Name: preparation of authigenic pyrite from methane-bearing sediments for in situ sulfur isotope analysis using sims
Uploaded: 2017-08-31T12:30:00
Description: Watch this Scientific Journal Video about Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS at JoVE.com

Denne forskningen i fellesskap ble finansiert og støttet av Natural Science Foundation of China (nei 91128101, 41273054 og 41373007), Kina geologiske undersøkelse prosjektet for Sørkinahavet gass hydrat ressurs leting (nr. DD20160211), grunnleggende forskning midler til sentral universitetene (nr. 16lgjc11) og Guangdong provinsen universiteter og høyskoler Perleflodens Scholar finansiert ordningen (nr 2011). Zhiyong Lin erkjenner økonomisk støtte fra Kina stipend rådet (nr. 201506380046). Yang Lu Takk Guangzhou Elite prosjektet (nr. JY201223) og Kina postdoktor Science Foundation (nr 2016 M 592565). Vi er takknemlige til Dr. Shengxiong Yang, Guangxue Zhang og Dr. Jinqiang Liang av Guangzhou Marine geologiske undersøkelse for prøver og verdifulle forslag. Vi takker Dr. Xianhua Li og Dr. Lei Chen Institutt for geologi og geofysikk Beijing kinesiske vitenskapsakademi, for hjelp med SIMS analyse. Dr. Xiaoping Xia er takket for gjør tilgjengelig SIMS laboratoriet av Guangzhou Institute av Geokjemi, kinesiske vitenskapsakademi, til innspillingen av denne artikkelen. Manuskriptet nytte kommentarer fra Dr. Alisha Dsouza, gjennomgå redaktør av JoVE og to anonyme dommere.

1. innsamling av prøver fra en Sediment Merk: kjernen HS148 ble Hentet fra et nettsted nær gass hydrat boring sone i området Shenhu Sør-Kinahavet, cruise av R/V Haiyang Sihao i 2006.
<ol><li>Kutt stempelet kjernen (her, HS148) i seksjoner i intervaller på 0,7 m fra toppen til bunnen (ombord fartøyet) og overføre delene til et kaldt rom (4 ° C) for lagring etter henting.</li>
	<li>Overføre delene kjernen til et kaldt rom (4 ° C) i land-baserte laboratoriet lagring etter cruise. Ta...

