CN1825086A - Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment - Google Patents
Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment Download PDFInfo
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- CN1825086A CN1825086A CN 200610038066 CN200610038066A CN1825086A CN 1825086 A CN1825086 A CN 1825086A CN 200610038066 CN200610038066 CN 200610038066 CN 200610038066 A CN200610038066 A CN 200610038066A CN 1825086 A CN1825086 A CN 1825086A
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- sample
- acid
- acetolysis
- acetic acid
- glacial acetic
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- WFDIJRYMOXRFFG-UHFFFAOYSA-N Acetic anhydride Chemical compound CC(=O)OC(C)=O WFDIJRYMOXRFFG-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000005852 acetolysis reaction Methods 0.000 title claims abstract description 26
- 239000013049 sediment Substances 0.000 title claims abstract description 10
- 239000000843 powder Substances 0.000 title 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 64
- 229960000583 acetic acid Drugs 0.000 claims abstract description 29
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 23
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002253 acid Substances 0.000 claims abstract description 12
- 238000004140 cleaning Methods 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 4
- 238000007873 sieving Methods 0.000 claims abstract description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 38
- 239000012535 impurity Substances 0.000 claims description 12
- 230000018044 dehydration Effects 0.000 claims description 11
- 238000006297 dehydration reaction Methods 0.000 claims description 11
- 239000002689 soil Substances 0.000 claims description 7
- 238000013459 approach Methods 0.000 claims description 6
- 229920002678 cellulose Polymers 0.000 claims description 6
- 239000001913 cellulose Substances 0.000 claims description 6
- 210000000805 cytoplasm Anatomy 0.000 claims description 6
- 238000012545 processing Methods 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- 239000010430 carbonatite Substances 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 claims description 3
- -1 protoplasm Substances 0.000 claims description 3
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000005119 centrifugation Methods 0.000 abstract description 3
- 238000001914 filtration Methods 0.000 abstract description 2
- 239000011435 rock Substances 0.000 abstract description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 abstract 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 abstract 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000007788 liquid Substances 0.000 abstract 1
- 238000007781 pre-processing Methods 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 238000005406 washing Methods 0.000 abstract 1
- 238000011160 research Methods 0.000 description 5
- 239000011521 glass Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- 235000002918 Fraxinus excelsior Nutrition 0.000 description 2
- 239000002956 ash Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 239000000356 contaminant Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000383 hazardous chemical Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- 239000004677 Nylon Substances 0.000 description 1
- 238000004026 adhesive bonding Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003245 coal Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000004069 differentiation Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 229920001778 nylon Polymers 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000011282 treatment Methods 0.000 description 1
- 210000005239 tubule Anatomy 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
- 239000000052 vinegar Substances 0.000 description 1
- 235000021419 vinegar Nutrition 0.000 description 1
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to acetolysis analysis method without acetic anhydride for spore and pollen in the Quaternary Period sediment. It includes the following steps: taking sample preprocessing: removing carbonate rock and silica by dilute hydrochloric acid and hydrofluoric acid, heating by thick hydrochloric acid, filtering; centrifugal dewatering; making solution of acetolysis analysis method without acetic anhydride from 75-85% glacial acetic acid, 15-25% vitriol; adding the solution into sample, whisking, heating, and the ratio is 1:2-3; adding water into the sample after cooling, centrifuging, pouring out the acid solution, adding water and taking centrifugation repeating for 2-3 times to remove acid liquid, adding little water into sample, washing in the ultrasonic wave cleaning machine, sieving, and taking centrifugation and storing. The optimized method the weight ratio of glacial acetic acid and vitriol is 80%: 20%. It is convenience to operate in lab.
Description
Technical field:
The present invention relates to the experimental technique of a kind of petrifactology fossil cryptogam, be specifically related to the acetolysis analytical approach of the cryptogam in a kind of improved quaternary sediment.
