CN111856048A - Altered carbonate automatic analysis device and analysis method - Google Patents
Altered carbonate automatic analysis device and analysis method Download PDFInfo
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- CN111856048A CN111856048A CN201910364521.8A CN201910364521A CN111856048A CN 111856048 A CN111856048 A CN 111856048A CN 201910364521 A CN201910364521 A CN 201910364521A CN 111856048 A CN111856048 A CN 111856048A
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- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 title claims abstract description 64
- 238000004458 analytical method Methods 0.000 title claims abstract description 44
- 238000010438 heat treatment Methods 0.000 claims abstract description 76
- 239000012159 carrier gas Substances 0.000 claims abstract description 28
- 239000007789 gas Substances 0.000 claims abstract description 25
- 238000001514 detection method Methods 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 13
- 238000000354 decomposition reaction Methods 0.000 claims description 9
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 4
- 239000001301 oxygen Substances 0.000 claims description 4
- 229910052760 oxygen Inorganic materials 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims 1
- 238000002347 injection Methods 0.000 claims 1
- 239000007924 injection Substances 0.000 claims 1
- 239000010453 quartz Substances 0.000 claims 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 1
- 239000003208 petroleum Substances 0.000 abstract description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 8
- 238000005259 measurement Methods 0.000 description 7
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 3
- 239000004215 Carbon black (E152) Substances 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 230000004075 alteration Effects 0.000 description 2
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 229930195733 hydrocarbon Natural products 0.000 description 2
- 150000002430 hydrocarbons Chemical class 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- 238000004448 titration Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 125000005587 carbonate group Chemical group 0.000 description 1
- 238000004587 chromatography analysis Methods 0.000 description 1
- 230000002860 competitive effect Effects 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000013508 migration Methods 0.000 description 1
- 230000005012 migration Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000012284 sample analysis method Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000011410 subtraction method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N35/10—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices
- G01N35/1081—Devices for transferring samples or any liquids to, in, or from, the analysis apparatus, e.g. suction devices, injection devices characterised by the means for relatively moving the transfer device and the containers in an horizontal plane
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N35/00—Automatic analysis not limited to methods or materials provided for in any single one of groups G01N1/00 - G01N33/00; Handling materials therefor
- G01N2035/00346—Heating or cooling arrangements
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
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Abstract
The invention belongs to the field of petroleum geology, and particularly relates to an altered carbonate automatic analysis device and an analysis method, wherein the altered carbonate automatic analysis device comprises the following components: the automatic sample feeding heating device comprises one or more automatic sample feeding heating units connected in parallel; each automatic sample introduction heating unit comprises an automatic sample introduction subunit and a heating subunit, the automatic sample introduction subunit comprises a cylinder, a cylinder electromagnetic valve and a cylinder air inlet system, the heating subunit comprises a sample frame, a heating part, a carrier gas electromagnetic valve and a carrier gas system, the cylinder is connected with the sample frame, and the heating part is provided with a sample frame inlet and outlet channel; CO 22The infrared gas analyzer is connected with the heating subunit of the automatic sample feeding heating unit; the control system is used for automatically controlling the automatic altered carbonate analysis device; a constant-temperature box is arranged in the constant-temperature box,is arranged outside the heating subunit. The invention has the advantages of simple operation, convenient use, small analysis error and high working efficiency.
Description
Technical Field
The invention belongs to the field of petroleum geology, and particularly relates to an automatic analysis device and an automatic analysis method for altered carbonate.
Background
Low molecular hydrocarbon gas from oil and gas reservoir reacts with oxygen to generate CO in the process of vertical migration to the earth surface2And H2O，CO2Continue to penetrate to the surface and react with some salt radicals H in the formation2The secondary carbonate is called altered carbonate, also called delta C, and is formed in cracks or crystal lattices of the silicate in a cementing state, and the decomposition temperature is 500-600 ℃. In oil and gas chemical exploration, the characteristic of altered carbonate (Delta C) is often utilized to carry out geochemical exploration, in particular to decompose and release CO at the temperature of 500-600 ℃ by the altered carbonate (Delta C)2The content is used for determining the amount of altered carbonate, and the index is used for delineating the abnormal chemical exploration and deducing a hydrocarbon gas substance source deep in the stratum.
