Name: measurement of h2s in crude oil and crude oil headspace using multidimensional gas chromatography, deans switching and sulfur-selective detection
Uploaded: 2015-12-10T15:00:00.000+00:00
Duration: 8 min 37 s
Description: Watch this Scientific Journal Video about Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection at JoVE.com

The authors would like to acknowledge support from the Government of Canada's interdepartmental Program of Energy Research and Development, PERD 113, Petroleum Conversion for Cleaner Air. N.E.H would like to acknowledge her Natural Sciences and Engineering Research Council of Canada Visiting Fellowship.

<ol>
	<li>Guidotti, T. L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Hydrogen+sulphide.">Hydrogen sulphide.</a> Occ. Med. 46, 367-371 (1996).</li><li>Reiffenstein, R. J., Hulbert, W. C., Roth, S. H. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Toxicology+of+Hydrogen+Sulfide.">Toxicology of Hydrogen Sulfide.</a> Annu. Rev. Pharmacol. Toxicol. , 109-134 (1992).</li><li>Qi, 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=Effect+of+Temperature+on+the+Corrosion+Behavior+of+Carbon+Steel+in+Hydrogen+Sulphide+Environments.">Effect of Temperature on the Corrosion Behavior of Carbon Steel in Hydrogen Sulphide Environments.</a> Int. J. Electrochem. Sci. 9, 2101-2112 (2014).</li><li>Ma, H., 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=The+influence+of+hydrogen+sulfide+on+corrosion+of+iron+under+different+conditions.">The influence of hydrogen sulfide on corrosion of iron under different conditions.</a> Corros. Sci. 42, 1669-1683 (2000).</li><li>Kallinikos, L. E., Jess, A., Papayannakos, N. G. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Kinetic+study+and+H2S+effect+on+refractory+DBTs+desulfurization+in+a+heavy+gasoil.">Kinetic study and H2S effect on refractory DBTs desulfurization in a heavy gasoil.</a> J. Catal. 269, 169-178 (2010).</li><li>Liu, B., 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=Kinetic+investigation+of+the+effect+of+H2S+in+the+hydrodesulfurization+of+FCC+gasoline.">Kinetic investigation of the effect of H2S in the hydrodesulfurization of FCC gasoline.</a> Fuel. 123, 43-51 (2014).</li><li>Si, X., Xia, D., Xiang, Y., Zhou, Y. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Effect+of+H2S+on+the+transformation+of+1-hexene+over+NiMoS/&#947;-Al2O3+with+hydrogen.">Effect of H2S on the transformation of 1-hexene over NiMoS/&#947;-Al2O3 with hydrogen.</a> J. Nat. Gas Chem. 19, 185-188 (2010).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Hydrogen Sulfide and Mercaptan Sulfur in Liquid Hydrocarbons by Potentiometric Titration. , UOP 163-10 (2010).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Standard Test Method for Determination of Hydrogen Sulfide in Fuel Oils by Rapid Liquid Phase Extraction. , ASTM D7621-10 (2010).</li><li>Lywood, W. G., Murray, D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> H2S in Crude Measurement Report. , (2012).</li><li>. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Standard Test Method for Sulfur Compounds in Light Petroleum Liquids by Gas Chromatography and Sulfur Selective Detection. , ASTM D7621-10 (2009).</li><li>Liu, W., Morales, M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=.">.</a> Detection of Sulfur Compounds According to ASTM D5623 in Gasoline with Agilent's Dual Plasma Sulfur Chemiluminescence Detector (G6603A) and an Agilent 7890A Gas Chromatograph. , (2008).</li><li>Barman, B. N., Cebolla, V. L., Membrado, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Chromatographic+Techniques+for+Petroleum+and+Related+Products.">Chromatographic Techniques for Petroleum and Related Products.</a> Crit. Rev. Anal. Chem. 30, 75-120 (2000).</li><li>Rodgers, R. P., McKenna, A. M. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Petroleum+Analysis.">Petroleum Analysis.</a> Anal. Chem. 83, 4665-4687 (2011).</li><li>Nizio, K. D., McGinitie, T. M., Harynuk, J. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Comprehensive+multidimensional+separations+for+the+analysis+of+petroleum.">Comprehensive multidimensional separations for the analysis of petroleum.</a> J. Chromatogr. A. 1255, 12-23 (2012).</li><li>Luong, J., Gras, R., Shellie, R. A., Cortes, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Tandem+sulfur+chemiluminescence+and+flame+ionization+detection+with+planar+microfluidic+devices+for+the+characterization+of+sulfur+compounds+in+hydrocarbon+matrices.">Tandem sulfur chemiluminescence and flame ionization detection with planar microfluidic devices for the characterization of sulfur compounds in hydrocarbon matrices.</a> J. Chromatogr. A. 1297, 231-235 (2013).</li><li>Di Sanzo, F. P., Bray, W., Chawla, B. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Determination+of+the+Sulfur+Components+of+Gasoline+Streams+by+Capillary+Column+Gas+Chromatography+with+Sulfur+Chemiluminescence+Detection.">Determination of the Sulfur Components of Gasoline Streams by Capillary Column Gas Chromatography with Sulfur Chemiluminescence Detection.