CN105424687A - Method for detecting biogenic silicon content in bottom sediment - Google Patents
Method for detecting biogenic silicon content in bottom sediment Download PDFInfo
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- CN105424687A CN105424687A CN201510764778.4A CN201510764778A CN105424687A CN 105424687 A CN105424687 A CN 105424687A CN 201510764778 A CN201510764778 A CN 201510764778A CN 105424687 A CN105424687 A CN 105424687A
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Abstract
The invention discloses a method for detecting the biogenic silicon content in bottom sediment. According to the method, a sample is subjected to one-step extraction after pretreatment, and testing of the sample in a day can be implemented. Meanwhile, the method is improved on the basis of the alkali dissolution spectrophotometric method, so that the minimum detectable concentration of dissolved silicon is 40 microgram/L, and the detectable upper limit is 2 mg/L. Test steps are easy and convenient to operate, one-time effective extraction is achieved, the biogenic silicon content in the bottom sediment of fresh water bodies such as lakes, rivers and reservoirs can be accurately, effectively and quickly tested, analyzed precision is higher, extraction of richer water body ecological environment change information is facilitated, water quality changes of water sources, landscape water bodies and aquatic water bodies can be monitored, and the biogenic silicon content can serve as an important environment monitoring index of water environment science and engineering reform.
Description
Technical field
The invention belongs to environmental monitoring field, relate to the method for Biogenic Silica in accurate and effective, the quick detection Sediments of a kind of energy, by pre-treatment and the final test method of bed mud, accurate test can be realized, realize rapid extraction water body environment change information.
Background technology
Biogenic opal (BSi, BiogenicSilica) also known as be biological opaline (abbreviation opaline).It is the important component part of lake, river, oceanic sediment, and its overwhelming majority derives from the deposition of dead diatom test.Diatom is a kind of phytoplankton (Phytoplankton), and it has photosynthetic pigments, and the differentiation of plant unrooted, stem, leaf, the rudimentary plant of the unicellular reproductive organs of tool, diatom lives in various types of water body.At present, diatom has been recorded and has had distinctive kind more than 100,000.
The research in biogenic opal field mainly concentrates in the research of oceanic sediment in the past, is used to refer to the change of sea surface yield-power.In geology, the Main Function of biogenic opal research is the Division and contrast on stratum and palaeoenvironmental recovery, is the Main Basis dividing some stratum: the historic change of solvable silicon in (1) record water body; (2) indispensable part in global silicon cycling research; (3) the Substitute Indexes effect in paleoclimatology research; (4) the paleolimnology meaning of biogenic opal.At present, the method for testing for Biogenic Silica is concluded and is mainly contained 7 kinds, respectively: (1) is X-ray diffraction method directly; (2) indirect X ray diffraction approach; (3) infrared measure; (4) total rock chemical element computing method; (5) difference wet method; (6) microfossil counting method; (7) the molten spectrophotometric method of alkali.These methods respectively have feature, and application is also wide, but the shortcoming such as ubiquity measuring accuracy is low, the test duration is long, testing cost is high; And being confined to geology, petrochemical complex, application is narrow.
The research effect of biogenic opal is by according to the mutual relationship between diatom group in Recent Lakes water body and its distribution, ecosystem environment, carry out the historical analogy of Water-Body Information, survey year data in conjunction with other Microfossils, chemical element, stable isotope, mineral, organic compound and nucleic, rebuild the change histories of different times water body environment.Due to following reason, biogenic opal research is not only in geology research, and also can play important effect in modern environment scientific and engineering: (1) diatom abundance in water body in lake is high, in lake sediment, the concentration of diatom is also very high equally.The almost full zeyssatite deposition be made up of diatom shell even can be formed under the environmental baseline be applicable to; (2) subtle change of the chemical composition of water body, salinity, pH value, nutritional labeling, illumination, temperature, the environmental baseline such as turbidity and the degree of depth, all may change the different degree of group splitting or integrating of diatom, sociales and concentration etc.; (3) compared with other algae or microfossil, the siliceous housing of diatom is easy to preserve in sediment; (4) widely dispersed of diatom, from desalination lake to high salinity salt lake, all may grow diatom from poor nutrition class lake to eutrophic lake; (5) because the classification of diatom is carried out according to shell characteristics, so Fossil Diatom and now raw diatom are easily identified.The research of biogenic opal is developed rapidly in recent years in following 8: (1) genealogical classification; (2) with the relation of envirment factor; (3) Lake Acidification; (4) eutrophication; (5) climate change; (6) transfer function; (7) resedimentation and dissolution; (8) biogenic opal and pigment comparative analysis etc.Mostly tradition monitoring water environment is to carry out for water body physics, chemistry, Biological indicators with analysis, seldom relate to the analysis of Biological indicators in sediment bed mud, the formulation that the foundation of biogenic opal method of testing can be monitoring water environment and water environment treatment engineering proposal plays an important role.
