31 and form 120 contained angles, sample dish 11 is rotatory 120, can accomplish the liquid feeding of round reaction vessel 2, and it is long when further shortening the liquid feeding, improves the treatment effeciency. By analogy, the liquid injection assemblies 31 can be four, five or more.
Next, examples of the reaction apparatus 1 are provided.
In another embodiment, shown in connection with FIG. 5, the sample sites are arranged to form a plurality of concentric rings, and the reaction apparatus 1 further comprises a heating member 14, the heating member 14 being in the shape of a ring, the heating member 14 being disposed between the two concentric rings. The annular heating member 14 uniformly heats the reaction vessels 2 arranged in an annular shape, thereby improving the heating uniformity.
The heating member 14 may be a heating wire, a heating pipe, or the like. The heating element 14 is connected to a temperature control panel 17 by temperature control wires to ensure that the heating element 14 heats or maintains the sample site. The sample tray 11 is provided with a communicating groove 18, the temperature control line is routed in the communicating groove 18, and the communicating groove 18 plays a role in protecting the temperature control line. Further, the communicating groove 18 is communicated with the first rotating shaft 12, and the temperature control line is routed in the communicating groove 18 and the first rotating shaft 12, so that the temperature control line is fully protected.
Further, the heating element 14 may directly heat the air in the sample tray 11, or may heat the solution in the sample tray 11 to form a water bath.
In another embodiment, the reaction apparatus 1 further comprises a filtrate tank 13, a filtrate chamber is formed in the filtrate tank 13, the filtrate tank 13 is fixedly connected to the sample plate 11, a through hole is formed in the sample site, the through hole communicates the filtrate tank 13 with the sample chamber 21 in the reaction container 2, and the filtrate tank 13 communicates with the drain 5.
Distilled water is added into the reaction vessel 2, the residual acid reagent in the rock sample is mixed with the distilled water to form filtrate, and the filtrate sequentially penetrates through the bottom and the through holes of the reaction vessel 2 and is infiltrated into a filtrate bin under the action of gravity.
Further, the filtrate tank 13 and the sample tray 11 may be an integrated structure, and the filtrate bin is formed into an inverted cone structure so as to guide the flow of the filtrate. That is, the projection view of the sample plate 11 and the filtrate tank 13 is a central ring structure, and the first rotating shaft 12 is connected to the filtrate tank 13 and the hollow cylindrical hole at the center of the sample plate 11.
Furthermore, a drainage rod 19 is connected to the sample tray 11, the drainage rod 19 is located at the position of the through hole, and the drainage rod guides the filtrate to the filtrate bin and accelerates the flow of the filtrate. Further, the drainage rod 19 extends to the inner wall of the filtrate tank 13 to drain the filtrate sufficiently.
The liquid drainage device 5 further comprises a liquid drainage pipeline 56, a filtrate collecting tank 51 and an ion detector 52, wherein the filtrate collecting tank 51 is connected with the bottom of the filtrate tank 13 through the liquid drainage pipeline 56, a pump body 54 is arranged on the liquid drainage pipeline 56, and the ion detector 52 is arranged on the filtrate collecting tank 51 through a lifting assembly 55. The drainage device 5 is responsible for collecting and monitoring the endpoint recognition indexes in real time, provides a judgment basis for the automatic process of the instrument, and collects the experimental waste liquid in a unified way.
In this embodiment, the filtrate in each cleaning cycle is accelerated by the pump 54, flows from the bottom of the filtrate tank along the drain line 56 into the filtrate collection tank 51, and undergoes pH and Cl processes in the filtrate collection tank 51-Ion concentration or other ion concentration detection. In this embodiment, the ion detector 52 may be a pH detector or Cl-A detector or other more durable detector, wherein the pH detector detects H+Or OH-And (4) concentration. The lifting assembly 55 employs a holder for holding the pH detector/Cl and an automatic lifting track-The detector moves up and down on the automatic lifting track and repeatedly enters the filtrate collecting tank 51 to carry out pH value and Cl on the filtrate-Detecting the ion concentration or other ion concentrations until the pH value and Cl-When the ion concentration or other ion concentrations are less than or equal to the set threshold, it is considered that the cleaning end point is reached, and at this time, the water injection path 33 does not perform the circulating water injection flow in the reaction container 2.
Furthermore, the filtrate tank 13 can be connected with a plurality of drainage pipelines 56, so that the drainage efficiency is improved.