<ol>
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G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+global+importance+and+context+of+methane+escape+from+the+seabed.">The global importance and context of methane escape from the seabed.</a> Geo-Mar Lett. 23 (3), 147-154 (2003).</li><li>Suess, E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Marine+cold+seeps+and+their+manifestations:+geological+control,+biogeochemical+criteria+and+environmental+conditions.">Marine cold seeps and their manifestations: geological control, biogeochemical criteria and environmental conditions.</a> Int J Earth Sci. 103 (7), 1889-1916 (2014).</li><li>Boetius, A., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+marine+microbial+consortium+apparently+mediating+anaerobic+oxidation+of+methane.">A marine microbial consortium apparently mediating anaerobic oxidation of methane.</a> Nature. 407 (6804), 623-626 (2000).</li><li>Orphan, V. 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Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=How+sulfate-driven+anaerobic+oxidation+of+methane+affects+the+sulfur+isotopic+composition+of+pyrite:+A+SIMS+study+from+the+South+China+Sea.">How sulfate-driven anaerobic oxidation of methane affects the sulfur isotopic composition of pyrite: A SIMS study from the South China Sea.</a> Chem Geol. 440, 26-41 (2016).</li><li>J&#248;rgensen, B. B., B&#246;ttcher, M. E., L&#252;schen, H., Neretin, L. N., Volkov, I. I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Anaerobic+methane+oxidation+and+a+deep+H2S+sink+generate+isotopically+heavy+sulfides+in+Black+Sea+sediments.">Anaerobic methane oxidation and a deep H2S sink generate isotopically heavy sulfides in Black Sea sediments.</a> Geochim Cosmochim Ac. 68 (9), 2095-2118 (2004).</li><li>Borowski, W. S., Rodriguez, N. M., Paull, C. K., Ussler, III, W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Are+34S-enriched+authigenic+sulfide+minerals+a+proxy+for+elevated+methane+flux+and+gas+hydrates+in+the+geologic+record?.">Are 34S-enriched authigenic sulfide minerals a proxy for elevated methane flux and gas hydrates in the geologic record?.</a> Mar Petrol Geol. 43, 381-395 (2013).</li><li>Canfield, D. E. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Isotope+fractionation+by+natural+populations+of+sulfate-reducing+bacteria.">Isotope fractionation by natural populations of sulfate-reducing bacteria.</a> Geochim Cosmochim Ac. 65 (7), 1117-1124 (2001).</li><li>McKibben, M. A., Eldridge, C. S. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Micron-scale+isotopic+zoning+in+minerals;+a+record+of+large-scale+geologic+processes.">Micron-scale isotopic zoning in minerals; a record of large-scale geologic processes.</a> Mineral Mag. 58A, 587-588 (1994).</li><li>Peevler, J., Fayek, M., Misra, K. C., Riciputi, L. 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R., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Charge-mode+electrometer+measurements+of+S-isotopic+compositions+on+SHRIMP-SI.">Charge-mode electrometer measurements of S-isotopic compositions on SHRIMP-SI.</a> Int J Mass Spectrom. 359, 26-37 (2014).</li><li>Pimminger, A., Grasserbauer, M., Schroll, E., Cerny, I. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microanalysis+in+galena+by+Secondary+Ion+Mass+Spectrometry+for+determination+of+sulfur+isotopes.">Microanalysis in galena by Secondary Ion Mass Spectrometry for determination of sulfur isotopes.</a> Anal Chem. 56 (3), 407-411 (1984).</li><li>Eldridge, C. S., Compston, W., Williams, I. S., Walshe, J. L., Both, R. A. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+microanalysis+for+34S/32S+ratios+using+the+ion+microprobe+SHRIMP.">In situ microanalysis for 34S/32S ratios using the ion microprobe SHRIMP.</a> Int J Mass Spectrom Ion Processes. 76 (1), 65-83 (1987).</li><li>Kozdon, R., Kita, N. T., Huberty, J. M., Fournelle, J. H., Johnson, C. A., Valley, J. W. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+sulfur+isotope+analysis+of+sulfide+minerals+by+SIMS:+precision+and+accuracy,+with+application+to+thermometry+of+3.5+Ga+Pilbara+cherts.">In situ sulfur isotope analysis of sulfide minerals by SIMS: precision and accuracy, with application to thermometry of 3.5 Ga Pilbara cherts.</a> Chem Geol. 275 (3-4), 243-253 (2010).</li><li>Farquhar, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pathways+for+Neoarchean+pyrite+formation+constrained+by+mass-independent+sulfur+isotopes.">Pathways for Neoarchean pyrite formation constrained by mass-independent sulfur isotopes.</a> Proc Natl Acad Sci USA. 110 (44), 17638-17643 (2013).</li><li>Whitehouse, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Multiple+sulfur+isotope+determination+by+SIMS:+evaluation+of+reference+sulfides+for+&#916;33S+with+observations+and+a+case+study+on+the+determination+of+&#916;36S.">Multiple sulfur isotope determination by SIMS: evaluation of reference sulfides for &#916;33S with observations and a case study on the determination of &#916;36S.</a> Geostand Geoanal Res. 37 (1), 19-33 (2013).</li><li>Chen, L., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Extreme+variation+of+sulfur+isotopic+compositions+in+pyrite+from+the+Qiuling+sediment-hosted+gold+deposit,+West+Qinling+orogen,+central+China:+an+in+situ+SIMS+study+with+implications+for+the+source+of+sulfur.">Extreme variation of sulfur isotopic compositions in pyrite from the Qiuling sediment-hosted gold deposit, West Qinling orogen, central China: an in situ SIMS study with implications for the source of sulfur.</a> Miner Depos. 50 (6), 643-656 (2015).</li><li>LaFlamme, C., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=In+situ+multiple+sulfur+isotope+analysis+by+SIMS+of+pyrite,+chalcopyrite,+pyrrhotite,+and+pentlandite+to+refine+magmatic+ore+genetic+models.">In situ multiple sulfur isotope analysis by SIMS of pyrite, chalcopyrite, pyrrhotite, and pentlandite to refine magmatic ore genetic models.</a> Chem Geol. 444, 1-15 (2016).</li><li>Peckmann, J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Methane-derived+carbonates+and+authigenic+pyrite+from+the+northwestern+Black+Sea.">Methane-derived carbonates and authigenic pyrite from the northwestern Black Sea.</a> Mar Geol. 177 (1-2), 129-150 (2001).</li><li>Zhang, M., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Morphology+and+formation+mechanism+of+pyrite+induced+by+the+anaerobic+oxidation+of+methane+from+the+continental+slope+of+the+NE+South+China+Sea.">Morphology and formation mechanism of pyrite induced by the anaerobic oxidation of methane from the continental slope of the NE South China Sea.</a> J Asian Earth Sci. 92, 293-301 (2014).</li><li>Lin, Z. Y., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Stable+isotope+patterns+of+coexisting+pyrite+and+gypsum+indicating+variable+methane+flow+at+a+seep+site+of+the+Shenhu+area,+South+China+Sea.">Stable isotope patterns of coexisting pyrite and gypsum indicating variable methane flow at a seep site of the Shenhu area, South China Sea.</a> J Asian Earth Sci. 123, 213-223 (2016).</li><li>Virtaslo, J. J., et al. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Pyritic+and+baritic+burrows+and+microbial+filaments+in+postglacial+lacustrine+clays+in+the+northern+Baltic+Sea.">Pyritic and baritic burrows and microbial filaments in postglacial lacustrine clays in the northern Baltic Sea.</a> J Geol Soc London. 167 (6), 1185-1198 (2010).</li><li>Kohn, M. J., Riciputi, L. R., Stakes, D., Orange, D. 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Svovel isotop analyse av svovelkis kan er en nyttig tilnærming og identifisere biogeochemical prosesser som påvirker pyritization. Men hvis bulk svovel isotop analyse, representerer innhentet svovel isotop signaturer vanligvis blandede signaler, som sedimentære svovelkis aggregater består vanligvis av flere tett interfingering generasjoner. Her presenterer vi en metode (dvs. SIMS analyse) for å analysere den i situ svovel isotopanrikning komposisjoner av ulike svovelkis generasjoner på mikro-skala...

