CN104897704B - A kind of shale components quantitative analysis method - Google Patents
A kind of shale components quantitative analysis method Download PDFInfo
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- CN104897704B CN104897704B CN201510349157.XA CN201510349157A CN104897704B CN 104897704 B CN104897704 B CN 104897704B CN 201510349157 A CN201510349157 A CN 201510349157A CN 104897704 B CN104897704 B CN 104897704B
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Abstract
The invention discloses a kind of quantitative analysis method of shale components, comprise the following steps:1) it is divided into two parts of A, B after choosing the 50g rock cores drying of shale interval, A part samples are milled to particle diameter and are less than 0.2mm；B parts sample comminution to particle diameter is less than 1mm；2) A sample 0.01g 1.00g are weighed, add excessive hydrochloric acid solution, reaction is complete.Then neutrality is washed to distillation, dried；3) sample made from 2) is subjected to rock organic carbon analysis with carbon and sulfur analytical instrument, determines the percentage composition W of organic matter in shale1；4) B part samples after processing are ground to whole particle diameters less than 40 μm；5) obtained powder sample in 4) is drawn to the percentage composition of various inorganic rock forming minerals；6) inorganic rock phase and organic matter total amount are normalized, then draws the percentage composition of various composition.The invention provides one kind can accurately reflect shale components composition and content, and and can is applied to the shale quantitative analysis method of comprehensive study.
Description
Technical field
The present invention relates to a kind of analysis method of material, and in particular to a kind of shale components quantitative analysis method, belongs to oil
Chemical analysis method in gas exploration and exploitation geology field.
Background technology
In shale Exploration of Oil And Gas and exploitation, the main preservation of petroleum resources is different from conventional oil gas reservoir in shale
Reservoir property.Deepen as the understanding of short source rock is continuous and what global unconventionaloil pool was explored gradually gos deep into, it is understood that shale
Oil-gas geology reserves it is bigger than conventional oil gas reservoir.The research of shale comes into vogue therewith, occupies the difference in geology research special column
Not capacity mostly.
A kind of good component quantifying analysis method should have scientific and practicality, can accurate characterization shale rock into
It is grouped into, and can extensive use.The difficulty that used shale components quantitative analysis method faces has following three points:(1) commonly use
Ordinary sheet identification method, due to the limitation of resolution ratio under microscope mirror, it is impossible to accurately distinguish particle diameter tiny shale and flour sand, nothing
Method realizes accurate quantitative analysis；(2) X- diffraction sample-pretreatment, although the composition relative amount of the energy inorganic rock phase of accurate quantitative analysis,
It is that can not identify organic matter fractions, the quantitative approach is not comprehensive enough；(3) organic carbon analysis method, organic matter fractions can only be provided
Content, it is impossible to mutually carried out qualitative and quantitative analysis to inorganic rock.Therefore, it is reasonable and comprehensive strong suitable to lack a kind of logic at present
Quantitative analysis method for research.
The content of the invention
The defects of purpose of the present invention exists aiming at prior art, there is provided one kind can accurately reflect shale components group
Into and content, and can be applied to comprehensive study shale quantitative analysis method, solve shale components quantitative analysis it is inaccurate, incomplete
The problem of face, for studying the classification of shale, and the formulation of later stage fracturing reform design can be instructed.
