{"id":1390,"date":"2012-04-17T19:25:39","date_gmt":"2012-04-17T23:25:39","guid":{"rendered":"http:\/\/blogs.vassar.edu\/magnes\/?p=1390"},"modified":"2013-07-11T10:29:36","modified_gmt":"2013-07-11T14:29:36","slug":"preliminary-results","status":"publish","type":"post","link":"https:\/\/pages.vassar.edu\/magnes\/2012\/04\/17\/preliminary-results\/","title":{"rendered":"Preliminary Results"},"content":{"rendered":"<p>The magnetic field inside an NMR spectrometer is generated by a superconducting solenoid. \u00a0The solenoid is cooled by a three-layer cooling system. \u00a0The outer layer is one of liquid nitrogen at 77K. \u00a0The middle layer is an evacuated cavity that prevents heat conduction by air. \u00a0The innermost layer contains the solenoid submerged in 4K liquid helium that is kept below atmospheric pressure. \u00a0Initially, the magnetic field in an NMR will not be homogenous because of interferences resulting from the magnetization of the sample, and environmental interferences like iron or other metals used in construction.<\/p>\n<p><strong>Initial NMR Magnetic Field<\/strong><\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Initial-NMR-Magnetic-Field3.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1410\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Initial-NMR-Magnetic-Field3.png\" alt=\"\" width=\"431\" height=\"406\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Initial-NMR-Magnetic-Field3.png 431w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Initial-NMR-Magnetic-Field3-300x282.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Initial-NMR-Magnetic-Field3-318x300.png 318w\" sizes=\"auto, (max-width: 431px) 100vw, 431px\" \/><\/a><\/p>\n<p>Sample NMR Starting Magnetic Field<\/p>\n<p>Note the somewhat ordered field that already exists in the Z-direction. \u00a0This is what the initial field looks like most of the time: \u00a0the inhomogeneities are a complex function in three dimensions. \u00a0In order to make the magnetic field homogenous, it is modified using the shim system. The shim system is a series of uncooled, current carrying coils that generate fields in all three directions. \u00a0Each coil attempts to create a field with a function that precisely cancels the imperfections. \u00a0Numerous simple 3-D functions like <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-6f905e538e3a99fb5efb28de521821ca_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#88;&#44;&#32;&#90;&#44;&#32;&#88;&#89;&#94;&#123;&#50;&#125;&#44;&#32;&#90;&#94;&#123;&#50;&#125;&#44;&#32;&#90;&#94;&#123;&#51;&#125;&#44;&#32;&#90;&#94;&#123;&#52;&#125;&#44;&#32;&#88;&#90;&#44;&#32;&#89;&#90;&#44;&#32;&#97;&#110;&#100;&#32;&#88;&#94;&#123;&#50;&#125;&#45;&#89;&#94;&#123;&#50;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"19\" width=\"343\" style=\"vertical-align: -4px;\"\/> are available to add to the magnetic field created by shimming. \u00a0Each set of coils creates a magnetic field gradient in its direction. \u00a0Below is a model of a correction field that uses the function <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-97c248672bafa4beb4177b1ccda167d7_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#90;&#94;&#123;&#50;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"15\" width=\"19\" style=\"vertical-align: 0px;\"\/>:<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Sample-Z-squared-Magnetic-Field.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1419\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Sample-Z-squared-Magnetic-Field.png\" alt=\"\" width=\"399\" height=\"393\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Sample-Z-squared-Magnetic-Field.png 399w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Sample-Z-squared-Magnetic-Field-300x295.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Sample-Z-squared-Magnetic-Field-304x300.png 304w\" sizes=\"auto, (max-width: 399px) 100vw, 399px\" \/><\/a><\/p>\n<p><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-97c248672bafa4beb4177b1ccda167d7_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#90;&#94;&#123;&#50;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"15\" width=\"19\" style=\"vertical-align: 0px;\"\/> Correction Field<\/p>\n<p>All but the most experienced and exacting users of NMR use functions other than <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-cc9f8fff9fd24060bc054e78f01d5bfb_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#90;\" title=\"Rendered by QuickLaTeX.com\" height=\"12\" width=\"12\" style=\"vertical-align: 0px;\"\/> and <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-97c248672bafa4beb4177b1ccda167d7_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#90;&#94;&#123;&#50;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"15\" width=\"19\" style=\"vertical-align: 0px;\"\/> in the correction field because the original field is usually close to homogenous. \u00a0The optimal field for doing NMR spectroscopy is shown below-it is perfectly homogenous and only in the Z-direction.