Utslipp av metan fra sedimenter er vanlige langs kontinental margene1,2. Men de fleste av metan i områder av diffusive seepage er oksidert på bekostning av sulfat i sedimenter, en prosess som kalles SO4- AOM (formel 1)3,4. Produksjon av sulfide under denne prosessen resulterer vanligvis i nedbør av svovelkis. Også kjører OSR også dannelsen av svovelkis ved å slippe sulfide (ligning 2)5.
CH4 + så42- → HS- + HCO3- + H2O (1)
2 kanalar2O + så42- → H2S + 2HCO3- (2)
Det er funnet at authigenic sulfide i sulfat-metan overgang sone (SMTZ) avslører høy ses34S verdier, som ble foreslått å være forårsaket av forbedret SO4- AOM i områder seepage6,7, 8. Derimot viser svovelkis indusert av OSR vanligvis lavere ses34S verdiene9. Men det er utfordrende for å identifisere ulike svovelkis generasjoner av prosessene (dvs. OSR og SO4- AOM) hvis bare en bulk svovel isotop måling brukes, siden den suksessivt dannet interfingering svovelkis generasjoner kjennetegnes ved forskjellige isotopanrikning komposisjoner. Mikroskala i situ svovel isotop analyse er derfor nødvendig å forbedre vår forståelse av selve mineralizing prosesser10,11,12. Som en allsidig teknikk for i situ isotop analyse krever SIMS bare noen nanograms av prøven, som førte sin betegnelse som en ikke-ødeleggende teknikk. En primær ion bjelke sputters målet, forårsaker utslipp av sekundær ioner som blir deretter transportert til en masse spectrometer for måling av13. I en tidlig i situ svovel isotop analyse av SIMS, Pimminger et al. ble analysert ses34S verdiene i galena ved hjelp av 10-30 µm-diameter stråle14. Denne tilnærmingen har blitt stadig mer brukt til microanalysis av svovel isotopanrikning komposisjoner i sulfides, med betydelige forbedringer i både måling presisjon og oppløsning11,12,13 , 14 , 15 , 16 , 17 , 18 , 19 , 20. svovelkis med ulike morfologiske attributter og distinkte svovel stabil isotop mønstre er rapportert fra sive og ikke-sive miljøer21,22,23,24. Imidlertid til best av vår kunnskap, før vår siste SIMS studie6, bare én studie brukt den i situ svovel isotop analyse av svovelkis fra sive miljøer og viste stor svovel isotop variasjon i biogene svovelkis25.
I denne studien brukt vi SIMS å analysere ses34S verdiene av ulike generasjoner av authigenic svovelkis fra en seepage området i Sør-Kinahavet, som tillot Mikroskala diskriminering av OSR- og SO4- AOM-avledet svovelkis.

