Dear Label_Name,

Greetings! I hope you are well.

I am writing on behalf of an international publishing house, Science and Education Publishing, USA (http://www.sciepub.com).

Science and Education Publishing (SciEP) is a multidisciplinary open access publisher of Journals covering the fields of Science, Technology and Medicine. All SciEP publications are subject to high-quality peer review, editorial and production processes and are freely available online.

Welcome to the April, 2013 edition of SciEP newsletter, providing monthly summaries of articles on science & education related topics of interest to scientist and professionals. The mission of our journals is to provide an open access forum for publishing new findings on issues pertinent to scientific and academic field. We also invite you to submit original research papers, review articles, short reports, or case studies are considered for publication in our Multidisciplinary Journals.

American Journal of Public Health Research
DOI: 10.12691/ajphr-1-1-3

The Implementation of a Tele-Homecare System with Service Oriented Architecture and HL7 Message Transmission Standard
Ching-Sung Wang

American Journal of Medical and Biological Research
DOI: 10.12691/ajmbr-1-1-2

The Influence of Ethanol on Pyruvate Kinases Activity in Vivo, in Vitro, in Silico
Lelevich Sergey Vladimirovich, Khrustalev Vladislav Victorovich, Barkovsky Eugene Victorovich, Shedogubova Tatyana Aleksandrovna

American Journal of Medical Sciences and Medicine
DOI: 10.12691/ajmsm-1-1-1

Clinical and Histological Features in Wegener Granulomatosis
Li Cavoli Gioacchino, Passantino Rita, Bono Luisa, Tortorici Calogera, Ferrantelli Angelo, Giammarresi Carlo, Rotolo Ugo

American Journal of Infectious Diseases and Microbiology
DOI: 10.12691/ajidm-1-1-2

The Curse of Lymphatic Filariasis: Would the Continual Use of Diethylcarbamazine Eliminate this Scourge in Papua New Guinea?
Anne Lanham, Lillian Mwanri

We have released issues of some journals on February 2013.
American Journal of Public Health Research
American Journal of Medical Sciences and Medicine
American Journal of Medical and Biological Research
American Journal of Pharmacological Sciences
American Journal of Clinical Medicine Research
American Journal of Nursing Research
American Journal of Cancer Prevention
American Journal of Medicine Studies
American Journal of Infectious Diseases and Microbiology
American Journal of Cardiovascular Disease Research
American Journal of Biomedical Research
American Journal of Mechanical Engineering
American Journal of Microbiological Research
Journal of Preventive Medicine
American Journal of Food and Nutrition
American Journal of Hypertension Research
American Journal of Sports Science and Medicine
Journal of Cancer Research and Treatment
American Journal of Zoological Research
Journal of Biomedical Engineering and Technology
American Journal of Microbiological Research
Biomedical Science and Engineering

We are pleased to announce that submissions are now being accepted for peer review for all the journals across all our subject areas in SciEP.

Please submit your manuscript via our online submission system:
http://www.sciepub.com/author/signin

To unsubscribe from our mailing list, please click on the following link: unsubscribe

I am looking forward to hearing from you.

Kind regards,

David Rain
Email:join@sciepub.com
Science and Education Publishing (http://www.sciepub.com)

Experimental Studies on Spectrophotometric Extraction for Estimation of Fe (III) Using an Analytical Reagent

Sonali S. Patil

Department of Chemistry, J.S.M. College, Alibag, Raigad, Maharashtra, India

Abstract: In the present experimental studies, a new reagent 2, 4-dimethyl -3H- 1, 5 benzodiazepine (DBA) is devised for the extractive estimation of Fe (III) from given sample and by use of spectrophotometer as analysis tool. In the laboratory work, the fresh reagent was prepared and its characterization has been carried out with the help of mass spectrophotometer and IR, NMR, elemental analysis. The created analytical reagent (DBA) when reacts with iron produces red complex, this complex can be extracted by using n-butanol as a selected solvent, maintained at constant pH 7.8. The Beer's law is followed in the concentration of 1-10 μg Lit⁻¹ of Fe (III) and the optimum values of maximum absorption, molar extinction coefficient, and sandal’s sensitivity to the red complex, are observed to be 430 nm, 4954 Lit mol⁻¹cm-2 and 0.01203 μg cm⁻² respectively. Accordingly to which it turned out that the reagent is the best for the assessment for estimation of Fe (III) from various sources of samples.