The technical scheme is that:
A kind of quantitative analysis method of shale components, comprises the following steps:
1) it is divided into two parts of A, B after choosing the 50g rock cores drying of shale interval, A part samples are milled to particle diameter and are less than 0.2mm,
The sample sieving ground, requires that quality is no less than 10g to strengthen the representativeness of sample；B parts sample comminution to particle diameter is less than
1mm, take 1-2g standby；
2) A sample 0.01g-1.00g are weighed, remaining sample remains repetition measurement, is accurate to 0.0001g, is fitted into container, slowly
Excessive hydrochloric acid solution is added, is placed on water-bath or electric hot plate, temperature control is at 60 DEG C -80 DEG C, molten sample more than 2 hours, extremely
(reacted untill visually observing bubble-free and producing) untill reaction completely, sample must not be spilt during molten sample；Then sample
It is placed in the porcelain crucible on nutsch filter, neutrality is washed to distillation.Finally dried with 60 DEG C -80 DEG C of temperature；
3) sample made from 2) is subjected to rock organic carbon analysis with carbon and sulfur analytical instrument, determines the percentage of organic matter in shale
Content W1；
4) by the B part sample grinders or agate mortar after processing, whole particle diameters are ground to less than 40 μm；
5) obtained powder sample in 4) is used into back pressure method film-making, analysis test is carried out with X- diffractometers, draw quartz,
Feldspar, calcite, pyrite ... wait percentage composition W2, W3, W4, W5 ... the Wn, wherein W2+W3+W4+ of the inorganic rock forming mineral of n kinds
W5+ ...+Wn=100%；
6) inorganic rock phase and organic matter total amount are normalized, then draws the percentage composition of various composition, i.e.,：
W2'=W2 × (1-W1)；
W3'=W3 × (1-W1)；
W4'=W4 × (1-W1)；
W5'=W5 × (1-W1)；
…
Wn'=Wn × (1-W1).
The invention provides one kind can accurately reflect shale components composition and content, and and can is applied to the page of comprehensive study
Rock quantitative analysis method, solves that shale components quantitative analysis is inaccurate, incomplete problem, for studying the classification of shale, and
The formulation of later stage fracturing reform design can be instructed.The quantitative analysis method of the present invention can reflect the inorganic rock of shale
Phase, and can reflection rock in organic matter fractions, suitable for the shale components quantitative analysis method of desk research, and formed shale into
Divide the method and step of quantitative analysis, a kind of side comprehensive, logic is reasonable and workable is provided for shale components quantitative analysis
Method, solve the problems, such as to neglect organic matter fraction, for instructing desk research and fracturing reform to work.
Brief description of the drawings
Fig. 1 is the peak group shale minerals constitutional diagram of JY41-5 wells five in the embodiment of the present invention；
Fig. 2 is the peak group shale components distribution map of JY41-5 wells five in the embodiment of the present invention.
Embodiment
The peak group of In The Southeast of Sichuan Basin Fuling block Ordovician system five is mainly deep shelf environment, develops big set shale, class
Type enriches and part shale gassiness.Below to the shale of the peak group of In The Southeast of Sichuan Basin Fuling block Ordovician system five with carrying out shale
Matter research, shale components quantitative analysis is carried out to the peak group of Fuling block Ordovician system five using the method for the present invention.
A kind of quantitative analysis method of shale components, comprises the following steps:
The first step, by core observation, it is divided into two parts of A, B, A part samples after choosing the 50g rock cores drying of same shale interval
Product are milled to particle diameter and are less than 0.2mm, the sample sieving ground, require that quality is no less than 10g to strengthen the representativeness of sample；
B parts sample comminution to particle diameter is less than 1mm, takes 1-2g standby；The present embodiment samples 10 parts altogether in diverse location, obtains 10 parts and treats point
Analyse sample.
Second step, A sample 0.01g-1.00g being taken, remaining sample remains repetition measurement, is accurate to 0.0001g, is fitted into container,
Be slowly added to excessive hydrochloric acid solution, be placed on water-bath or electric hot plate, temperature control at 60 DEG C -80 DEG C, molten sample 2 hours with
On, (reacted untill visually observing bubble-free and producing) untill reaction is completely.Sample must not be spilt during molten sample.Then
Sample is placed in the porcelain crucible on nutsch filter, and neutrality is washed to distillation.Finally dried with 60 DEG C -80 DEG C of temperature.
Obtained sample is subjected to rock organic carbon analysis with carbon and sulfur analytical instrument, determines the percentage composition of organic matter in shale
(table 1).
