Electrochemical Analysis: Studies of Acids, Bases, and Salts by Emf, Conductance, Optical, and Kinetic Methods July 1965 to June 1966

Total Page:16

File Type:pdf, Size:1020Kb

Electrochemical Analysis: Studies of Acids, Bases, and Salts by Emf, Conductance, Optical, and Kinetic Methods July 1965 to June 1966 onal Bureau 01 avauuo*" jibrary, N.W. Bldg NBS 400 ELECTROCHEMICAL ANALYSIS: STUDIES OF ACIDS, BASES, AND SALTS BY EMF, CONDUCTANCE, OPTICAL, AND KINETIC METHODS JULY 1965 TO JUNE 1966 1: I Edited by Roger G. Bates IBSI Hi '.:::.: +** ° F t *oA U.S. DEPARTMENT OF COMMERCE National Bureau of Standards ' *<">cau of THE NATIONAL BUREAU OF STANDARDS The National Bureau of Standards is a principal focal point in the Federal Government for assur- ing maximum application of the physical and engineering sciences to the advancement of technology in industry and commerce. Its responsibilities include development and maintenance of the national standards of measurement, and the provisions of means for making measurements consistent with those standards; determination of physical constants and properties of materials; development of methods for testing materials, mechanisms, and structures, and making such tests as may be neces- sary, particularly for government agencies; cooperation in the establishment of standard practices for incorporation in codes and specifications; advisory service to government agencies on scientific and technical problems; invention and development of devices to serve special needs of the Govern- ment; assistance to industry, business, and consumers in the development and acceptance of com- mercial standards and simplified trade practice recommendations; administration of programs in cooperation with United States business groups and standards organizations for the development of international standards of practice; and maintenance of a clearinghouse for the collection and dissemination of scientific, technical, and engineering information. The scope of the Bureau's activities is suggested in the following listing of its three Institutes and their organizational units. Institute for Basic Standards. Applied Mathematics. Electricity. Metrology. Mechanics. Heat. Atomic Physics. Physical Chemistry. Laboratory Astrophysics.* Radiation Physics. Radio Standards Laboratory:* Radio Standards Physics; Radio Standards Engineering. Office of Standard Reference Data. Institute for Materials Research. Analytical Chemistry. Polymers. Metallurgy. Inorganic Mate- rials. Reactor Radiations. Cryogenics.* Materials Evaluation Laboratory. Office of Standard Refer- ence Materials. Institute for Applied Technology. Building Research. Information Technology. Performance Test Development. Electronic Instrumentation. Textile and Apparel Technology Center. Technical Analysis. Office of Weights and Measures. Office of Engineering Standards. Office of Invention and Innovation. Office of Technical Resources. Clearinghouse for Federal Scientific and Technical Information.** Located at Boulder, Colorado, 80302. ** Located at 5285 Port Royal Road, Springfield, Virginia, 22151. UNITED STATES DEPARTMENT OF COMMERCE • John T. Connor, Secretary NATIONAL BUREAU OF STANDARDS • A. V. Astin, Director NBS TECHNICAL NOTE 400 Issued September 6, 1966 ELECTROCHEMICAL ANALYSIS: STUDIES OF ACIDS, BASES, AND SALTS BY EMF, CONDUCTANCE, OPTICAL, AND KINETIC METHODS JULY 1965 TO JUNE 1966 Edited by Roger G. Bates Electrochemical Analysis Section Analytical Chemistry Division Institute for Materials Research NBS Technical Notes are designed to supplement the Bureau's regular publications program. They provide a means for making available scientific data that are of transient or limited interest. Technical Notes may be listed or referred to in the open literature. For sale by the Superintendent of Documents, U.S. Government Printing Office Washington, D.C., 20402 - Price 55 cents FOREWORD The Analytical Chemistry Division was established as a separate division at the National Bureau of Standards on September 1, 196j>, and became part of the Institute for Materials Research in the February 1, 1964, reorganization. It consists at present of nine sections and about 100 tech- nical personnel encompassing some 45 different analytical competences from activation analysis and atomic absorption to vacuum fusion and X-ray spectroscopy. These competences, and in turn the sections which they comprise, are charged with research at the forefront of analysis as well as aware- ness of the practical sample, be it standard reference material or service analysis. In addition it is their responsibility to inform others of their efforts. Formal publication in scientific periodicals is highly important. In addition, however, it has been our experi- ence that informal, annual summaries of progress describing efforts of the past year can be very valuable in disseminat- ing information. At the National Bureau of Standards