At present, the detection method about bed mud biogenic opal focuses mostly among the bed mud of ocean, has no the report relating to the poisons in freshwaters such as river, lake, reservoir.Detection difficulty for bed mud biogenic opal mainly concentrates on: the test duration is long, test result is forbidden, the present invention provides a kind of detection method being applicable to Biogenic Silica in freshwater sediment sediment first.
Summary of the invention
Technical matters to be solved by this invention is to provide a kind of method detecting Biogenic Silica in Sediments, the method accurately, fast, effectively, can within a short period of time, test organisms silicone content more quickly and accurately, the environmental information of research Sediments, all can accurately, rapidly, effectively be used the Inspect and control water body eutrophication such as (Important Water Source, lake, river, reservoir poisons in freshwater).Applicant by the improvement of sample pre-treatments and final experimental test procedures, perfect lacustrine deposit biogenic opal laboratory determination method, the shortcoming such as the precision that the inconvenience in the method for testing of overcoming over, complicated, failure, error cause more greatly is low.
For solving above-mentioned technical matters, technical solution of the present invention is:
Detect a method for Biogenic Silica in Sediments, comprise the following steps:
(1) freezing-dry: the freezing 48h of-80 DEG C, sample, after dry, sample water percentage remains on 1%-5%, and sample is placed on sealing in zip lock bag, and room temperature (25-28 DEG C) balance 12-24h, crosses 100-150 mesh sieves;
(2) take sample 180-200mg and put into 50mL polypropylene centrifuge tube;
(3) H of 4-5mL9%-11% is added
2o
2(must the same day configuration) Yu Guanzhong, leaves standstill 30-40min, and then adds 4-6mL1.00-1.50mol/LHCL, and ultrasonic 40kHz (220-240w) vibrates 25-30min;
(4) add 18-20mL deionized water, under eccentricity 4200-4500g, outwell supernatant after centrifugal 5-8min, deposited material can not disturbance, if there is deposited material disturbance, repeats step 2-3 time; Centrifuge tube containing deposited material is placed in 50-60 DEG C of baking ovens and dries 10-12h;
(5) accurately 36.0-40.0mL2mol/LNa is drawn
2cO
3in centrifuge tube after step (4) is dried, ultrasonic 40kHz (220-240w) vibrates to be placed in the water-bath of 80-85 DEG C after 5-8min and (adds a cover) heated at constant temperature;
(6) with 2-3h for interval, with sticking plaster agitating solution manually, after 5-6h, take out pipe, and rapid centrifugal 5-10min under 4200-4500g;
(7) shift out 4-6mL supernatant fast, and be kept in polypropylene tube in order to measuring;
(8) through above step, in sediment, biogenic opal dissolves completely, and by there is not diatom test in light microscopy sediment residue, after qualitative detection completes, employing silicon molybdenum blue colourimetry quantitatively detects.
In above-described scheme, storage of samples does not contact with glassware with testing process.If use glassware, first carry out full procedure blank test, eliminate the interference of glassware by the method that deduction is blank.Reagent preparation water should be distilled water.
In above-described scheme, described bed mud is take from the bed mud in the poisons in freshwaters such as Important Water Source, river, lake or reservoir.