<table border="0" cellpadding="0" cellspacing="0" width="835">
	<tbody>
		<tr height="21">
			<td height="21" style="height:21px;width:363px;">secondary ion mass spectroscopy</td>
			<td style="width:128px;">Cameca</td>
			<td style="width:179px;">&#160;IMS-1280</td>
			<td style="width:167px;"></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">&#160;thermal field emission scanning electron microscopy</td>
			<td>Quanta</td>
			<td>Quanta 400F</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">elemental analyser - isotope ratio mass spectrometry</td>
			<td>ThermoFinnigan</td>
			<td colspan="2">ThermoFinnigan Delta Plus</td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">binocular microscope</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">reflected light microscope</td>
			<td>Carl Zeiss</td>
			<td>3519001617</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">polishing machicine</td>
			<td>Struers</td>
			<td>60210535</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">cutting machicine</td>
			<td>Struers</td>
			<td>50110202</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">carbon/gold coating machicine</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">ethanol</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">acetic acid&#160;</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">zinc acetate solution (3%)&#160;&#160;&#160;</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">HCl solution (25%)</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">1 M CrCl2 solution</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">0.1 M AgNO3 solution</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="25">
			<td height="25" style="height:25px;">V2O5 powder</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">pure nitrogen</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">syringe</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">filter(&#60;0.45 &#181;m)</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">tin cups</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">round bottom flasks</td>
			<td>any</td>
			<td>NA</td>
			<td></td>
		</tr>
		<tr height="21">
			<td height="21" style="height:21px;">epoxy</td>
			<td>Struers</td>
			<td>41000004</td>
			<td></td>
		</tr>
	</tbody>
</table>

preparation of authigenic pyrite from methane-bearing sediments for in situ sulfur isotope analysis using sims

Forskjellige svovel isotop komposisjoner av authigenic svovelkis vanligvis skyldes sulfat-drevet anaerob oksidasjon av metan (SO4- AOM) og organiclastic sulfate reduksjon (OSR) i marine sedimenter. Men er rakne den komplekse pyritization sekvensen en utfordring på grunn av en sameksistens av ulike sekvensielt dannet svovelkis faser. Dette manuskriptet beskriver et eksempel forberedelse prosedyre som gjør bruk av sekundære ion masse spectroscopy (SIMS) å få i situ ses34S verdier av ulike svovelkis generasjoner. Dette gjør at forskere å begrense hvordan så4- AOM påvirker pyritization i metan-bærende sedimenter. SIMS analyse viste en ekstrem rekkevidde i ses34S verdier, som spenner fra-41.6 til + 114.8‰, som er mye større enn området ses34S verdier ved tradisjonelle bulk svovel isotop analyse av samme prøvene. Svovelkis i grunne sedimentet består hovedsakelig av 34S-utarmet framboids, foreslå tidlig diagenetic dannelsen av OSR. Dypere i sedimentet, mer svovelkis oppstår som overgrowths og euhedral krystaller, som viser mye høyere SIMS ses34S enn framboids. Slike 34S-beriket svovelkis gjelder forbedret SO4- AOM på sonen sulfat-metan overgangen postdating OSR. Høy oppløsning i situ SIMS svovel isotop analyser tillate for gjenoppbyggingen av pyritization prosesser, som ikke kan løses av bulk svovel isotop analyse.

Data uttrykk - Bulk svovel isotoper:
Bulk svovel isotop forholdet er uttrykt i forhold til den Wien Canyon Diablo Troilite (V-CDT) standard, og analytisk presisjon er bedre enn ±0.3‰. Svovel isotop målingene ble kalibrert med internasjonale referansemateriale: IAEA-S1 (ses34S = - 0.30‰), IAEA-S2 (ses34S = - 21.55‰), IAEA-S3 (ses34S = - 31.4‰), og NBS 127 (ses34S = 20.30‰). ...

Watch this Scientific Journal Video about Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS at JoVE.com

Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS

Analyser av svovel isotopanrikning sammensetningen (ses34S) av svovelkis fra metan-bærende sedimenter har vanligvis fokusert på bulk prøver. Her brukt vi sekundære ion masse spectroscopy å analysere ses34S verdiene av ulike svovelkis generasjoner å forstå diagenetic historien til pyritization.

Utarbeidelse av Authigenic svovelkis fra metan-bærende sedimenter for In Situ svovel isotop analyse ved hjelp av SIMS

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and ...

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Preparation of Authigenic Pyrite from Methane-bearing Sediments for In Situ Sulfur Isotope Analysis Using SIMS

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