Keywords: Fe (III), Spectrophotometric determination, DBA reagent, molar absorptivity

Received July 22, 2022; Revised August 24, 2022; Accepted September 05, 2022

Citation: Sonali S. Patil, Experimental Studies on Spectrophotometric Extraction for Estimation of Fe (III) Using an Analytical Reagent. Applied Ecology and Environmental Sciences, 10 (9). 568-572. January 2022. doi:10.12691/aees-10-9-2

1. Introduction

The traditional methods such as ion exchange, membrane separations, solvent extraction, and chemical adsorption for removal of heavy metals from industrial wastewater are being used [1,2]. The removal of heavy metals from industrial effluents, to control environmental pollution liquid-liquid extraction is one of the cheapest and effective techniques commonly employed [3-11].

Iron (Fe) is the commonly found metal, in the Pharmaceutical waste, chemical waste and industrial waste. Several research findings show various analytical methods developed for estimation Fe (III) [12,13,14,15,16,17,18]. A spectrophotometric extraction research work formation of a complex between Fe (III) and analytical reagent was studied by Micheal and Dermot [19]. Various analytical reagents were suggested by several researchers to estimate Fe (III) in various samples by spectrophotometric extraction [20,21,22,23].

The above literature survey shows that till date, no work has reported for predications of Fe (III) metal ions by using DBA as an analytical novel reagent. Hence, the attempt is made in present work on the 2, 4 dimethyl-3H-1,5 benzodiazepine fresh, novel reagent for the estimation of minute level quantities of Fe (III) using spectrophotometric extraction.

2. Methodology

2.1. Instrumentation for Experimental Research

During the experimentation the absorbance was measured by using calibrated UV, visible spectrophotometer (Shimadzu 2450 UV-Visible with 10 mm quartz cell) and pH was maintained by using calibrated digital pH meter (Elico LI-120). The parameters maintained during experimentation are depicted in Table 1.

Table 1. Experimental parameters

2.2. Preparation of Analytical Reagent

The analytical reagent is prepared by mixing 1 mole of o-phenylenediamine and 2 moles of Acetyl acetone in the Ethanol as solvent. The mixture obtained is then refluxed for the duration of 2 hrs in the round bottom glass flask. The obtained solution from above process is poured on ice to get crystals. This results a solid product, which is crystallized by using ethanol as a solvent. Further, it is then synthesized and characterized and used as analytical reagent for spectrophotometric identification of Fe (III) ions. A stock solution of above analytical reagent concentration of 0.05% was made ready in a methanol. The reaction scheme is as indicated in Figure 1.

2.3. Stock Solution

An accurately measured amount of ferric chloride was added to purified water, and then diluted to desired quantity.

Figure 1. Reaction for preparation of analytical Reagent 2, 4-Dimethyl -3h- 1,5 benzodiazepine (DBA)

2.4. Effect of pH on Extraction

In this study, different Buffer solutions were used for Fe (III) extraction with varied range of pH from 1 to 11, maintaining constant molar ratio 1:1 between organic phase and an aqueous phase. Figure 2 indicates the variation of absorbance with pH. It is observed from this figure that absorbance increases with increasing pH and touches maximum to the corresponding value of pH 7.8 and thereafter rise in pH, reduces absorbance significantly. Hence, the value of pH 7.8 was used in further investigations

Figure 2. Variation of Absorbance with pH

2.5. Selection Solvent

Different organic solvents were tested in this experimental work to identify the suitability of solvent and presented in Figure 3. The n-butanol is seems to be suitable solvent as indicated in the same figure.

Figure 3. Selection of Solvent

2.6. Selection of Wavelength

We will notice the absorbance in a Figure 4 that increases with increasing wavelength and attains a maximum value of absorbance at the corresponding wavelength of 430 nm for n-butanol as a solvent. Further, increase in wavelength reduces absorbance. This value of wavelength was recommended for further investigations.

Figure 4. Variation of Absorbance with Wavelength

3. Experimental Procedures

In a beaker mix 1 ml solution of ferric chloride (1 to 100 mg), and 0.05% reagent in methanol is thoroughly mixed. The pH is then adjusted to 7.8 by adding the buffer solution. The above solution is then added to separating glass funnel with 10 ml n-butanol. The organic and aqueous phases were separated. The organic phase is then subjected to spectrophotometer at a wavelength of 430 nm.

