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Extraction of OM Rock-Eval (Pyrolysis) Elemental analysis GC, HPLC & MS SIRMS
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Extraction of OM Outline of extraction procedures in IHSS method Step 1. Equilibrate the sample to a pH value between 1-2 with 1 M HCl at room teperature. Adjust solution volume with 0.1 M HCl to provide a final concentration that has ratio of 10 mL liquid/1 g dry sample. Shake the suspencion for 1 hour. Step 2. Separate supernatant from the residue by decantation after allowing solution to settle (or by low speed centrifugation). Save supernatant for XAD-8 isolation. Step 3. Neutralize the soil residue with 1 M NaOH to pH=7.0 then add 0.1 NaOH under an athmosphere of N2 to give a final extractant to soil ratio of 10:1. Step 4. Extract the suspension under N2 with intermittent shaking for a minimum of 4 hours. Allow the alkaline suspension to settle overnight and collect the supernatant by means of decantation or centrifugation. Step 5. Acidify the supernatant with 6 M HCl with constant stirring to pH=1.0 and then allow the suspension to stand for 12-16 hours. Step 6. Centrifuge to separate the humic acid (precipitate) and fulvic acid (supernatant - FA Extract 2) fractions. Step 7. Redissolve the humic acid fraction by adding a minimum volume of 0.1 M KOH under N2. Add solid KCl to attain 0.3 M (K+) and then centrifuge at high speed to remove suspended solids.
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Step 8. Reprecipitate the humic acid as in step 5. Centrifuge and discard supernatant. Step 9. Suspend the humic acid precipitate in 0.1 M HCl/0.3 M HF solution in a plastic container. Shake overnight at room temperature. Step 10. Centrifuge and repeat HCl/HF treatment(step 9), if necessary, until the ash content is below 1 percent. Step 11. Transfer the precipitate to a Visking dialysis tube by slurring wiyh water and dialyze against distilled water until the dialysis watr gives a nagative Cl- test with the AgNO3. Step 12. Freeze-dry the humic acid. Step 13. Pass the supernatant from step 2 through a column of XAD-8 (0.15 ml of resin per gram of initial sample dry weight at a flow rate of 15 bed volumes per hour). Discard the effluent, rinse the XAD-8 column containing sorbed fulvic acid with 0.65 column volumes of distilled water. Step 14. Back elute the XAD-8 column with 1 column volume of 0.1 M NaOH, followed by 2-3 column volumes of distilled water. Step 15. Immediately acidify with 6 M HCl to pH=1. Add concentrated HF to a final concentration of 0.3 M HF. Solution volume should be sufficient to maintain fulvic acid solubility. Step 16. Pass the supernatant from step 6 through a column of XAD-8 (1.0 mL of resin per gram of initial sample dry weight). Step 17. Repeat steps 14 and 15
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Step 18. Combine the final eluates from steps 15 and 17 and pass this solution through XAD-8 resin in glass column (column volume should be 1/5 of sample volume). Rinse with 0.65 column volumes of distilled water. Step 19. Back elute with 1 column volume of 0.1 M NaOH followed by 2 column volumes of distilled water. Pass eluate through H+- saturated cation exchange resin (Bio-Rad AG-MP-5) using three times the mole of Na ions in solution). Step 20. Freeze-dry the eluate to recover the H+- saturated fulvic acid. from http://karnet.up.wroc.pl/~weber/ekstrak2.htm
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http://karnet.up.wroc.pl/~weber/ekstrak2.htm
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http://jmbe.asm.org/index.php/jmbe/article/view/656/html Soxhlet extraction
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Rock-Eval (pyrolysis) 무산소 가열로 유기물의 분해를 측정하는 것. 근 원암의 평가에 많이 이용 http://www.vinci-technologies.com/product s-explo.aspx?IDR=82289&idr2=82568&ID M=536784 http://wiki.aapg.org/Rock-Eval_pyrolysis
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PeakIs a measurement of…Comment S1 mg Hc/g rock The free hydrocarbons present in the sample before the analysis Can be thought of as a residual hydrocarbon phase. When S1 is large relative to S2, an alternative source such as migrated hydrocarbons or contamination should be suspected S2 mg Hc/g rock The volume of hydrocarbons that formed during thermal pyrolysis of the sample Used to estimate the remaining hydrocarbon generating potential of the sample S3 mg Co2/g rock The CO 2 yield during thermal breakdown of kerogen Most prevalent in calcareous source rocks. S4 mg carbon/g rock The residual carbon content of the sample Residual carbon content of sample has little or no potential to generate hydrocarbons due to a lack of hydrogen and the chemical structure of the molecule %TOC=[0.082(S1+S2)+S4]/10 http://wiki.aapg.org/Rock-Eval_pyrolysis
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http://www-odp.tamu.edu/publications/tnotes/tn30/tn30_f5.htm
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Elemental analysis Combustion CHNX analysis http://www.chemistryland.com/CHM151S/03-Counting/ElementalAnalysis/ElementalAnalysis.htm
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http://facstaff.gpc.edu/~mkim/C1211&1212Lec/C1211_Lecture.htm
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http://www.weiku.com/products/10367454/Automatic_Carbon_Hydrogen_Nitrogen_Analyzer_SDCH235.html
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Elemental Analyzer (EA) The elemental analyzer is for routine analysis of organic samples for δ15/14N, δ13/12C, %N, and % C. A sample is combusted in an Oxygen stream at 1100C,then passed through oxidation and reductio n tubes to form CO2 and N2 gas. The peaks are separated on a chromatography column allowing bot h C and N isotope composition to be determined on a single sample. The precision is better than 0.2 f or C and 0.4 for N. The disadvantage of the elemental analyzer is that it is not as precise as the dual i nlet. The advantages are that sample prep is much easier, many more samples can be analyzed per da y, and δ15/14N, δ13/12C, %N, and %C are measured on each sample. http://www.uark.edu/ua/isotope/equipment.php
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http://cool.conservation-us.org/jaic/articles/jaic33-02-008.html http://www.rsic.iitb.ac.in/Chn.html
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GC-MS Combination of GC and MS http://en.wikipedia.org/wiki/Gas_chromatography%E2%80%93mass_spectrometry
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http://academics.wellesley.edu/Chemistry/chem211lab/Orgo_Lab_Manual/Appendix/Appendix/Instruments/GCMS/gcms.html
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http://blog.restek.com/wp-content/uploads/2011/03/chromatogram-fig21.jpg
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www.avivanalytical.com
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SIRMS Nowadays, combined w/ EA, Laser, GC, etc http://inside.mines.edu/~jhumphre/Isotope_Lab.html
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http://www.gwadi.org/tools/tracers/methods
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Others IR NMR ESR XRD UV etc.
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