In long-term oil and gas exploration practice, the research on the altered carbonate indexes is also great, and CN101226180A provides a modified carbonate standard substance for conveniently comparing the altered carbonate measurement results in oil and gas exploration in different areas, accurately calibrating a measurement instrument, monitoring the measurement results and providing a basis for standardizing the admission conditions and the competitive conditions of the oil and gas exploration object market. CN202837262U provides a split type for alteration carbonate analysis schizolysis bottle to the defect of the split type for alteration carbonate analysis schizolysis bottle that uses now, and this schizolysis bottle has overcome split type schizolysis bottle ground part sealing difficulty through the shape that changes the bottle lid and its connected mode with the body, and the gas that the schizolysis produced leaks easily, causes sample schizolysis link once the qualification rate is low, outstanding problems such as complex operation. CN206862878U is a novel six-channel altered carbonate analyzer which can improve the testing efficiency, utilize the carbon dioxide infrared detector to measure and get rid of the influence of human and environmental factors caused by the titration method. Meanwhile, a plurality of researches are carried out on the detection method of altered carbonate, and the existing detection methods comprise a chromatography method, a nonaqueous volume method, a subtraction method, an infrared method, a nonaqueous titration method, a carbon isotope ratio method and the like, but the detection methods are all manual detection, only one group of samples can be measured at one time, and because the accuracy and the stability of the detection are greatly influenced by human factors, some unpredictable deviations are easy to appear in the detection result, and when the analysis amount is large, the manual detection also influences the research progress to a great extent because the detection efficiency is low.
Disclosure of Invention
In order to solve the problems, the invention provides an automatic analysis device and an automatic analysis method for altered carbonate, which are simple to operate, convenient to use, small in analysis error and high in working efficiency.
An aspect of the present invention provides an apparatus for automatically analyzing altered carbonate, including:
the automatic sample feeding heating device comprises one or more automatic sample feeding heating units connected in parallel; each automatic sample feeding heating unit comprises an automatic sample feeding subunit and a heating subunit,
the automatic sample introduction subunit comprises a cylinder, a cylinder electromagnetic valve and a cylinder air inlet system,
the heating subunit comprises a sample rack, a heating part, a carrier gas electromagnetic valve and a carrier gas system, the air cylinder is connected with the sample rack, and the heating part is provided with a sample rack inlet and outlet channel;
CO2the infrared gas analyzer is connected with the heating subunit of the automatic sample feeding heating unit;
the control system is used for automatically controlling the automatic altered carbonate analysis device;
and the constant temperature box is arranged outside the heating subunit.
According to the invention, preferably, an inlet carrier gas solenoid valve and an outlet carrier gas solenoid valve are respectively arranged at two ends of the heating part, and the carrier gas system is connected with the inlet carrier gas solenoid valve.
In the invention, a sample boat can be arranged on the sample rack, and the air cylinder drives the sample boat on the sample rack to enter and exit the heating part, so as to realize heating and recovery of the altered carbonate sample.
In the present invention, in order to ensure the normal operation of the cylinder, preferably, the cylinder air intake system is connected with an air compressor. In order to ensure the purity of the incoming gas in the carrier gas system, in the present invention, it is preferable that the carrier gas system is further provided with a purifier.
Another aspect of the present invention provides an automatic altered carbonate analysis method performed in the automatic altered carbonate analysis apparatus, the automatic altered carbonate analysis method including:
setting the sample decomposition temperature, the sample introduction interval time, the sample collection time and the sample detection time on a control system, introducing replacement gas into the heating part to completely discharge air in the heating part, and then sequentially placing the pretreated altered carbonate samples into each sample holder;
after the heating part is preheated to the decomposition temperature of the sample, the cylinder in the first automatic sample introduction heating device pushes the sample holder to enter the heating part, and the altered carbonate sample is heated in the heating part to decompose and release CO 2When the set sample collection time is reached, the carrier gas electromagnetic valve is opened, and the replacement gas pushes to release CO2Into CO2The infrared gas analyzer analyzes the sample, and when the set sample detection time is reached, the carrier gas electromagnetic valve is closed;
the sample holders in the other automatic sample feeding heating devices are sequentially pushed into the heating part according to the set sample feeding interval time, and the process of the first automatic sample feeding heating device is sequentially repeated until all samples are completely analyzed;
wherein the replacement gas is a carbon dioxide-free gas.
Before the automatic analysis of altered carbonate, the sample of altered carbonate is generally pretreated, and in the present invention, the pretreatment step preferably comprises: the altered carbonate samples were heated to 490-510 ℃ and then oxidized under oxygen for 50-70 min.
According to the present invention, it is preferred that the altered carbonate sample has a decomposition temperature of 590-610 ℃.
In order to ensure that the analysis of each altered carbonate sample is orderly carried out, the sample rack in the next group of automatic sample feeding heating devices needs to wait for the sample rack to enter the heating part after the analysis of the previous group of altered carbonate samples is finished. When a group of samples are analyzed, preferably, the method for automatically analyzing the altered carbonate further comprises recovering the altered carbonate sample, specifically, pulling the sample holder by the air cylinder to pull the altered carbonate sample out of the heating part, and manually recovering the altered carbonate sample when the temperature of the sample is reduced to the normal temperature.
