CN109883788A - A oxidation unit for shale organic carbon survey - Google Patents
A oxidation unit for shale organic carbon survey Download PDFInfo
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- CN109883788A CN109883788A CN201910219243.7A CN201910219243A CN109883788A CN 109883788 A CN109883788 A CN 109883788A CN 201910219243 A CN201910219243 A CN 201910219243A CN 109883788 A CN109883788 A CN 109883788A
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Abstract
The invention discloses an oxidation device for determining organic carbon in shale, which comprises a closed reaction kettle and a stirring mechanism arranged in the reaction kettle, wherein an openable feeding door and an air vent for introducing oxygen are arranged on the reaction kettle in a closed manner; the stirring mechanism comprises a stirring shaft which is rotatably vertically arranged in the reaction kettle, a first magnet is installed at the upper end of the stirring shaft, the first magnet is formed by radially extending the stirring shaft and is a strip-shaped magnetic strip part, a support is further arranged at the top of the reaction kettle, a motor which is vertically downwards arranged is installed on the support, an output shaft of the motor is coaxially arranged with the stirring shaft, a second magnet is fixedly installed below the output shaft of the motor, and the second magnet is the same as the projection of the first magnet on the vertical direction and is located in the magnetic field range of the first magnet. The invention can stir the sample, increase the contact area of the sample and oxygen, and ensure the sufficient oxidation of the sample, thereby improving the precision of the detection result.
Description
Technical field
The present invention relates to rock physics research fields, and in particular to a kind of oxidation unit for shale organic carbon determination.
Background technique
With the high speed development of global economy, shows energy supply and demand problem day and protrude, the continuous growth of petroleum resources demand, page
Rock gas succeeds exploitation in north America region as a kind of unconventional petroleum resources having a high potential, becomes global Oil Gas
The frontier of exploration and development, and have wide development prospect, cause the attention of countries in the world rapidly.Currently, east China
The ground such as Eastern Sag in Liaohe Depression, western Sichuan and the Erdos basin Liang Ge become the key area of shale gas exploration and development.
Total organic carbon (TOC) content is the material base of shale anger in shale, determines the angry ability of shale, is that evaluation shale is organic
The important parameter of matter abundance and Gas-generating Potentiality.Total content of organic carbon is higher, and the ability of shale adsorbed gas is stronger, contains in organic matter
There is a large amount of micropore, it has stronger adsorption capacity, while dissolution of the hydrocarbon gas in bituminite to gas
Increase suction-operated of the shale to gas.Total content of organic carbon and shale have positive correlation to the adsorption capacity of natural gas in shale
System, therefore rapid and accurate determination shale organic Geochemical Characteristics parameter organic carbon content, Reserves Assessment and production to shale gas
Gas merit rating, and then study lithological composition, origin cause of formation source, occurrence form, accumulation feature, the accumulating condition, page of shale gas reservoir
Rock air content etc. is of great significance.
Currently, organic carbon content measurement mainly uses potassium dichromate oxidation and calcination method, wherein potassium dichromate oxidation
It is that redox reaction occurs with the organic carbon of the strong potassium bichromate sulfuric acid solution of oxidisability and sample to be tested, exists between them
Quantitative relationship, then remaining potassium bichromate is titrated with standard restoration agent (ferrous sulfate), the content of organic carbon can be obtained, but should
Method is complicated for operation, time-consuming, measurement result poor reproducibility, and pollutes larger；Calcination method be oxygen abundance in the case where,
Using carbon and sulphur detector or carbon determinator etc., by the total organic carbon in sample, oxygenolysis is carbon dioxide under the high temperature conditions,
And its content is measured, the content of organic carbon is finally calculated, but this method is incomplete to the oxidation of organic matter, it is especially to be measured
When object content is more, error is larger, causes testing result inaccurate.