Described silicon molybdenum blue colourimetry, comprises the following steps:
(1) utilize HCl to regulate solution ph to 6.80-7.20, adopt after the yellow silicon-molybdenum heteropoly acid of formation and add 1,2, during 4-amino naphthol sulfonic acid reductive agent, be reduced to silicon molybdenum blue, adopt silicon molybdenum blue colourimetry to carry out colorimetric test, thus improve measurement sensitivity;
(2) preparation of reductive agent, dissolves 500mg1-amino-beta naphthal-4-sulfonic acid (1-amino-2-naphthol-4-sulfonicacid) and 1gNa
2sO
3yu Shuizhong, can heat, then add solution containing 30gNaHSO
3150mL aqueous solution in, be filtered in polyethylene solution, put into refrigerator and keep in Dark Place, if find that solution colour deepens to stop using and again prepares;
(3) silicon dioxide standard solution, gets every milliliter of stock solution 10.00mL containing 1.00mg silicon dioxide and moves in 1000mL volumetric flask, be diluted to graticule, preserve with polyethylene bottle sealing.In this solution, every milliliter contains 10.0 μ g silicon dioxide;
(4) other preparation of reagents, ammonium molybdate reagent: dissolve 10g ammonium molybdate and (stir and low-grade fever) in water, be diluted to 100mL, can filter if any insolubles, reconcile to pH7-8 with ammoniacal liquor.1+1 hydrochloric acid solution 5mL.Oxalic acid solution, 75g/L: dissolve 7.50g oxalic acid in water, be diluted to 100mL.Silicon dioxide stock solution: take glass sand (silicon dioxide) 0.2500g and be placed in platinum crucible (30-50mL), add natrium carbonicum calcinatum 4g, mixing, put into muffle furnace at 1000 DEG C of melting 1h, put into the leaching of plastic beaker hot water after taking out cooling, wash clean crucible and lid with water, move in 250mL volumetric flask, be diluted with water to graticule, mixing.Store in tygon, sealing is preserved, and this solution every milliliter is containing 1.00mg silicon dioxide.
(5) drafting of typical curve, get silicon dioxide standard solution 0,0.10,0.50,1.00,3.00,5.00,7.00,10.00mL, move respectively in 50mL color comparison tube, be diluted with water to graticule.Add 1+1 hydrochloric acid solution 1.0mL and ammonium molybdate reagent 2.0mL successively rapidly, fully mix, then place 10-15min.Add 2.0mL oxalic acid solution, fully mix.After 5-10min, being 650-660nm place at spectrophotometer absorption peak, using 10mm cuvette, take water as reference, measures absorbance.Calibration curve is drawn after blank correction.
(6) mensuration of water sample, getting appropriate as clear as crystal water sample (or through 0.45 μm of membrane filtration) in 50mL color comparison tube, measuring according to drawing identical method of operating with calibration curve.If water sample has color, then water sampling 2 parts, 1 part of test use, other 1 part does not add ammonium molybdate, and all the other operations are all drawn identical with calibration curve.The absorbance recorded by the former, after deducting the absorbance of the water sample not adding ammonium molybdate, checks in final content, eliminates the interference of colourity.
In the above scheme, preferred:
(1) freezing-dry :-80 DEG C of freezing 48h, after dry, sample water percentage remains on 3%, and sample is placed on sealing in zip lock bag, and 26 DEG C of balance 24h, cross 120 mesh sieves;
(2) take sample 200mg and put into 50mL polypropylene centrifuge tube;
(3) H of 5mL10% is added
2o
2(w/v; Must configuration on the same day) in centrifuge tube, leave standstill 30min, and then add 5mL1mol/LHCL, ultrasonic 40kHz (220-240w) vibrates 30min;
(4) 20mL deionized water is added, under eccentricity 4300g, outwell supernatant after centrifugal 5min, deposited material can not disturbance, if there is deposited material disturbance, can repeat to add water centrifugal 2-3 times, the centrifuge tube containing deposited material is placed in 55 DEG C of baking ovens and dry 10h;
(5) accurately 40.0mL2mol/LNa is drawn
2cO
3in the centrifuge tube of step (4), ultrasonic 40kHz (220-240w) is vibrated to be placed in the water-bath of 83 DEG C after 5min and (is added a cover) heated at constant temperature;
(6) be interval agitating solution with 2h, after 5h, take out pipe, and centrifugal 5min under 4300g rapidly;
(7) shift out 5mL supernatant fast, and be kept in polypropylene tube in order to measuring;
Utilize above-mentioned optimal parameter method, minimum concentrations is 40 μ g/L, and detecting the upper limit is 2mg/L.
