{"status":"ok","message-type":"work","message-version":"1.0.0","message":{"indexed":{"date-parts":[[2026,4,17]],"date-time":"2026-04-17T22:47:57Z","timestamp":1776466077805,"version":"3.51.2"},"reference-count":43,"publisher":"Wiley","issue":"11","license":[{"start":{"date-parts":[[2007,10,8]],"date-time":"2007-10-08T00:00:00Z","timestamp":1191801600000},"content-version":"vor","delay-in-days":0,"URL":"http:\/\/onlinelibrary.wiley.com\/termsAndConditions#vor"}],"content-domain":{"domain":[],"crossmark-restriction":false},"short-container-title":["Magnetic Reson in Chemistry"],"published-print":{"date-parts":[[2007,11]]},"abstract":"<jats:title>Abstract<\/jats:title><jats:p>Hydrogen cyanide, cyanogen chloride and phosgene are produced in tremendously large quantities today by the chemical industry. The compounds are also particularly attractive to foreign states and terrorists seeking an inexpensive mass\u2010destruction capability. Along with contemporary warfare agents, therefore, the US Army evaluates protective equipment used by warfighters and domestic emergency responders against the compounds, and requires their certification at \u2265 95 carbon atom % before use. We have investigated the <jats:sup>13<\/jats:sup>C spin\u2010lattice relaxation behavior of the compounds to develop a quantitative NMR method for characterizing chemical lots supplied to the Army. Behavior was assessed at 75 and 126 MHz for temperatures between 5 and 15 \u00b0C to hold the compounds in their liquid states, dramatically improving detection sensitivity. <jats:italic>T<\/jats:italic><jats:sub>1<\/jats:sub> values for cyanogen chloride and phosgene were somewhat comparable, ranging between 20 and 31 s. Hydrogen cyanide values were significantly shorter at 10\u201318 s, most likely because of a <jats:sup>1<\/jats:sup>H\uf8ff<jats:sup>13<\/jats:sup>C dipolar contribution to relaxation not possible for the other compounds. The <jats:italic>T<\/jats:italic><jats:sub>1<\/jats:sub> measurements were used to derive relaxation delays for collecting the quantitative <jats:sup>13<\/jats:sup>C data sets. At 126 MHz, only a single data acquisition with a cryogenic probehead gave a signal\u2010to\u2010noise ratio exceeding that necessary for certifying the compounds at \u2265 95 carbon atom % and 99% confidence. Data acquired at 75 MHz with a conventional probehead, however, required \u2265 5 acquisitions to reach this certifying signal\u2010to\u2010noise ratio for phosgene, and \u2265 12 acquisitions were required for the other compounds under these same conditions. In terms of accuracy and execution time, the NMR method rivals typical chromatographic methods. Published in 2007 by John Wiley &amp; Sons, Ltd.<\/jats:p>","DOI":"10.1002\/mrc.2081","type":"journal-article","created":{"date-parts":[[2007,10,8]],"date-time":"2007-10-08T08:16:49Z","timestamp":1191831409000},"page":"954-961","source":"Crossref","is-referenced-by-count":19,"title":["Purity analysis of hydrogen cyanide, cyanogen chloride and phosgene by quantitative <sup>13<\/sup>C NMR spectroscopy"],"prefix":"10.1002","volume":"45","author":[{"given":"Terry J.","family":"Henderson","sequence":"first","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]},{"given":"David B.","family":"Cullinan","sequence":"additional","affiliation":[],"role":[{"role":"author","vocabulary":"crossref"}]}],"member":"311","published-online":{"date-parts":[[2007,10,8]]},"reference":[{"key":"e_1_2_1_2_2","unstructured":"Convention on the Prohibition of the Development Production Stockpiling and Use of Chemical Weapons and their Destruction signed January 1993 in Paris France and entered into force on 29 April1997. Printed and distributed by the Provisional Technical Secretariat for the Preparatory Commission for the Organization for the Prohibition of Chemical Weapons. Depositary of the Convention is the Secretary\u2010General of the United Nations."},{"key":"e_1_2_1_3_2","doi-asserted-by":"publisher","DOI":"10.1016\/0079-6565(77)80003-4"},{"key":"e_1_2_1_4_2","doi-asserted-by":"publisher","DOI":"10.1021\/ac50036a025"},{"key":"e_1_2_1_5_2","doi-asserted-by":"crossref","first-page":"1793","DOI":"10.1051\/jcp\/1995921793","volume":"92","author":"Jan S","year":"1995","journal-title":"J. Chim. Phys. Phys.\u2010 Chim. Biol."},{"key":"e_1_2_1_6_2","first-page":"232","volume":"37","author":"Kestner TA","year":"1996","journal-title":"Polym. Prepr. (Am. Chem. Soc., Div. Polym. Chem.)"