scholarly journals Derivative Zero - Crossing Spectrophotometry Of Binary Mixtures Of Acetyl Acetonates Of Micro – Amounts Of Mn (Ii) And Al (Iii).

2013 ◽  
Vol 10 (3) ◽  
pp. 866-882
Author(s):  
Baghdad Science Journal

New derivative molecular absorption spectrophotometric methods have been developed for the determination of Al (III) , Mn (II) , individually and binary mixtures . The aim of this model of study is to obtain analytical results characterized by adequate standard of analytical figures of merits through application of derivative Spectrophotometry (dnA/d?n). The two metals acetyl acetonates are chemically stable and are widely used as catalysts . Where Interferences are probable due to very close or nearby peaks or Summits, the Zero – Crossing derivative measurement technique is used to avoid interfering effects between two metals pairs.

1992 ◽  
Vol 75 (4) ◽  
pp. 678-684 ◽  
Author(s):  
Espinosa A Mansilla ◽  
F Salinas ◽  
Berzas J J Nevado

Abstract Derivative spectrophotometric methods have been developed for determining furfural and hydroxymethylfurfural and for resolving their binary mixtures on the basis of the UV spectra and the Winkler reaction. The latter method permits the simultaneous determination of both compounds in orange and grapefruit juices without previous separations.


2014 ◽  
Vol 2014 ◽  
pp. 1-11 ◽  
Author(s):  
Fatma Turak ◽  
Mithat Dinç ◽  
Öznur Dülger ◽  
Mahmure Ustun Özgür

Four simple, rapid, and accurate spectrophotometric methods were developed for the simultaneous determination of two food colorants, Carmoisine (E122) and Ponceau 4R (E124), in their binary mixtures and soft drinks. The first method is based on recording the first derivative curves and determining each component using the zero-crossing technique. The second method uses the first derivative of ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of the binary mixture by that of one of the components. The third method, derivative differential procedure, is based on the measurement of difference absorptivities derivatized in first order of solution of drink samples in 0,1 N NaOH relative to that of an equimolar solution in 0,1 N HCl at wavelengths of 366 and 451 nm for Carmoisine and Ponceau 4R, respectively. The last method, based on the compensation method is presented for derivative spectrophotometric determination of E122 and E124 mixtures with overlapping spectra. By using ratios of the derivative maxima, the exact compensation of either component in the mixture can be achieved, followed by its determination. These proposed methods have been successfully applied to the binary mixtures and soft drinks and the results were statistically compared with the reference HPLC method (NMKL 130).


2013 ◽  
Vol 2013 ◽  
pp. 1-9 ◽  
Author(s):  
Fatma Turak ◽  
Mahmure Ustun Ozgur

Two simple spectrophotometric methods have been proposed for simultaneous determination of two colorants (Indigotin and Brilliant Blue) and two sweeteners (Acesulfame-K and Aspartame) in synthetic mixtures and chewing gums without any prior separation or purification. The first method, derivative spectrophotometry (ZCDS), is based on recording the first derivative curves (for Indigotin, Brillant Blue, and Acesulfame-K) and third-derivative curve (for Aspartame) and determining each component using the zero-crossing technique. The other method, ratio derivative spectrophotometry (RDS), depends on application ratio spectra of first- and third-derivative spectrophotometry to resolve the interference due to spectral overlapping. Both colorants and sweeteners showed good linearity, with regression coefficients of 0.9992–0.9999. The LOD and LOQ values ranged from 0.05 to 0.33 μgmL−1and from 0.06 to 0.47 μgmL−1, respectively. The intraday and interday precision tests produced good RSD% values (<0.81%); recoveries ranged from 99.78% to 100.67% for all two methods. The accuracy and precision of the methods have been determined, and the methods have been validated by analyzing synthetic mixtures containing colorants and sweeteners. Two methods were applied for the above combination, and satisfactory results were obtained. The results obtained by applying the ZCDS method were statistically compared with those obtained by the RDS method.


2013 ◽  
Vol 96 (6) ◽  
pp. 1377-1386 ◽  
Author(s):  
Fatma Turak ◽  
Mahmure Ustun Ozgur

Abstract Four simple, rapid, sensitive, and accurate spectrophotometric methods were developed for the simultaneous determination of Allura Red (AR) and Ponceau 4R (P) without previous chemical separation. The first method, derivative spectrophotometry, depends on first derivative spectrophotometry with zero-crossing and peak-to-base measurement. The second method, derivative ratio spectrophotometry, uses the first derivative of the ratio spectra. The ratio spectra are obtained by dividing the absorption spectra of a binary mixture by that of one of the components. The third method, differential derivative spectrophotometry, is based on the measurement of the difference absorptivities derivatized in the first order of a sample extract in 0.1 M NaOH relative to that of an equimolar solution in 0.1 M HCI. The fourth method, based on the compensation technique, is presented for the derivative spectrophotometric determination of binary mixtures with overlapping spectra by using ratios of the derivative maximum or minimum; the exact compensation of either component in the mixture can be achieved, followed by its determination. All the proposed methods were successfully applied to the determination of the colorants in their laboratory mixtures and granulated drinks without any interference by the ingredients. AR and P showed good linearity, with regression coefficients of 0.9994–0.9999. The LOD and LOQ values ranged from 0.059 to 0.102 and 0.198 to 0.341 μg/mL, respectively. The intraday and interday precision tests produced good RSD values (&lt;1.37%); recoveries ranged from 98.75 to 100.37% for all four methods. The common ingredients and additives did not interfere in the AR and P determination. The results of the proposed methods were statistically compared with the results of an HPLC method given in the literature (Nordic Committee on Food Analysis; NMKL 130) at the 95% confidence level by Student's t-test and the variance ratio F-test. No statistically significant difference was found among these methods.


