...CHEM 5 Quantitative Analysis Laboratory Outline. 55labout.doc 02/06/05 Objectives: • development of quantitative laboratory skills • introduction to modern analytical science • Approach: • solve a series of chemical analysis problems with various techniques and instruments • certify laboratory instruments and standards • maintain laboratory records in compliance with Good Laboratory Practice Guidelines Schedule: Weeks 1-6 - Perform a Basic Set of 8 fundamental experiments (Series A) Weeks 5-15 Two parallel activities will be sustained: - Perform a series of quantitative studies (Series B) - Calibration of laboratory instruments (Each student or student group will perform each experiment in the B-series.) (Each student or student group will perform the calibration of laboratory instruments __________________________________________________________________ Series A. Basic Quantitative Techniques Introductory Experiments (A-1) Experiment 1 Use of the Analytical Balance (page 727) (A-2) Experiment 2 Use of the Pipet and Buret and Statistical Analysis (page 729) Gravimetric Analysis (A-3) Experiment 3 Gravimetric Determination of Chloride (page 730) Volumetric Analysis Acid-Base Titrations Neutralization Titrations (A-4) Experiment 6 Determination of Replaceable Hydrogen in Acid by Titration with Sodium Hydroxide (page 736) (A-5) Experiment...
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...Bulk Polymerization of Styrene Bulk polymerization of styrene will be conducted with different initial initiator concentrations. The polymers will be analyzed for their MW and PDI by size exclusion chromatography (SEC) using a calibration curve. The MW dependence on conversion will be investigated. The effect of the initiator concentration on polymer MW will be examined. Materials. Azobisisobutyronitrile (AIBN) and toluene (HPLC) were purchased from Sigma-Aldrich and used as received. Styrene (Sigma-Aldrich) was purified by passing through a silica column to remove inhibitors. CDCl3 was purchased from Cambridge Isotope and was used as received. Methods. Reaction procedure. To a vial charged with freshly purified styrene (10 g) was AIBN (0.7g, 0.35g or 0.17g) added at room temperature. The mixtures are then heated at 80˚C in an oil bath. Seven aliquots of the reaction mixture are removed at fixed time intervals (e.g., 0, 20, 40, 60, 80,100 min, 1 week) and analyzed by 1H NMR spectroscopy for conversion and SEC for polymer MW and PDI. Sample preparation for SEC analysis. An aliquot of the reaction mixture (3mg) is dissolved in THF(1mL) and was filtered through a syringe membrane filter prior to injection into SEC column. Sample preparation for 1H NMR analysis. An aliquot of the reaction mixture (0.1-0.5 mg) is dissolved in CDCl3 (1mL) and is transferred into a NMR tube for conversion analysis. Lab report write-up. Summarize and discuss your experimental...
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...Chemistry Modern Analytical Chemistry David Harvey DePauw University Boston Burr Ridge, IL Dubuque, IA Madison, WI New York San Francisco St. Louis Bangkok Bogotá Caracas Lisbon London Madrid Mexico City Milan New Delhi Seoul Singapore Sydney Taipei Toronto McGraw-Hill Higher Education A Division of The McGraw-Hill Companies MODERN ANALYTICAL CHEMISTRY Copyright © 2000 by The McGraw-Hill Companies, Inc. All rights reserved. Printed in the United States of America. Except as permitted under the United States Copyright Act of 1976, no part of this publication may be reproduced or distributed in any form or by any means, or stored in a data base or retrieval system, without the prior written permission of the publisher. This book is printed on acid-free paper. 1 2 3 4 5 6 7 8 9 0 KGP/KGP 0 9 8 7 6 5 4 3 2 1 0 ISBN 0–07–237547–7 Vice president and editorial director: Kevin T. Kane Publisher: James M. Smith Sponsoring editor: Kent A. Peterson Editorial assistant: Jennifer L. Bensink Developmental editor: Shirley R. Oberbroeckling Senior marketing manager: Martin J. Lange Senior project manager: Jayne Klein Production supervisor: Laura Fuller Coordinator of freelance design: Michelle D. Whitaker Senior photo research coordinator: Lori Hancock Senior supplement coordinator: Audrey A. Reiter Compositor: Shepherd, Inc. Typeface: 10/12 Minion Printer: Quebecor Printing Book Group/Kingsport Freelance cover/interior designer: Elise Lansdon Cover image: © George Diebold/The...