</a> J. High Res. Chromatog. 17, 255-258 (1994).</li><li>Deans, D. R. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=A+new+technique+for+heart+cutting+in+gas+chromatography.">A new technique for heart cutting in gas chromatography.</a> Chromatographia. 1, 18-22 (1968).</li><li>Hinshaw, J. V. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Valves+for+Gas+Chromatography,+Part+III:+Fluidic+Switching+Applications.">Valves for Gas Chromatography, Part III: Fluidic Switching Applications.</a> LC GC N. Am. 29, 988-994 (2011).</li><li>Seeley, J. V., Micyus, N. J., Bandurski, S. V., Seeley, S. K., McCurry, J. D. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Microfluidic+Deans+Switch+for+Comprehensive+Two-Dimensional+Gas+Chromatography.">Microfluidic Deans Switch for Comprehensive Two-Dimensional Gas Chromatography.</a> Anal. Chem. 79, 1840-1847 (2007).</li><li>Tranchida, P. Q., Sciarrone, D., Dugo, P., Mondello, L. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Heart-cutting+multidimensional+gas+chromatography:+A+review+of+recent+evolution,+applications,+and+future+prospects.">Heart-cutting multidimensional gas chromatography: A review of recent evolution, applications, and future prospects.</a> Anal. Chim. Acta. 716, 66-75 (2012).</li><li>Armstrong, D. W., Reid, G. L., Luong, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Gas+Separations:+A+Comparison+of+GasPro&#8482;+and+Aluminum+Oxide+PLOT+Columns+for+the+Separation+of+Highly+Volatile+Compounds.">Gas Separations: A Comparison of GasPro&#8482; and Aluminum Oxide PLOT Columns for the Separation of Highly Volatile Compounds.</a> Curr. Sep. 15, 5-11 (1996).</li><li>Ellis, J., Vickers, A. K., George, C. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Capillary+Column+Selectivity+and+Inertness+for+Sulfur+Gas+Analysis+in+Light+Hydrocarbon+Streams+by+Gas+Chromatography.">Capillary Column Selectivity and Inertness for Sulfur Gas Analysis in Light Hydrocarbon Streams by Gas Chromatography.</a> Fuel Chemistry Division Preprints. 47, 703-704 (2002).</li><li>Ji, Z., Majors, R. E., Guthrie, E. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Porous+layer+open-tubular+capillary+columns:+preparations,+applications+and+future+directions.">Porous layer open-tubular capillary columns: preparations, applications and future directions.</a> J. Chromatogr. A. 842, 115-142 (1999).</li><li>Luong, J., Gras, R., Shellie, R. A., Cortes, H. J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Applications+of+planar+microfluidic+devices+and+gas+chromatography+for+complex+problem+solving.">Applications of planar microfluidic devices and gas chromatography for complex problem solving.</a> J. Sep. Sci. 36, 182-191 (2013).</li><li>Hildmann, F., Kempe, G., Speer, K. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Application+of+the+precolumn+back-flush+technology+in+pesticide+residue+analysis:+A+practical+view.">Application of the precolumn back-flush technology in pesticide residue analysis: A practical view.</a> J. Sep. Sci. 36, 2128-2135 (2013).</li><li>Gray, B. P., Teale, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=The+use+of+a+simple+backflush+technology+to+improve+sample+throughput+and+system+robustness+in+routine+gas+chromatography+tandem+mass+spectrometry+analysis+of+doping+control+samples.">The use of a simple backflush technology to improve sample throughput and system robustness in routine gas chromatography tandem mass spectrometry analysis of doping control samples.</a> J. Chromatogr. A. 1217, 4749-4752 (2010).</li><li>Hayward, T., Gras, R., Luong, J. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Characterization+of+selected+oxidation+inhibitors+in+transformer+oils+by+multidimensional+gas+chromatography+with+capillary+flow+technology.">Characterization of selected oxidation inhibitors in transformer oils by multidimensional gas chromatography with capillary flow technology.</a> Anal. Methods. 6, 8136-8140 (2014).</li><li>Hutte, R. S., Johansen, N. G., Legier, M. F. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Column+Selection+and+Optimization+for+Sulfur+Compound+Analyses+by+Gas+Chromatography.">Column Selection and Optimization for Sulfur Compound Analyses by Gas Chromatography.</a> J. High Res. Chromatog. 13, 421-426 (1990).</li><li>Yan, X. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Unique+selective+detectors+for+gas+chromatography:+Nitrogen+and+sulfur+chemiluminescence+detectors.">Unique selective detectors for gas chromatography: Nitrogen and sulfur chemiluminescence detectors.</a> J. Sep. Sci. 29, 1931-1945 (2006).</li><li>Araujo, P. <a target="_blank" href="http://www.ncbi.nlm.nih.gov/entrez/query.fcgi?db=PubMed&cmd=Search&doptcmdl=Citation&defaultField=Title+Word&term=Key+aspects+of+analytical+method+validation+and+linearity+evaluation.">Key aspects of analytical method validation and linearity evaluation.</a> J. Chromatogr. B. 877, 2224-2234 (2009).</li></ol>