The invention adopts automatic sample introduction, automatic analysis and automatic sample discharge to keep the heat release time of the sample consistent, and solves the problems of low efficiency and large error in manual measurement. Meanwhile, by arranging a plurality of groups of automatic sample introduction heating units connected in parallel, automatic analysis of a plurality of groups of altered carbonates is realized, the defect that only one sample can be manually tested each time in the existing analysis and measurement technology is overcome, and the working efficiency is improved on the premise of ensuring the analysis quality.
Additional features and advantages of the invention will be set forth in the detailed description which follows.
Drawings
The above and other objects, features and advantages of the present invention will become more apparent by describing in more detail exemplary embodiments thereof with reference to the attached drawings, in which like reference numerals generally represent like parts throughout.
Fig. 1 shows a schematic diagram of an automatic sample feeding heating device according to an embodiment of the present invention.
Fig. 2 shows a schematic diagram of an apparatus for automatically analyzing altered carbonate according to an embodiment of the present invention.
Description of reference numerals:
1. a cylinder; 2. a sample holder; 3. a heating member; 4. a carrier gas solenoid valve; 5. an air cylinder electromagnetic valve; 6. a pressure reducing valve; 7. a thermostat; 8. a cylinder air intake system; 9. a carrier gas system; 10. CO 2 2A detector.
Detailed Description
Preferred embodiments of the present invention will be described in more detail below. While the following describes preferred embodiments of the present invention, it should be understood that the present invention may be embodied in various forms and should not be limited by the embodiments set forth herein.
Examples
The automatic altered carbonate analysis device shown in figure 2 is adopted to carry out automatic altered carbonate analysis, the automatic altered carbonate analysis device comprises 16 automatic sample introduction heating units which are connected in parallel, each automatic sample introduction heating unit is shown in figure 1 and comprises an automatic sample introduction subunit and a heating subunit, the automatic sample introduction subunit comprises an air cylinder 1, an air cylinder electromagnetic valve 5 and an air cylinder air inlet system 8, and the heating subunit and CO are connected with each other2The infrared gas analyzer is connected with the infrared gas analyzer and comprises a sample rack 2, a heating part 3, a carrier gas electromagnetic valve 4 and a carrier gas system 9, wherein the cylinder 1 is connected with the sample rack 2, the heating part 3 is provided with an inlet and outlet channel of the sample rack 2, the two ends of the heating part are respectively provided with the carrier gas electromagnetic valve 4, and the outside of the heating part is provided with a heat preservation box.
The automatic altered carbonate analysis device is also provided with a control system for automatic control of the automatic altered carbonate analysis device.
Altered carbonate sample analysis method:
The altered carbonate samples were tested in the above-described apparatus for 16 replicates.
Pretreatment: the altered carbonate samples were heated to 490-510 ℃ and then oxidized under oxygen for 50-70 min.
After the pretreatment is finished, setting the sample decomposition temperature of 600 ℃, the sample introduction interval time, the sample collection time and the sample detection time on a control system, introducing nitrogen into the heating part to completely discharge air in the heating part, and then sequentially placing the pretreated altered carbonate samples into each sample rack;
after the heating part is preheated to the decomposition temperature of the sample, the cylinder in the first automatic sample introduction heating device pushes the sample holder to enter the heating part, and the altered carbonate sample is heated in the heating part to decompose and release CO2When the set sample collection time is reached, the carrier gas electromagnetic valve is opened, and the nitrogen pushes to release CO2Into CO2And (3) analyzing by an infrared gas analyzer, closing the carrier gas electromagnetic valve when the set sample detection time is reached, pulling the sample frame 2 by the air cylinder 1, pulling the altered carbonate sample out of the heating part 3, and manually recovering the sample when the sample is cooled to normal temperature.