The peak group shale organic carbon analysis tables of data of table 1JY41-5 wells five
3rd step, by the B part sample grinders or agate mortar after processing, whole particle diameters are ground to less than 40 μm.Will
Obtained powder sample uses back pressure method film-making, carries out analysis test with X- diffractometers, draws quartz, feldspar, calcite, Huang Tie
Ore deposit ... waits percentage composition W2, W3, W4, W5 ... the Wn, wherein W2+W3+W4+W5+ ...+Wn=100% of the inorganic rock forming mineral of n kinds.
(table 2, accompanying drawing 1)；
The peak group shale X- diffraction total rock analytical datas of table 2JY41-5 wells five
3rd step, total rock ensaying and organic carbon analysis result are handled by data normalization, carry out shale components and determine
Amount analysis (table 3, accompanying drawing 2).
The peak group shale components quantitative analytical data table (normalization) of table 3JY41-5 wells five
The quantitative analysis method of the present invention can reflect the inorganic rock phase of shale, and and can reflects organic matter portion in rock
Point, suitable for the shale components quantitative analysis method of desk research, and the method and step of shale components quantitative analysis is formed, be page
The analysis of rock component quantifying provides a kind of method comprehensive, logic is reasonable and workable, and solution neglects organic matter fraction
Problem, for instructing desk research and fracturing reform to work.
Claims (1)
1. a kind of quantitative analysis method of shale components, it is characterised in that comprise the following steps：
1) it is divided into two parts of A, B after choosing the 50g rock cores drying of shale interval, A part samples are milled to particle diameter and are less than
0.2mm, the sample quality ground are no less than 10g；B parts sample comminution to particle diameter is less than 1mm, takes 1-2g standby；
2) A sample 0.01g-1.00g are weighed, 0.0001g is accurate to, is fitted into container, it is molten to be slowly added to excessive hydrochloric acid
Liquid, it is placed on water-bath or electric hot plate, temperature control is at 60 DEG C -80 DEG C, molten more than sample 2h, and reaction is to visually observing nothing
It is untill reacting completely that bubble, which produces,；Sample must not be spilt during molten sample；Then the porcelain crucible that sample is placed on nutsch filter
In, it is washed to neutrality with distillation；Finally dried with 60 DEG C -80 DEG C of temperature；
3）By 2）Obtained sample carries out rock organic carbon analysis with carbon and sulfur analytical instrument, determines that the percentage of organic matter in shale contains
Measure W1；
4）By the B part sample grinders or agate mortar after processing, whole particle diameters are ground to less than 40 μm；
5）By 4）In obtained powder sample use back pressure method film-making, carry out analysis test with X- diffractometers, draw in shale
The percentage composition W of the inorganic rock forming mineral of n-1 kinds2、W3、W4、W5…Wn, wherein W2+W3+W4+W5+…+Wn=100%；
6) inorganic rock phase and organic matter total amount are normalized, then draws the percentage composition of various composition, i.e.,：
W2’=W2×（1-W1）；
W3’=W3×（1-W1）；
W4’=W4×（1-W1）；
W5’=W5×（1-W1）；
…
Wn’=Wn×（1-W1）.
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| CN105842417A (en) * | 2016-03-17 | 2016-08-10 | 成都创源油气技术开发有限公司 | Method for accurately measuring organic carbon content of shale |
| CN106006655B (en) * | 2016-05-16 | 2019-02-26 | 南华大学 | The method of Ostracode microfossil is extracted from black shale |
| CN106442096B (en) * | 2016-09-26 | 2019-02-19 | 中国石油化工股份有限公司 | The measuring method of total organic carbon in a kind of sedimentary rock |
| CN106841004A (en) * | 2017-01-25 | 2017-06-13 | 中国石油大学(北京) | Shale preserves capacity judging method |
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| CN103344541A (en) * | 2013-07-08 | 2013-10-09 | 中国石油大学(华东) | Method for measuring total porosity of shale |
| CN103411848B (en) * | 2013-07-25 | 2015-05-27 | 中国石油大学(华东) | Method used for evaluating shale gas adsorption capacity of shale |
| CN104020276B (en) * | 2014-06-24 | 2015-08-12 | 中国石油大学(北京) | The defining method of transverse isotropy shale reservoir rock mechanics parameter |
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