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 forskning er i fællesskab finansieret og støttet af den Natural Science Foundation of China (Nej 91128101, 41273054 og 41373007), Kina geologiske undersøgelse projekt for Sydkinesiske Hav Gas hydrat ressource udforskning (nr. DD20160211), grundforskning midler til Central universiteter (nr. 16lgjc11), og Guangdong provinsen universiteter og Colleges Pearl River Scholar finansieret ordning (nr. 2011). Zhiyong Lin anerkender den finansielle støtte fra Kina stipendium Rådet (nr. 201506380046). Yang Lu tak Guangzhou Elite projekt (nr. JY201223) og Kina postdoc Science Foundation (nr. 2016 M 592565). Vi er taknemmelige for Dr. Shengxiong Yang, Guangxue Zhang og Dr. Jinqiang Liang af Guangzhou Marine Geological Survey for at give prøver og værdifulde forslag. Vi takker Dr. Xianhua Li og Dr. Lei Chen fra Instituttet for geologi og geofysik (Beijing), kinesiske Academy of Sciences, hjælp til SIMS analyse. Dr. Xiaoping Xia er takkede for tilrådighedsstillelse SIMS Lab af Geokemi Guangzhou-Institut, kinesiske Academy of Sciences, til optagelserne af denne artikel. Håndskriftet har nydt godt af kommentarer fra Dr. Alisha Dsouza, anmeld redaktør af JoVE og to anonyme dommere.

1. indsamling af prøver fra et Sediment Core Bemærk: core HS148 blev indhentet fra et sted i nærheden af gas hydrat boring zone i området Shenhu, Sydkinesiske Hav, under en sejltur med R/V Haiyang Sihao i 2006.
<ol><li>Cut stempel core (her, HS148) i sektioner med mellemrum på 0,7 m fra toppen til bunden (ombord skibet) og overføre sektionerne til et koldt rum (4 ° C) til opbevaring efter hentning.</li>
	<li>Overføre core sektioner til et koldt rum (4 ° C) i land-baserede lab til ...

<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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Svovl isotop analyser af Pyrit er en nyttig tilgang og kan hjælpe med at identificere de biogeokemiske processer, der påvirker pyritization. Men hvis bulk svovl isotop analyser anvendes, opnåede svovl isotop signaturer almindeligt repræsenterer blandede signaler, som sedimentære pyrit aggregater typisk består af flere nøje interfingering generationer. Her præsenterer vi en metode (dvs. SIMS analyse) til at analysere i situ svovl isotopiske kompositioner af forskellige pyrit generationer på mikr...