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...Equipment Qualification Good Laboratory Practices About About Labcompliance Contact Labcompliance Scope Tax/Bank Information All come with 10+ Best Practice Documents: SOPs, Checklists, Examples Transfer of Analytical Procedures According to the New USP Chapter <1224> With SOPs, templates and examples for easy implementation March 21, 2013 Quality by Design (QbD) for Analytical Method Development and Validation Learn how to design robustness for easy transfer and to avoid OOS situations Recorded, available at any time Validation of Analytical Methods for GLP and Clinical Studies Learn how to design, prepare, conduct and document for FDA compliance Recorded, available at any time Eight Steps for Cost-effective Laboratory Compliance Up-to-date overview, hot topics and trends. Recorded, available at any time Verification of Compendial Methods according to the New USP Chapter <1226> Understand the new risk based approach and and get real world case studies for testing Recorded, available at any time Effective HPLC Method Development and Validation Preparation, conduct and documentation for FDA/EMA Compliance Recorded, available at any time Validation of Analytical Methods and Procedures Conduct and Document for Efficiency and FDA, USP/EP and ISO 17025 Compliance Recorded, available at any time Development and Validation of Stability...
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...biamperometry. The monitor applies a voltage between two identical electrodes, which causes the reduced mediator formed during the incubation period to be reconverted to an oxidized mediator. This generates a small current that is read by the monitor. If controls do not fall within the acceptable range after one repeat 1 Do not report the patient results (this would be if the operatoris running controls for the purpose of checking the meter; otherwise, the QC lockout would not have allowed the patient to be tested prior to getting the controls in acceptable range). 2 Review the test policy and procedure. 3 To get a trade, take all of the reagents and supplies out of the drawer and take the entire GTS to the High Volume Lab of Chemistry, 5th floor McCullough Bldg. 4 If feasible for the testing site, the Nurse Manager/designee or Clinic Manager can authorize the borrowing of a GTS unit from another location. cont. NOTE: The proper comment code (09) identifying a temporary GTS unit is being used should be entered after the patient result is displayed and before it is "entered" by the operator. Point of Care should be notified that the assigned GTS unit is not performing satisfactorily. 5 Control testing should be repeated with the borrowed monitor, and, if acceptable, patient testing can be performed and reported. 6 If the problem cannot be resolved with a borrowed monitor, a patient sample should be collected and sent to the clinical...
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...Method Number: EPA 200.7 Revision Number: 3.0 Date: September 3, 2010 Clinical Laboratory of San Bernardino, Inc. Standard Operating Procedure for the Determination of Metals by Inductively Coupled Plasma Spectroscopy 1. SCOPE AND APPLICATION: 1.1 This method provides procedures for the determination of dissolved elements in ground waters, surface waters, and drinking water supplies. It may also be used for the determination of total recoverable element concentrations in these waters and wastewaters. Dissolved elements can be determined after suitable filtration and acid preservation. Acid digestion procedures are required prior to the determination of total recoverable elements. To reduce potential interference, dissolved solids should be < 0.2% (w/v). Prepared samples may require dilution prior to analysis to avoid physical interferences. The method is applicable to the following analytes: Chemical Abstract Services Registry Numbers (CAS-No.) 7429-90-5 7440-39-3 7440-42-8 7440-70-2 7440-48-4 7440-50-8 7439-89-6 7439-95-4 7439-96-5 7439-98-7 7440-41-7 7440-43-9 7440-47-3 7440-02-0 7440-22-4 7440-09-7 7631-86-9 7440-23-5 7440-66-6 Dectection Limit of Reporting (DLR) 50 ppb 100 ppb 100 ppb 1 ppm 10 ppb 50 ppb 100 ppb / 40 ppb 1 ppm 20 ppb / 4 ppb 10 ppb 1.0 ppb 1.0 ppb 10 ppb 10 ppb 10 ppb 1 ppm 0.5 ppm 1 ppm 50 ppb 1.2 1.3 1.4 Analyte Aluminum (Al) Barium (Ba) Boron (B) Calcium (Ca) Cobalt (Co) Copper (Cu) Iron (Fe) Magnesium (Mg) Manganese (Mn) Molybdenum (Mo) Beryllium...