The authors have nothing to disclose.

من أجل تحقيق القياس الأمثل لH 2 S، وهذا الأسلوب يستخدم مفتاح عمداء، backflushing وكشف عن التوهج الكبريت (SCD). ويستخدم العمود dimethylpolysiloxane كأول عمود البعد GC، ويعمل على إعاقة حركة الهيدروكربونات الأثقل الموجودة في العينة بحيث لا تلوث العمود المؤامرة. ومما يعزز هذا التأثير ...

تحليل دقيق للنفط الخام أمر ضروري لصناعة النفط والغاز، والأنظمة واقتصاديات الصحة والسلامة هي وظائف ذات نوعية النفط. من أجل حماية نقل العينات الخام، فمن الضروري تحديد خصائص العينات الخام لتطوير أنظمة السلامة لتنفيذها في حال إطلاق سراح المتهم أو التسرب. على وجه الخصوص، وتحديد حجم كبريتيد الهيدروجين (H 2 S) هو المهم، نظرا لسميته العالية في الطور الغازي. التعرض منخفضة تصل إلى 100 ​​جزء في المليون يمكن أن تكون قاتلة (http://www.cdc.gov/niosh/idlh/7783064.html) 1،2. ويعتبر المنحل H 2 S في عينات الخام عموما أن يكون تآكل 3،4، ويمكن تنشيط المواد الحفازة المستخدمة لعلاج النفط 5-7. إزالة H 2 S من تيارات النفط الخام مثالية، ولكن دون وسيلة لقياس المنحل H 2 S، فإنه من الصعب تقييم مدى نجاح العلاج لإزالة. لهذه الأسباب، وقد وضعت هذا البروتوكول لقياس dissolved H 2 S في عينات النفط الخام الثقيلة مثل الرمال النفطية الكندية خامات. ويوجد عدد من الطرق القياسية لتقدير حجم H 2 S في عينات البترول أو الوقود استنادا أخف وزنا، ولكن لم يتم التحقق من صحة أي للاستخدام مع الخامات الثقيلة المستخرجة عادة من الرمال النفطية الكندية. يتم تحديد H 2 S والمركبتان باستخدام تقنية المعايرة التي كتبها العالمي للمنتجات النفط (UOP) طريقة 163 8، ولكن يعاني هذا الأسلوب من التحيز المستخدم التفسير الذي ينتج من القراءة اليدوية من منحنيات المعايرة. يستخدم معهد البترول (IP) طريقة 570 تخصص H 2 S محلل أن ارتفاع درجات الحرارة عينات زيت الوقود 9، ويستفيد من البساطة وقابلية، لكنه يفتقر الى الدقة مع عينات أثقل 10. الجمعية الأمريكية للاختبارات والمواد (ASTM) طريقة D5623 يستخدم اللوني للغاز (GC) مع التبريد المبردة والكبريت الكشف الانتقائي لقياس H 2 S في السوائل النفطية الخفيفة11،12. ويمكن تحسين هذا المعيار لاستخدام العازل المحيط وأيضا أن تطبق على النفط الخام الأثقل، لذلك كان يستخدم كأساس لبروتوكول مناقشتها هنا. GC هو أسلوب يستخدم بشكل كبير لتحليل عينات البترول. يتم تبخيرها العينات في مدخل الساخنة، ويحدث فصل في الطور الغازي. فصل الطور الغازي GC يجعل مثالية لتحليل H 2 S، كما تتحرر بسهولة من العينة السائلة أثناء التسخين في المدخل. طرق GC يمكن إنشاؤها خصيصا لعينات مختلفة، اعتمادا على برامج درجة الحرارة المستخدمة، والأعمدة تنفيذها، واستخدام اللوني متعدد الأبعاد 13-15. كان هناك عدد من التطورات الأخيرة لقياس H 2 S باستخدام GC. لونغ وآخرون أظهرت H 2 S وغيرها من قياس مركب الكبريت الخفيف في ضوء ونواتج التقطير باستخدام GC متعدد الأبعاد وعمداء التبديل، ولكن الطريقة لميتم تطبيقها على أثقل خامات 16. دي سانزو وآخرون. H كميا أيضا 2 S في البنزين باستخدام GC، إلا أنه أيضا لم يتم استخدامه على الخامات الثقيلة، ويتطلب تبريد 17 الفرعية المحيطة. طريقة عرض هنا يوضح قتا طويلا إنقاذ أكثر هذه الأساليب السابقة، مع فترة التحليل الكامل لمدة 5 دقائق، مقارنة ب 10 دقيقة (لونج) و 40 دقيقة (دي سانزو). للأسف، كان تنفيذ هذه الطرق في مختبرنا لمقارنة دقة يكن من الممكن بسبب المعدات والوقت القيود. GC متعدد الأبعاد يسمح للمستخدم لاستغلال الانتقائية من عمودين، بدلا من عمود واحد. في GC التقليدية، يحدث الانفصال على عمود واحد. في حالة GC متعدد الأبعاد، يتم فصل العينة على عمودين المختلفة، وتعزيز الفصل والانتقائية. مفتاح عمداء هو جهاز واحد يستخدم لتوظيف تكوين عمود ثنائي الأبعاد. يستخدم مفتاح صمام الخارجي لخيمةتدفق الغاز ط م من مدخل على التحول الى واحد من اثنين من الموانئ منفذ 18-20. النفايات السائلة من العمود الأول يمكن أن توجه في أي من الاتجاهين. في هذه الحالة، غازات الكبريت الخفيفة هي &quot;قطع القلب&quot; 21 من الفصل الأول إلى طبقة مسامية أنبوبي المفتوحة (مؤامرة) عمود الفصل الثانوي، وهو ما ثبت لتكون ممتازة لفصل H 2 S من غيره من غازات الكبريت الخفيف (http://www.chem.agilent.com/cag/cabu/pdf/gaspro.pdf) 22-24. ويستخدم للكشف عن التوهج الكبريت للكشف، وتوفير الانتقائية لمركبات الكبريت والقضاء على تدخل محتمل من أي الغازات الخفيفة الأخرى التي قد تم نقلها إلى العمود مؤامرة خلال قطع القلب. يتم الاحتفاظ الهيدروكربونات من العينة النفط الخام على عمود البعد الأول وتتم إزالة أثناء إجراء backflush. هذا يحمي العمود مؤامرة من أي تلوث 25-27. كما تم تنفيذ هذا النهج بنجاح لالشرجيسيس مثبطات أكسدة في زيوت المحولات 28. هنا، يتم توظيف طريقة GC ثنائي الأبعاد لتحليل وتقدير حجم المذاب H 2 S في عينات النفط الخام الثقيل. يتم عرض طريقة قابلة للتطبيق على نطاق واسع من H 2 S تركيزات، ويمكن أيضا أن تستخدم لقياس H 2 S في عينات المرحلة الغازية.