such publications fit logically into the category of a Technical Note. In 1966 we plan to issue these summaries for all of our sections. The following is the second annual report on progress of the Electrochemical Analysis Section. W. Wayne Meinke, Chief Analytical Chemistry Division ii PREFACE This is the second in a series of annual progress reports of the Electrochemical Analysis Section of the Analytical Chemistry Division. The report covers the fiscal year 1966, which "began on July 1, 1965, and ended on June 30, 1966. Many of the processes and reactions of analytical interest take place in solutions, and a large fraction of these involve ionized solutes. If the research programs of the Electrochemical Analysis Section were to "be placed in a single broad category, undoubtedly "Solution Electro- chemistry" would "be a. fair choice, with primary emphasis on acid-base phenomena, solvent effects on the behavior of electrolytes, and potentiometry with reversible electrodes. Competence in polarography and coulometry exists elsewhere in the Analytical Chemistry Division] hence, these areas are not a part of the research activity of the Electro- chemical Analysis Section. In line with a uniform policy of the Division, the Section's programs have both research and sample aspects. During the fiscal year Just ending, about 70 percent of the total effort was devoted to re- search, while 20 percent was devoted to programs on Standard Reference Materials and 10 percent to Other-Agency programs. The outstanding event of the present year was the long- awaited move to the excellent new facility at Gaithersburg, Md. The move and the attendant loss of time during re- settlement have inevitably left their mark on the Section's activity* More serious, however, has been a shortage of personnel. Two project leaders, Dr. Robert Gary and Dr. Richard K. Wolford, were chosen as Science and Technology Fellows and were assigned elsewhere in the Department of Commerce for 10 months of the reporting period. iii A third, Dr. Marion M. Davis, retired from the Section on December J51, 1965. On the other hand, Dr. Paul W. Schindler spent nine months in the Section as a guest worker supported by the Swiss National Foundation. The purpose of this report is to summarize the broad program of the Electrochemical Analysis Section and to convey also the manner in which the individual projects contribute to the whole. An attempt is made to set forth in a rather complete way the entire year's activity of the Section and to reveal the ways in which this specialized group contributes to the missions of the Division and Institute of which it is a part. In order to specify adequately the procedures, it has been necessary occasionally to identify commercial materi- als and equipment in this report In no case does such identification imply recommendation or endorsement by the National Bureau of Standards, nor does it imply that the material or equipment identified is necessarily the best available for the purpose. The assistance of Mrs. Rosemary Maddock and Mrs. Marguerite Rauderibush in the preparation of this report is gratefully acknowledged. Roger G. Bates, Chief Electrochemical Analysis Section Washington, D.C. June , 1966 IV TABLE OF CONTENTS PAGE 1. FACILITIES AND EQUIPMENT 1 The Gaithersburg Laboratories ........ 1 Plans and Needs 5 2. MEASUREMENT OF ACIDITY 5 Concepts and Program 5 pH Standards 10 Redetermination of the pH of Potassium Hydrogen Phthalate, Primary pH Standard 10 Method ..... 10 Procedures 11 Results 11 Certification of a New Lot of Potassium Dihydrogen Phosphate ..... 1^ Sodium Hydrogen Succinate, a New Standard Reference Material for pH Measurements . 15 Standard pH Values for 4-Aminopyridine Buffers in 50 Percent Methanol 17 Standards for a pD Scale in Deuterium Oxide. 19 A Scale of Acid Strengths in Benzene 21 Experimental 21 Discussion 22 3. SOLVENT EFFECTS ON ACID-BASE PROCESSES .... 25 Dissociation of Positively-Charged Acids in Methanol-Water Solvents 25 Ammonium Ion 28 Tris (hydroxymethyl )methylammonium Ion 30 Solubility Studies of the Medium Effect ^2 Parameters for the Solvent Effect. 35 Isotope Effects on the Dissociation of Acetic Acid in Water and Deuterium Oxide . 59 v PAGE Acid-Base Behavior in Organic Solvents with Low Dielectric Constants . 45 Spectrophotometry Studies of the Dissociation of Phenols 46 4. EQUILIBRIUM STUDIES OP SYSTEMS OF ANALYTICAL INTEREST 48 Thermodynamics of the Dissociation of Morpholinium Ion in Water ......... 48 Ionization Constant of Deuterium Oxide from 5 to 50 °C 51 Response of the Glass Electrode in Heavy Water 56 5. THERMODYNAMIC STUDIES OF AQUEOUS SOLUTIONS OF MIXED SALTS . 60 6. CONDUCTOMETRIC DETERMINATION OF TRACES OF WATER 63 Objectives and Principle of Method ...... 63 Modification of Apparatus 63 Calibration with Water 68 Analysis of Errors ..... 71 Status of the Project ...... 73 7. KINETIC TECHNIQUES IN TRACE ANALYSIS 74 8.
