Mineralogical Analysis of Historical Mortars by FTIR

A method for quantitative mineralogical analysis by ATR-FTIR [1] has been used first time for analysis of historical mortars. Mixtures of different minerals and gypsum were used in order to measure the minimum band intensity that must be considered for calculations and the detection limit. In this way, the molar absorptivity coefficient in the Lambert–Beer law and the components of a mixture in mol percentage can be calculated. The GAMS equation modeling environment and the NLP solver CONOPT (©ARKI Consulting and Development) were used to correlate the experimental data in the samples considered. The characterization of the vernacular mortars by FTIR analysis identifies the predominant minerals of the samples, and in conjunction with XRF and XRD, shows the exact composition of historical mortars, which will optimize the restoration and conservation of monuments, preserving our heritage.

Measurement of Capsaicinoids in Chiltepin Hot Pepper: A Comparison Study between Spectrophotometric Method and High Performance Liquid Chromatography Analysis

Direct spectrophotometric determination of capsaicinoids content in Chiltepin pepper was investigated as a possible alternative to HPLC analysis. Capsaicinoids were extracted from Chiltepin in red ripe and green fruit with acetonitrile and evaluated quantitatively using the HPLC method with capsaicin and dihydrocapsaicin standards. Three samples of different treatment were analyzed for their capsaicinoids content successfully by these methods. HPLC-DAD revealed that capsaicin, dihydrocapsaicin, and nordihydrocapsaicin comprised up to 98% of total capsaicinoids detected. The absorbance of the diluted samples was read on a spectrophotometer at 215–300 nm and monitored at 280 nm. We report herein the comparison between traditional UV assays and HPLC-DAD methods for the determination of the molar absorptivity coefficient of capsaicin (ε280=3,410andε280=3,720 M−1 cm−1) and dihydrocapsaicin (ε280=4,175andε280=4,350 M−1 cm−1), respectively. Statistical comparisons were performed using the regression analyses (ordinary linear regression and Deming regression) and Bland-Altman analysis. Comparative data for pungency was determined spectrophotometrically and by HPLC on samples ranging from 29.55 to 129 mg/g with a correlation of 0.91. These results indicate that the two methods significantly agree. The described spectrophotometric method can be routinely used for total capsaicinoids analysis and quality control in agricultural and pharmaceutical analysis.

A High Molar Extinction Coefficient Ru(II) Complex Functionalized withcis-Dithiocyanato-bis-(9-anthracenyl-10-(2-methyl-2-butenoic acid)-1,10-phenanthroline): Potential Sensitizer for Stable Dye-Sensitized Solar Cells

New heteroleptic ruthenium(II) complex was formulated as [Ru(L1)2(NCS)2], where L1= 9-anthracenyl-10-(2-methyl-2-butenoic acid)-1,10-phenanthroline was synthesized and its photophysical properties were studied and compared to previously reported analogue complex containing no anthracene moiety [Ru(L2)2(NCS)2], L2= (2-methyl-2-butenoic acid)-1,10-phenanthroline. The two complexes though exhibit very strong molar extinction coefficient values; however, [Ru(L1)2(NCS)2] shows better characteristic broad and intense metal-to-ligand charge transfer (MLCT) absorption band and higher molar absorptivity coefficient at (λmax=522 nm,ε=6.60×104 M−1 cm−1) than that of [Ru(L2)2(NCS)2] complex, (λmax=446 nm,ε=4.82×104 M−1 cm−1). At room temperature, long wavelength emissions with strong intensity ratio centered at 660 nm were recorded for [Ru(L1)2(NCS)2] complex with a bathochromic shift (λem=700 nm) for [Ru(L2)2(NCS)2] complex. It was shown that the luminescence wavelength characteristic of the complexes may be a function relating to the increasing length ofπ-conjugation and/or molecular weight. A preliminary cyclic voltammetry of [Ru(L1)2(NCS)2] complex also exhibits good electroredox activity with oxidation potential of about 1.04 V, significantly better than other Ru(II) polypyridine complexes containing bidentate ligands.