3.1. Development of Calibration Curve

Figure 5 shows the variation of absorbance with concentration of Fe (III) ions. By following the same method as demonstrated in experimental procedures, the samples of Fe (III) with different concentrations were prepared and its absorbance was measured for development of Calibration curve.

Figure 5. Development of Calibration Curve

3.2. Selection of Molar Ratio between Fe (III) and Analytical Reagent

Figure 6 shows the selection of molar ratio between Fe (III) and analytical reagent using various methods. The Job’s continuous variation method was extensively used for fixation of the composition ratio of the extracted species, and the same results were further validated by using, mole ratio method and slope ratio method. From, these methods a molar ratio between Fe (III) and analytical reagent to be fixed as1: 1.

Figure 6. Selection of molar ratio between Fe (III) and analytical reagent

3.3. Study of the Equilibrium Time

The influence of pulsating time on the extraction was studied in the range of few seconds to 60 minutes. From Figure 7 it was observed that the quantitative extraction was achieved after 10 seconds. The further shaking time has no effect on the percentage extraction of the Fe (III).

Figure 7. Study of Equilibrium time on Fe (III): DBA

3.4. Stability of the Complex with Time

Figure 8 presents the effect of time on stability of extracted species; the stability of extracted species is noticed up to 36 hours. Due to this reason, during the experimentation absorbance measurement was done within 1.25 hour time span.

Figure 8. Influence of time on the stability of extracted species

3.5. Effect of Diverse Ions

Various ions interfere at different concentration range estimation of Fe (III).The positive and negative ions were tested to find their limit in the prediction of Fe (III).The details of such ions and their tolerance limit with minimum error are reported in Table 2. These ions are further suppressed during actual prediction of Fe (III) and presented in Table 3.

Table 2. Influence of diverse ions

Table 3. Suppressing reagents

3.6. Analytical Reagents and Their Limitations

Table 4 presents the comparison between different analytical reagents used in the earlier study and proposed analytical reagent used in the present work. This table clearly indicates that the proposed analytical reagent is appears to perform well over the earlier reported data.

Table 4. Analytical reagents and their limitations

4. Uses of Present Study

This experimental investigation for detection of Fe (III), find a wide application in the areas of industrial, food, and environmental. The proposed analytical reagent seems to be superior as compared to earlier reported data.

Table 5. Use of present study

5. Conclusion

In the present experimental studies, a new organic compound 2, 4-dimethyl -3H- 1, 5 benzodiazepine (DBA) was devised to estimate Fe (III) by using spectrophotometer. The fresh organic compound is observed to be more effective over literature data. The present method is found to be best, simple and effectively applied for estimation of Fe (III) from various sources of samples.

Acknowledgements

The research work was successfully done by Dr. S. S. Patil at the Chemistry Laboratory of JSM College Alibag. The author is thankful to the authorities of the institution; for giving support and cooperation.

Conflict of Interests

With reference to publication of the present paper, author hereby state that no sort of conflict of interest associated to this work.