Compared with prior art, the present invention has the following advantages:
(1) the present invention has done part improvement on the molten spectrophotometric method basis of alkali, and utilize silicon molybdenum blue colorimetric method for determining Biogenic Silica, precision is higher.Traditional method of testing many employings molybdenum yellow method, under certain acidity, silicic acid and ammonium molybdate generate yellow silicon-molybdenum heteropoly acid H
8[Si (Mo
2o
7)
6], i.e. molybdenum yellow, can carry out the colorimetric estimation of silicon.But molybdenum yellow is unstable, sensitivity is not high yet, and molybdenum yellow photometry concentration limit is only 0.4mg/L, and determination of the upper limit is only 25mg/L.So, with reductive agent, it must be reduced into blue silicon-molybdenum heteropoly acid, namely silicon molybdenum blue.Finally, utilize silicon molybdenum blue colorimetric method for determining dissolves silicon content, the minimum concentrations of silicon molybdenum blues photometry is 40 μ g/L, and detecting the upper limit is 2mg/L.
(2) test duration is shorter, carries out onestep extraction after pre-treatment, can realize the test to sample in 1 day, obtain final test data by freeze drier to sample.The mainly common seasoning that past adopts is all carry out at more than 0 DEG C or higher temperature usually.In general, after dry, the product of gained occurs that volume-diminished, quality are hardening, and volatile component can lose, and the material generation sex change of thermal sensitivity, inactivation, even there occurs oxidation.Therefore, dried product, compared with before drying, proterties has very large difference.For bed mud, after adopting freeze drier freeze-drying, dried bed mud is loose porous, in spongy, dissolve rapidly and completely, almost recover original proterties immediately after adding water.
(3) data can flexible conversion, and the data tested out are percentage composition, both can independently use; Also can be converted into qualitative data rapidly, thus realize and the large aggregation of data analysis on the biometric platform of the qualitative data of other physics, chemistry, Biological indicators, realize environmental monitoring.
(4) method of testing is easy, is easy to grasp, and difficulty is lower, overcomes over and tests lab assistant and the high shortcoming of appointed condition requirement, can apply to domestic most Routine Test Lab.
(5) method provided by the invention simplifies step while ensure that accuracy rate, have compressed the time, and the process for sample can guarantee Sample storage shape invariance; Silicon molybdenum blue method replaces the use of molybdenum yellow method, ensures that measuring accuracy increases substantially.
Accompanying drawing explanation
Fig. 1 is biogenic opal method of testing schematic flow sheet in lake sediment.
Fig. 2 is biogenic opal (BSi) detection record figure.
Embodiment
Set forth content of the present invention below in conjunction with embodiment further for somewhere, Hubei bottom mud in lake biogenic opal, but the present invention uses category to be not only confined to the following examples.