Recommended publications
  • Chemistry Grade Level 10 Units 1-15
    COPPELL ISD SUBJECT YEAR AT A GLANCE ​ ​ ​ ​​ ​ ​​ ​ ​ ​ ​ ​ ​ GRADE HEMISTRY UNITS C LEVEL 1-15 10 Program Transfer Goals ​ ​ ​ ​ ● Ask questions, recognize and define problems, and propose solutions. ​ ​​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ● Safely and ethically collect, analyze, and evaluate appropriate data. ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ● Utilize, create, and analyze models to understand the world. ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ● Make valid claims and informed decisions based on scientific evidence. ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ● Effectively communicate scientific reasoning to a target audience. ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ PACING 1st 9 Weeks 2nd 9 Weeks 3rd 9 Weeks 4th 9 Weeks ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ Unit 1 Unit 2 Unit 3 Unit 4 Unit 5 Unit 6 Unit Unit Unit Unit Unit Unit Unit Unit Unit ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ 7 8 9 10 11 12 13 14 15 1.5 wks 2 wks 1.5 wks 2 wks 3 wks 5.5 wks ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ 1.5 2 2.5 2 wks 2 2 2 wks 1.5 1.5 ​ ​ ​ ​ wks wks wks wks wks wks wks Assurances for a Guaranteed and Viable Curriculum ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ Adherence to this scope and sequence affords every member of the learning community clarity on the knowledge and skills ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ on which each learner should demonstrate proficiency. In order to deliver a guaranteed and viable curriculum, our team ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ commits to and ensures the following understandings: ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ ​ Shared Accountability: Responding
    [Show full text]
  • Chapter 9 Titrimetric Methods 413
    Chapter 9 Titrimetric Methods Chapter Overview Section 9A Overview of Titrimetry Section 9B Acid–Base Titrations Section 9C Complexation Titrations Section 9D Redox Titrations Section 9E Precipitation Titrations Section 9F Key Terms Section 9G Chapter Summary Section 9H Problems Section 9I Solutions to Practice Exercises Titrimetry, in which volume serves as the analytical signal, made its first appearance as an analytical method in the early eighteenth century. Titrimetric methods were not well received by the analytical chemists of that era because they could not duplicate the accuracy and precision of a gravimetric analysis. Not surprisingly, few standard texts from the 1700s and 1800s include titrimetric methods of analysis. Precipitation gravimetry developed as an analytical method without a general theory of precipitation. An empirical relationship between a precipitate’s mass and the mass of analyte— what analytical chemists call a gravimetric factor—was determined experimentally by taking a known mass of analyte through the procedure. Today, we recognize this as an early example of an external standardization. Gravimetric factors were not calculated using the stoichiometry of a precipitation reaction because chemical formulas and atomic weights were not yet available! Unlike gravimetry, the development and acceptance of titrimetry required a deeper understanding of stoichiometry, of thermodynamics, and of chemical equilibria. By the 1900s, the accuracy and precision of titrimetric methods were comparable to that of gravimetric methods, establishing titrimetry as an accepted analytical technique. 411 412 Analytical Chemistry 2.0 9A Overview of Titrimetry We are deliberately avoiding the term In titrimetry we add a reagent, called the titrant, to a solution contain- analyte at this point in our introduction ing another reagent, called the titrand, and allow them to react.