<table><tbody><tr><td>Deans switch</td><td>Agilent</td><td>G2855A</td><td>Or equivalent flow switching device</td></tr><tr><td>Restrictor tubing&amp;nbsp;</td><td>Agilent</td><td>160-2615-10</td><td>Fused silica, deactivated, 180 &amp;micro;m</td></tr><tr><td>HP-PONA column</td><td>Agilent</td><td>19091S-001</td><td></td></tr><tr><td>GasPro column</td><td>Agilent</td><td>113-4332</td><td></td></tr><tr><td>Sulfur chemiluminescence detector, 355</td><td>Agilent/Sievers</td><td>G6603A</td><td></td></tr><tr><td>H&lt;sub&gt;2&lt;/sub&gt;S calibration standard, in He</td><td>Air Liquide</td><td>Custom order</td><td>211 ppm H&lt;sub&gt;2&lt;/sub&gt;S</td></tr><tr><td>CS&lt;sub&gt;2&lt;/sub&gt;</td><td>Fisher Scientific</td><td>C184-500</td><td></td></tr><tr><td>Toluene, HPLC grade</td><td>Fisher Scientific</td><td>T290-4</td><td></td></tr><tr><td>Gas bag, 2 L</td><td>Calibrated Instruments, Inc.</td><td>GSB-P/2</td><td>Twist on/off nozzle</td></tr><tr><td>250 &amp;micro;l gas tight syringe</td><td>Hamilton</td><td>81130</td><td></td></tr><tr><td>500 ml amber glass bottle</td><td>Scientific Specialties</td><td>N73616</td><td></td></tr><tr><td>Open top screw caps</td><td>Scientific Specialties</td><td>169628</td><td></td></tr><tr><td>Tegrabond disc for screw caps</td><td>Chromatographic Specialties</td><td>C889125C</td><td>25 mm, 10/90 MIL</td></tr><tr><td>1 ml gas tight syringe</td><td>Hamilton</td><td>81330</td><td></td></tr><tr><td>2.5% H&lt;sub&gt;2&lt;/sub&gt;S in He gas standard</td><td>Air Liquide</td><td>Custom order</td><td></td></tr></tbody></table>

measurement of h2s in crude oil and crude oil headspace using multidimensional gas chromatography, deans switching and sulfur-selective detection