Technical background:
Spore-pollen analysis is that the scientific research personnel studies the plant spore preserved in the stratum and the application work of pollen, vegetation differentiation and climatic variation for the geologize period of history are significant, and play an important role on geologic prospecting, searching coal, oil, the energy and other mineral reserve simultaneously.And as the prerequisite that cryptogam is studied, be that the method for what use is made of chemistry, physics is extracted the fossil cryptogam from rock, and make the thin slice that can forever preserve, promptly usually said spore-pollen analysis.This is a kind of special technology, is the Palynology important component part.Equally, the fossil cryptogam also is the important content of stratigraphy study in the Quaternary period, has important science and using value.The usual method of spore-pollen analysis is to remove dead matter with hydrochloric acid and hydrofluorite, and obtains acidproof organic wall fossil.And have a large amount of undegradable canebreaks and organic impurities the Quaternary period in the cryptogam, therefore the effect of impact analysis processing at first will eliminate the interference of these organic impurities greatly.Normally by acetolysis method, to the organic impurities purified treatment in quaternary sediment and the table earth sample.Acetolysis method is the glass Kroes card Ya method (glass Kroes card Ya work " pollen analysis " in 1956) of invention just of the Soviet Union in 1956: after sample is washed method through dehydration, vinegar, prepare 9 to 1 acetic anhydride, sulfuric acid solution again and add in the test tube, heat then.In preparation, safe operation is required high, can not there be naked light to occur, therefore operate abnormally dangerously, and be difficult to grasp, therefore be not easy to promote.Secondly, acetic anhydride is the inflammable thing of national appointment, belongs to national control, usually must the unit lertter of introduction and report the approval of public security bureau, so the laboratory formality buys very loaded down with trivial detailsly, has a strong impact on the time and the efficient of experimental analysis.Therefore, pressed for and improved one's methods, and the used alternative reagent of improving one's methods must safe and reliable, easy purchase.
Summary of the invention:
The objective of the invention is traditional acetolysis method is improved, overcome the disadvantage that it uses the hazardous chemicals acetic anhydride, with the acetic anhydride in the medicine replacement classic method of safety, with the management of convenient breadboard operation and medicine.
The core content of this method is that scheme is with the acetic anhydride in the glacial acetic acid replacement classic method:
The acetolysis analytical approach of the no acetic anhydride of the cryptogam in the quaternary sediment, concrete steps be,
Sample pre-treatments: the cryptogam sample is removed carbonatite with watery hydrochloric acid, gets rid of siliceous composition with hydrofluorite, use the concentrated hydrochloric acid heat treated again after, filter to concentrate;
Will be through the sample of above-mentioned processing, centrifugal dehydration is washed once with acetic acid again, and acetic acid is removed in same centrifugal dehydration;
The preparation of the acetolysis method solution of no acetic anhydride: add sulfuric acid in proportion in glacial acetic acid, stir, the mass ratio of glacial acetic acid and sulfuric acid is glacial acetic acid 75～85%, sulfuric acid 15～25%;
The acetolysis method solution for preparing is added in the sample that dewaters fully, stir, heated about 10 minutes, cellulose, protoplasm, soil ulmin and some impurity are fully dissolved, the mass ratio of sample and acetolysis method solution is 1: 2～3;
With cooled sample thin up, centrifugal, acid solution is outwelled, thin up and centrifugal 2-3 time repeatedly, is removed acid solution again;
With adding low amounts of water in the sample, in supersonic wave cleaning machine, clean, pour into again in 10 microns sieves and sieve.Purpose: the sample through after the processing of acetolysis method, some tiny chip and ashes are arranged, the sieve of at this moment using suitable aperture is with contaminant filter, and remaining is exactly the fossil cryptogam;
The sample that obtains sieving is concentrated and just can film-making forever be preserved after the centrifugal dehydration once more.
The glacial acetic acid in the above scheme and the optimum quality ratio of sulfuric acid, the application recommends: glacial acetic acid 80%, sulfuric acid 20%.