In another embodiment, the drain line 56 is a flexible line or a removable sleeve. When the sample disk 11 and the filtrate tank 13 are integrated, that is, the filtrate tank 13 can rotate synchronously with the sample disk 11, and a certain amount of movement needs to be left in the drainage pipeline 56 during the rotation of the filtrate tank 13, so that the drainage pipeline 56 is a flexible pipeline or a movable sleeve to cooperate with the rotation of the sample disk 11. The movable sleeve comprises a sleeve structure formed by at least two sections of rotatably connected pipe fittings.
In another embodiment, the filtrate tank 13 is further connected with a negative pressure component, and the reaction device 1 further comprises a first sealing component 15, wherein the first sealing component 15 seals the opening above the reaction device 1, so that a closed environment is formed in the reaction device 1, and the negative pressure component accelerates the percolation of the liquid.
In the process of repeated water addition, in order to avoid overflow caused by excessive water in the reaction vessel 2, the water added each time needs to be completely percolated in the water addition period as much as possible, so that a negative pressure component needs to be started in addition to controlling the water addition amount each time, negative pressure is provided for the liquid in the reaction vessel 2 to the process of percolation in the filtrate bin, percolation of the liquid is accelerated, and efficiency is improved. Wherein, negative pressure assembly includes vacuum pump and negative pressure pipeline 41, and the vacuum pump passes through negative pressure pipeline 41 and filtrate storehouse intercommunication, starts the vacuum pump, makes filtrate storehouse form the negative pressure through negative pressure pipeline 41. In addition, the pretreatment system is further provided with a pressure control panel 42, the negative pressure module is connected with the pressure control panel 42, and the pressure control panel 42 is used for controlling and displaying the pressure state of the negative pressure module.
Further, the negative pressure pipeline 41 is a flexible pipeline or a movable sleeve. The negative pressure line 41 is connected to a portion of the filtrate tank 13 above the filtrate tank 13 to prevent the negative pressure line 41 from sucking the liquid in the filtrate tank 13 as much as possible. When the sample disk 11 and the filtrate tank 13 are integrated, that is, the filtrate tank 13 can rotate synchronously with the sample disk 11, and a certain amount of movement needs to be left in the negative pressure pipeline 41 during the rotation of the filtrate tank 13, so that the negative pressure pipeline 41 is a flexible pipeline or a movable sleeve to cooperate with the rotation of the sample disk 11. The movable sleeve comprises a sleeve structure formed by at least two sections of rotatably connected pipe fittings.
Furthermore, a plurality of negative pressure pipelines 41 can be connected to the filtrate tank 13 so as to facilitate multi-directional suction and facilitate uniform pressure distribution in the filtrate tank.
Two examples of sample trays 11 are provided below.
In another embodiment, as shown in fig. 1 and 2, a fixing groove 111 is formed at the sample site, a separate sample chamber is formed in the fixing groove 111, a first sealing member 15 is provided at an upper opening of the fixing groove 111, and the reaction vessel 2 is provided in the fixing groove 111. All form an independent space in every fixed slot 111, the first seal assembly 15 of upper end opening part butt of fixed slot 111 promptly, reaction vessel 2 is in fixed slot 111 internal reaction, avoids mutual interference between reaction vessel 2, guarantees to detect the accuracy. And a through hole is provided below each fixing groove 111 so that the filtrate flows out.
The first sealing assembly 15 comprises a first sealing gasket 151, a pressing plate 152 and a locking member 153, the first sealing gasket 151 is laid on the notch of the fixing groove 111, the pressing plate 152 is pressed on the first sealing gasket 151, and the pressing plate 152 is fixedly connected with the sample tray 11 through the locking member 153. Further, the lower end of the reaction vessel 2 is hermetically connected to the fixing groove 111, a second sealing assembly 16 is disposed in the fixing groove 111, and the second sealing assembly 16 is used for sealing the fixing groove 111 and the bottom of the reaction vessel 2. The second sealing assembly 16 includes a second sealing gasket disposed in the fixing groove 111, the reaction vessel 2 being placed on the second sealing gasket, and a gasket located between the reaction vessel 2 and the second sealing gasket. The arrangement of the first sealing member 15 and the second sealing member 16 ensures the environmental sealing in each fixing groove 111, and improves the flexibility of the choice of the reaction vessel 2 and the adaptability in the production practice.
Further, the reaction vessel 2 also abuts against the first sealing assembly 15, and the opening of the reaction vessel 2 is connected with the first sealing assembly 15 in a sealing manner, so that the stability of the reaction vessel 2 in the first sealing assembly 15 is improved.