وهناك طريقة لتحليل كبريتيد الهيدروجين المذاب في عينات النفط الخام ويتجلى ذلك باستخدام الكروماتوغرافيا الغازية. من أجل القضاء على التدخل بفعالية، يستخدم تكوين العمود الأبعاد، مع التحول عمداء تستخدم لنقل كبريتيد الهيدروجين من الأول إلى العمود الثاني (قطع القلب). يتم فصل العينات الخام السائلة أولا على عمود dimethylpolysiloxane، والغازات الخفيفة وكذلك فصل على عمود المستعبدين طبقة مسامية أنبوبي المفتوحة (مؤامرة) التي هي قادرة على فصل كبريتيد الهيدروجين من الأنواع الخفيفة الأخرى الكبريت قطع القلب. ثم يتم الكشف عن كبريتيد الهيدروجين مع كاشف التوهج الكبريت، إضافة طبقة إضافية من الانتقائية. بعد الانفصال والكشف عن كبريتيد الهيدروجين، وbackflushed النظام لإزالة المواد الهيدروكربونية العالية الغليان الموجودة في العينات الخام والحفاظ على سلامة الكروماتوغرافي. تم كميا المنحل كبريتيد الهيدروجين في عينات السائل 1،1 حتي 500 صمساء، مما يدل على تطبيق واسع لمجموعة من العينات. طريقة كما تم تطبيقها بنجاح لتحليل عينات الغاز من أكياس فراغ الرأس النفط الخام والغاز العملية، مع قياس من 0.7 إلى 9700 جزء في المليون كبريتيد الهيدروجين.

من أجل الحصول على تقدير موثوق من H 2 S لعينات كلا السائل والغاز والمعايرة المناسبة أمر ضروري. لحقن المعايرة وحقن عينة، وS الذروة H 2 يجب أن لا تكون متداخلة مع القمم المجاورة وينبغي أن يكون منطقة ذروة استنساخه. ويبين الشكل 3 حقنة لعينة الغاز حيث الغاز ?...

Watch this Scientific Journal Video about Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection at JoVE.com

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

A multidimensional gas chromatography method for the analysis of dissolved hydrogen sulfide in liquid crude oil samples is presented. A Deans switch is used to heart-cut light sulfur gases for separation on a secondary column and detection on a sulfur chemiluminescence detector.

قياس H<sub&gt; 2</sub&gt; S في النفط الخام والنفط الخام فراغ الرأس عن طريق المتعددة الأبعاد الغاز اللوني، عمداء التبديل والكبريت انتقائية الكشف

A method for the analysis of dissolved hydrogen sulfide in crude oil samples is demonstrated using gas chromatography. In order to effectively eliminate ...

measurement-h2s-crude-oil-crude-oil-headspace-using-multidimensional

Research

JoVE Journal

Environment

Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

19.1K Views.  Natural Resources Canada. A multidimensional gas chromatography method for the analysis of dissolved hydrogen sulfide in liquid crude oil samples is presented. A Deans switch is used to heart-cut light sulfur gases for separation on a secondary column and detection on a sulfur chemiluminescence detector. 

Video: Measurement of H2S in Crude Oil and Crude Oil Headspace Using Multidimensional Gas Chromatography, Deans Switching and Sulfur-selective Detection

Quantitative Detection of Trace Explosive Vapors by Programmed Temperature Desorption Gas Chromatography-Electron Capture Detector

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive vapor samples. The direct liquid deposition method yields a higher fidelity between the analysis of vapor samples and the analysis of solution standards than using separate injection methods for vapors and solutions, i.e., samples collected on vapor collection tubes and standards prepared in solution vials. Additionally, the method can account for instrumentation losses, which makes it ideal for minimizing variability and quantitative trace chemical detection. Gas chromatography with an electron capture detector is an instrumentation configuration sensitive to nitro-energetics, such as TNT and RDX, due to their relatively high electron affinity. However, vapor quantitation of these compounds is difficult without viable vapor standards. Thus, we eliminate the requirement for vapor standards by combining the sensitivity of the instrumentation with a direct liquid deposition protocol to analyze trace explosive vapor samples.