The sample holders in the rest automatic sample feeding heating devices are sequentially pushed into the heating part according to the set sample feeding interval time, and the process of the first automatic sample feeding heating device is sequentially repeated until all samples are completely analyzed, and the detection results are shown in the following table 1:
TABLE 1
| Serial number | Peak number | Retention time (min) | Peak height (mv) | Peak area (mv. s)-1) | Content (10)-2) |
| 1 | 1 | 1.065 | 6090.892 | 168058.406 | 3.2530 |
| 2 | 2 | 3.440 | 6166.949 | 172616.297 | 3.3412 |
| 3 | 3 | 5.965 | 6415.639 | 175249.094 | 3.3921 |
| 4 | 5 | 8.798 | 6961.170 | 188839.031 | 3.6552 |
| 5 | 7 | 10.165 | 6378.726 | 178900.063 | 3.4628 |
| 6 | 9 | 14.932 | 6580.640 | 190192.656 | 3.6814 |
| 7 | 10 | 17.898 | 6539.281 | 195114.828 | 3.7767 |
| 8 | 11 | 20.665 | 5521.574 | 151129.719 | 2.9253 |
| 9 | 13 | 23.932 | 5859.930 | 154228.109 | 2.9853 |
| 10 | 15 | 25.332 | 5950.127 | 161804.109 | 3.1319 |
| 11 | 16 | 30.332 | 5493.843 | 163060.844 | 3.1562 |
| 12 | 17 | 31.865 | 5572.888 | 164582.656 | 3.1857 |
| 13 | 18 | 33.332 | 4951.540 | 150498.953 | 2.9131 |
| 14 | 19 | 34.932 | 5949.978 | 178962.594 | 3.4640 |
| 15 | 20 | 36.598 | 5777.809 | 176060.234 | 3.4078 |
| 16 | 21 | 39.998 | 6285.865 | 163664.000 | 3.1679 |
The average value of 16 measurement data is 3.31, the standard deviation is 0.26, the maximum error of the sample content is 0.86 & lt 2, and the method error is met.
The embodiment shows that the automatic analysis device for altered carbonate can realize the automatic analysis of a plurality of groups of altered carbonate samples, the heat release time of the samples is kept consistent, the problems of low efficiency and large error in manual measurement are solved, and the working efficiency is improved.
Having described embodiments of the present invention, the foregoing description is intended to be exemplary, not exhaustive, and not limited to the embodiments disclosed. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments.
Claims (10)
1. An apparatus for automatically analyzing altered carbonate, comprising:
the automatic sample feeding heating device comprises one or more automatic sample feeding heating units connected in parallel; each automatic sample introduction heating unit comprises an automatic sample introduction subunit and a heating subunit, the automatic sample introduction subunit comprises a cylinder, a cylinder electromagnetic valve and a cylinder air inlet system, the heating subunit comprises a sample frame, a heating part, a carrier gas electromagnetic valve and a carrier gas system, the cylinder is connected with the sample frame, and the heating part is provided with a sample frame inlet and outlet channel;
CO2The infrared gas analyzer is connected with the heating subunit of the automatic sample feeding heating unit;
the control system is used for automatically controlling the automatic altered carbonate analysis device;
and the constant temperature box is arranged outside the heating subunit.
2. The altered carbonate automatic analysis device according to claim 1, wherein an inlet carrier gas solenoid valve and an outlet carrier gas solenoid valve are respectively arranged at two ends of the heating component, and the carrier gas system is connected with the inlet carrier gas solenoid valve.
3. The altered carbonate automatic analysis device according to claim 1, wherein a sample boat is further disposed on the sample holder, and the sample boat is made of quartz or ceramic.
4. The altered carbonate automatic analysis device according to claim 1, wherein the carrier gas system is further provided with a purifier.
5. The altered carbonate automatic analysis device of claim 1, wherein the cylinder air intake system is connected to an air compressor.
6. An automatic altered carbonate analysis method performed in the automatic altered carbonate analysis device according to any one of claims 1 to 5, the automatic altered carbonate analysis method comprising:
Setting the sample decomposition temperature, the sample introduction interval time, the sample collection time and the sample detection time on a control system, introducing replacement gas into the heating part to completely discharge air in the heating part, and then sequentially placing the pretreated altered carbonate samples into each sample holder;
after the heating part is preheated to the decomposition temperature of the sample, the cylinder in the first automatic sample introduction heating device pushes the sample holder to enter the heating part, and the altered carbonate sample is heated in the heating part to decompose and release CO2When the set sample collection time is reached, the carrier gas electromagnetic valve is opened, and the replacement gas pushes to release CO2Into CO2The infrared gas analyzer analyzes the sample, and when the set sample detection time is reached, the carrier gas electromagnetic valve is closed;
the sample holders in the other automatic sample feeding heating devices are sequentially pushed into the heating part according to the set sample feeding interval time, and the process of the first automatic sample feeding heating device is sequentially repeated until all samples are completely analyzed;
wherein the replacement gas is a carbon dioxide-free gas.
7. The automated altered carbonate analysis method of claim 6, wherein the step of pre-treating comprises: the altered carbonate samples were heated to 490-510 ℃ and then oxidized under oxygen for 50-70 min.
8. The method of claim 6, wherein the decomposition temperature of the altered carbonate sample is 590-610 ℃.
9. The method of claim 6, wherein the sample injection interval time is greater than the sample detection time.
10. The method of claim 6, further comprising recovering the sample of altered carbonate.
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