Methanemissionerne fra sedimenter er fælles langs kontinentale margener1,2. Men de fleste af metan i områder af diffuserende nedsivning oxideres på bekostning af sulfat i sedimenter, en proces kendt som SO4- AOM (ligning 1)3,4. Produktionen af sulfid i denne proces medfører almindeligvis udfældning af pyrit. Også, OSR også drev dannelsen af pyrit ved at frigive sulfid (ligning 2)5.
CH4 + så42 – → HS- + HCO3- + H2O (1)
2ch2O + så42 – → H2S + 2HCO3- (2)
Man fandt at authigenic sulfid i sulfat-methan overgang zone (SMTZ) afslører høj δ34S værdier, som blev foreslået at være forårsaget af forbedrede SO4- AOM i områder af nedsivning6,7, 8. Derimod viser pyrit induceret af OSR almindeligt lavere δ34S værdier9. Men det er udfordrende for at identificere forskellige pyrit generationer induceret af disse processer (dvs., OSR og SO4- AOM) Hvis der kun en bulk svovl isotop måling anvendes, da den successivt dannede interfingering pyrit generationer er karakteriseret ved forskellige isotopiske kompositioner. Derfor er individuel i situ svovl isotop analyser nødvendige for at forbedre vores forståelse af den faktiske mineralizing processer10,11,12. Som en alsidig teknik til i situ isotop analyser kræver SIMS kun et par nanogram af prøven, som udløste dens betegnelse som en ikke-destruktiv teknik. En primær ion stråle sputters mål, forårsager emission af sekundære ioner, der transporteres derefter til et massespektrometer til måling af13. I en tidlig i situ svovl stråle isotop analyser anvendelse af SIMS, Pimminger et al. held analyseret δ34S værdier i galena ved hjælp af en 10-30 µm-diameter14. Denne tilgang er blevet i stigende grad anvendt til mikroanalyser af svovl isotopiske kompositioner i sulfider, med betydelige forbedringer i begge måling præcision og opløsning11,12,13 , 14 , 15 , 16 , 17 , 18 , 19 , 20. pyrit med forskellige morfologiske attributter og særskilte svovl stabil isotop mønstre er blevet rapporteret fra sive og ikke-sive miljøer21,22,23,24. Men til bedst af vores viden, før vores seneste SIMS undersøgelse6, kun én undersøgelse anvendes i situ svovl isotop analyser af pyrit fra sive miljøer og afslørede store svovl isotop variabilitet i biogene pyrit25.
I denne undersøgelse anvendte vi SIMS til at analysere δ34S værdier af forskellige generationer af authigenic pyrit fra en nedsivning websted i det Sydkinesiske Hav, hvilket gav mulighed for individuel forskelsbehandling af OSR- og SO4- AOM-afledte pyrit.

<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

Forskellige svovl isotop kompositioner af authigenic pyrit typisk skyldes sulfat-drevet anaerob iltning af methan (SO4- AOM) og organiclastic sulfat reduktion (OSR) i marine sedimenter. Men optrævling den komplekse pyritization sekvens er en udfordring på grund af sameksistensen af forskellige sekventielt dannede pyrit faser. Dette manuskript beskriver et eksempel forberedelse procedure, der giver mulighed for brug af sekundære ion masse spektroskopi (SIMS) at få i situ δ34S værdier af forskellige pyrit generationer. Dette gør det muligt for forskere at begrænse hvordan så4- AOM påvirker pyritization i methan-bærende sedimenter. SIMS analyse afslørede en ekstrem rækkevidde i δ34S værdier, der spænder fra-41.6 til + 114.8‰, som er meget bredere end δ34S værdiområdet fremstillet ved traditionelle bulk svovl isotop analyser af de samme prøver. Pyrit i den lavvandede sedimenter består hovedsageligt af 34S-forarmet framboids, hvilket tyder på tidlig diagenetic dannelsen af OSR. Dybere i sedimentet, flere pyrit opstår som overgrowths og euhedral krystaller, der viser meget højere SIMS δ34S værdier end framboids. Sådanne 34S-beriget Pyrit er relateret til øget SO4- AOM på overgangszone sulfat-methan postdating OSR. Høj opløsning i situ SIMS svovl isotop analyser giver mulighed for genopbygningen af pyritization processer, som ikke kan løses af bulk svovl isotop analyser.

Data udtryk - Bulk svovl isotoper:
Bulk svovl isotopforhold er udtrykt i forhold til den Wien Canyon Diablo jernsulfid (V-CDT) standard, og den analytiske præcision er bedre end ±0.3‰. Svovl isotop målinger blev kalibreret med internationale referencematerialer: IAEA-S1 (δ34S = - 0.30‰), IAEA-S2 (δ34S = - 21.55‰), IAEA-S3 (δ34S = - 31.4‰), og NBS 127 (δ34S = 20.30‰). 
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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 af svovl-isotopsammensætning (δ34S) af pyrit fra metan-bærende sedimenter har typisk fokus på bulk prøver. Her, anvendte vi sekundære ion masse spektroskopi til at analysere δ34S værdier af forskellige pyrit generationer til at forstå pyritization diagenetic historie.

Forberedelse af Authigenic pyrit fra metan-bærende sedimenter for In Situ svovl isotop analyser ved hjælp af 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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