CN102183391A - Scanning electron microscope-energy spectrum online rock sample preparation method - Google Patents
Scanning electron microscope-energy spectrum online rock sample preparation method Download PDFInfo
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- CN102183391A CN102183391A CN 201110038881 CN201110038881A CN102183391A CN 102183391 A CN102183391 A CN 102183391A CN 201110038881 CN201110038881 CN 201110038881 CN 201110038881 A CN201110038881 A CN 201110038881A CN 102183391 A CN102183391 A CN 102183391A
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Abstract
The invention provides a scanning electron microscope-energy spectrum online rock sample preparation method which comprises the following steps: a. using the fresh, representative and even cross section of a rock sample containing oil as an observation surface and bonding the rock sample on a sample pile; b. after the rock sample is naturally dried or placed into an oven at 50 DEG C, washing off the oil on the rock sample containing the oil; and c. blowing off the dust on the surface of the rock sample with the oil washed off by washing ear balls and plating gold or plating carbon in a vacuum film plating machine. In the oil washing of the step b, a tetrahydrofuran solvent is used as a crude oil extraction solvent and added to the evaporator of a Soxhlet extractor, and the rock sample is added to a crude oil extractor; the evaporator is electrically heated; the steam is blown into a condenser through an adapting pipe; the tetrahydrofuran solvent after being condensed flows into the crude oil extractor to dissolve the crude oil in the rock sample; and finally, the tetrahydrofuran solvent which is dissolved with the crude oil flows back to the evaporator through siphons at the sides of the evaporator.
Description
Technical field:
The present invention relates to the petro-technology field, further relate to rock sample is analyzed experimental technique, the online rock sample preparation method of particularly a kind of scanning electron microscope-power spectrum.
Background technology:
In petroleum industry, scanning electron microscope-power spectrum on line analytical processing is indispensable analytical technology.This technology can be studied the type and the distribution of grain fabric feature, pore constriction feature and the cementing matter of rock, for reservoir evaluation and reservoir protection provide the important theory foundation.In high vacuum scanning electron microscope-power spectrum was online, laboratory sample was rock core or the landwaste that oil bearing grade does not wait mostly, can not directly carry out Analysis and Identification, need carry out following specimen preparation program according to the regulation of Chinese industry standard SY/T 5162-1997 the 4th part:
1. extracting (washing oil): containing oil samples needs first washing oil.
2. select sightingpiston: representative, smooth fresh section as sightingpiston.
3. go up stake: sample is bonded in the sample stake.
4. dry: as to dry naturally or put into baking oven and dry down at 50 ℃.
5. dedusting: the dust that blows sample surfaces with ear washing bulb off.
6. plated film: gold-plated or plating carbon in vacuum coating equipment.
In the rock sample preparation flow, the rock sample washing oil is finished in Soxhlet extractor, rock sample could be cleaned to fluorescence below three grades in average 6 days, and most of specimen preparation time accounts for.
In addition, the former oil extraction of rock sample is for organic principles such as the oil in the rock sample, colloid and bituminous matter are separated with the inorganic constituents of rock, satisfying the mensuration to the various physicochemical property of rock or crude oil, and then instructs petroleum exploration and development.Principle such as Fig. 1 of Soxhlet extractor extracting crude oil, basic process is: the solvent for preparing is packed in the extraction flask (evaporator) of Soxhlet extractor, then rock sample is packed in the crude oil extraction tube (extraction apparatus), connect condensate water to condenser and heat just can for the energising of extracting bottle.After the reagent boiling, steam enters the condenser from adapting pipe, and condensed solvent flows in the crude oil extraction apparatus, and the submergence rock sample also slowly dissolves the crude oil in the rock sample gradually.When reagent arrived certain height in the rock sample extraction tube, U trap was back in the extraction flask through the side, and carried institute's dissolved substances, as crude oil and water (perhaps other organic substance etc.).Reagent just moves in the closed system that Soxhlet extractor forms like this: evaporation, and---condensation---backflow---is evaporated again, moves in circles, till the former oil extraction in the rock sample is clean.But in whole crude oil extractive process, the contour malicious chemicals solvent of benzene and methenyl choloride can evaporate in the air by various approach, and air is polluted and destroys, and the staff is caused serious or even fatal harm.In addition, because it is all moisture usually in the rock sample, and benzene and methenyl choloride are all water insoluble, make solvent be difficult to enter in the rock sample, therefore must add a certain amount of alcohol in the solvent moisture is carried out extracting, otherwise extraction efficiency descends greatly, the adding of alcohol simultaneously, the volatilization that has further strengthened the contour malicious chemicals solvent of benzene and methenyl choloride.
