In the paper by Asiri et al. [Acta Cryst. (2012), E68, o1154], the title and the chemical name of one of the reagents used in the synthesis are corrected.[This corrects the article DOI: 10.1107/S1600536812011579.].
Mixed reagents for the Glucose-6-phosphate dehydrogenase (G6PD) deficiency fluorescent screening test were freeze-dried in plastic tubes. The reagents were then reconstituted with distilled water and the test was performed in the usual way. Initial testing with the freeze-dried mixed reagents gave consistent positive reaction to 12 normal blood samples and negative reaction to 9 G6PD deficient blood samples. This will enable a laboratory with freeze-drying facilities to prepare reagent tubes in bulk. As these tubes can be kept at 4 degrees C and do not require to be stored at -20 degrees C, a major laboratory can prepare these tubes and supply small laboratories for screening purposes.
A series of chelating reagents, 1-phenyl-3-methyl-4-(2-fluorobenzoyl)-5-pyrazolone, 1-phenyl-3-methyl-4-(3-fluorobenzoyl)-5-pyrazolone and 1-phenyl-3-methyl-4-(4-fluorobenzoyl)-5-pyrazolone, has been synthesized. The extraction of Ln(III), (Ln = La, Eu and Lu) into chloroform with these reagents at 30 +/- 1 degrees has been studied. The composition of the complexes extracted has been determined by the slope method, and the extraction constants K(ex), were measured. The presence of the fluorine atom in the reagents does not make the K(ex), values much different from those obtained with the parent pyrazolone.
A brief survey to assess the sensitivity and efficacy of some common etching reagents for revealing obliterated engraved marks on Al-Si alloy surfaces is presented. Experimental observations have recommended use of alternate swabbing of 10% NaOH and 10% HNO(3) on the obliterated surfaces for obtaining the desired results. The NaOH etchant responsible for bringing back the original marks resulted in the deposition of some dark coating that has masked the recovered marks. The coating had been well removed by dissolving it in HNO(3) containing 10-20% acid. However, the above etching procedure was not effective on aluminium (99% purity) and Al-Zn-Mg-Cu alloy surfaces. Also the two reagents (i) immersion in 10% aq. phosphoric acid and (ii) alternate swabbing of 60% HCl and 40% NaOH suggested earlier for high strength Al-Zn-Mg-Cu alloys [23] were quite ineffective on Al-Si alloys. Thus different aluminium alloys needed different etching treatments for successfully restoring the obliterated marks. Al-Si alloys used in casting find wide applications especially in the manufacture of engine blocks of motor vehicles. Hence, the results presented in this paper are of much relevance in serial number restoration problems involving this alloy.
Restoration of obliterated engraved marks on high strength Al-Zn-Mg-Cu alloy (AA7010) surfaces by etching technique was studied. The alloy surfaces were mechanically engraved with some identification marks using "Gravograph". The marks were then erased by removing the metal to different levels up to and below the depth of engraving. Five metallographic reagents were tested on the obliterated surfaces by etching. The following two methods (i) immersion in 10% aq. phosphoric acid and (ii) alternate swabbing of 60% HCl and 40% NaOH were found to be quite effective to reveal the obliterated marks. These two procedures were also able to show effectively the marks obliterated by over-engraving and centre punching. Of the two techniques immersion in phosphoric acid provided more contrast. Interestingly, alternate swabbing of 60% HCl and 40% NaOH presented itself to be the common reagent for restoration on pure aluminium as well as its alloy surfaces. This is evident from our own current experiments and those of earlier researchers [G. Peeler, S. Gutowski, H. Wrobel, G. Dower, The restoration of impressed characters on aluminium alloy motor cycle frames, J. Forensic Ident. 58 (1) (2008) 27-32; M. Izhar M. Baharum, R. Kuppuswamy, A.A. Rahman, Restoration of engraved marks on aluminium surfaces by etching technique, Forensic Sci. Int. 177 (2008) 221-227]. The findings have assumed importance as engines and chassis of cars and frames of firearms are currently made of high strength aluminium alloys and recovery on these surfaces by current methods is not satisfactory.
