Constructing flow-through reactors for chemiluminescence detection by machining channels into polymer disks has enabled the exploration of new configurations and materials that can improve signal intensity beyond that attainable with the traditional coiled-tubing design. Several approaches to merge reactant solutions were examined: an intersection, chamber or deeper well in the centre of a serpentine configuration flow-cell (directly in front of a photomultiplier tube), or a confluence point outside the detection zone. For several analytically useful, rapid chemiluminescence reactions, the single-inlet flow-cell with external Y-piece was most suitable, but for others (such as KMnO(4)/Mn(II) with morphine, and [Ir(f-ppy)(2)BPS](-) with fluoroquinolones) the dual-inlet configuration provided greater signals. The introduction of central mixing zones with larger widths than the channel reduced the chemiluminescence response. The reversing turns of a serpentine channel promote efficient mixing and greater chemiluminescence intensities than a spiral channel, but increasing the sharpness of the turns created areas of poor solution flow and decreased the chemiluminescence response. Teflon disks impregnated with glass microspheres increased the chemiluminescence signals by 13%-17%, due to the greater reflection of stray light towards the photodetector.
ABSTRACT: A rapid method for screening drug seizure samples for 3,6‐diacetylmorphine (heroin), which consists of a simple hydrolysis procedure and flow‐injection analysis with two chemiluminescence reagents, is described. Before hydrolysis, 3,6‐diacetylmorphine evokes an intense response with a tris(2,2′‐bipyridyl)ruthenium(III) reagent (prepared by dissolving the perchlorate salt in acetonitrile), and a relatively weak chemiluminescence response with a second reagent: potassium permanganate in an aqueous acidic polyphosphate solution. However, the permanganate reagent is extremely sensitive toward the hydrolysis products of 3,6‐diacetylmorphine (i.e., 6‐monoacetylmorphine and morphine). Some compounds commonly found in drug laboratories may cause false positives with tris(2,2′‐bipyridyl)ruthenium(III), but do not produce the markedly increased response with the permanganate reagent after the hydrolysis procedure. The combination of these two tests therefore provides an effective presumptive test for the presence of 3,6‐diacetylmorphine, which we have verified with 14 samples obtained from a forensic science laboratory.
This review describes developments in all aspects of atomisation and excitation related to atomic spectroscopy reported in the Atomic Spectrometry Updates References in JAAS, Volume 3 (88/930–88/2393) and Volume 4 (89/C1–89/C1658). Thus it follows the review published last year (J. Anal. At. Spectrom., 1988, 3, 133R). The full references, names and adresses of authors can be readily found from the Atomic Spectrometry Updates references in the relevant issues of JAAS. However, as an additional service to readers an abbreviated form of each literature reference quoted (except for those to Conference Proceedings) is given at the end of the review. Comments as to possible improvements in future reviews are always welcome.