    [Show full text]
  • Titration Endpoint Challenge
    Analytical and Bioanalytical Chemistry (2019) 411:1–2 https://doi.org/10.1007/s00216-018-1430-y ANALYTICAL CHALLENGE Titration endpoint challenge Diego Alejandro Ahumada Forigua1 & Juris Meija2 Published online: 1 January 2019 # Springer-Verlag GmbH Germany, part of Springer Nature 2018 We would like to invite you to participate in the Analytical practical aspects related to the sources of uncertainty of Challenge, a series of puzzles to entertain and challenge our this technique. readers. This special feature of “Analytical and Bioanalytical Origins of titrimetry date back to 1690s, when Wilhelm Chemistry” has established itself as a truly unique quiz series, Homberg (1652–1715) published the first report related to with a new scientific puzzle published every three months. an acidity measurement [1]. Several decades later Claude Readers can access the complete collection of published prob- Geoffroy (1729–1753) used this method to determine the lems with their solutions on the ABC homepage at http://www. strength of vinegar by adding small amounts of potassium springer.com/abc. Test your knowledge and tease your wits in carbonate until the no further effervescence was observed diverse areas of analytical and bioanalytical chemistry by [2]. William Lewis (1708–1781), who is also considered one viewing this collection. of the early pioneers of titration, recognized the difficulty in In the present challenge, titration is the topic. And please determining the endpoint of the titration through the process note that there is a prize to be won (a Springer book of your of cessation of effervescence, so he suggested the use of color choice up to a value of €100).
    [Show full text]
  • Analytical Chemistry Laboratory Manual 2
    ANALYTICAL CHEMISTRY LABORATORY MANUAL 2 Ankara University Faculty of Pharmacy Department of Analytical Chemistry Analytical Chemistry Practices Contents INTRODUCTION TO QUANTITATIVE ANALYSIS ......................................................................... 2 VOLUMETRIC ANALYSIS .............................................................................................................. 2 Volumetric Analysis Calculations ................................................................................................... 3 Dilution Factor ................................................................................................................................ 4 Standard Solutions ........................................................................................................................... 5 Primary standard .............................................................................................................................. 5 Characteristics of Quantitative Reaction ......................................................................................... 5 Preparation of 1 L 0.1 M HCl Solution ........................................................................................... 6 Preparation of 1 L 0.1 M NaOH Solution ....................................................................................... 6 NEUTRALIZATION TITRATIONS ...................................................................................................... 7 STANDARDIZATION OF 0.1 N NaOH SOLUTION ......................................................................
    [Show full text]
  • Comparison of Vitamin C Content in Citrus Fruits by Titration and High Performance Liquid Chromatography (HPLC) Methods
    International Food Research Journal 24(2): 726-733 (April 2017) Journal homepage: http://www.ifrj.upm.edu.my Comparison of vitamin C content in citrus fruits by titration and high performance liquid chromatography (HPLC) methods 1Fatin Najwa, R. and 1,2*Azrina, A. 1Department of Nutrition and Dietetics, Faculty of Medicine and Health Sciences, 43400 UPM Serdang, Selangor, Malaysia 2Research Centre of Excellence, Nutrition and Non-communicable Diseases, Faculty of Medicine and Health Sciences, Universiti Putra Malaysia, 43400 UPM Serdang, Selangor, Malaysia Article history Abstract Received: 29 June 2015 Vitamin C is one of the essential vitamins for human and animal. Many methods were Received in revised form: developed for the determination of vitamin C such as spectrophotometry, electrophoresis, 23 March 2016 titration, and high performance liquid chromatography (HPLC). This study aims to compare Accepted: 4 April 2016 vitamin C content of citrus fruits (orange, grapefruit, lemon, lime, kaffir lime and musk lime) using indophenol titration and HPLC-PDA methods. In the titration method, orange has the highest vitamin C content (58.30 mg/100g) followed by grapefruit (49.15 mg/100g), lemon Keywords (43.96 mg/100g), kaffir lime (37.24 mg/100g), lime (27.78 mg/100g) and musk lime (18.62 Vitamin C mg/100g). While, in the HPLC method orange also leads with the highest vitamin C content Ascorbic acid (43.61 mg/100g) followed by lemon (31.33 mg/100g), grapefruit (26.40 mg/100g), lime (22.36 Citrus fruits mg/100g), kaffir lime (21.58 mg/100g) and musk lime (16.78 mg/100g).
