CN1825086B - 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
- Publication number
- CN1825086B CN1825086B CN2006100380665A CN200610038066A CN1825086B CN 1825086 B CN1825086 B CN 1825086B CN 2006100380665 A CN2006100380665 A CN 2006100380665A CN 200610038066 A CN200610038066 A CN 200610038066A CN 1825086 B CN1825086 B CN 1825086B
- Authority
- CN
- China
- Prior art keywords
- sample
- acid
- acetolysis
- acetic acid
- glacial acetic
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- 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 10 milliliters of little centrifuge tubes 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 the quaternary sediment, concrete steps are 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 and 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 impurity, and described impurity includes cellulose, protoplasm, soil ulmin; 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 |
Applications Claiming Priority (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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1825086A CN1825086A (en) | 2006-08-30 |
| CN1825086B true CN1825086B (en) | 2010-07-07 |
Family
ID=36935861
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2006100380665A Expired - Fee Related CN1825086B (en) | 2006-01-26 | 2006-01-26 | Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1825086B (en) |
Families Citing this family (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
Non-Patent Citations (2)
| Title |
|---|
| 何翠玲.微体样品化学处理中的小管净化.中国古生物学会第九届全国会员代表大会暨中国古生物学会第二十三次学术年会论文摘要集无 无.2005,123. |
| 何翠玲.微体样品化学处理中的小管净化.中国古生物学会第九届全国会员代表大会暨中国古生物学会第二十三次学术年会论文摘要集无 无.2005,123. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1825086A (en) | 2006-08-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Zhao et al. | Experiments for improving phytolith extraction from soils | |
| BR112013024126B1 (en) | method for the recovery of oil from the production of ethanol from corn | |
| CN104142321A (en) | Method for fast detecting surface enhancing Raman spectrums of pesticide residues in tea leaves | |
| CN108129547B (en) | Method for extracting extracellular polymeric substance of zoogloea | |
| CN101817526A (en) | Method for recovering polyethylene glycol and silicon carbide from silicon crystal cutting waste liquid | |
| CN106349486B (en) | A kind of sludge and fulvic acid XAD resin fractional extraction method in stalk hybrid composting | |
| CN101726438B (en) | Method for analyzing glass fiber in paper | |
| CN1825086B (en) | Acetolysis analyzing method without acetic anhydride for spore powder in quaternary sediment | |
| TAKAHASHI et al. | An improved method for estimating the number of resting spores of Plasmodiophora brassicae in soil | |
| CN106053175B (en) | The simple and easy method of carbide in a kind of extractor tool steel | |
| CN115557508B (en) | Method for purifying siliceous sponge spicules in marine sediments | |
| CN105038848B (en) | A kind of preprocess method of biomass pyrolytic tar | |
| CN105675375A (en) | Separating medium of inactivated nematode in dead masson pine wood and separation method and kit | |
| CN109110765B (en) | Method for extracting silicon powder and silicon carbide from silicon wafer cutting waste sand mixture | |
| CN203007255U (en) | Quick extracting device for pine wood nematode nucleic acid in wood | |
| JI et al. | Efficient separation of phenols from phenols-containing oil mixtures via forming hydrogen bonds | |
| CN113049324A (en) | Pretreatment method suitable for aquatic product anesthetic or veterinary drug | |
| US20150361018A1 (en) | Process for cleaning contaminated fluids | |
| KR101148482B1 (en) | Chlorophyll extraction method from silksorm excrements | |
| CN108548704A (en) | A kind of peat cryptogam rapid extracting method | |
| CN108918486A (en) | Method and device for measuring crude oil content in oily sludge | |
| Green et al. | Extraction techniques for palaeobotanical and palynological material | |
| CN109030162A (en) | A kind of full-automatic preprocessing system of oil inclusions group constituent analysis and method | |
| CN103344519B (en) | A kind of silit chemical analysis method | |
| CN109078508A (en) | A kind of preparation method of the arsenic removal film for mine arsenic-containing waste water |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20100707 Termination date: 20110126 |