Paper spray ionization (PSI) mass spectrometry (MS) is an emerging tool for ambient reaction monitoring via microdroplet reaction acceleration. PSI-MS was used to accelerate and monitor the time course of the reaction of dansyl chloride with aniline, in acetonitrile, to produce dansyl aniline. Three distinct PSI arrangements were explored in this study representing alternative approaches for sample loading and interaction; conventional single tip as well as two novel setups, a dual-tip and a co-axial arrangement were designed so as to limit any on-paper interaction between reagents. The effect on product abundance was investigated using these different paper configurations as it relates to the time course and distance of microdroplet travel. It was observed that product yield increases at a given distance and then decreases thereafter for all PSI configurations. The fluorescent property of the product (dansyl aniline) was used to visually inspect the reaction progress on the paper substrate during the spraying process. Amongst the variety of sample loading methods the novel dual-tip arrangement showed an increased product yield and microdroplet density, whilst avoiding any on-paper interaction between the reagents.
Indoles are amongst the most important class of heteroaromatics in organic chemistry, being commonly found in biologically active natural products and therapeutically useful compounds. The synthesis of indoles is therefore important and several methods for their synthesis that make use of silver(I) catalysts and reagents have been developed in recent years. This Focus Review contains, to the best of our knowledge, a comprehensive coverage of silver-mediated indole forming reactions since the first reaction of this type was reported in 2004.
In this study, a simple, selective and sensitive method, for spectrophotometric determination of As(III) with gallocyanine as the sensitive reagent was developed. The wavelength of an analytical measurement, for the determination of As (III), using gallocyanine was at 630 nm with an optimum response at pH 2. The RSD for the reproducibility of 100 ppm As (III) was 2.3%. The LOD was 0.04 ppm with linear dynamic range in As(III) concentration of 0.2 - 1.5 ppm. The developed method has been validated against Atomic Absorption Spectrophotometry (AAS). The interference study of several metal ions was carried out and it revealed that that Mn (II) ion was interfered the most.
Nanoporous materials such as Mobil composite material number 41 (MCM-41) are attractive for applications such as catalysis, adsorption, supports, and carriers. Green synthesis of MCM-41 is particularly appealing because the chemical reagents are useful and valuable. We report on the eco-friendly synthesis of MCM-41 nanoporous materials via multi-cycle approach by re-using the non-reacted reagents in supernatant as mother liquor after separating the solid product. This approach was achieved via minimal requirement of chemical compensation where additional fresh reactants were added into the mother liquor followed by pH adjustment after each cycle of synthesis. The solid product of each successive batch was collected and characterized while the non-reacted reagents in supernatant can be recovered and re-used to produce subsequent cycle of MCM-41. The multi-cycle synthesis is demonstrated up to three times in this research. This approach suggests a low cost and eco-friendly synthesis of nanoporous material since less waste is discarded after the product has been collected, and in addition, product yield can be maintained at the high level.
Most of the automotive companies use cast iron for their engine blocks. Restoration of obliterated number on these iron surfaces by chemical etching is known to be quite difficult. Heating of the obliterated surface using oxyacetylene flame is an alternative recovery treatment suggested in literature and used in practice. However chemical etching has been established to be the most sensitive technique for detection of metal deformation present under stamped serial numbers. Hence, the current work investigated the suitability of some common etchants on cast iron surfaces with a view to determining the most suitable one for revealing the obliterated marks. The reagents tested were mostly copper containing Fry's reagent and its modifications. Two cast iron engine blocks (3.29%C and 3.1%C) of two cars--a Proton Saga and a Toyota--were utilized for the experiments. The engine blocks were cut into several small plates and each plate was stamped with some numerical characters at 8 kN load using Instron Table Mounted Universal Testing Machine. The depth of stamping impression varied between 0.2 mm and 0.3 mm. The stamped number was completely ground off manually using a metal file. The grounded surface was then polished smooth using emery papers and etched with a few selected reagents mostly by swabbing. Experimental results showed that a modified Fry's composition consisting of 4 5g CuCl(2), 100 mL HCl, and 180 mL H(2)O restored the number with better contrast at a reasonably shorter time. The above reagent is a slightly modified form of one of the Fry's original compositions--45 g CuCl(2), 180 mL HCl, and 100 mL H(2)O. Quite importantly the proposed reagent restored the original stamped numbers of both Proton and Toyota cars and also a Mitsubishi car that had been obliterated. The most widely used Fry's composition (90 g CuCl(2), 120 mL HCl and 100 mL H(2)O), although recovered the obliterated number, did not cause the desired contrast.
