Gas chromatographic determination of water in organic compounds and of organic compounds in water after steam distillation

dc.contributor.advisor James S. Fritz Dix, Kevin
dc.contributor.department Chemistry 2018-08-16T15:51:30.000 2020-07-02T06:10:48Z 2020-07-02T06:10:48Z Sun Jan 01 00:00:00 UTC 1989 1989
dc.description.abstract <p>A gas chromatograph (GC) with a flame ionization detector (FID) is shown to be effective in the determination of water in organic compounds. Since the FID gives little response for water, a reaction is needed to convert water into a detectable species. The ketal, 2,2-dimethoxypropane (DMP), reacts quantitatively with water to yield the products methanol and acetone when an acid catalyst is present. Acetone is easily determined with a GC equipped with a capillary column and FID. A solid acid catalyst, Nafion, has been effective and is easily separated before sample introduction into the GC;Several organic solvents were analyzed using this indirect method for determining water. The method is effective for determining water from 0.001-3.5% w/w. Larger concentrations of water can be determined by reducing the sample size. Solid samples were also analyzed and the water found in additional spikes agreed with the amount added;Simple steam distillation is used for the isolation and concentration of organic compounds from water matrices. Organic compounds are spiked into a flask containing water and the mixture is then boiled. Typical distillation times take less than 25 minutes. The condensate is collected in a small collection tube and a portion is injected into a GC containing a capillary column. The recovery of most compounds with boiling points from 77 to 238°C is better than 90% and a concentration effect of ten is realized. This method is very effective for phenols which traditionally have been difficult to distill;When compounds are present at concentrations in the part-per-billion range, a further concentration is necessary. Steam distillation combined with solid phase extraction is shown to be effective in isolating and concentrating compounds from water at these low concentrations. A simple interface between the boiling apparatus and resin collection column is presented. Once the organic analytes are boiled and collected on the resin, they are removed with a small amount of ethyl acetate. The ethyl acetate solution is then injected into a GC. Compounds with boiling points above 400°C can be determined by turning off the flow of cold water in the condenser. Recoveries are better than 80% for compounds with boiling points between 132 to 404°C. ftn*DOE Report IS-T 1396. This work was performed under Contract W-7405-Eng-82 with the Department of Energy.</p>
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dc.identifier archive/
dc.identifier.articleid 10032
dc.identifier.contextkey 6348096
dc.identifier.s3bucket isulib-bepress-aws-west
dc.identifier.submissionpath rtd/9033
dc.language.iso en
dc.source.bitstream archive/|||Sat Jan 15 02:27:23 UTC 2022
dc.subject.disciplines Analytical Chemistry
dc.subject.keywords Chemistry
dc.subject.keywords Analytic
dc.subject.keywords Chemistry
dc.title Gas chromatographic determination of water in organic compounds and of organic compounds in water after steam distillation
dc.type article
dc.type.genre dissertation
dspace.entity.type Publication
relation.isOrgUnitOfPublication 42864f6e-7a3d-4be3-8b5a-0ae3c3830a11 dissertation Doctor of Philosophy
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