Embodiment 1:
Detect a method for Biogenic Silica in Sediments, comprise the following steps:
The bed mud of piston type profile lead to the less waters of the artificial interference in the natural lake of Hubei is adopted to sample, layering is sampled according to (0-10cm/ layer), load in plastics zip lock bag and take back, sample is carried out freeze-dried :-80 DEG C of freezing 48h, after dry, sample water percentage remains on 3%, sample is placed on sealing in zip lock bag, and 26 DEG C of balance 24h, cross 120 mesh sieves;
(1) take sample 200mg and put into 50mL polypropylene centrifuge tube;
(2) H of 5mL10% is added
2o
2(must the same day configuration) Yu Guanzhong, leaves standstill 30min, and then adds 5mL1mol/LHCL, and ultrasonic 40kHz (220-240w) vibrates 30min;
(3) add 20mL deionized water, under eccentricity 4300g, outwell supernatant after centrifugal 5min, deposited material can not disturbance, if there is deposited material disturbance, can repeat step 2-3 time, be placed in 55 DEG C of baking ovens and dry 10h;
(4) accurately 40mL2mol/LNa is drawn
2cO
3yu Guanzhong, ultrasonic 40kHz (220-240w) vibrate to be placed in the water-bath of 83 DEG C after 5min and (add a cover) heated at constant temperature;
(5) be interval agitating solution with 2h, after 5h, take out pipe, and centrifugal 5min under 4300g rapidly;
(6) shift out 5mL supernatant fast, and be kept in polypropylene tube in order to measuring;
(7) through above step, in sediment, biogenic opal dissolves completely, by there is not diatom test in light microscopy sediment residue, enters quantitative detecting step after qualitative detection completes;
(8) utilize HCl to regulate solution ph to 6.80-7.20, when employing adds 1,2,4-amino naphthol sulfonic acid reductive agent after forming yellow silicon-molybdenum heteropoly acid, be reduced to silicon molybdenum blue, adopt silicon molybdenum blue colourimetry to carry out colorimetric test; (absorption peak is 650nm, detects and is limited to 10 to adopt Japanese Shimadzu UV-260 spectrophotometer to carry out measuring in the present embodiment
-8g).
(9) preparation of reductive agent, dissolves 500mg1-amino-beta naphthal-4-sulfonic acid (1-amino-2-naphthol-4-sulfonicacid) and 1gNa
2sO
3yu Shuizhong, can heat, then add solution containing 30gNaHSO
3150mL aqueous solution in, be filtered in polyethylene solution, put into refrigerator and keep in Dark Place, if find that solution colour deepens to stop using and again prepares;
(10) silicon dioxide standard solution, gets every milliliter of stock solution 10.00mL containing 1.00mg silicon dioxide and moves in 1000mL volumetric flask, be diluted to graticule, preserve with polyethylene bottle sealing.In this solution, every milliliter contains 10.0 μ g silicon dioxide;
(11) other preparation of reagents, ammonium molybdate reagent: dissolve 10g ammonium molybdate and (stir and low-grade fever) in water, be diluted to 100mL, can filter if any insolubles, be adjusted to pH7-8 with ammoniacal liquor.1+1 hydrochloric acid solution 5mL.Oxalic acid solution, 75g/L: dissolve 7.50g oxalic acid in water, be diluted to 100mL.Silicon dioxide stock solution: take glass sand (silicon dioxide) 0.2500g and be placed in platinum crucible (30-50mL), add natrium carbonicum calcinatum 4g, mixing, put into muffle furnace at 1000 DEG C of melting 1h, put into the leaching of plastic beaker hot water after taking out cooling, wash clean crucible and lid with water, move in 250mL volumetric flask, be diluted with water to graticule, mixing.Store in tygon, sealing is preserved, and this solution every milliliter is containing 1.00mg silicon dioxide.
(12) drafting of typical curve, get silicon dioxide standard solution 0,0.10,0.50,1.00,3.00,5.00,7.00,10.00mL, move respectively in 50mL color comparison tube, be diluted with water to graticule.Add 1+1 hydrochloric acid solution 1.0mL and ammonium molybdate reagent 2.0mL successively rapidly, fully mix, then place 10-15min.Add 2.0mL oxalic acid solution, fully mix.After 5-10min, being 650-660nm place at spectrophotometer absorption peak, using 10mm cuvette, take water as reference, measures absorbance.Calibration curve is drawn after blank correction.