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...Based on my observation, marijuana leaves exhibits a warty appearance due to the presence of non glandular hairs which at their base contains a spheriodal cystollith of calcium carbonate while on the other sample of marijuana seeds I observed the lacy and hair like. During the Chemical Test of the Fast Blue Salt or FBS Test on the Marijuana seeds, hashish cake and hashish candy I observed that there was a reaction on the test conducted due to the appearance of purple color or violet. On the Marquis test conducted for Morphine, Shabu and Ephedrine there were reaction with the two sample wherein the morphine turned to purple, shabu became orange and lately turned to red dark brown in color while the Ephedrine had no reaction at all. On the Simmon’s test, the color of shabu became blue in color. On the other test in Chen Kao 123, the Ephedrine has a reaction and the color of the sample became purple. The last examination conducted was the Benzidine test- to test whether the stain is blood or not. A stain sample rub with a filter paper and added with 1-2 drops of Benzidine Reagent and 1-2 drops of hydrogen peroxide on the filter paper, instant blue color indicates the presence of blood. CONCLUSION: Based on my observation of the chemical examination or test of prohibited drugs, therefore I conclude that the Marijuana leaves and marijuana seeds are not the same in characteristics. In the chemical test conducted, all the samples reacted...
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...ANALYTICAL BIOCHEMISTRY Analytical Biochemistry 334 (2004) 196–198 www.elsevier.com/locate/yabio Notes & Tips A spectrophotometric assay for the quantiWcation of polyethylenimine in DNA nanoparticles Martin Bertschinger, Sophie Chaboche, Martin Jordan¤, Florian M. Wurm Swiss Federal Institute of Technology Lausanne, Laboratory of Cellular Biotechnology, Lausanne VD1015, Switzerland Received 29 April 2004 Available online 28 August 2004 Since the Wrst description of polyethylenimine (PEI)1 as a gene delivery vehicle, there has been a strong interest in its use for in vivo and in vitro transfections of mammalian cells [1]. The mechanism of gene transfer by PEI is still unclear, and little is known about the formation of PEI– DNA nanoparticles. Such questions are diYcult to address because a rapid and sensitive assay for the quantiWcation of PEI in diVerent transfection media is not available. The only spectrophotometric assay for the quantiWcation of PEI is based on the dark blue cuprammonium complex that is formed when copper(II) ions are added to PEI [2,3]. This complex has a strong absorbance peak at 285 nm and a weaker one at 630 nm. Unfortunately, the absorption maximum at 285 nm is close to that of DNA (260 nm). In addition, most cell culture media contain components that absorb at this wavelength. At 630 nm, there is much less interference from biological molecules, but the signal from the cuprammonium complex is also low. We successfully adapted a commercially...
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...This experiment will separate the components of a mixture on the basis of their differing absorptive tendencies on a stationary phase, which is the method of chromatography. The mobile phase will consist of four distinct transition metal cations dissolved in an acetone-hydrochloric acid eluent, along with three unknown solutions; the identities of these will be determined based on a comparison of the Rf value of these to the known cations. First to be prepared was the stationary phase, or chromatographic paper, which in this case was filter paper. Given only large sheets, it was cut into a rectangle with 20 cm length and 10 cm width. Before cutting, though gloves were put on so that skin oil would not stain the filter paper. Also, the filter paper was not laid on the lab table, but on a paper towel. With a pencil, a line was drawn 2 cm from the bottom edge of the paper. Marks were put on the line, 2 cm apart, and labeled with the appropriate cations and the unknowns labeled as U1, U2, and U3. The stationary phases were then spotted with the corresponding knowns and unknowns, then dried under a heat lamp. This spotting process was repeated 3 times. It was done using glass capillary tubes; these used adhesive and cohesive forces to draw up the cation solutions into the tube and subsequently released them onto the filter paper when touch. With the stationary prepared, the developing chamber was made. In a 600-ml beaker 9 ml of acetone and 1ml of 6 M HCl were combined (under...