    [Show full text]
  • Determination and Identification of Fundamental Amino Acids by Thermometric Titration and Nuclear Magnetic Resonance Spectroscopy
    Louisiana State University LSU Digital Commons LSU Historical Dissertations and Theses Graduate School 1967 Determination and Identification of Fundamental Amino Acids by Thermometric Titration and Nuclear Magnetic Resonance Spectroscopy. William Yong-chien Wu Louisiana State University and Agricultural & Mechanical College Follow this and additional works at: https://digitalcommons.lsu.edu/gradschool_disstheses Recommended Citation Wu, William Yong-chien, "Determination and Identification of Fundamental Amino Acids by Thermometric Titration and Nuclear Magnetic Resonance Spectroscopy." (1967). LSU Historical Dissertations and Theses. 1274. https://digitalcommons.lsu.edu/gradschool_disstheses/1274 This Dissertation is brought to you for free and open access by the Graduate School at LSU Digital Commons. It has been accepted for inclusion in LSU Historical Dissertations and Theses by an authorized administrator of LSU Digital Commons. For more information, please contact [email protected]. This dissertation has been microfilmed exactly as received 67-8805 WU, William Yong-Chien, 1939- DETERMINATION AND IDENTIFICATION OF FUNDAMENTAL AMINO ACIDS BY THERMOMETRIC TITRATION AND NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY. Louisiana State University and Agricultural and Mechanical College, Ph.D., 1967 Chemistry, analytical University Microfilms, Inc., Ann Arbor, Michigan Reproduced with permission of the copyright owner. Further reproduction prohibited without permission. DETERMINATION AND IDENTIFICATION OF FUNDAMENTAL AMINO ACIDS BY THERMOMETRIC TITRATION AND NUCLEAR MAGNETIC RESONANCE SPECTROSCOPY A Dissertation Submitted to the Graduate Faculty of the Louisiana State University and Agricultural and Mechanical College in partial fulfillment of the requirements for the degree of Doctor of Philosophy in The Department of Chemistry by William Yong-Chien Wu B.A., Hardin Simmons University, I96I January, I967 Reproduced with permission of the copyright owner.
    [Show full text]
  • Determination of the Chemical Concentrations
    American Journal of Analytical Chemistry, 2014, 5, 205-210 Published Online February 2014 (http://www.scirp.org/journal/ajac) http://dx.doi.org/10.4236/ajac.2014.53025 Online Process Control of Alkaline Texturing Baths: Determination of the Chemical Concentrations Martin Zimmer, Katrin Krieg, Jochen Rentsch Department PV Production Technology and Quality Assurance, Fraunhofer Institute for Solar Energy Systems, Freiburg, Germany Email: [email protected] Received December 16, 2013; revised January 20, 2014; accepted January 28, 2014 Copyright © 2014 Martin Zimmer et al. This is an open access article distributed under the Creative Commons Attribution License, which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. In accor- dance of the Creative Commons Attribution License all Copyrights © 2014 are reserved for SCIRP and the owner of the intellectual property Martin Zimmer et al. All Copyright © 2014 are guarded by law and by SCIRP as a guardian. ABSTRACT Almost every monocrystalline silicon solar cell design includes a wet chemical process step for the alkaline tex- turing of the wafer surface in order to reduce the reflection of the front side. The alkaline texturing solution contains hydroxide, an organic additive usually 2-propanol and as a reaction product silicate. The hydroxide is consumed due to the reaction whereas 2-propanol evaporates during the process. Therefore, the correct reple- nishment for both components is required in order to achieve constant processing conditions. This may be sim- plified by using analytical methods for controlling the main components of the alkaline bath. This study gives an overview for a successful analytical method of the main components of an alkaline texturing bath by titration, HPLC, surface tension and NIR spectrometry.