A study has been made of the characteristics of restoration of obliterated engraved marks on aluminium surfaces by etching technique. By etching different reagents on 0.61mm thick sheets of aluminium (99wt%) on which some engraved marks had been erased to different depths it was found that the reagent 60% hydrochloric acid and 40% sodium hydroxide on alternate swabbing on the surfaces was found to be the most sensitive one for these metal surfaces. This reagent was able to restore marks in the above plates erased down to 0.04mm below the bottom of the engraving. The marks also presented excellent contrast with the background. This reagent was further experimented with similar aluminium surfaces, but of relatively greater thickness of 1.5mm. It was noticed that the recovery depth increased slightly to 0.06mm; this suggested the dependence of recovery depth on the thickness of the sheet metal. Further, the depth of restoration decreased in cases where the original number was erased and over which a new number was engraved; the latter results are similar to those of steel surfaces reported earlier [M.A.M. Zaili, R. Kuppuswamy, H. Harun, Restoration of engraved marks on steel surfaces by etching technique, Forensic Sci. Int. 171 (2007) 27-32].
A shelf-stable loop-mediated isothermal amplification (LAMP) reagent for Burkholderia pseudomallei detection is described. The coupling of LAMP reagents with the indirect colorimetric indicator and consequently its lyophilization enable the simple evaluation of results without the need for any advance laboratory instruments. The reagents were found to have a stable shelf life of at least 30 days with well-maintained sensitivity and specificity.
This paper reports the application of hexamethyldisilazane-trimethylsilyl trifluoromethanesulfonate (HMDS-TMSOTf) for the simultaneous silylation of 3-monochloro-1,2-propanediol (3-MCPD) and 1,3-dicholoropropanol (1,3-DCP) in solid and liquid food samples. 3-MCPD and 1,3-DCP are chloropropanols that have been established as Group 2B carcinogens in clinical testing. They can be found in heat-processed food, especially when an extended high-temperature treatment is required. However, the current AOAC detection method is time-consuming and expensive. Thus, HMDS-TMSOTf was used in this study to provide a safer, and cost-effective alternative to the HFBI method. Three important steps are involved in the quantification of 3-MCPD and 1,3-DCP: extraction, derivatization and quantification. The optimization of the derivatization process, which involved focusing on the catalyst volume, derivatization temperature, and derivatization time was performed based on the findings obtained from both the Box-Behnken modeling and a real experimental set up. With the optimized conditions, the newly developed method was used for actual food sample quantification and the results were compared with those obtained via the standard AOAC method. The developed method required less samples and reagents but it could be used to achieve lower limits of quantification (0.0043mgL(-1) for 1,3-DCP and 0.0011mgL(-1) for 3-MCPD) and detection (0.0028mgL(-1) for 1,3-DCP and 0.0008mgL(-1) for 3-MCPD). All the detected concentrations are below the maximum tolerable limit of 0.02mgL(-1). The percentage of recovery obtained from food sample analysis was between 83% and 96%. The new procedure was validated with the AOAC method and showed a comparable performance. The HMDS-TMSOTf derivatization strategy is capable of simultaneously derivatizing 1,3-DCP and 3-MCPD at room temperature, and it also serves as a rapid, sensitive, and accurate analytical method for food samples analysis.
Chrome azurol S immobilised on XAD-2 has been used in this study as a reagent phase for the development of an optical fibre Al(III) sensor. Using a kinetic approach, this sensor was able to give a linear response in the Al(III) concentration range of 1.3 x 10(-5)-2.0 x 10(-4) M with a limit of detection of 1.0 x 10(-4) M. The optimum responses were obtained at pH 6.0 and when the solution was stirred. The sensor response was found to have a repeatability and reproducibility of 1.6% and 5.8%, respectively. The results obtained for Al(III) determination in aqueous sample were in good agreement with those obtained using graphite furnace-atomic absorption spectrometry.
One of the most crucial attributes of synthetic organic chemistry is to design organic reactions under the facets of green chemistry for the sustainable production of chemicals. Thus, due to the intensified environmental and safety concern, the need for new technologies for conducting chemical transformation has grown. In this regard, there is enormous interest in the use of heterogeneous catalysts as they generally avoid the generation of waste, require fewer toxic reagents, as well as entail easier separation and recycling of the catalyst. α,β-Unsaturated acids have been widely used in various industrial applications and have been identified as one of the most promising chemicals obtained via the Knoevenagel condensation reaction. This review aims to discuss the most pertinent heterogeneous catalytic systems such as zeolites, mesoporous silica, ionic liquids, metal oxides, and graphitic carbon nitride-based catalysts in the Knoevenagel reaction. Ultimately, this review focuses not only on the catalyst but also provides an overall idea and guide for the preparation of new catalysts with outstanding properties by looking at the chemical and engineering aspects such as the reaction conditions and the mechanisms.