Summary of the invention:
The purpose of this invention is to provide a kind of saving rock sample scavenging period, thereby greatly accelerate the rock sample preparation time, the online rock sample preparation method of the scanning electron microscope-power spectrum of increasing work efficiency.This preparation method also can not cause any pollution to environment in addition.
Purpose of the present invention can realize by following technical measures:
This rock sample is the preparation method carry out as follows:
A. get representative, the smooth fresh section of oil-containing rock sample as sightingpiston, and rock sample is bonded in the sample stake;
B. through drying naturally or putting into baking oven after oven dry under 50 ℃, again the oil-containing rock sample is carried out washing oil;
C. blow the dust on rock sample surface earlier off with ear washing bulb through the rock sample of washing oil, more gold-plated or plating carbon in vacuum coating equipment.
Purpose of the present invention also can realize by following technical measures:
The described washing oil of b step is to get tetrahydrofuran solvent earlier to join as former oil extraction solvent in the evaporator of Soxhlet extractor, and rock sample is joined in the former oil extractor; Then evaporator is carried out electrical heating, steam enters in the condenser by adapting pipe, and condensed tetrahydrofuran solvent flows into the crude oil in the former oil extractor dissolving rock sample; The tetrahydrofuran solvent that will be dissolved with crude oil at last is back in the evaporator through the side U trap, and tetrahydrofuran solvent recycles.
The present invention will go up stake behind the first washing oil in the original sample preparation procedure, change into and go up stake back washing oil earlier.After rock sample washing oil flow process is adjusted,,, promptly rise to present 180 by original each 30 so the sample blocks number of a washing oil has increased by 5 times because the single sample volume of selecting significantly reduces.And because the rock sample volume is little, adds and use the rock sample of tetrahydrofuran cleaning efficiently irreducible oil that washing oil is taken time and reduced half, promptly is kept to present 3 days by original 6 days.COMPREHENSIVE CALCULATING, rock sample washing oil are increased to 60 of present every days by 5 of original average every days, are equivalent to sample washing oil piece number and have turned over 12 times.In addition, as former oil extraction solvent, benzene, the contour malicious chemicals solvent of methenyl choloride have been replaced, with nontoxic tetrahydrofuran solvent without any environmental pollution.
Description of drawings:
Fig. 1 is the washing oil principle schematic.
Embodiment:
Embodiment 1:
This rock sample is the preparation method carry out as follows:
A. get representative, the smooth fresh section of oil-containing rock sample as sightingpiston, and rock sample is bonded in the sample stake;
B. through drying naturally or putting into baking oven after oven dry under 50 ℃, again the oil-containing rock sample is carried out washing oil;
C. blow the dust on rock sample surface earlier off with ear washing bulb through the rock sample of washing oil, more gold-plated or plating carbon in vacuum coating equipment.
Purpose of the present invention also can realize by following technical measures:
The described washing oil of b step is to get tetrahydrofuran solvent earlier to join as former oil extraction solvent in the evaporator of Soxhlet extractor, and rock sample is joined in the former oil extractor; Then evaporator is carried out electrical heating, steam enters in the condenser by adapting pipe, and condensed tetrahydrofuran solvent flows into the crude oil in the former oil extractor dissolving rock sample; The tetrahydrofuran solvent that will be dissolved with crude oil at last is back in the evaporator through the side U trap, and tetrahydrofuran solvent recycles.