(13) mensuration of water sample, getting appropriate as clear as crystal water sample (or through 0.45 μm of membrane filtration) in 50mL color comparison tube, measuring according to drawing identical method of operating with calibration curve.If water sample has color, then water sampling 2 parts, 1 part of test use, other 1 part does not add ammonium molybdate, and all the other operations are all drawn identical with calibration curve.The absorbance recorded by the former, after deducting the absorbance of the water sample not adding ammonium molybdate, checks in final content, eliminates the interference of colourity.
Utilize said method, 3 reperformance tests have been done at total 10 sediment samples of holing to Z-1 and the Z-2 in lake, Hubei, test result mean deviation is less, SPSS12.0 is used to carry out statistical study to sampled point Z-1 and Z-2, result shows there was no significant difference between sampled point (P > 0.05) (table 1, Fig. 2), show that method accuracy provided by the invention is high, reproducible.
Table 1
Claims (5)
1. detect a method for Biogenic Silica in Sediments, comprise the following steps:
(1) freezing-dry: the freezing 48h of-80 DEG C, sample, after dry, sample water percentage remains on 1%-5%, and sample is placed on sealing in zip lock bag, and equilibrium at room temperature 12-24h crosses 100-150 mesh sieves;
(2) take sample 180-200mg and put into 50mL polypropylene centrifuge tube;
(3) H of 4-5mL9%-11% is added
2o
2yu Guanzhong, leaves standstill 30-40min, and then adds 4-6mL1.00-1.50mol/LHCL, ultrasonic 40kHz vibration 25-30min;
(4) add 18-20mL deionized water, under eccentricity 4200-4500g, outwell supernatant after centrifugal 5-8min, deposited material can not disturbance, if there is deposited material disturbance, repeats this step of step 2-3 times; Centrifuge tube containing deposited material is placed in 50-60 DEG C of baking ovens and dries 10-12h;
(5) 36.0-40.0mL2mol/LNa is drawn
2cO
3in centrifuge tube after step (4) is dried, after ultrasonic 40kHz vibration, be placed on heated at constant temperature in the water-bath of 80-85 DEG C;
(6) with 2-3h for interval, with sticking plaster agitating solution manually, after 5-6h, take out pipe, and rapid centrifugal 5-10min under 4200-4500g;
(7) shift out 4-6mL supernatant fast, and be kept in polypropylene tube in order to measuring;
(8) through above step, in sediment, biogenic opal dissolves completely, and by there is not diatom test in light microscopy sediment residue, after qualitative detection completes, employing silicon molybdenum blue colourimetry quantitatively detects.
2. method according to claim 1, storage of samples does not contact with glassware with testing process; If use glassware, first carry out full procedure blank test, eliminate the interference of glassware by the method that deduction is blank; Reagent preparation water is distilled water.
3. method according to claim 1, described bed mud is take from the bed mud in Important Water Source, river, lake or reservoir poisons in freshwater.
4. method according to claim 1, described silicon molybdenum blue colourimetry, comprises the following steps:
(1) utilize HCl to regulate solution ph to 6.80-7.20, when employing adds 1,2,4-amino naphthol sulfonic acid reductive agent after forming yellow silicon-molybdenum heteropoly acid, be reduced to silicon molybdenum blue, adopt silicon molybdenum blue colourimetry to carry out colorimetric test, thus improve measurement sensitivity;
(2) preparation of reductive agent, dissolves 500mg1-amino-beta naphthal-4-sulfonic acid and 1gNa
2sO
3yu Shuizhong, can heat, then add solution containing 30gNaHSO
3150mL aqueous solution in, be filtered in polyethylene solution, put into refrigerator and keep in Dark Place, if find that solution colour deepens to stop using and again prepares;
(3) silicon dioxide standard solution, gets every milliliter of stock solution 10.00mL containing 1.00mg silicon dioxide and moves in 1000mL volumetric flask, be diluted to graticule, preserve with polyethylene bottle sealing; In this solution, every milliliter contains 10.0 μ g silicon dioxide;