Phenylmethoxybis(tetrazolium) ion-association complexes with an anionic indium(III) — 4-(2-pyridylazo)resorcinol chelate

Complex formation and liquid-liquid extraction were studied in systems containing indium(III), 4-(2-pyridylazo)resorcinol (PAR), phenylmethoxybis(tetrazolium) salt (MBT), water and chloroform. The following MBTs, which differ only by the number of -NO2 groups in their cationic parts, were used: 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis(2,5-diphenyl-2H-tetrazolium chloride) (Blue Tetrazolium chloride, BT), 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis[2-(4-nitrophenyl)-5-phenyl-2H-tetrazolium chloride] (Nitro Blue Tetrazolium chloride, NBT) and 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)bis[2,5-di(4-nitrophenyl)-2H-tetrazolium chloride] (Tetranitro Blue Tetrazolium chloride, TNBT). The composition of the formed ternary complexes was determined, In:PAR:MBT=1:2:2, and the optimum conditions for their extraction found: pH, shaking time, concentration of the reagents and the sequence of their addition. Some key constants were estimated: constants of extraction (Kex), constants of association (β) and constants of distribution (KD). BT appears to be the best MBT for extraction of the In(III)-PAR species, [In3+(OH)3(PAR)2]4−, (Log Kex=10.9, Log β=9.8, Log KD=1.12, R%=92.7%). Several additional characteristics concerning its application as extraction-spectrophotometric reagent were calculated: limit of detection (LOD = 0.12 µg cm−3), limit of quantification (LOD = 0.40 µg cm−3) and Sandell’s sensitivity (SS =1.58 ng cm−2); Beer’s law is obeyed for In(III) concentrations up to 3.2 µg mL−1 with a molar absorptivity coefficient of 7.3×104 L mol−1 cm−1 at λmax=515 nm.

Photometric Analysis Reagents of Rare Earths and their Application in Metallurgical Analysis

In this paper, photometric analysis reagents of rare earths and their application in metallurgical analysis at home and abroad in the past 10 years was reviewed, pertaining especially to various coloring reagents of rare earths and its conditions of coloring reaction, the maximum absorption wavelength, molar absorptivity coefficient, limit of detaction, as well as interference and application of corresponding methods. The key application in the determination of actual samples was summarized for it is very important to eliminate the effect of interfering ions. The purpose is to provide help to establish new analysis methods of high sensitivity and selectivity in the future. 52 references are cited.

Ternary complexes of vanadium(IV) with 4-(2-pyridylazo)-resorcinol (PAR) and ditetrazolium chlorides (DTC)

Complex formation and liquid-liquid extraction have been studied for ternary complexes of vanadium(IV) with 4-(2-pyridylazo)-resorcinol (PAR) and ditetrazolium chlorides (DTC) in a water-chloroform medium. The specific ditetrazolium compounds investigated were i) 3,3′-(4,4′-biphenylene)-bis(2,5-diphenyl-2H-tetrazolium) chloride (Neotetrazolium chloride, NTC); ii) 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)-bis(2,5-diphenyl-2H-tetrazolium) chloride (Blue Tetrazolium chloride, BTC); and iii) 3,3′-(3,3′-dimetoxy-4,4′-biphenylene)-bis[2-(4-nitrophenyl)-5-phenyl-2H-tetrazolium] chloride (Nitro Blue Tetrazolium chloride, NBT). Molar absorptivity coefficients and the composition of the complexes have been calculated. Association constants (β) have also been obtained for the interactions between the vanadium(IV) — PAR anionic chelates [VO(PAR)2]2− (I) and [VO(OH)2(PAR)2]4− (II), and ditetrazolium cations (DT2+). Some special features of NBT as an extraction-spectrophotometric reagent for vanadium(IV) have been discussed. Unlike NTC and BTC which form complexes with both I and II, NBT associates only with II. The pH interval for complete extraction of (NBT2+)2[VO(OH)2(PAR)2] is broader and allows work at lower pH values the other ion-associates of V(IV,V)-PAR that were studied. NBT is -therefore the appropriate reagent both for direct V(IV) determination and for V(IV)/V(V) separation. Some additional characteristics for the V(IV)-PAR-NBT-water-chloroform system have been determined: extraction constant, distribution constant, recovery factor, limit of detection and limit of quantification. Beer’s law is valid up to 1.4 μg mL−1 vanadium(IV) with molar absorptivity coefficient of 3.55×104 L mol−1 cm−1 at λmax=559 nm.