2019 ◽  
Vol 2019 ◽  
pp. 1-11
Author(s):  
Shilan A. Omer ◽  
Nabil A. Fakhre

In this study, three simple and accurate spectrophotometric methods for simultaneous determination of pyriproxyfen and chlorothalonil residues in cucumbers and cabbages grown in experimental greenhouse were studied. The first method was based on the zero-crossing technique measurement for first and second derivative spectrophotometry. The second method was based on the first derivative of the ratio spectra. However, the third method was based on mean centering of ratio spectra. These procedures lack any previous separation steps. The calibration curves for three spectrophotometric methods are linear in the concentration range of 1–30 μg·mL−1 and 0.5–7 μg·mL−1 for pyriproxyfen and chlorothalonil successively. The recoveries ranged from 82.12–97.40% for pyriproxyfen and 81.51–97.04% for chlorothalonil with relative standard deviations less than 4.95% and 5.45% in all instances for pyriproxyfen and chlorothalonil, respectively. The results obtained from the proposed methods were compared statistically by using one-way ANOVA, and the results revealed there were no significant differences between ratio spectra and mean centering methods with the zero-crossing technique. The proposed methods are successfully applied for the simultaneous estimation of the residue of both pesticides in cucumber and cabbage samples.


2007 ◽  
Vol 90 (1) ◽  
pp. 128-141 ◽  
Author(s):  
Abd El-Maaboud I Mohamed ◽  
Osama H Abdelmageed ◽  
Ibrahim H Refaat

Abstract Simple chemometrics-assisted spectrophotometric methods are described for determination of 2 antibacterial binary mixtures. The mixtures are composed of norfloxacin in combination with tinidazole and erythromycin (as ethylsuccinate ester or stearate salt) in combination with trimethoprim. The normal UV absorption spectra of each pair of drugs in the studied mixtures, in the range of 200-400 nm, showed a considerable degree of spectral overlapping: 77.5% for the norfloxacintinidazole mixture and 84.3% for the erythromycintrimethoprim mixture. Resolution of the norfloxacintinidazole mixture and trimethoprim in the presence of erythromycin was accomplished successfully by using zero-crossing first derivative (1D), classical least-squares (CLS) regression analysis, and principal component regression (PCR) analysis methods. In addition, an alternative simple and accurate colorimetric method was developed for the determination of erythromycin in the presence of trimethoprim using 2,4-dinitrophenylhydrazine. All variables affecting the development of the colored chromogen were studied and optimized, and the product was measured at 526-529 and 538-542 nm for erythromycin stearate and erythromycin ethylsuccinate, respectively. For zero-crossing, first derivative technique Beer’s law was obeyed in the general concentration range of 250 μg/mL for norfloxacin, tinidazole, and trimethoprim with good correlation coefficients (0.9994-0.9996). Overall limits of detection (LOD) and quantification (LOQ) ranged from 0.59 to 2.81 and 1.96 to 9.33 μg/mL, respectively. The obtained results from CLS and PCR were compared with those obtained from a 1D spectrophotometric method. With the exception of erythromycin, overall recoveries in the average range of 97.33-103.0% were obtained with a considerable degree of accuracy when the suggested methods were applied to analysis of synthetic binary mixtures, some commercial dosage forms such as tablets and oral suspension without interference from the commonly encountered excipients and additives. For the colorimetric method, Beer's law was obeyed in the general concentration range of 7.21-28.84 μg/mL erythromycin with good correlation coefficients (0.9980-0.9996). Overall LOD and LOQ ranged from 0.73 to 1.65 and 2.43-5.49 μg/mL, respectively. Erythromycin derivatives were determined in the commercial dosage form, without interference from trimethoprim-encountered excipients and additives. The obtained results, with both chemometric and colorimetric methods, have been compared with those obtained from reported methods, and proper F- and t-values were observed, indicating no significant difference between the results of the suggested methods and reported method(s). The good percentage recoveries and proper statistical data obtained proved the efficiency of the proposed procedures for the determination of the studied drugs in their binary mixtures as well as in the commercial dosage forms with quite satisfactory precision.


2009 ◽  
Vol 74 (12) ◽  
pp. 1455-1465 ◽  
Author(s):  
Valéria Guzsvány ◽  
Zsigmond Papp ◽  
Sanja Lazic ◽  
Ferenc Gaál ◽  
Luka Bjelica ◽  
...  

A simple first-order derivative spectrophotometric method was developed for the simultaneous determination of imidacloprid and 6-chloronicotinic acid (6-CNA). By using the zero-crossing approach, imidacloprid was determined at 249 nm and 6-CNA at 236 nm with detection limits of 0.32 and 0.17 ?g mL-1, respectively, and relative standard deviations not exceeding 1.2 % in the case of model systems. The proposed method was applied for the determination of imidacloprid and 6-CNA in commercial formulations. A conventional spectrophotometric method (at 270 nm) was also employed for the determination of the content of imidacloprid in the same commercial formulations. The results of the developed spectrophotometric methods were in good agreement with those obtained by the high-performance liquid chromatographic method.


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