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...Gunshot Residue Analysis You are provided with cotton balls that were used to swab 2 suspect’s hands for the presence of gunshot residue. Determine, by atomic absorption spectroscopy, if either of the 2 have fired a gun recently. To do this you will first extract the lead residue off of the cotton ball and then you will run the lead samples and a lead positive sample and a blank to determine if there is lead in the residue from the suspect’s hands. Extraction/Sample Prep: 1.) Use tweezers or forceps to remove the cotton ball from its container and place it into a plastic centrifuge tube. Add 10 mL of 1% nitric acid and shake well. Continue shaking occasionally for 10 minutes. 2.) Remove the supernatant (the liquid in the tube) with a transfer pipet and place it into a labeled 25 mL volumetric flask. 3.) Add 1 mL of Ammonium dihydrogen phosphate solution. 4.) Dilute the contents of the flask with 1% nitric acid. 5.) Label the flask(s) as unknowns (1,2). Positive and negative control samples: 1.) Add 1 mL of lead standard to a 25 mL volumetric flask. 2.) Add 1 mL of Ammonium dihydrogen phosphate solution. 3.) Dilute the contents of the flask with 1% nitric acid. 4.) Label the flask as positive control #1 5.) Add 0.5 mL of lead standard to a 25 mL volumetric flask. 6.) Add 1 mL of Ammonium dihydrogen phosphate solution. 7.) Dilute the contents of the flask with 1% nitric acid. 8.) Label the flask as positive control #2 9.) Add 1 mL of Ammonium dihydrogen phosphate solution. 10.)...
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...Statement of Goals The goal of the group project was to calculate the percent calcium in a natural calcium tablet from Prime Eastern Pharmaceuticals in order to compare it with the reported amount of 800 mg of calcium per tablet to determine the validity of complaints regarding a reduced amount of mineral in the multivitamin. The quantitative determination of the analyte was accomplished through three experiments: complexometric titrimetry, flame atomic absorption analysis, and potentiometry using an Ion Selective Electrode. The complexometric titrimetry involved titrating the unknown calcium solution made from the calcium tablet with standardized EDTA. Quantitative determination of the analyte calcium was possible due to the stable and quick formation of the metal-EDTA complex with a 1:1 reaction stoichiometry. Flame atomic absorption analysis is useful in determining the amount of analyte in an unknown because the measure absorbances of standard solutions can be used to plot a calibration curve that can be used to determine the concentration of the metal in an unknown solution. Potentiometry is useful for determination of analyte when an ion sensitive electrode is used to find the amount of ion in standard solutions. Week 1: Introduction and Background The first test for calcium in the multivitamin was complexometric titrimetry, a titration of a solution of calcium tablet with a standardized solution of EDTA. EDTA forms a stable complex with calcium metal with a reaction...
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...Chromatography is commonly used to separate mixtures to determine different chemical components. The main types of chromatography include gas, thin layer, paper and column chromatography. Generally used most, paper has a stationery phase and a mobile phase in a chromatographical experiment. The stationery phase is the paper itself absorbing the solvent, while the mobile phase is the solute moving up the strip of paper. Solvents are solids, liquids or gasses that dissolve the solute, in this instance it separates the pigments of the ink so you can see what colours make the solute. (ABC, 2018) Each solvent has a different structure based on their dielectric constant. The solvents being used in this experiment are acetone, acetic acid (5%) and water. The dielectric constant states how polar each solvent is, showing whether or not it will have a better reaction with the inks tested. The measurement of the solute and the solvent is calculated in this equation: The Rf value (retention value) is the distance at which the solute has travelled (Mobile phase). This is a useful technique as it can determine the polarities of the solvents. Determining whether the solvents are polar or non-polar is through their chemical structure and electronegativity charges. Electronegativity is a measure of the tendency of an atom to attract a bonding pair of electrons. (Clark, 2000) Firstly, if the electronegativity difference is greater than 0.5, then it is considered as a polar bond and if it below...