    [Show full text]
  • Superacid Chemistry
    SUPERACID CHEMISTRY SECOND EDITION George A. Olah G. K. Surya Prakash Arpad Molnar Jean Sommer SUPERACID CHEMISTRY SUPERACID CHEMISTRY SECOND EDITION George A. Olah G. K. Surya Prakash Arpad Molnar Jean Sommer Copyright # 2009 by John Wiley & Sons, Inc. All rights reserved Published by John Wiley & Sons, Inc., Hoboken, New Jersey Published simultaneously in Canada No part of this publication may be reproduced, stored in a retrieval system, or transmitted in any form or by any means, electronic, mechanical, photocopying, recording, scanning, or otherwise, except as permitted under Section 107 or 108 of the 1976 United States Copyright Act, without either the prior written permission of the Publisher, or authorization through payment of the appropriate per-copy fee to the Copyright Clearance Center, Inc., 222 Rosewood Drive, Danvers, MA 01923, (978) 750-8400, fax (978) 750-4470, or on the web at www.copyright.com. Requests to the Publisher for permission should be addressed to the Permissions Department, John Wiley & Sons, Inc., 111 River Street, Hoboken, NJ 07030, (201) 748-6011, fax (201) 748-6008, or online at http://www.wiley.com/go/permission. Limit of Liability/Disclaimer of Warranty: While the publisher and author have used their best efforts in preparing this book, they make no representations or warranties with respect to the accuracy or completeness of the contents of this book and specifically disclaim any implied warranties of merchantability or fitness for a particular purpose. No warranty may be created or extended by sales representatives or written sales materials. The advice and strategies contained herein may not be suitable for your situation.
    [Show full text]
  • The Birth of Titrimetry: William Lewis and the Analysis of American Potashes
    66 Bull. Hist. Chem., VOLUME 26, Number 1 (2001) THE BIRTH OF TITRIMETRY: WILLIAM LEWIS AND THE ANALYSIS OF AMERICAN POTASHES Frederick G. Page, University of Leicester. William Lewis (1708- In order to place 1781), was a physician, author, Lewis’s work in the context and an experimental chemist. of the early beginnings of Sometime after 1730 he gave the industrial revolution in public lectures in London on Britain, Sivin (4) has used a chemistry and the improve- chronological argument; he ment of pharmacy and manu- cites Ashton’s suggestion facturing arts (1). With a grow- (5) that 1782 was the begin- ing reputation as a chemical ning of the industrial revo- experimentalist he was elected lution because in that year F.R.S., on October 31,1745, most statistics indicated a and was then living in Dover sharp increase in industrial Street, London. In 1747 he production. But, as Sivin moved to Kingston-upon- argues, it seems reasonable Thames, where he set up a to assume that by the time well-equipped laboratory and such early statistics became presumably continued in medi- available, those industries cal practice. From about 1750 that had created salable until his death in 1781 Lewis products had already be- employed Alexander Chisholm come established and were as his assistant in chemical and no longer in their early literary works (2). These im- years of founding. On this proved the knowledge and basis the industrial revolu- practice of pharmacy, but as a tion must have begun ear- practical consulting chemist lier. By the middle of the Lewis has received little bio- eighteenth century the so- graphical recognition.
    [Show full text]
  • High Performance Liquid Chromatographic Assay of Chlorpropamide, Stability Study and Its Application to Pharmaceuticals and Urine Analysis
    Open Access Austin Journal of Analytical and Pharmaceutical Chemistry Research Article High Performance Liquid Chromatographic Assay of Chlorpropamide, Stability Study and its Application to Pharmaceuticals and Urine Analysis Basavaiah K1* and Rajendraprasad N2 1Department of Chemistry, University of Mysore, Mysuru, Abstract Karnataka, India Chlorproamide (CLP) is a sulphonyl-urea derivative used in the treatment 2PG Department of Chemistry, JSS College of Arts, of type 2 diabetes mellitus. A rapid, sensitive and specific HPLC method with Commerce & Science, B N Road, Mysuru, Karnataka, uv detection is described for the determination of CLP in bulk and tablet forms. India The assay was performed on an Inertsil ODS 3V (150mm × 4.6mm; 5µm *Corresponding author: Basavaiah K, Department particle size) column using a mixture of phosphate buffer (pH 4.5), methanol of Chemistry, University of Mysore, Manasagangothri, and acetonitrile (30:63:7v/v/v) as mobile phase at a flow rate of 1mLmin-1 and Mysuru, Karnataka, India with uv detection at 254nm. The column temperature was 30ᴼC and injection volume was 20µL. The retention behaviour of CLP as a function of mobile phase Received: February 27, 2017; Accepted: March 16, pH, composition and flow rate was carefully studied, and chromatographic 2017; Published: March 22, 2017 conditions, yielding a symmetric peak with highest number of theoretical plates, were optimized. The calibration curve was linear (r = 0.9999) over the concentration range 0.5 – 300 µgmL-1. The limits of detection (LOD) and quantification (LOQ) were found to be 0.1 and 0.3 µgmL-1, respectively. Both intra-day and inter-day precisions determined at three concentration levels were below 1.0% and the respective accuracies expressed as %RE were ≤1.10%.