Trace explosive vapors of TNT and RDX collected on sorbent-filled thermal desorption tubes were analyzed using a programmed temperature desorption system coupled to GC with an electron capture detector. The instrumental analysis is combined with direct liquid deposition method to reduce sample variability and account for instrumentation drift and losses.

الكشف عن كمية من المتفجرات عن طريق تتبع الأبخرة درجة الحرارة المبرمجة الامتزاز الغاز اللوني-الكترون التقاط الكاشف

The direct liquid deposition of solution standards onto sorbent-filled thermal desorption tubes is used for the quantitative analysis of trace explosive ...

Chemistry

Light-driven Enzymatic Decarboxylation

Oxidoreductases belong to the most-applied industrial enzymes. Nevertheless, they need external electrons whose supply is often costly and challenging. Recycling of the electron donors NADH or NADPH requires the use of additional enzymes and sacrificial substrates. Interestingly, several oxidoreductases accept hydrogen peroxide as electron donor. While being inexpensive, this reagent often reduces the stability of enzymes. A solution to this problem is the in situ generation of the cofactor. The continuous supply of the cofactor at low concentration drives the reaction without impairing enzyme stability. This paper demonstrates a method for the light-catalyzed in situ generation of hydrogen peroxide with the example of the heme-dependent fatty acid decarboxylase OleTJE. The fatty acid decarboxylase OleTJE was discovered due to its unique ability to produce long-chain 1-alkenes from fatty acids, a hitherto unknown enzymatic reaction. 1-alkenes are widely used additives for plasticizers and lubricants. OleTJE has been shown to accept electrons from hydrogen peroxide for the oxidative decarboxylation. While addition of hydrogen peroxide damages the enzyme and results in low yields, in situ generation of the cofactor circumvents this problem. The photobiocatalytic system shows clear advantages regarding enzyme activity and yield, resulting in a simple and efficient system for fatty acid decarboxylation.

We describe a protocol for the light-catalyzed generation of hydrogen peroxide &#8212; a cofactor for oxidative transformations.

مدفوعة خفيفة الأنزيمية نزع الكربوكسيل

Oxidoreductases belong to the most-applied industrial enzymes. Nevertheless, they need external electrons whose supply is often costly and challenging. ...

Chemical Analysis of Water-accommodated Fractions of Crude Oil Spills Using TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system requires the careful preparation of the sample in order to accurately replicate the natural formation of the water-accommodated fraction that occurs in nature. Low-energy water-accommodated fractions (LEWAF) are carefully prepared by mixing crude oil and water at a set ratio. Aspirator bottles are then irradiated, and at set time points, the water is sampled and extracted using standard techniques. A second challenge is the representative characterization of the sample, which must take into consideration the chemical changes that occur over time. A targeted analysis of the aromatic fraction of the LEWAF can be performed using an atmospheric-pressure laser ionization source coupled to a custom-built trapped ion mobility spectrometry&#8211;Fourier transform&#8211;ion cyclotron resonance mass spectrometer (TIMS-FT-ICR MS). The TIMS-FT-ICR MS analysis provides high-resolution ion mobility and ultrahigh-resolution MS analysis, which further allow the identification of isomeric components by their collision cross-sections (CCS) and chemical formula. Results show that as the oil-water mixture is exposed to light, there is significant photo-solubilization of the surface oil into the water. Over time, the chemical transformation of the solubilized molecules takes place, with a decrease in the number of identifications of nitrogen- and sulfur-bearing species in favor of those with a greater oxygen content than were typically observed in the base oil.

The low-energy water-accommodated fraction (LEWAF) of crude oil is a challenging system to analyze, because over time, this complex mixture undergoes chemical transformations. This protocol illustrates methods for the preparation of the LEWAF sample and for performing photo-irradiation and chemical analysis by trapped ion mobility spectrometry&#8211;FT-ICR MS.

التحليل الكيميائي للالكسور-استيعاب المياه من النفط الخام التسربات عن طريق TIMS-FT-ICR MS

Multiple chemical processes control how crude oil is incorporated into seawater and also the chemical reactions that occur overtime. Studying this system ...