<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1435\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1.png\" alt=\"\" width=\"365\" height=\"362\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1.png 365w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1-150x150.png 150w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1-300x297.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Normal-Magnetic-Field1-302x300.png 302w\" sizes=\"auto, (max-width: 365px) 100vw, 365px\" \/><\/a><\/p>\n<p>Optimal NMR Magnetic Field<\/p>\n<p>Once the magnetic field is homogenized, the analysis of a sample can begin. \u00a0Each nucleus in the atom to be tested has its own resonant frequency somewhere in the radio section of the electromagnetic spectrum. \u00a0NMR takes advantage of this frequency&#8217;s dependence on the strength on an external magnetic field to gather information about each single nucleus, all at one time. \u00a0When the sample is placed in the now-homogenized magnetic field, the electrons around each nucleus become a current, and generate their own magnetic field in the opposite direction. \u00a0This effect is shown below, where the field of the NMR is blue, and the field created by the sample is red.<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Magnetic-Field-of-a-Sample.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1437\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Magnetic-Field-of-a-Sample.png\" alt=\"\" width=\"433\" height=\"375\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Magnetic-Field-of-a-Sample.png 433w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Magnetic-Field-of-a-Sample-300x259.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Magnetic-Field-of-a-Sample-346x300.png 346w\" sizes=\"auto, (max-width: 433px) 100vw, 433px\" \/><\/a>Magnetic field generated by a sample<\/p>\n<p>The smaller, red magnetic field decreases the influence of the NMR&#8217;s magnetic field on each nucleus and causes a very small shift in their resonant frequencies. \u00a0These shifts, which are dependent on the electron density around each nucleus, are calculated using the equation:<\/p>\n<p class=\"ql-center-displayed-equation\" style=\"line-height: 21px;\"><span class=\"ql-right-eqno\"> (1) <\/span><span class=\"ql-left-eqno\"> &nbsp; <\/span><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-6ade1ddca3de922823c2680fd8bcfb74_l3.png\" height=\"21\" width=\"121\" class=\"ql-img-displayed-equation \" alt=\"&#92;&#98;&#101;&#103;&#105;&#110;&#123;&#101;&#113;&#117;&#97;&#116;&#105;&#111;&#110;&#42;&#125; &#92;&#100;&#101;&#108;&#116;&#97;&#61;&#49;&#48;&#94;&#123;&#54;&#125;&#40;&#92;&#115;&#105;&#103;&#109;&#97;&#95;&#123;&#48;&#125;&#45;&#92;&#115;&#105;&#103;&#109;&#97;&#41; &#92;&#101;&#110;&#100;&#123;&#101;&#113;&#117;&#97;&#116;&#105;&#111;&#110;&#42;&#125;\" title=\"Rendered by QuickLaTeX.com\"\/><\/p>\n<p>The peaks that appear on NMR spectra are created when radio waves that match the now-altered resonant frequencies are absorbed and reradiated by the nuclei. \u00a0The four NMR spectra collected for 3,3-dimethyl-2-butanol are shown below as a sample of the gathered data.<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Slide51.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-2246\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/Slide51.png\" alt=\"\" width=\"283\" height=\"208\" \/><\/a>\u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 \u00a0 3,3-dimethyl-2-butanol<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1511\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR.png\" alt=\"\" width=\"3300\" height=\"2550\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR.png 3300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR-300x231.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR-1024x791.png 1024w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-Whole-H-NMR-388x300.png 388w\" sizes=\"auto, (max-width: 3300px) 100vw, 3300px\" \/><\/a><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-d12612c700f99e015f6937d86076b314_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#94;&#123;&#49;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"10\" width=\"5\" style=\"vertical-align: 5px;\"\/>H-NMR Spectrum of 3,3-dimethyl-2-butanol<\/p>\n<p>Each peak in a <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-d12612c700f99e015f6937d86076b314_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#94;&#123;&#49;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"10\" width=\"5\" style=\"vertical-align: 5px;\"\/>H-NMR spectrum\u00a0represents a certain number of hydrogen nuclei and describes their neighborhood in the molecule.<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1543\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR.png\" alt=\"\" width=\"3300\" height=\"2550\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR.png 3300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR-300x231.