Nuclear magnetic resonance (NMR) spectrometry has been applied to a wide variety of quantitative organic problems, but an intensity standard is required to obtain higher precision (7). The standard compound can be added to each sample as an internal standard or in a separate tube as an external standard. In the latter case there is a possibility of instrumental variation during the interval between the time when the spectra of the sample and the standard are obtained, while in the case of an internal standard the contamination of a sample by the reference compound cannot be avoided. We have developed an analytical technique for the determination of a molecular species in a mixture using an external standard in a precision coaxial tubing (Wilmad Glass Co., inside diameter: inner tube 1.3 mm, outer tube 4.2 mm.). The method has also been used for the elemental determination of hydrogen. In addition, we have developed an analytical method for some binary mixtures by the measurement of chemical shift using this precision coaxial tubing. © 1969, American Chemical Society. All rights reserved.