Summary of the invention
In view of the above shortcomings of the prior art, the purpose of the present invention is to provide one kind to stir sample
It mixes, increases the contact area of sample and oxygen, guarantee that sample is fully oxidized, to improve the shale organic carbon of testing result precision
The oxidation unit of measurement.
In order to solve the above-mentioned technical problem, the present invention adopts the following technical scheme: it is a kind of for shale organic carbon determination
Oxidation unit, it is closed on the reaction kettle to be provided with including closed reaction kettle and the rabbling mechanism being arranged in reaction kettle
Openable feeding gate and blow vent for being passed through oxygen；The rabbling mechanism is described anti-including being rotationally vertically provided at
The agitating shaft in kettle is answered, the upper end of the agitating shaft is equipped with the first magnet, the first magnet radially extending along agitating shaft
The magnetic stripe portion in a strip shape formed, the radially mounted paddle having for stirring test sample on the agitating shaft；It is described anti-
It answers and is additionally provided with bracket at the top of kettle, vertically down-set motor, the output shaft of the motor are installed on the bracket
It is coaxially disposed with the agitating shaft, is fixedly installed with the second magnet, second magnet and institute below the output shaft of the motor
It is identical to state the projection of the first magnet vertically, and first magnet is in the magnetic field range of the second magnet.In this way, when second
Electromagnet rotates under motor control, and then changes its magnetic direction, and then the first magnet is under the magnetic fields of the second magnet
It rotates, and drives agitating shaft and paddle to rotate simultaneously, therefore the stirring action to sample to be tested may be implemented.And lead to
Crossing magnetic fields realizes driving motor and the untouchable setting of pyroreaction kettle, avoids in reaction kettle hot environment to motor
It influences and damages.
Preferably, first magnet and the second magnet it is close to each other one end polarity it is opposite.In this way, increasing the second magnetic
Interaction force between iron and the first magnet.
Preferably, paddle is to be evenly distributed the fan leaf being arranged on the agitating shaft；The paddle is located at
The lower end of the agitating shaft, and the paddle is in contact with the bottom surface of the reaction kettle, in this way, increasing mixing area and
Evenness increases the contact area of sample to be tested and oxygen, keeps its oxidation more abundant.
Preferably, the magnetic stripe portion be uniformly arranged along the circumferential direction of first magnet it is multiple.In this way, can be by setting
The magnetic stripe portion quantity on the second magnet and the first magnet is set, to regulate and control amount of force between the two, therefore can be
In the identical situation of electrode power, master regulation mixing speed is come from according to the amount of sample to be tested.
Preferably, being provided with check valve at the blow vent.In this way, avoiding the sample to be tested in reaction kettle with air-flow band
Out outside reaction kettle.
Compared with prior art, the invention has the following beneficial effects:
1, the oxidation unit tested provided by the present invention for shale organic carbon, including reaction kettle, rabbling mechanism and motor,
The contact area and response area for greatly increasing sample to be tested and oxygen, improve reaction efficiency, shorten the reaction time,
Keep organic oxidation of coal more complete.Compared with the carbon and sulfur analytical instrument in primary standard measures shale organic carbon, standard GB/ is eliminated
Filtration washing step as defined in T19145-2003 reduces the labor intensity of staff, improves testing efficiency；Also save
Addition fluxing agent step cleans combustion tube step, has opened up the new direction of shale organic carbon detection technique.With existing mechanism phase
Than, which passes through the interaction of the first magnet and the second magnet, the rotation of paddle in pyroreaction kettle is realized,
This is simple in sturcture, ingenious in design, easy to operate, and the present invention is according to " 3 times of principles of method whole process zero standard deviation " detection limit
Up to 0.162%, preci-sion and accuracy is all satisfied the limit value requirement of preci-sion and accuracy in standard GB/T19145-2003.This
Invention improves accuracy, reliability and the detection efficiency of institute's sample organic carbon content, so to the Reserves Assessment of shale gas and
Correct analysis is made in gas deliverability evaluation.