},{"key":"e_1_2_1_7_2","doi-asserted-by":"publisher","DOI":"10.1002\/star.19950471205"},{"key":"e_1_2_1_8_2","doi-asserted-by":"publisher","DOI":"10.1007\/BF02523385"},{"key":"e_1_2_1_9_2","first-page":"5569","volume":"50","author":"Orejuela LM","year":"1996","journal-title":"Holzforschung"},{"key":"e_1_2_1_10_2","doi-asserted-by":"publisher","DOI":"10.1039\/a705178f"},{"key":"e_1_2_1_11_2","doi-asserted-by":"publisher","DOI":"10.1021\/ac010809"},{"key":"e_1_2_1_12_2","doi-asserted-by":"publisher","DOI":"10.1021\/jf00054a023"},{"key":"e_1_2_1_13_2","doi-asserted-by":"publisher","DOI":"10.1016\/0031-9422(96)00283-X"},{"key":"e_1_2_1_14_2","doi-asserted-by":"publisher","DOI":"10.1038\/nbt1290-1282"},{"key":"e_1_2_1_15_2","first-page":"291","volume":"22","author":"Tugnait M","year":"1992","journal-title":"Methodol. Surv. Biochem. Anal."},{"key":"e_1_2_1_16_2","doi-asserted-by":"publisher","DOI":"10.1006\/abio.1993.1451"},{"key":"e_1_2_1_17_2","doi-asserted-by":"publisher","DOI":"10.1002\/mrc.1260310810"},{"key":"e_1_2_1_18_2","doi-asserted-by":"publisher","DOI":"10.1023\/A:1018914215345"},{"key":"e_1_2_1_19_2","doi-asserted-by":"publisher","DOI":"10.1021\/ef960045e"},{"key":"e_1_2_1_20_2","doi-asserted-by":"publisher","DOI":"10.1007\/BF00009561"},{"key":"e_1_2_1_21_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0922-3487(96)80051-7"},{"key":"e_1_2_1_22_2","doi-asserted-by":"publisher","DOI":"10.1021\/ac980573i"},{"key":"e_1_2_1_23_2","doi-asserted-by":"publisher","DOI":"10.1021\/ac50048a040"},{"key":"e_1_2_1_24_2","first-page":"278","volume-title":"Pulse and Fourier Transform NMR","author":"Farrar TC","year":"1967"},{"key":"e_1_2_1_25_2","doi-asserted-by":"publisher","DOI":"10.1016\/0022-2364(83)90035-5"},{"key":"e_1_2_1_26_2","doi-asserted-by":"publisher","DOI":"10.1063\/1.432503"},{"key":"e_1_2_1_27_2","doi-asserted-by":"publisher","DOI":"10.1016\/0079-6565(79)80013-8"},{"key":"e_1_2_1_28_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0065-2318(08)60192-4"},{"key":"e_1_2_1_29_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja00443a016"},{"key":"e_1_2_1_30_2","doi-asserted-by":"publisher","DOI":"10.1021\/bi00600a027"},{"key":"e_1_2_1_31_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0021-9258(19)41076-4"},{"key":"e_1_2_1_32_2","first-page":"6","volume-title":"CRC Handbook of Chemistry","author":"Lide DR","year":"1995"},{"key":"e_1_2_1_33_2","doi-asserted-by":"publisher","DOI":"10.1103\/PhysRev.86.1055.3"},{"key":"e_1_2_1_34_2","first-page":"367","volume":"99","author":"Uike M","year":"1992","journal-title":"J. Magn. Reson."},{"key":"e_1_2_1_35_2","doi-asserted-by":"publisher","DOI":"10.1006\/jmre.1997.1215"},{"key":"e_1_2_1_36_2","doi-asserted-by":"publisher","DOI":"10.1006\/jmre.1998.1476"},{"key":"e_1_2_1_37_2","doi-asserted-by":"publisher","DOI":"10.1006\/jmre.1998.1516"},{"key":"e_1_2_1_38_2","doi-asserted-by":"publisher","DOI":"10.1006\/jmre.1999.1833"},{"key":"e_1_2_1_39_2","doi-asserted-by":"publisher","DOI":"10.1016\/S0009-2614(96)01336-X"},{"key":"e_1_2_1_40_2","doi-asserted-by":"publisher","DOI":"10.1021\/ci980017p"},{"key":"e_1_2_1_41_2","doi-asserted-by":"publisher","DOI":"10.1021\/ac00238a010"},{"key":"e_1_2_1_42_2","doi-asserted-by":"publisher","DOI":"10.1021\/ja039261"},{"key":"e_1_2_1_43_2","first-page":"3140","volume-title":"The United States Pharmacopoeia","year":"1992"},{"key":"e_1_2_1_44_2","volume-title":"British Pharmacopoeia","year":"1988"}],"container-title":["Magnetic Resonance in Chemistry"],"original-title":[],"language":"en","link":[{"URL":"https:\/\/api.wiley.com\/onlinelibrary\/tdm\/v1\/articles\/10.1002%2Fmrc.2081","content-type":"unspecified","content-version":"vor","intended-application":"text-mining"},{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/pdf\/10.1002\/mrc.2081","content-type":"unspecified","content-version":"vor","intended-application":"similarity-checking"}],"deposited":{"date-parts":[[2025,10,20]],"date-time":"2025-10-20T11:15:35Z","timestamp":1760958935000},"score":1,"resource":{"primary":{"URL":"https:\/\/analyticalsciencejournals.onlinelibrary.wiley.com\/doi\/10.1002\/mrc.2081"}},"subtitle":[],"short-title":[],"issued":{"date-parts":[[2007,10,8]]},"references-count":43,"journal-issue":{"issue":"11","published-print":{"date-parts":[[2007,11]]}},"alternative-id":["10.1002\/mrc.2081"],"URL":"https:\/\/doi.org\/10.1002\/mrc.2081","archive":["Portico"],"relation":{},"ISSN":["0749-1581","1097-458X"],"issn-type":[{"value":"0749-1581","type":"print"},{"value":"1097-458X","type":"electronic"}],"subject":[],"published":{"date-parts":[[2007,10,8]]}}}