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

Different sulfur isotope compositions of authigenic pyrite typically result from the sulfate-driven anaerobic oxidation of methane (SO4-AOM) and organiclastic sulfate reduction (OSR) in marine sediments. However, unravelling the complex pyritization sequence is a challenge because of the coexistence of different sequentially formed pyrite phases. This manuscript describes a sample preparation procedure that enables the use of secondary ion mass spectroscopy (SIMS) to obtain in situ &#948;34S values of various pyrite generations. This allows researchers to constrain how SO4-AOM affects pyritization in methane-bearing sediments. SIMS analysis revealed an extreme range in &#948;34S values, spanning from -41.6 to +114.8&#8240;, which is much wider than the range of &#948;34S values obtained by the traditional bulk sulfur isotope analysis of the same samples. Pyrite in the shallow sediment mainly consists of 34S-depleted framboids, suggesting early diagenetic formation by OSR. Deeper in the sediment, more pyrite occurs as overgrowths and euhedral crystals, which display much higher SIMS &#948;34S values than the framboids. Such 34S-enriched pyrite is related to enhanced SO4-AOM at the sulfate-methane transition zone, postdating OSR. High-resolution in situ SIMS sulfur isotope analyses allow for the reconstruction of the pyritization processes, which cannot be resolved by bulk sulfur isotope analysis.

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

Analyses of the sulfur isotopic composition (&#948;34S) of pyrite from methane-bearing sediments have typically focused on bulk samples. Here, we applied secondary ion mass spectroscopy to analyze the &#948;34S values of various pyrite generations to understand the diagenetic history of pyritization.

إعداد البايرايت أوثيجينيك من الرواسب الحاملة لغاز الميثان للنظائر في الموقع الكبريت في تحليل استخدام سيمز

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

On-line Analysis of Nitrogen Containing Compounds in Complex Hydrocarbon Matrixes

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The composition of heavy crude oils and shale oils varies substantially depending on the origin of the mixture. In particular they contain an increased amount of nitrogen containing compounds compared to the conventionally used sweet crude oils. As nitrogen compounds have an influence on the operation of thermal processes occurring in coker units and steam crackers, and as some species are considered as environmentally hazardous, a detailed analysis of the reactions involving nitrogen containing compounds under pyrolysis conditions provides valuable information. Therefore a novel method has been developed and validated with a feedstock containing a high nitrogen content, i.e., a shale oil. First, the feed was characterized offline by comprehensive two-dimensional gas chromatography (GC &#215; GC) coupled with a nitrogen chemiluminescence detector (NCD). In a second step the on-line analysis method was developed and tested on a steam cracking pilot plant by feeding pyridine dissolved in heptane. The former being a representative compound for one of the most abundant classes of compounds present in shale oil. The composition of the reactor effluent was determined via an in-house developed automated sampling system followed by immediate injection of the sample on a GC &#215; GC coupled with a time-of-flight mass spectrometer (TOF-MS), flame ionization detector (FID) and NCD. A novel method for quantitative analysis of nitrogen containing compounds using NCD and 2-chloropyridine as an internal standard has been developed and demonstrated.

A method combining comprehensive two-dimensional gas chromatography with nitrogen chemiluminescence detection has been developed and applied to on-line analysis of nitrogen containing compounds in a complex hydrocarbon matrix.

على الخط تحليل النيتروجين التي تحتوي على مركبات في مصفوفة الهيدروكربونية مجمع

The shift to heavy crude oils and the use of alternative fossil resources such as shale oil are a challenge for the petrochemical industry. The ...

Seawater Sampling and Collection

This video documents methods for collecting coastal marine water samples and processing them for various downstream applications including biomass concentration, nucleic acid purification, cell abundance, nutrient and trace gas analyses. For today's demonstration samples were collected from the deck of the HMS John Strickland operating in Saanich Inlet. An A-frame derrick, with a multi-purpose winch and cable system, is used in combination with Niskin or Go-Flo water sampling bottles. Conductivity, Temperature, and Depth (CTD) sensors are also used to sample the underlying water mass. To minimize outgassing, trace gas samples are collected first.  Then, nutrients, water chemistry, and cell counts are determined. Finally, waters are collected for biomass filtration. The set-up and collection time for a single cast is ~1.5 hours at a maximum depth of 215 meters. Therefore, a total of 6 hours is generally needed to complete the collection series described here.

This video documents methods for collecting coastal marine water samples and processing them for various downstream applications including biomass concentration, nucleic acid purification, cell abundance, nutrient and trace gas analyses.

أخذ عينات مياه البحر وكوكتيل

This video documents methods for collecting coastal marine water samples and processing them for various downstream applications including biomass ...