2, provided by the present invention for the oxidation unit of shale organic carbon test, equipment is simple, at low cost, easy to control, can
Mixing speed can be regulated and controled, in conjunction with ventilating mode, greatly by the quantity for adjusting output power of motor size and/or magnetic stripe portion
The big contact area and response area for increasing sample to be tested and oxygen, improves reaction efficiency, shortens the reaction time, because
This present invention can realize the complete oxidation of organic carbon in the short time at a lower temperature, reduce energy consumption, and by that will react
The setting of kettle and driving mechanism non-direct contact avoids influence and damage of the high-temp combustion to driving device, extends the equipment
Service life.The new direction of shale organic carbon detection technique has been opened up, there is good application prospect.
Detailed description of the invention
Fig. 1 is the structural schematic diagram that oxidation unit is tested for shale organic carbon；
Fig. 2 is the structural schematic diagram of the first magnet (the second magnet)；
Fig. 3 is CO2Response and temperature of reaction kettle variation relation figure.
Specific embodiment
Present invention will be further explained below with reference to the attached drawings and examples.
One, a kind of oxidation unit for shale organic carbon determination
Referring to Fig. 1 and Fig. 2, including closed reaction kettle 1 and the rabbling mechanism 2 being arranged in reaction kettle, the reaction
It is closed on kettle 1 to be provided with openable feeding gate and the blow vent for being passed through oxygen；The rabbling mechanism includes rotationally
The agitating shaft 3 being vertically provided in the reaction kettle, the upper end of the agitating shaft 3 are equipped with the first magnet 4, first magnet
It is radially mounted on the agitating shaft to have for stirring detection along the magnetic stripe portion 5 in a strip shape to be formed that radially extends of agitating shaft
The paddle 6 of sample；It is additionally provided with bracket 7 at the top of the reaction kettle, is equipped on the bracket vertically down-set
Motor 8, the output shaft of the motor and the agitating shaft are coaxially disposed, and are fixedly installed with second below the output shaft of the motor
Magnet 9, second magnet 9 is identical as the projection of first magnet 4 vertically, and first magnet is in the second magnet
Magnetic field range in.
Two, a kind of shale organic carbon determination method, comprising the following steps:
1) pre-treatment of sample: it is 80~200 mesh that shale to be measured, which is ground to granularity, is placed in the porcelain boat of pre-burn
In, excessive hydrochloric acid solution is added, there is no until bubble wait react；Porcelain boat is placed in 100~120 DEG C of heating plates be evaporated it is molten
Liquid；
2) oxidation processes are carried out by above-mentioned oxidation unit: are heated at high temperature the reaction kettle, and are continually fed into oxygen to it,
To Tail gas measuring less than carbon dioxide until, then will treated that sample is placed in the reaction kettle；
3) start motor, agitating shaft rotates under magnet effect, and paddle is driven to stir sample to be tested；
4) after reaction, the carbon dioxide generated in step 2) reaction kettle is discharged, repeats step 2) until reaction
It is discharged in kettle without carbon dioxide, then detects the amount of total CO 2, the content of total organic carbon in shale can be obtained.
When implementation, first magnet and the second magnet it is close to each other one end polarity it is opposite.In this way, increasing the second magnet
With the interaction force between the first magnet.
When implementation, the paddle is to be evenly distributed the fan leaf being arranged on the agitating shaft；The paddle position
In the lower end of the agitating shaft, and the paddle is in contact with the bottom surface of the reaction kettle, in this way, increase mixing area and
The uniformity increases the contact area of sample to be tested and oxygen, keeps its oxidation more abundant.
When implementation, the magnetic stripe portion has been uniformly arranged multiple along the circumferential direction of first magnet.In this way, setting can be passed through
Magnetic stripe portion quantity on second magnet and the first magnet, to regulate and control amount of force between the two, therefore can be in electricity
In the identical situation of pole power, master regulation mixing speed is come from according to the amount of sample to be tested.