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...Maria Vasilenko 223901 Feasibility of using biosensors for heavy metal detection in complex matrices such as bio-slurries. Master of Science Thesis Examiners: Professor Matti Karp Professor Raghida Lepistö Examiner and topic approved in The Science and Bioengineering Department Council meeting on 7.11.2012 Abstract TAMPERE UNIVERSITY OF TECHNOLOGY Master‟s Degree Programme in Science and Bioengineering Vasilenko Maria: Feasibility of using biosensors for heavy metal detection in complex matrices such as bio-slurries. Seminar paper, 97 pages November 2012 Major: Biotechnology Examiners: Matti Karp, Raghida Lepisto Keywords: environmental pollution, heavy metals, biosensors, slurries The quality of bioslurries that are used in industrial production and agriculture need to be watched very closely to avoid spreading of contaminants on area and poisoning of humans and animals. Because heavy metals are very stable and toxic in many chemical compositions, their amount should be estimated very thoroughly. A new approach that involved biosensors was tested in this study. Because the slurries are complex non-unified matrices which composed of two phases – solid and liquid, the cell behavior can varies a lot from the one that explained in water and so the estimation of ion concentration can be not reliable. It was shown that the cell actually behave different in the slurries. Normally the dissolved compounds suppress the biosensor activity and, in the same time, the ions in the...
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...Food Chemistry Food Chemistry 101 (2007) 397–400 www.elsevier.com/locate/foodchem Analytical, Nutritional and Clinical Methods Method development for the determination of manganese in wheat flour by slurry sampling flame atomic absorption spectrometry ´ Rennan G.O. Araujo, Fabio de S. Dias, Samuel M. Macedo, ´ Walter N.L. dos Santos, Sergio L.C. Ferreira * ´ ˆ ´ ´ ´ Universidade Federal da Bahia, Instituto de Quımica, Nucleo de Excelencia em Quımica Analıtica da Bahia, ´ Campus Universitario de Ondina, 40170-290 Salvador, Bahia, Brasil Received 23 June 2005; received in revised form 25 October 2005; accepted 25 October 2005 Abstract The wheat is one of the cereals more consumed in the human food in all worlds. In the form of flour it is used for preparation of breads, cookies, pizzas, cakes, and etc. This way, the knowledge of the mineral content this cereal and its flour is very important. Considering it, methods for determination of metals in these matrices are opportune and several papers have been performed. In this paper, a slurry sampling flame atomic absorption spectrometric method for the determination of manganese in wheat flour is proposed. The optimization step was performed using univariate methodology involving the variables: nature and concentration of the acid solution for slurry preparation, sonication time and sample mass. The established experimental conditions after optimization recommend a sample mass of 0.5 g, 2.0 mol LÀ1nitric acid solution and a sonication...
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...solution to that of standards. Beer-Lambert law ( A = abc Where: A ( is the absorbance (in absorbance units) at a specific wavelength; a: is the absorptivity at a specific wavelength; when expressed in units of L/mol-cm it is the molar absorptivity (ε); c: is the concentration of the absorbing species, usually expressed in units of mol/L; b: is the pathlength of the sample through which the light beam passes, usually expressed in units of cm. ✓ Procedure a) Preparation of solution : 1) Prepare a standard iron solution containing about 0.0702 g of iron per 1000 mL by first calculating the required amount of pure ferrous ammonium sulfate [Fe(NH4)2(SO4)2C6H2O] (FW=392.14). Weigh out the sample using an analytical balance and dissolve this in about 200 mL of deionized water containing 2.5 mL of H2SO4 in a 1 L volumetric flask. Dilute with water to the mark and mix thoroughly by inverting the stoppered flask several times. Do not dry the ferrous ammonium sulfate before weighing. This solution will be used in a subsequent analysis. Note:...
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