    [Show full text]
  • Title a Hydronium Solvate Ionic Liquid
    A Hydronium Solvate Ionic Liquid: Facile Synthesis of Air- Title Stable Ionic Liquid with Strong Bronsted Acidity Kitada, Atsushi; Takeoka, Shun; Kintsu, Kohei; Fukami, Author(s) Kazuhiro; Saimura, Masayuki; Nagata, Takashi; Katahira, Masato; Murase, Kuniaki Journal of the Electrochemical Society (2018), 165(3): H121- Citation H127 Issue Date 2018-02-22 URL http://hdl.handle.net/2433/240665 © The Author(s) 2018. Published by ECS. This is an open access article distributed under the terms of the Creative Commons Attribution 4.0 License (CC BY, Right http://creativecommons.org/licenses/by/4.0/), which permits unrestricted reuse of the work in any medium, provided the original work is properly cited. Type Journal Article Textversion publisher Kyoto University Journal of The Electrochemical Society, 165 (3) H121-H127 (2018) H121 A Hydronium Solvate Ionic Liquid: Facile Synthesis of Air-Stable Ionic Liquid with Strong Brønsted Acidity Atsushi Kitada, 1,z Shun Takeoka,1 Kohei Kintsu,1 Kazuhiro Fukami,1,∗ Masayuki Saimura,2 Takashi Nagata,2 Masato Katahira,2 and Kuniaki Murase1,∗ 1Department of Materials Science and Engineering, Kyoto University, Yoshida-honmachi, Sakyo, Kyoto 606-8501, Japan 2Institute of Advanced Energy, Gokasho, Uji, Kyoto 611-0011, Japan + A new kind of ionic liquid (IL) with strong Brønsted acidity, i.e., a hydronium (H3O ) solvate ionic liquid, is reported. The IL can + + be described as [H3O · 18C6]Tf2N, where water exists as the H3O ion solvated by 18-crown-6-ether (18C6), of which the counter – – + anion is bis(trifluoromethylsulfonyl)amide (Tf2N ;Tf= CF3SO2). The hydrophobic Tf2N anion makes [H3O · 18C6]Tf2N stable + in air.
    [Show full text]
  • Solvent Effects on the Thermodynamic Functions of Dissociation of Anilines and Phenols
    University of Wollongong Research Online University of Wollongong Thesis Collection 1954-2016 University of Wollongong Thesis Collections 1982 Solvent effects on the thermodynamic functions of dissociation of anilines and phenols Barkat A. Khawaja University of Wollongong Follow this and additional works at: https://ro.uow.edu.au/theses University of Wollongong Copyright Warning You may print or download ONE copy of this document for the purpose of your own research or study. The University does not authorise you to copy, communicate or otherwise make available electronically to any other person any copyright material contained on this site. You are reminded of the following: This work is copyright. Apart from any use permitted under the Copyright Act 1968, no part of this work may be reproduced by any process, nor may any other exclusive right be exercised, without the permission of the author. Copyright owners are entitled to take legal action against persons who infringe their copyright. A reproduction of material that is protected by copyright may be a copyright infringement. A court may impose penalties and award damages in relation to offences and infringements relating to copyright material. Higher penalties may apply, and higher damages may be awarded, for offences and infringements involving the conversion of material into digital or electronic form. Unless otherwise indicated, the views expressed in this thesis are those of the author and do not necessarily represent the views of the University of Wollongong. Recommended Citation Khawaja, Barkat A., Solvent effects on the thermodynamic functions of dissociation of anilines and phenols, Master of Science thesis, Department of Chemistry, University of Wollongong, 1982.
    [Show full text]