When implementation, check valve is provided at the blow vent.In this way, the sample to be tested in reaction kettle is avoided to take out of with air-flow
Outside reaction kettle.
Three, the condition optimizing of shale organic carbon test macro
1, the determination of ignition temperature
Accurately weigh 105 DEG C~110 DEG C dry 2h to constant weight GBW07430 (GSS-16, carbon content are 1.0 ± 0.15%)
90mg, according to operating process, at being 600 DEG C, 700 DEG C, 800 DEG C, 850 DEG C, 900 DEG C, 1000 DEG C in temperature of reaction kettle respectively into
Sample measures CO2Response.
According to CO2Response is with temperature of reaction kettle variation relation figure and measurement result table 1 and Fig. 3 it is found that sample is at 600 DEG C
It burns at~1000 DEG C, CO2Peak height increase with the raising of temperature, the time used is being reduced with the raising of temperature；700 DEG C and
CO after 600 DEG C of burnings2Peak area be respectively after completely burned 92.5%, 95.1%, i.e., at low ambient temperatures, organic carbon
Efficiency is also very high.When reaction temperature is greater than 800 DEG C, the oxidation efficiency of organic carbon is greater than 98% or more.
1 temperature of reaction kettle experiment status data of table summarizes
2, the determination of oxygen ventilation amount
Experimental program: 105 DEG C~110 DEG C dry 2h to constant weight GBW07430 (GSS-16, carbon contents 1.0 are accurately weighed
± 0.15%) 90mg, according to operating process, it is 800 DEG C that temperature of reaction kettle, which is arranged, changes oxygen ventilation amount, respectively in 150m L/
min；200m L/min；3 measurements, shadow of the observation oxygen ventilation amount size to measurement result are carried out under 250m L/min flow
It rings.
2 oxygen ventilation amount of table influences experimental data situation
From measurement result table 2, it can be concluded that, oxygen ventilation amount has a certain impact to organic Carbon analysis, and ventilatory capacity exists
Measured value under 150mL/min flow is 0.661%, is lower than standard substance Determination Limit 0.85%, flow 200mL/min,
Measured value under 250m L/min is respectively 0.922% and 0.881%, in the uncertain value model of standard value 0.85%-1.15%
In enclosing.Therefore, oxygen ventilation amount is set in 200mL/min~250mL/min range.
3, the pre-treating method of sample
In the practical application of measurement organic carbon, the inorganic carbonate in sample is generally removed using hydrochloric acid.This be because
There is no oxidisability for hydrochloric acid, inorganic carbonate can be removed, while preferably retaining organic matter component again.The selection of acid concentration:
First: to avoid concentration conversion, facilitating experimental implementation, the expression of acid concentration uses volume ratio；Second: because residual is in the sample
Hydrochloric acid, HCL is converted into after heating further to be removed with copper wire, and concentration is bigger, and cost is higher；Third: residual is in the sample
Hydrochloric acid can to reaction kettle generate corrosion failure.Therefore the present invention from concentration of hydrochloric acid be VHydrochloric acid:VWater=1:7 (reference standard GB/T
It 19145-2003) is verified, if experimental study is met the requirements, concentration of hydrochloric acid is not further added by.
Experimental program:
Non-quantitative weighs standard substance 100mg or so, is placed in the porcelain boat of pre-burn, and it is molten that excessive hydrochloric acid is added
Liquid (VHydrochloric acid:VWater=1:7), to (there is no bubbles) after the reaction was completed, it is placed in 105 DEG C of heating plates and is evaporated.
3 pre-treatment experimental data situation of table
By the test data table 3 of soil and stream sediment as can be seen that using concentration of hydrochloric acid VHydrochloric acid:VWater=1:7 is carried out
In 7 standard substance samples of pre-treatment, the requirement that result substantially meets standard value uncertainty is measured.Therefore sample removes nothing
It is V that machine carbon, which can choose concentration of hydrochloric acid,Hydrochloric acid:VWater=1:7.