References

[1]   | Blais, J.F., Dufresne. S. and Mercier G., (1999). State of the art of technologies for metal removal from industrial effluents, Journal of Water Science, 12(4), 687-711.
[2]   | Guards R.L. and Coutinho A.P., (2008). A group contribution method for viscosity estimation of ionic liquids, 266, 195-201.
[3]   | Sosaari P., Srivastava V. and Sillanpää M., (2008). Ionic liquid-based water treatment technologies for organic pollutants: Current status and future prospects of ionic liquid mediated technologies, Science of the Total Environment, 690, 604–619.
[4]   | Gunatilake S.K., (2005).Methods of removing heavy metals from industrial wastewater, Multidisciplinary Engineering Science Studies (JMESS), 1(1), 12-18.
[5]   | Babel, S., and Kurniawan. T.A., (2004). Cr (VI) removal from synthetic wastewater using coconut shell charcoal and commercial activated carbon modified with oxidizing agent’s and/or Chitosan, Chemosphere, 54(7), 951-967.
[6]   | Faur-Brasquet, C., Kadirvelu K., and Le Cloirec, P., (2002). Removal of metal ions from aqueous solutions by adsorption: competition with organic matter, Carbon, 40, 2387-2392.
[7]   | Fu F., and Wang Q., (2011). Removal of heavy metal ions from wastewaters: A review, Journal of Environmental Management, 92(3), 407-418.
[8]   | He J, Yang J., Sarwar M.T., Duan C. and Zhao Y.,(2003). Comparative investigation on copper leaching efficiency from waste mobile phones using various types of ionic liquids, Journal of Cleaner Production, 256, 348-368.
[9]   | Kenntner N., Krone O., Altenkamp R. and Tataruch F., (2003). Environmental contaminants in liver and kidney of free- ranging Northern Goshawks (Accipiter gentilis) from three regions of Germany, Archives of Environmental Contamination and Toxicology, 45(1), 128-135.
[10]   | Li C., and Trost B.M, (2008). Green chemistry for chemical synthesis, 105(36), 13197-13202.
[11]   | Patil S.S. and Lokhande R.S., (2013). Development of an Extractive Spectrophotometric Method for Determination of Cr (VI) using 2, 4-dimethyl -3H- 1, 5 benzodiazepine, International Journal of Applied Chemistry, 9(2), 133-140.
[12]   | P. G. T. Fogg, and R. J. Hall, (1971). Kinetics of the formation of monocomplexes of iron(III) with salicylic acid, sulphosalicylic acid, 8-hydroxyquinoline, and salicylaldehyde, Journal of Chemical Society A, 1365-1370.
[13]   | F. P. Cavasino and E. Di Dio., (1971). Kinetics of the formation of iron(III) monochelates with substituted malonic acids, Journal of Chemical Society A, 3176-3180.
[14]   | N. Kujundzie and M. Pribanic., (1978). Rate and mechanism of the formation of the monohydroxamato complexes of iron(III), Journal of Inorganic and Nuclear Chemistry, 40, 729-731.
[15]   | K. Kustin, R. F. Pastemack, and E. M. Weinstock, (1966). Steric effects in fast metal complex substitution reaction. I, Journal of American Chemical Society, 88, 4610-4615.
[16]   | A. Kowalak, K. Kustin, R. F. Pastemack and S. Petruci., (1967). Steric effects in fast metal complex substitution reactions. II, Journal of American Chemical Society, 89, 3126-3130.
[17]   | P. T. Thomas, and K. N. Raymond., (1981). Coordination chemistry of microbial iron transport compounds Kinetics and mechanism of iron exchange in hydroxamate siderophore complexes, Journal of American Chemical Society, 103, 6617-6624.
[18]   | M. Birus, N. Kujundzik, and M. Pribanic.,(1984). Iron (III) complexation by desferrioxamine B in acidic aqueous solutions. Kinetics and mechanism of the formation and hydrolysis of the binuclear complex diferrioxamine B, Inorganic Chemistry, 23, 2170-2191.

[19]  
J. H. Micheal, and F. K. Dermot., (1991).Reactions of metal ions with protonated ligands. Kinetics and mechanisms of the reactions of iron(III) with heptane-2,4,6-trione (H2hto), 1-phenylhexane 1,3,5-trione (H2phto) and 1,5-diphenylpentane1,3,5-trione (H2dppto) in methanol-water (70: 30 vol./vol.) at 25°C and I=0.5 mol dm-3, Inorganica Chimica Acta, 187, 159-165.

[20]   | K. Ogava, and N. Tobe., (1966). A spectrophotometric study of the complex formation between Iron (III) and sulfosalicylic acid, Bulletin of Chemical Society of Japan, 39, 223-227.
[21]   | Lutfullah, S. Sharma, N. Rahman, S. N. H. Azmi, H. J. S. Al Hidaifi, and M. E. M. Alqasmi., (2010). Spectrophotometric determination of Fe(III) via complexation with piroxicam in synthetic mixture and soil samples, Journal of Scientific and Industrial Research, 69: 135-141.
[22]   | M. Sun, and M. Lu., (2016). Spectrophotometric determination of trace iron in Fe (III)-potassium thiocyanate methyl violet polyvinyl alcohol system, Indian Journal of Advances in Chemical Science 4(3), 302-307.
[23]   | S. Khan, R. Dashora, A. K. Goswamy, and D. N. Purohith., (2004). Review of spectrophotometric methods for determination of iron, Reviews in Analytical Chemistry 23, 1-4.