Claims (2)
1. online rock sample preparation method of scanning electron microscope-power spectrum is characterized in that this rock sample preparation method carries out as follows:
A. get representative, the smooth fresh section of oil-containing rock sample as sightingpiston, and rock sample is bonded in the sample stake;
B. through drying naturally or putting into baking oven after oven dry under 50 ℃, again the oil-containing rock sample is carried out washing oil;
C. blow the dust on rock sample surface earlier off with ear washing bulb through the rock sample of washing oil, more gold-plated or plating carbon in vacuum coating equipment.
2. the online rock sample preparation method of a kind of scanning electron microscope-power spectrum according to claim 1, it is characterized in that the described washing oil of b step is to get tetrahydrofuran solvent earlier to join as former oil extraction solvent in the evaporator of Soxhlet extractor, joins rock sample in the former oil extractor; Then evaporator is carried out electrical heating, steam enters in the condenser by adapting pipe, and condensed tetrahydrofuran solvent flows into the crude oil in the former oil extractor dissolving rock sample; After the side U trap will be dissolved with the tetrahydrofuran solvent of crude oil and be back in the evaporator, tetrahydrofuran solvent recycles.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110038881 CN102183391A (en) | 2011-02-16 | 2011-02-16 | Scanning electron microscope-energy spectrum online rock sample preparation method |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110038881 CN102183391A (en) | 2011-02-16 | 2011-02-16 | Scanning electron microscope-energy spectrum online rock sample preparation method |
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| CN102183391A true CN102183391A (en) | 2011-09-14 |
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| CN 201110038881 Pending CN102183391A (en) | 2011-02-16 | 2011-02-16 | Scanning electron microscope-energy spectrum online rock sample preparation method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048858A (en) * | 2013-03-13 | 2014-09-17 | 中国石油天然气股份有限公司 | Method for plating copper on rock sample for scanning electron microscope |
| CN111157305A (en) * | 2019-08-15 | 2020-05-15 | 中国石油天然气股份有限公司 | Preparation and treatment method of conglomerate sample for scanning electron microscope |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4920792A (en) * | 1988-03-04 | 1990-05-01 | Shell Oil Company | Method for determining the amount of fluid in a core |
| WO2009048701A1 (en) * | 2007-10-12 | 2009-04-16 | Prad Research And Development Limited | Methods for characterizing heavy oils |
| CN101788410A (en) * | 2010-02-10 | 2010-07-28 | 中国石油天然气股份有限公司 | Method for extracting oil sample inside hydrocarbon inclusion in groups |
-
2011
- 2011-02-16 CN CN 201110038881 patent/CN102183391A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4920792A (en) * | 1988-03-04 | 1990-05-01 | Shell Oil Company | Method for determining the amount of fluid in a core |
| WO2009048701A1 (en) * | 2007-10-12 | 2009-04-16 | Prad Research And Development Limited | Methods for characterizing heavy oils |
| CN101788410A (en) * | 2010-02-10 | 2010-07-28 | 中国石油天然气股份有限公司 | Method for extracting oil sample inside hydrocarbon inclusion in groups |
Non-Patent Citations (2)
| Title |
|---|
| 《中华人民共和国石油天然气行业标准》 19971231 魏宝和 等 SY/T 5162-1997岩石样品扫描电子显微镜分析方法 , * |
| 《石油炼制》 19821231 葛家齐 等 五种国产减压渣油的分子量分布 , 第12期 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104048858A (en) * | 2013-03-13 | 2014-09-17 | 中国石油天然气股份有限公司 | Method for plating copper on rock sample for scanning electron microscope |
| CN104048858B (en) * | 2013-03-13 | 2016-07-13 | 中国石油天然气股份有限公司 | A kind of copper electroplating method of scanning electron microscope rock sample |
| CN111157305A (en) * | 2019-08-15 | 2020-05-15 | 中国石油天然气股份有限公司 | Preparation and treatment method of conglomerate sample for scanning electron microscope |
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Application publication date: 20110914 |