4, the selection of sample granularity
Granule size will affect the removal degree of inorganic carbon, and then influence the test accuracy of organic matter.In national standard GB/
, it is specified that the sample granularity for measuring organic carbon is no more than 80 mesh (partial sizes in the measurement of T19145-2003 sedimentary rock total organic carbon
0.2mm), to chemistry and spectral analysis sample, most common granularity is the grain after 160 mesh or the processing of 200 mesh Geological Standard Materials
Degree is general to be required to reach -200 mesh (ratio is greater than 95%).Accordingly, following experimental program is selected.
Experimental program: 2 samples of selection are prepared into two kinds of granularities of 80 mesh and 200 mesh respectively, are tested with laser particle size analyzer
The volume distribution situation of two kinds of granularities is demonstrate,proved, while under other experiment conditions and the identical situation of step, sample is carried out organic
Carbon measurement.
4 sample granularity of table analyzes situation
Find out from 4 result of organic carbon test table of two kinds of granularities of 80 mesh and 200 mesh, two kinds of granularity organic carbon test results
Deviation (requires≤0.24 according to the repeatability of standard) within the scope of the quality requirement of standard GB/T19145-2003.Therefore, root
Data-speculative is factually tested, 200 mesh of sample granularity of organic carbon can satisfy the requirement of test completely.
Four, efficiency evaluation is carried out to the detection method of foundation
For the effective implementations for further verifying detection method, respectively to the characteristic index method detection limit of method, precision
4 degree, accuracy and measurement range elements are verified.
1, detection limit is evaluated
Method detection limit is the important indicator of chemical analysis.According to the detection limit of method by whole process reagent blank and instrument
The control of device sensitivity determines that method uses in blank assay and detects object: according to the Overall Steps of sample analysis, repeating
Each measurement result is scaled concentration or content in sample, calculates the standard deviation of parallel determination, press by n >=7 time blank test
Formula (3.20) calculation method detection limit.
MDL=t(n-1,0.99)×S (3.20)
In formula: MDL --- method detection limit；
The parallel determination number of n --- sample；
T --- freedom degree n-1, t when confidence level is 99% are distributed (unilateral side)；
The standard deviation that S --- n times are measured in parallel.
Wherein, the t value when freedom degree is n-1, and confidence level is 99% can refer to table 3-6 value.
Method detection limit confirmatory experiment: weigh 0.0100g GSD2a standard substance (standard value: 0.26 ± 0.02%, content
It is lower to be considered as blank), carry out independent measurement 8 times according to testing process, table look-up t value is 2.998.The revision of the convention is 3.Usually said
According to method whole process zero standard 3 times of principles of deviation, the method detection for calculating solid sample is limited to 0.162%, as a result sees
Table 5.
5 analysis method detection limit verification result of table
2, precision is evaluated
Precision refers under prescribed conditions, the consistent degree between independent test result.To the sample of certain level concentration
N times parallel determination is carried out in i-th laboratory, relative standard deviation is calculated as follows in laboratory:
In formula: xkThe kth time measurement result that a certain concentration level sample is carried out in --- -- i-th of laboratory；
To the average value of a certain concentration level sample test in --- -- i-th of laboratory；
SiTo the standard deviation of a certain concentration level sample test in --- --- i-th of laboratory；
RSDiTo the relative standard deviation of a certain concentration level sample test in --- -- i-th of laboratory.
Precision confirmatory experiment: the standard substance of the high, medium and low 3 different contents level of selection, it is each according to testing process
Sample carries out independent measurement 3 times, calculates the absolute difference of average value and unitary determination result and mean value.The verifying of method precision
Result data is as shown in table 6 below.