Find by test: replace the method for acetic anhydride feasible fully with glacial acetic acid, because glacial acetic acid and acetic anhydride all are weak acid, and sulfuric acid be a kind of strong acid can and any acetate mix and form solution, according to their feature: two kinds of weak acid all have the function of purification sample; And glacial acetic acid is not inflammable thing, and promptly safety is reliable again in process for preparation.By experiment repeatedly, draw in test: the optimum reagent ratio of glacial acetic acid+sulfuric acid=8 to 2, can remove protoplasm, cellulose, soil ulmin and other impurity in the sample.Sample is again in conjunction with ultrasonic cleaning, handle with sieve after cleaning, the fossil cryptogam that deals is all very clear and inclusion-free is infected with on structure, the surface texturing internally, especially the impurity that is attached on the fossil sporoderm can both be removed fully, the SPORO-POLLEN FOSSILS AND form that obtains is clear, there is no fine impurities is infected with, be beneficial to very much fossil evaluation and statistics, greatly reduce the labor capacity of researcher, and improved the accuracy of research.Therefore this invention has purposes widely in quaternary research, is the important breakthrough of continuing to use traditional acetolysis method in the Quaternary period in 50 years, therefore has very important science and productive value.Overcome the disadvantage of using the hazardous chemicals acetic anhydride simultaneously, made things convenient for the management of breadboard operation and medicine.
Embodiment:
Embodiment 1, the acetolysis analytical approach of the no acetic anhydride of the cryptogam in the quaternary sediment,
During a collection of fossil sample of every processing, all have and to make the thin slice of permanent preservation then through focusing in the little centrifuge tube behind chemistry and physics and the cleaning sample.In general, for the not too tight cave of gluing, lake sediment or there is not the table soil sample of diagenesis, contain more protoplasm, cellulose, soil ulmin etc. and other impurity in them.This sample must be used acetolysis method after handling with conventional method, particularly analyzes modern pollen, must carry out with the method, just can reach the effect of fossil cryptogam sharpness.Step is as follows:
1. sample pre-treatments: the cryptogam sample is removed carbonatite with 10% watery hydrochloric acid usually, gets rid of siliceous composition with 42% hydrofluorite, use concentrated hydrochloric acid 36-38% heat treated again after, concentrated through 10 microns sieves (nylon) filtration.Contain soil ulmin, cellulose, protoplasm and other organic impurities in the remaining sample that obtains, above chemicals can't be removed it.Therefore to remove with acetolysis method.
2. the preparation of Gai Liang acetolysis method solution: glacial acetic acid (C
4H
6O
2Chemical pure; Concentration: 99%)+sulfuric acid (H
2SO
4Chemical pure; Concentration: 98%)=8 to 2: pouring 8 parts of glacial acetic acid in the ready graduated cylinder into, and then add 2 parts of sulfuric acid that need, mix up with glass bar again and but can.
3. will put into the little centrifuge tube of 10 milliliters, directly centrifugal dehydration, centrifugation time 3 minutes (2000 rev/mins) through the sample of handling well behind persalt and the hydrofluorite removal inorganics.Wash sample one time with acetic acid again after the dehydration, acetic acid is removed in same centrifugal dehydration.
4. suck the acetolysis method solution for preparing in the little centrifuge tube of 10 milliliters of the sample that dewaters fully with dropper, suck the 2-3 solution doubly of sample, stir with little glass bar, after making sample in the tubule obtain reaction, electric furnace heating about 10 minutes fully is dissolved among the sample cellulose, protoplasm, soil ulmin and some impurity.
5. with the direct thin up acid solution of sample in cooled 10 milliliters of little centrifuge tubes, centrifugal 3 minutes (2000 rev/mins) outwell acid solution, and thin up is also centrifugal again, and 2-3 can remove acid solution repeatedly.