The second is sealed fills up for elasticity seat and is sealed the pad, and elasticity seat is the conical surface with 2 complex surfaces of reaction vessel, can adapt to the 2 external diameters of different reaction vessel, sets up annular gasket group between the bottom surface of elasticity seat pad and reaction vessel 2 for adjust reaction vessel 2's height, make reaction vessel 2 flush as far as possible with the top surface of fixed slot 111. The first sealing gasket is an elastic sealing gasket, the opening of the reaction vessel 2 after being sealed and the notches of the fixing grooves 111 around the opening are provided with the elastic sealing gasket, a rigid compacting plate is placed above all the elastic sealing gaskets, and the rigid compacting plate is fastened with the sample tray 11 by a locking piece at the edge of the rigid compacting plate.
In this embodiment, since the outer diameter of the reaction vessel 2 is smaller than the inner diameter of the fixing groove 111, a gap exists between the reaction vessel 2 and the fixing groove 111, and in order to ensure the airtightness of the reaction apparatus 1, the first sealing member 15 is provided to isolate the inner space of the reaction apparatus 1 from the outside; the second sealing assembly 16 is arranged to isolate the gap between the fixing groove 111 and the bottom of the reaction container 2 from the inner space of the filtrate bin, so that the sealing effect is optimized.
In another embodiment, the difference from the above embodiment is that, as shown in fig. 3 and 4, the fixing groove 111 (not shown) need not be formed at the sample site. In particular, the sample tray 11 is formed with a connected sample chamber, i.e. a connected chamber space is formed on the whole sample tray 11, instead of the plurality of independent spaces in the above-described embodiment. The first sealing assembly 15 is sealed above the reaction container 2, the reaction container 2 is communicated with the sample bin and the filtrate bin, the first part of side wall of the reaction container 2 is communicated with the sample bin, the second part of side wall is communicated with the filtrate bin, namely, liquid in the sample bin permeates into the sample cavity 21 of the reaction container 2 through the first part of side wall, and liquid in the sample cavity 21 seeps out through the second part of side wall and flows into the filtrate bin. In order to supply liquid in the sample bin conveniently, the reaction device 1 is also connected with a liquid supply assembly, and the liquid supply assembly is communicated with the sample bin and supplies liquid to the sample bin.
In this embodiment, the sample chamber and the filtrate chamber can be understood as two independent spaces in the reaction device 1, and the sample chamber and the filtrate chamber are communicated through the reaction container 2.
During the use, hold the rock sample in the sample chamber 21, supply sour reagent to the sample storehouse in through the feed line way, in sour reagent permeates sample chamber 21 through first part lateral wall, sour reagent reacts with the sample in with to get rid of inorganic carbon, sour reagent permeates the filtrate storehouse from the second part lateral wall again. In the acid adding process, reverse percolation is adopted to replace direct dripping, so that the contact time of an acid reagent and a rock sample is prolonged, the reaction rate is further delayed, and the reaction intensity is reduced. For the mode of direct dropwise add acid reagent in to sample cavity 21 among the prior art, this embodiment makes acid reagent and reaction vessel 2's outer wall direct contact, carries out reverse osmosis, has avoided the sample to splash, and the test result is more accurate relatively.
Further, the liquid supply assembly can be used for adding a cleaning agent (such as distilled water) into the sample bin, and cleaning the rock sample after removing the inorganic carbon.
The reverse osmosis principle is that the reaction intensity is controlled by delaying the contact between reactants and prolonging the reaction time, so that the treatment efficiency is lower than that of a direct dropwise adding mode. This embodiment cooperation negative pressure subassembly, negative pressure subassembly promote the interior acid reagent of sample storehouse to flow in reaction vessel 2 to reaction rate is accelerated to a certain extent within range, raises the efficiency.
Further, as shown in fig. 3 and 4, a flow guide surface gradually decreasing along the outer circumference of the sample tray 11 toward the center is formed in the sample chamber, which facilitates the liquid to flow into and fill the sample chamber.
Further, a third sealing member 6 is arranged between the reaction vessel 2 and the sample site (the third sealing member 6 replaces the second sealing member 16 in the above-described embodiment), and the third sealing member 6 is arranged between the first part side wall and the second part side wall. The third seal 6 seals the outer wall of the reaction vessel 2 to the sample tray 11 to prevent liquid in the sample compartment from flowing into the filtrate compartment without entering the sample chamber 21.
Wherein, the inner wall of third sealing member 6 is laminated with reaction vessel 2 mutually and is sealed, and high foot seat packing is selected for use to third sealing member 6, and the top edge of third sealing member is higher than 1/4 of reaction vessel 2 height at least to guarantee sealed effect.
