Design, validation, and implementation of a rapid-injection NMR system

Journal of Organic Chemistry

Volumn 75, Issue 16, 2010, Pages 5558-5572

  Denmark, Scott E ^a   Williams, Bruce J ^a   Eklov, Brian M ^a   Pham, Son M ^a   Beutner, Gregory L ^a  

^a UNIVERSITY OF ILLINOIS AT URBANA CHAMPAIGN   (United States)

Author keywords

[No Author keywords available]

Indexed keywords

CHEMICAL PROCESS; CHEMICAL REAGENTS; DESIGN CRITERION; NMR SPECTROSCOPY; NMR TUBES; ORGANIC REACTION MECHANISMS; RAPID ACQUISITION; REAL TIME; REPRODUCIBILITIES; RESEARCH PROBLEMS;

NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY;

INSTRUMENTS;

REAGENT;

ARTICLE; CALIBRATION; CHEMICAL REACTION; EVOLUTION; KINETICS; NUCLEAR MAGNETIC RESONANCE; NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY; RAPID INJECTION NUCLEAR MAGNETIC RESONANCE; RELIABILITY; REPRODUCIBILITY; TEMPERATURE; VALIDATION PROCESS;

CALIBRATION; EQUIPMENT DESIGN; ETHERS; MAGNETIC RESONANCE SPECTROSCOPY; MOLECULAR STRUCTURE; SILANES; STEREOISOMERISM; TEMPERATURE;

EID: 77955680491     PISSN: 00223263     EISSN: 15206904     Source Type: Journal    
DOI: 10.1021/jo100837a     Document Type: Article

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36. Digispense 2000 fitted with a size A alumina ceramic piston and an optional gland seal. The size A piston is rated from 1 to 2000 μL with 0.1 μL resolution. Contact IVEK Corp. at (800) 356-4746 or visit www.ivek.com.
37. The rates of travel are controllable, but increasing or decreasing them too far can cause the pistons to not seat properly, leaving them in an intermediary position and unable to move without resetting them manually.
38. Titanium tubing was made of A40 (<0.04% iron), 0.083′′ o.d., 0.063′′ i.d., 60′′ long.
39. Although more costly and more difficult to machine than stainless steel or brass, initial testing with stainless steel tubing resulted in poor line shape, even at room temperature.
40. In practice, small changes to this lateral alignment can be made manually as needed.
41. Later designs also required a slight modification: A small amount of the inside of the sleeve was removed to compensate for the braise point where the tip was attached to the injector tube.
42. The wires used for cleaning microliter syringes can also be useful in clearing clogged ports.
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