6. with the sample in 10 milliliters of little centrifuge tubes, pour in 200 milliliters the small beaker, add low amounts of water, in supersonic wave cleaning machine, cleaned 20 seconds, pour into again in 10 microns sieves and sieve.Purpose: the sample through after the processing of acetolysis method, some tiny chip and ashes are arranged, the sieve of at this moment using suitable aperture is with contaminant filter, and remaining is exactly the fossil cryptogam.The sample that obtains sieving is concentrated and is put into 10 milliliters of centrifuge tubes, just can film-making forever preserve after the centrifugal dehydration once more.The SPORO-POLLEN FOSSILS AND form that obtains is clear, there is no fine impurities is infected with, and is beneficial to very that fossil is identified and statistics, greatly reduces the labor capacity of researcher, and has improved the accuracy of research.Therefore this invention has purposes widely in quaternary research, is the important breakthrough of continuing to use traditional acetolysis method in the Quaternary period in 50 years, therefore has very important science and productive value.
Embodiment 2, and is substantially the same manner as Example 1, but glacial acetic acid and the mass ratio of sulfuric acid be: glacial acetic acid 85%, sulfuric acid 15%.
Embodiment 3, and is substantially the same manner as Example 1, but glacial acetic acid and the mass ratio of sulfuric acid be: glacial acetic acid 75%, sulfuric acid 25%.
Claims (2)
1, the acetolysis analytical approach of the no acetic anhydride of the cryptogam in a kind of quaternary sediment, concrete steps be,
Sample pre-treatments: the cryptogam sample is removed carbonatite with watery hydrochloric acid, gets rid of siliceous composition with hydrofluorite, use the concentrated hydrochloric acid heat treated again after, filter to concentrate;
Will be through the sample of above-mentioned processing, centrifugal dehydration is washed once with acetic acid again, and acetic acid is removed in same centrifugal dehydration;
The preparation of the acetolysis method solution of no acetic anhydride: add sulfuric acid in proportion in glacial acetic acid, stir, the mass ratio of glacial acetic acid and sulfuric acid is glacial acetic acid 75～85%, sulfuric acid 15～25%;
The acetolysis method solution for preparing is added in the sample that dewaters fully, stir, heating is fully dissolved cellulose, protoplasm, soil ulmin and some impurity, and the mass ratio of sample and acetolysis method solution is 1: 2～3;
With cooled sample thin up, centrifugal, acid solution is outwelled, thin up and centrifugal 2～3 times repeatedly, is removed acid solution again;
With adding low amounts of water in the sample, in supersonic wave cleaning machine, clean, pour into again in 10 microns sieves and sieve;
The sample that obtains sieving, film-making is preserved after the concentrated centrifugal dehydration once more.
2, according to the acetolysis analytical approach of the no acetic anhydride of the cryptogam in the described quaternary sediment of claim 1, it is characterized in that the mass ratio of described glacial acetic acid and sulfuric acid is: glacial acetic acid 80%, sulfuric acid 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100380665A CN1825086B (en) | 2006-01-26 | 2006-01-26 | Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2006100380665A CN1825086B (en) | 2006-01-26 | 2006-01-26 | Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment |
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| Publication Number | Publication Date |
|---|---|
| CN1825086A true CN1825086A (en) | 2006-08-30 |
| CN1825086B CN1825086B (en) | 2010-07-07 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN2006100380665A Expired - Fee Related CN1825086B (en) | 2006-01-26 | 2006-01-26 | Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108548704A (en) * | 2018-04-18 | 2018-09-18 | 中国科学院东北地理与农业生态研究所 | A kind of peat cryptogam rapid extracting method |
-
2006
- 2006-01-26 CN CN2006100380665A patent/CN1825086B/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108548704A (en) * | 2018-04-18 | 2018-09-18 | 中国科学院东北地理与农业生态研究所 | A kind of peat cryptogam rapid extracting method |
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| CN1825086B (en) | 2010-07-07 |
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Granted publication date: 20100707 Termination date: 20110126 |