(4) other preparation of reagents, ammonium molybdate reagent: dissolve 10g ammonium molybdate in water, be diluted to 100mL, can filter if any insolubles, be adjusted to pH7-8 with ammoniacal liquor; 1+1 hydrochloric acid solution 5mL; Oxalic acid solution, 75g/L: dissolve 7.50g oxalic acid in water, be diluted to 100mL; Silicon dioxide stock solution: take glass sand 0.2500g and be placed in platinum crucible, add natrium carbonicum calcinatum 4g, mixing, puts into muffle furnace at 1000 DEG C of melting 1h, put into plastic beaker hot water after taking out cooling to leach, wash clean crucible and lid with water, move in 250mL volumetric flask, be diluted with water to graticule, mixing, store in tygon, sealing is preserved, and this solution every milliliter is containing 1.00mg silicon dioxide;
(5) drafting of typical curve, get silicon dioxide standard solution 0,0.10,0.50,1.00,3.00,5.00,7.00,10.00mL, move respectively in 50mL color comparison tube, be diluted with water to graticule, add 1+1 hydrochloric acid solution 1.0mL and ammonium molybdate reagent 2.0mL successively rapidly, abundant mixing, then place 10-15min, add 2.0mL oxalic acid solution, fully mix, after 5-10min, be 650-660nm place at spectrophotometer absorption peak, using 10mm cuvette, take water as reference, measure absorbance, after blank correction, draw calibration curve;
(6) mensuration of water sample, gets appropriate as clear as crystal water sample in 50mL color comparison tube, measures according to drawing identical method of operating with calibration curve; If water sample has color, then water sampling 2 parts, 1 part of test use, other 1 part does not add ammonium molybdate, and all the other operations are all drawn identical with calibration curve; The absorbance recorded by the former, after deducting the absorbance of the water sample not adding ammonium molybdate, checks in final content, eliminates the interference of colourity.
5. method according to claim 1, is characterized in that:
(1) freezing-dry :-80 DEG C of freezing 48h, after dry, sample water percentage remains on 3%, and sample is placed on sealing in zip lock bag, and 26 DEG C of balance 24h, cross 120 mesh sieves;
(2) take sample 200mg and put into 50mL polypropylene centrifuge tube;
(3) H of 5mL10% is added
2o
2in centrifuge tube, leave standstill 30min, and then add 5mL1mol/LHCL, ultrasonic 40kHz vibration 30min;
(4) add 20mL deionized water, under eccentricity 4300g, outwell supernatant after centrifugal 5min, deposited material can not disturbance, if there is deposited material disturbance, can repeat to add water centrifugal 2-3 times, the centrifuge tube containing deposited material is placed in 55 DEG C of baking ovens and dry 10h;
(5) accurately 40.0mL2mol/LNa is drawn
2cO
3in the centrifuge tube of step (4), after ultrasonic 40kHz vibration 5min, be placed on heated at constant temperature in the water-bath of 83 DEG C;
(6) be interval agitating solution with 2h, after 5h, take out pipe, and centrifugal 5min under 4300g rapidly;
(7) shift out 5mL supernatant fast, and be kept in polypropylene tube in order to measuring.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN108508182A (en) * | 2018-03-16 | 2018-09-07 | 中石化江汉石油工程有限公司测录井公司 | Quickly determine the survey logging method of Biogenic Silica in the hot shale of graptolitic facies |
| CN108918816A (en) * | 2018-04-24 | 2018-11-30 | 中石化石油工程技术服务有限公司 | Determine the survey logging method of five peak shale Biogenic Silicas |
| CN111982887A (en) * | 2019-05-24 | 2020-11-24 | 中国石油化工股份有限公司 | Method for measuring content of biological silicon in sedimentary rock |
| CN110243936A (en) * | 2019-06-14 | 2019-09-17 | 中国科学院水生生物研究所 | A kind of method of original position enabling non-destructive determination biomass of submerged plant |
| CN110243936B (en) * | 2019-06-14 | 2021-05-28 | 中国科学院水生生物研究所 | Method for in-situ nondestructive determination of biomass of submerged plant |
| CN110361383A (en) * | 2019-06-19 | 2019-10-22 | 广州大学 | A kind of lake historical ecology health assessment method based on sedimentary column snapshot |
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