Negative temperature programming using microwave open tubular gas chromatography.

A microwave gas chromatography (GC) column oven is engineered to generate a uniform microwave field around an open tubular column with the elimination of cold spots, which are common in a domestic microwave oven. Short cool-down time in microwave heating makes it possible to employ negative temperature programming for the enhanced separation of compounds during the process. The feasibility of negative temperature programming in microwave GC is investigated for the analysis and quantitation of four different pairs of nonvolatile and volatile compounds. The influence of intermediate column cooling rate, holding time in the cooling ramp, and reheating rate after the cooling ramp for enhanced resolution are investigated. The results obtained from negative temperature programming are compared with those from positive temperature programming. Negative temperature programming affords greater resolution of some critical pairs of analytes.

Isolation of tetra-acyl sucrose esters from turkish tobacco using supercritical fluid CO2 and comparison with conventional solvent extraction.

Pure supercritical CO2 at various pressures and temperatures was used to effect the fractionation of tetra-acyl sucrose esters (SE) from dried, ground Turkish tobacco without any further pretreatment of the matrix. It was determined that SE cannot be extracted using low density CO2 (150 atm, 60 degrees C, and 0.62 gm/mL or 200 atm, 100 degrees C, and 0.49 gm/mL), whereas other analytes, which strongly interfere with the conventional solvent extraction of SE, can be easily removed under the same conditions. At the higher temperature (100 degrees C), these same analytes that interfere with the conventional solvent extraction of SE are even more readily removed, while the very poor extractability of SE is not affected. It was demonstrated, however, that SE can be removed from the pre-extracted tobacco with supercritical CO2 if the density is greater than (or equal to) 0.73 gm/mL. The supercritical fluid extraction method has been compared with other previous extraction methods that employ conventional solvents. This study provides one of the clearest examples of how the variable density property of a supercritical fluid can be utilized to effect the fractionation of a complex mixture.

Feasibility of supercritical fluid extraction with on-line coupling of reversed-phase liquid chromatography for quantitative analysis of polymer additives.

An on-line analytical method for determining polymer additives which incorporates (a) sample preparation and concentration, (b) chromatographic separation, and (c) UV detection is presented. The on-line system which combines supercritical fluid extraction (SFE) and high-performance liquid chromatography (LC) allows analytes to first be extracted and transferred to the SFE sorbent trap, then desorbed from the trap and presented to the LC system. No UV detector interference from residual dissolved CO2 in the mobile phase was observed since CO2 is eliminated by a pre-wash of the sorbent trap with a small amount of water. Reversed-phase LC with a mobile phase gradient of acetonitrile-water was employed. The described method allows a complete analysis to be processed in less than 30 min.

Polymer-additive extraction via pressurized fluids and organic solvents of variously cross-linked poly(methylmethacrylates).

Variously cross-linked poly(methylmethacrylates) (PMMAs) are synthesized with three additives incorporated at theoretically 1000 microg of the additive per gram of prepared polymer. The additives are Irganox 1010, Irganox 1076, and Irgafos 168. The in-house" synthesized polyacrylates are then subjected to supercritical fluid extraction (SFE) to determine if additive recovery is a function of percent cross-linking. Although considerable work in this regard has been performed with non-cross-linked polyolefins, the literature is lacking regarding polyacrylates. Some additive degradation apparently occurs during the synthesis, as judged by the increased complexity of the extract high-performance liquid chromatographic trace and the low percent recoveries observed especially for the Irganoxes. For low polymer cross-linking (1%), it appears that both PMMA synthetic reproducibility and readily observed polymer swelling during SFE are serious issues that adversely affect additive percent recovery and precision of results. Higher percent cross-linking yields more consistent analytical data than low percent cross-linking, even though the amount of additive extracted in all PMMA samples (regardless of cross-linking percentage) is essentially the same whether the extraction is via SFE or liquid-solid extraction with methylene chloride. Results for comparably cross-linked poly(ethylmethacrylate) and poly(butylmethacrylate) are similar to PMMA.

Delayed chest wall pain after coronary artery bypass.

The author describes a patient who has a successful coronary artery bypass. Six weeks later, after a physical examination of the chest, she had unbearable sharp, stabbing pain around the incision which was not responding to nerve blocks, analgesics, nonsteroidal anti inflammatory agents, and epidural blocks. The pain was responsive to mexilitine and disappeared after three weeks of treatment.

Suggested new operative approach in the treatment of Lutembacher's syndrome, with moderately hypoplastic left ventricle.

Lutembacher's syndrome or ASD secondum and rheumatic mitral stenosis is treated with surgery but in some instances of presence of small left ventricle surgery will lead to death. Nazem's approach which is our Staged Suggested Method has saved several patients with this kind of pathology.

Suggested approach for end to side anastomosis to the abdominal aorta in aorto-femoral bypass grafting for aorto-iliac occlusive disease.

For surgical treatment of aorto-iliac occlusive diseases the prosthetic grafts are used for aorto-femoral bypass in which the end to side anastomoses are done on anterior aspect of aorta. But this approach is leading to some disadvantages caused by gravity or pressure imposed by abdominal viscera and resulting to kinking to the anastomotic area between the vertebral column and viscera which brings about turbulence, platelet aggregation, thrombus formation, and its organization which finally occludes the lumen. Nazem's method of lateral end-to-side anastomosis preferably to the left side of aorta will be without the mentioned bad on sequences, thereby greatly reducing mortality and morbidity. We recommend the interested academic groups use our method, which follows and we welcome them sharing their results with us.