Further, the heating element 14 is arranged in the sample tray 11, liquid in the sample bin forms a water bath environment, and the heating element 14 forms water bath heating to enable heat to be uniformly diffused, so that the problem of nonuniform heat distribution is avoided.
Furthermore, a temperature sensor is arranged in the sample bin and is used for measuring the temperature of the liquid in the sample bin so as to accurately ensure that the temperature of the liquid in the sample bin is within a set range. And the power or heating time of the heating member 14 can be adjusted based on the readings of the temperature sensor.
Furthermore, a liquid level detector 113 is arranged in the sample bin, and the liquid level detector 113 detects the height of the acid reagent or the distilled water in the sample bin, so that the liquid level height of the sample bin is always kept at a set value according to the detection result of the liquid level detector 113.
The sample tray 11 is provided with a liquid inlet 112 and a liquid outlet 114, the sample tray 11 is further provided with a first switch and a second switch, the first switch is located at the liquid inlet 112, the second switch is located at the liquid outlet 114, the first switch is communicated with the liquid supply assembly and the sample bin, and the second switch is communicated with the sample bin and the filtrate bin.
When the liquid level in the sample bin exceeds a first set value, the first switch is closed, the second switch is opened, the liquid in the sample bin is discharged to the filtrate bin, and then the filtrate bin is discharged to the liquid discharging device 5. And when the liquid level in the sample bin is lower than a second set value, the first switch is opened, the second switch is closed, and liquid is supplied to the sample bin.
The liquid supply assembly comprises a liquid supply pipeline, an intermediate container and a liquid supply pump, the liquid supply pipeline is connected with the liquid supply pump and the intermediate container, the intermediate container is connected with the first switch, and the liquid supply pipeline is connected with the acid injection passage 32 or the water injection passage 33 so as to introduce an acid reagent or a cleaning agent into the sample bin.
It should be noted that both the liquid supply assembly and the liquid adding device can be used for adding liquid into the reaction container 2, and the liquid adding operations of the two-part structure are mutually independent, and in the using process, one of the two parts can be selected. When the liquid supply assembly carries out reverse osmosis acid addition, the sample disc and the liquid adding device are both kept in a static state, so that the problem of pipeline winding in the rotating process is avoided.
During operation of the above embodiment, the liquid level in the reaction vessel 2 does not exceed 2/3, which is the total height thereof. On one hand, the phenomenon that the liquid level is too high and carries the sample to float upwards is avoided, and further the experiment failure caused by sample loss is avoided; on the other hand, because the sample below the reaction vessel 2 burns more fully in the follow-up test, if the sample height is too high or the height is not uniform, there is the potential risk of insufficient burning, and then lead to that the test value has data quality problems such as error, data reliability are not high.
Furthermore, the pretreatment device also comprises an occupying container which is used for filling the empty sample. The space-occupying container has the functions of: when the sample amount of the batch is less than the number of sample positions in the instrument, an occupying container is added at the sample position without the sample, so that the local closed space required by negative pressure and/or reverse osmosis is ensured, and the experiment is smoothly carried out.
The space occupying container can be made of acid-resistant stainless steel, corrosion-resistant organic materials, high-temperature fired ceramic materials and the like.
The lower level will be described in detail with reference to fig. 2, taking the sample sites arranged to form a plurality of circular rings as an example.
The sample sites are arranged in a circular ring shape, and the number of the sample sites on the sample disk 11 can be increased to 120. And (3) adding liquid by using the single liquid injection assembly 31, optionally performing natural infiltration, wherein the liquid adding time of each sample is 20-30 s, the sample plate 11 rotates for 360 degrees, the total time is 40-60 min, and the time interval is enough for completing the natural infiltration of the sample in the initial sample position. The multiple liquid injection assemblies 31 are used for liquid injection, accelerated percolation can be selected, namely, the negative pressure assembly is started, and the efficiency is improved; taking two liquid injection assemblies 31 as an example, in order to complete liquid injection and detection of all samples, the sample tray 11 only needs to rotate 180 degrees, and the time is consumed for 20-30 min; the four liquid injection assemblies 31 only need to rotate 90 degrees, the time is consumed for 10-15 min, and the treatment efficiency is obviously improved.
The reaction vessel 2 at the sample site is understood to be arranged in polar coordinates, and the liquid adding device 3 (acid adding "sample dissolving"/water adding "sample washing") needs to adjust the polar diameter (the position of the liquid injecting head 311 on the guide rail 312) and the polar angle (the rotation angle of the guide rail 312).