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR-1024x791.png 1024w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-C-13-NMR-388x300.png 388w\" sizes=\"auto, (max-width: 3300px) 100vw, 3300px\" \/><\/a><img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-da2979ed4cdf09c04247f6962db549d8_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#94;&#123;&#49;&#51;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"10\" width=\"13\" style=\"vertical-align: 5px;\"\/> C-NMR spectrum of 3,3-dimethyl-2-butanol<\/p>\n<p>Each peak in a <img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-da2979ed4cdf09c04247f6962db549d8_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#94;&#123;&#49;&#51;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"10\" width=\"13\" style=\"vertical-align: 5px;\"\/> C-NMR spectrum\u00a0represents a specific &#8220;type&#8221; of carbon in the molecule. \u00a0One peak can represent more than one carbon nucleus if they have the same electron densities.<\/p>\n<p>The two spectra below are meant to be read together.<\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1550\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351.png\" alt=\"\" width=\"3300\" height=\"2550\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351.png 3300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351-300x231.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351-1024x791.png 1024w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-1351-388x300.png 388w\" sizes=\"auto, (max-width: 3300px) 100vw, 3300px\" \/><\/a><\/p>\n<p><a href=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902.png\"><img loading=\"lazy\" decoding=\"async\" class=\"alignnone size-full wp-image-1551\" src=\"http:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902.png\" alt=\"\" width=\"3300\" height=\"2550\" srcset=\"https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902.png 3300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902-300x231.png 300w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902-1024x791.png 1024w, https:\/\/pages.vassar.edu\/magnes\/files\/2012\/04\/33-dimethyl-2-butanol-DEPT-902-388x300.png 388w\" sizes=\"auto, (max-width: 3300px) 100vw, 3300px\" \/><\/a>Top: \u00a0DEPT-135 Spectrum; Bottom: \u00a0DEPT-90 Spectrum<\/p>\n<p>The peaks on these spectra describe the number of hydrogen atoms bound to each carbon atom. \u00a0The frequencies of the peaks are the same as they are on the\u00a0<img loading=\"lazy\" decoding=\"async\" src=\"https:\/\/pages.vassar.edu\/magnes\/wp-content\/ql-cache\/quicklatex.com-da2979ed4cdf09c04247f6962db549d8_l3.png\" class=\"ql-img-inline-formula \" alt=\"&#94;&#123;&#49;&#51;&#125;\" title=\"Rendered by QuickLaTeX.com\" height=\"10\" width=\"13\" style=\"vertical-align: 5px;\"\/>C-NMR.<\/p>\n<p>More information on exactly how to interpret each spectrum, and translate all of their information into a molecular structure, is forthcoming.<\/p>\n<p>&nbsp;<\/p>\n","protected":false},"excerpt":{"rendered":"<p>The magnetic field inside an NMR spectrometer is generated by a superconducting solenoid. \u00a0The solenoid is cooled by a three-layer cooling system. \u00a0The outer layer is one of liquid nitrogen at 77K. \u00a0The middle layer is an evacuated cavity that prevents heat conduction by air. \u00a0The innermost layer contains the solenoid submerged in 4K liquid [&hellip;]<\/p>\n","protected":false},"author":912,"featured_media":0,"comment_status":"open","ping_status":"closed","sticky":false,"template":"","format":"standard","meta":{"footnotes":""},"categories":[4101,64,29905],"tags":[],"class_list":["post-1390","post","type-post","status-publish","format-standard","hentry","category-advanced-em","category-michael","category-spring-2012"],"_links":{"self":[{"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/posts\/1390","targetHints":{"allow":["GET"]}}],"collection":[{"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/posts"}],"about":[{"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/types\/post"}],"author":[{"embeddable":true,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/users\/912"}],"replies":[{"embeddable":true,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/comments?post=1390"}],"version-history":[{"count":57,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/posts\/1390\/revisions"}],"predecessor-version":[{"id":2405,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/posts\/1390\/revisions\/2405"}],"wp:attachment":[{"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/media?parent=1390"}],"wp:term":[{"taxonomy":"category","embeddable":true,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/categories?post=1390"},{"taxonomy":"post_tag","embeddable":true,"href":"https:\/\/pages.vassar.edu\/magnes\/wp-json\/wp\/v2\/tags?post=1390"}],"curies":[{"name":"wp","href":"https:\/\/api.w.org\/{rel}","templated":true}]}}