Biology

<meta charset="utf8"></head><body>إعداد عملي ومنخفض التكلفة لقياس الميثان في العينات المائية

Measuring Dissolved Methane in Aquatic Ecosystems Using An Optical Spectroscopy Gas Analyzer

Measuring greenhouse gas (GHG) fluxes and pools in ecosystems are becoming increasingly common in ecological studies due to their relevance to climate change. With it, the need for analytical platforms adaptable to measuring different pools and fluxes within research groups also grows. This study aims to develop a procedure to use portable optical spectroscopy-based gas analyzers, originally designed and marketed for gas flux measurements, to measure GHG concentrations in aqueous samples. The protocol involves the traditional headspace equilibration technique followed by the injection of a headspace gas subsample into a chamber connected through a closed loop to the inlet and outlet ports of the gas analyzer. The chamber is fabricated from a generic mason jar and simple laboratory supplies, and it is an ideal solution for samples that may require pre-injection dilution. Methane concentrations measured with the chamber are tightly correlated (r2 &#62; 0.98) with concentrations determined separately through gas chromatography-flame ionization detection (GC-FID) on subsamples from the same vials. The procedure is particularly relevant for field studies in remote areas where chromatography equipment and supplies are not readily available, offering a practical, cheaper, and more efficient solution for measuring methane and other dissolved greenhouse gas concentrations in aquatic systems.

<meta charset="utf8"></head><body>قياس الميثان المذاب في النظم البيئية المائية باستخدام محلل غاز التحليل الطيفي البصري

This study demonstrates an approach to measure methane gas concentrations in aqueous samples using portable optical analyzers coupled to an injection chamber in a closed loop. The results are similar to conventional gas chromatography, presenting a practical and low-cost alternative particularly suitable for remote field studies.

قياس الميثان المذاب في النظم البيئية المائية باستخدام محلل غاز التحليل الطيفي البصري

Measuring greenhouse gas (GHG) fluxes and pools in ecosystems are becoming increasingly common in ecological studies due to their relevance to climate ...

Qualitative Characterization of the Aqueous Fraction from Hydrothermal Liquefaction of Algae Using 2D Gas Chromatography with Time-of-flight Mass Spectrometry

Two-dimensional gas chromatography coupled with time-of-flight mass spectrometry is a powerful tool for identifying and quantifying chemical components in complex mixtures. It is often used to analyze gasoline, jet fuel, diesel, bio-diesel and the organic fraction of bio-crude/bio-oil. In most of those analyses, the first dimension of separation is non-polar, followed by a polar separation. The aqueous fractions of bio-crude and other aqueous samples from biofuels production have been examined with similar column combinations. However, sample preparation techniques such as derivatization, solvent extraction, and solid-phase extraction were necessary prior to analysis. In this study, aqueous fractions obtained from the hydrothermal liquefaction of algae were characterized by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry without prior sample preparation techniques using a polar separation in the first dimension followed by a non-polar separation in the second. Two-dimensional plots from this analysis were compared with those obtained from the more traditional column configuration. Results from qualitative characterization of the aqueous fractions of algal bio-crude are discussed in detail. The advantages of using a polar separation followed by a non-polar separation for characterization of organics in aqueous samples by two-dimensional gas chromatography coupled with time-of-flight mass spectrometry are highlighted.

A two-dimensional gas chromatography-time-of-flight mass spectrometry method is described for characterization of the aqueous fraction of bio-crude produced from hydrothermal liquefaction of algae. This protocol can also be employed to analyze the aqueous fraction of liquid products from fast pyrolysis, catalytic fast pyrolysis, catalytic deoxygenation and hydro-treating.

توصيف نوعي لكسر مائي من الحرارية المائية لتسييل من الطحالب عن طريق 2D اللوني للغاز مع الوقت من الطيران الطيف الكتلي

Two-dimensional gas chromatography coupled with time-of-flight mass spectrometry is a powerful tool for identifying and quantifying chemical components in ...

قياس H

Summary

Explore More Videos

Chapters in this video

الكشف عن كمية من المتفجرات عن طريق تتبع الأبخرة درجة الحرارة المبرمجة الامتزاز الغاز اللوني-الكترون التقاط الكاشف

مدفوعة خفيفة الأنزيمية نزع الكربوكسيل

التحليل الكيميائي للالكسور-استيعاب المياه من النفط الخام التسربات عن طريق TIMS-FT-ICR MS

إعداد البايرايت أوثيجينيك من الرواسب الحاملة لغاز الميثان للنظائر في الموقع الكبريت في تحليل استخدام سيمز

على الخط تحليل النيتروجين التي تحتوي على مركبات في مصفوفة الهيدروكربونية مجمع

أخذ عينات مياه البحر وكوكتيل

قياس الميثان المذاب في النظم البيئية المائية باستخدام محلل غاز التحليل الطيفي البصري

قياس الميثان المذاب في النظم البيئية المائية باستخدام محلل غاز التحليل الطيفي البصري

قياس الميثان المذاب في النظم البيئية المائية باستخدام محلل غاز التحليل الطيفي البصري

توصيف نوعي لكسر مائي من الحرارية المائية لتسييل من الطحالب عن طريق 2D اللوني للغاز مع الوقت من الطيران الطيف الكتلي