Interpretation of result: from the data and allowable value of the absolute deviation of high, medium and low 3 different contents level standard substance
It is found that method precision meets the requirement in standard GB/T19145-2003, data are shown, method precision is in different contents
It is worth level requirement difference, the maximum deflection difference value of each content section test far smaller than allows difference, and deviation is permission difference
1/2 to 1/3 between.Such as deviation 0.02 and allowed limit 0.07；Deviation 0.05 and allow limit 0.13；Deviation 0.08 and permit
Perhaps 0.24 is limited.
The verification result of 6 method precision of table
3, accuracy estimating
The standard substance for choosing GBW07423, GBW07428, GBW07309, GBW07360 totally 4 kinds of different content levels, is pressed
It is independently measured 4 times according to each sample of testing process, specific test data is as shown in table 7 below.
It is good to can be seen that the case where method accuracy validation is carried out using standard substance from the test data in table 3-9.
The absolute deviation of the measured value of 4 selected different content ladder standards matter is in the uncertain region of standard value.Far
Far meet the reproducibility R requirement that GB/T19145-2003 is measured using carbon and sulfur analytical instrument.
7 method accuracy validation result data of table
Using standard GB/T 19145-2003 as principle, respectively to foundation in terms of detection limit, preci-sion and accuracy three
Method evaluated.The result shows that: this method is according to " 3 times of principles of method whole process zero standard deviation " calculation method
Detection is limited to 0.162%.Preci-sion and accuracy is all satisfied precision and accurate limit value in standard GB/T19145-2003 and wants
It asks.
Finally, it should be noted that technical side the above examples are only used to illustrate the technical scheme of the present invention and are not limiting
Case, those skilled in the art should understand that, modification or equivalent replacement of the technical solution of the present invention are made for those, and
The objective and range for not departing from the technical program, are intended to be within the scope of the claims of the invention.
Claims (6)
1. a kind of oxidation unit for shale organic carbon determination, which is characterized in that including closed reaction kettle (1) and setting
Rabbling mechanism (2) in reaction kettle, it is closed on the reaction kettle (1) to be provided with openable feeding gate and for being passed through oxygen
Blow vent；The rabbling mechanism includes the agitating shaft (3) being rotationally vertically provided in the reaction kettle, the agitating shaft
(3) upper end is equipped with the first magnet (4), and first magnet radially extends the magnetic stripe portion in a strip shape to be formed along agitating shaft
(5), the radially mounted paddle (6) having for stirring test sample on the agitating shaft；The top of the reaction kettle is also set
It is equipped with bracket (7), vertically down-set motor (8) is installed on the bracket, the output shaft of the motor is stirred with described
Mix axis coaxial arrangement, be fixedly installed with the second magnet (9) below the output shaft of the motor, second magnet (9) with it is described
The projection of first magnet (4) vertically is identical, and first magnet is in the magnetic field range of the second magnet.
2. being used for the oxidation unit of shale organic carbon determination according to claim 1, which is characterized in that first magnet
(4) and the second magnet (9) it is close to each other one end polarity it is opposite.
3. being used for the oxidation unit of shale organic carbon determination according to claim 1, which is characterized in that the paddle (6)
To be evenly distributed the fan leaf being arranged on the agitating shaft (3).
4. being used for the oxidation unit of shale organic carbon determination according to claim 1, which is characterized in that the stirring parts (6)
Positioned at the lower end of the agitating shaft (3), and the paddle is in contact with the bottom surface of the reaction kettle.
5. being used for the oxidation unit of shale organic carbon determination according to claim 1, which is characterized in that the magnetic stripe portion (5)
It has been uniformly arranged along the circumferential direction of first magnet (4) multiple.
6. being used for the oxidation unit of shale organic carbon determination according to claim 1, which is characterized in that set at the blow vent
It is equipped with check valve.
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Cited By (1)
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| CN114734367A (en) * | 2022-04-22 | 2022-07-12 | 盐城苏高汽睿科技有限公司 | Intelligent automobile muffler production welding system |
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