Calix[4]azulene

Azulene reacts with paraformaldehyde in the presence of florisil to give excellent yields of calix[4]azulene.     

The effects of gamma irradiation on the microbiological, physical and sensory qualities of diced tomatoes

Diced Roma tomatoes were treated with gamma irradiation and evaluated for changes in microbial, physical, chemical and sensory properties. Dosages for Trial 1 were 0.0, 0.39, 0.56 and 1.82 kGy and in Trial 2, 0.0, 0.50, 1.24 and 3.70 kGy. Irradiation at 3.70 kGy resulted in no aerobic populations through day 12 and significantly fewer colonies through day 15 whereas yeast and mold populations experienced a 2 log reduction through day 12. Color, titratable acidity, and °Brix were not significantly affected by irradiation. Tissue firmness decreased with increasing dose but not with storage time. Treatment with 3.7 kGy decreased firmness by 50% and 20% with 0.5 kGy, however, the reduced firmness induced by 0.50 kGy was undetected by a 9 member trained sensory panel. A significant (p0.05) inverse correlation between changes in texture and water-soluble pectin (WSP) was determined while total pectin remained relatively constant and oxalate soluble pectin content decreased slightly with irradiation dose. The significant inverse correlation between the loss of firmness and WSP indicates that the changes in WSP play an important role in the tissue softening of tomatoes, This study indicates that irradiation at 0.5 kGy can reduce microbial counts substantially to improve microbial shelf life without adverse effects on sensory qualities.     

QSAR modeling of flotation collectors using principal components extracted from topological indices

Several topological indices were calculated for substituted-cupferrons that were tested as collectors for the froth flotation of uranium. The principal component analysis (PCA) was used for data reduction. Seven principal components (PC) were found to account for 98.6% of the variance among the computed indices. The principal components thus extracted were used in stepwise regression analyses to construct regression models for the prediction of separation efficiencies (Es) of the collectors. A two-parameter model with a correlation coefficient of 0.889 and a three-parameter model with a correlation coefficient of 0.913 were formed. PCs were found to be better than partition coefficient to form regression equations, and inclusion of an electronic parameter such as Hammett sigma or quantum mechanically derived electronic charges on the chelating atoms did not improve the correlation coefficient significantly. The method was extended to model the separation efficiencies of mercaptobenzothiazoles (MBT) and aminothiophenols (ATP) used in the flotation of lead and zinc ores, respectively. Five principal components were found to explain 99% of the data variability in each series. A three-parameter equation with correlation coefficient of 0.985 and a two-parameter equation with correlation coefficient of 0.926 were obtained for MBT and ATP, respectively. The amenability of separation efficiencies of chelating collectors to QSAR modeling using PCs based on topological indices might lead to the selection of collectors for synthesis and testing from a virtual database.     

Two polymorphs and the diethylammonium salt of the barbiturate eldoral

Polymorph (Ia) of eldoral [5‐ethyl‐5‐(piperidin‐1‐yl)barbituric acid or 5‐ethyl‐5‐(piperidin‐1‐yl)‐1,3‐diazinane‐2,4,6‐trione], C₁₁H₁₇N₃O₃, displays a hydrogen‐bonded layer structure parallel to (100). The piperidine N atom and the barbiturate carbonyl group in the 2‐position are utilized in N—H...N and N—H...O=C hydrogen bonds, respectively. The structure of polymorph (Ib) contains pseudosymmetry elements. The two independent molecules of (Ib) are connected via N—H...O=C(4/6‐position) and N—H...N(piperidine) hydrogen bonds to give a chain structure in the [100] direction. The hydrogen‐bonded layers, parallel to (010), formed in the salt diethylammonium 5‐ethyl‐5‐(piperidin‐1‐yl)barbiturate [or diethylammonium 5‐ethyl‐2,4,6‐trioxo‐5‐(piperidin‐1‐yl)‐1,3‐diazinan‐1‐ide], C₄H₁₂N⁺·C₁₁H₁₆N₃O₃⁻, (II), closely resemble the corresponding hydrogen‐bonded structure in polymorph (Ia). Like many other 5,5‐disubstituted derivatives of barbituric acid, polymorphs (Ia) and (Ib) contain the R₂²(8) N—H...O=C hydrogen‐bond motif. However, the overall hydrogen‐bonded chain and layer structures of (Ia) and (Ib) are unique because of the involvement of the hydrogen‐bond acceptor function in the piperidine group.     

A Simple Strategy to Improve the Accuracy of the Injection Step in Batch Injection Analysis Systems with Amperometric Detection

In this study, we describe for the first time the application of an internal standard method to compensate for random errors associated with the injection procedure in batch injection analysis (BIA) systems with multiple pulse amperometric detection. A sequence of potential pulses was selected in such a way that the internal standard (IS) compound was detected individually at one potential pulse and both the IS and analyte, were detected at another potential pulse. The current ratio (I_IS+analyte/I_IS) was used in the construction of the calibration curve and then to compensate for random errors. The use of disposable syringes or manual pipettes in BIA systems increases the robustness of the method and dispenses with skilled operators.     

Salmonella in foods: new enrichment procedure for TECRA Salmonella Visual Immunoassay using a single rv(R10) only, TT only, or dual rv(R10) and TT selective enrichment broths (AOAC official method 998.09): collaborative study

A collaborative study was conducted to compare a new enrichment procedure for the TECRA Salmonella Visual Immunoassay (TSVIA) with the reference method given in the U.S. Food and Drug Administration's Bacteriological Analytical Manual (7th Ed.). Three food types (milk powder, pepper, and soy flour) were analyzed in Australia and 3 food types (milk chocolate, dried egg, and raw turkey) were analyzed in the United States. Thirty-eight collaborators participated in the study. The TECRA method was evaluated using both Rappaport-Vassiliadis R10 (RV(R10)) and tetrathionate (TT) broths for selective enrichment. M broth cultures arising from each of the 2 selective enrichment broths were tested in the TSVIA using 2 individual wells, one for each selective broth, and a single well to test the pooled selective enrichment broths. The results for the pooled enrichment broths were reported elsewhere. This study presents the results for the use of single enrichment broths, i.e., RV(R10) only or TT only, with the TSVIA. No significant differences (p > 0.05) were observed for the pairwise comparison of the proportion of positive samples for either RV(R10) or TT used as a single enrichment broth for the TSVIA with that for the reference method.     

A very efficient,copper-free palladium catalyst for the Sonogashira reaction with aryl halides

The new complex [Pd[t-Bu2PCH2N(CH2Ph)CH2P t-Bu2](OAc)2] is a very efficient catalyst for the Sonogashira cross-coupling reaction of aryl halides with acetylenes at room temperature, without co-catalyst.