The specific use steps of the liquid adding process are as follows:
one is as follows: the whole liquid injection assembly 31 moves from the upper part of the reset groove 34 to the upper part of the sample plate 11, and initial position calibration is carried out; specifically, the guide rail 312 is rotated and adjusted to an appropriate polar angle, and the liquid injection head 311 slides to an appropriate polar diameter, so that the liquid injection head 311 is positioned above the annularly-distributed reaction vessels 2;
the second step is as follows: the addition of the first reaction vessel 2 on the ring is carried out;
and thirdly: fixing the pole diameter, rotating the sample disc 11, and sequentially completing liquid adding of all sample grades on the circular ring;
fourthly, the polar diameter is sequentially adjusted to complete the liquid adding of all the reaction containers 2; the diameter control can be from outside to inside or from inside to outside;
and fifthly: the priming assembly 31 is returned to the reset tank 34.
The above embodiments are merely illustrative of the present invention and are not to be construed as limiting the invention. Although the present invention has been described in detail with reference to the embodiments, it should be understood by those skilled in the art that various combinations, modifications or equivalents may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, and the technical solution of the present invention is covered by the claims of the present invention.

Claims (11)

1. A pre-processing system for total organic carbon testing, comprising:
the reaction device comprises a sample disc, the sample disc is connected to a first rotating shaft, a plurality of sample sites are arranged on the sample disc in an annular mode, and the sample sites are used for containing reaction containers;
the liquid adding device comprises a liquid injection assembly, an acid injection passage and a water injection passage, wherein the liquid injection assembly is provided with a liquid injection head, the liquid injection head is connected with the acid injection passage and the water injection passage, and the liquid injection head moves to the sample grade and is aligned to the reaction container.
2. The pretreatment system for testing total organic carbon according to claim 1, wherein the liquid injection assembly further comprises a guide rail connected to the second rotating shaft, and the guide rail is slidably connected with a CO2The detector and the liquid injection head, the guide rail drives the CO2The detector and the liquid injection head rotate to the upper part of the reaction vessel, and CO is discharged2The detector and/or the injection head are/is slidably adjusted to be aligned with the reaction vessel.
3. The pretreatment system for total organic carbon test according to claim 1, wherein the liquid injection head includes a first liquid injection port and a second liquid injection port, the first liquid injection port is connected to the acid injection passage, and the second liquid injection port is connected to the water injection passage.
4. The pretreatment system for testing total organic carbon according to claim 1, wherein a plurality of liquid injection assemblies are uniformly distributed on the periphery of the reaction device.
5. The pretreatment system for testing total organic carbon according to claim 1, wherein the sample stage is arranged to form a plurality of concentric rings, and the reaction apparatus further comprises a heating member having a ring shape, the heating member being disposed between two of the concentric rings.
6. The pretreatment system for testing total organic carbon according to claim 1, wherein the reaction device further comprises a filtrate tank, a filtrate bin is formed in the filtrate tank, the filtrate tank is fixedly connected with the sample tray, a through hole is formed in the sample level, the through hole communicates the filtrate tank with a sample cavity in the reaction container, and the filtrate tank communicates with a liquid discharge device.
7. The pretreatment system for testing total organic carbon according to claim 6, wherein a negative pressure component is further connected to the filtrate tank, and the reaction device further comprises a first sealing component which closes an opening above the reaction device.
8. The pretreatment system for testing total organic carbon according to claim 7, wherein a fixing groove is formed at the sample position, a separate sample chamber is formed in the fixing groove, the first sealing member is disposed at an upper opening of the fixing groove, and the reaction vessel is disposed in the fixing groove.
9. The pretreatment system for total organic carbon testing of claim 7, wherein the sample tray is formed with a communicating sample compartment thereon; a flow guide surface gradually decreasing towards the center direction along the periphery of the sample disc is formed in the sample bin;
the first sealing component is sealed above the reaction container, and the reaction container is communicated with the sample bin and the filtrate bin;
the reaction device is also connected with a liquid supply assembly, and the liquid supply assembly is communicated with the sample bin and supplies liquid to the sample bin.
10. The pretreatment system for testing total organic carbon according to claim 7, wherein the negative pressure assembly comprises a negative pressure pipeline connected to the filtrate tank, and the negative pressure pipeline is a flexible pipeline or a movable sleeve; the liquid drainage device comprises a liquid drainage pipeline connected with the filtrate tank, and the liquid drainage pipeline is a flexible pipeline or a movable sleeve.
11. The pretreatment system for total organic carbon testing of claim 1, further comprising an placeholder container for filling with the sample grade that is empty.
CN201911402465.9A 2019-12-30 2019-12-30 Pretreatment system for total organic carbon test Pending CN110987570A (en)

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