CHEM 5 Quantitative Analysis
Laboratory Outline.
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02/12/16
Objectives:
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development of quantitative laboratory skills
introduction to modern analytical science
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Approach:
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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
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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
Volumetric Analysis
Acid-Base Titrations
(A-4) Experiment 6
(A-5)
Experiment 7
Gravimetric Determination of Chloride (page 730)
Neutralization Titrations
Determination of Replaceable Hydrogen in Acid by Titration with Sodium
Hydroxide (page 736)
Determination of Total Alkalinity of Soda Ash (page 738)
Complexometric Titrations
(A-6) Experiment 9 Determination of Water Hardness with EDTA (page 742)
Precipitation Titrations
(A-7) Experiment 11 Determination of Chloride in a Soluble Chloride: Fajan’s Method (page 745)
Statistical Comparison of the results obtained from Exp 3 and Exp 11
Reduction-Oxidation Titrations
(A-8) Experiment 15 Analysis of Commercial Hypochlorite or Peroxide Solution by Iodometric
Titration (page 753)
Series B.
Quantitative Analytical Studies
The following experiments will be conducted simultaneously, with each student or student group
signing up for available time on required equipment.
(Due dates for results will be indicated by the Lab Instructor.)
(B-1)
Potentiometric Titrations
Experiment 19 pH Titration of Unknown Soda Ash (page 762)
(NOTE: Calibration of the pH electrode and Drop Counter is a required part of this experiment.)
(B-2)
Potentiometric Determination of Cl in Solid Mixtures
(NOTE: Calibration of the chloride electrode is a required part of this experiment.)
(B-3)
Reduction-Oxidation Titrations and the use of ORP Electrode and Drop Counter in the
Analysis of An Iron Alloy or Ore by Titration with Potassium Dichromate (page 750 plus Hand
outs)
(B-4)
Water Quality Index (Group Project) Field Analysis
(NOTE: Set-up and calibration of numerous electrodes is a required part of this experiment.)
Experiment 22 Determination of Nitrate Nitrogen in Water (page 766)
Experiment 24 Spectrophotometric Determination of Inorganic Phosphorus in Serum and
Water (page 769)
(B-5)
(B-6)
Spectrophotometric Measurements
Experiment 21 Spectrophotometric Determination of Iron (page 765)
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(B-7)
Infrared Spectrophotometric Determination of a Mixture of Xzylene Isomers (page 774)
(B-8)
Separation Analysis Methods
Experiment 31 Thin-Layer Chromatographic Separation of Amino Acids (page 780)
Gas-Liquid Chromatography
Experiment 32 Gas Chromatographic Analysis of Tertiary Mixture (page 781)
(B-9)
Determination of Lead in Water using Anodic Stripping Voltammetry
(B-10) Polarimetric Determination of the Mutarotation Constant of Glucose
(B-11) Kinetics Analysis
Experiment 35 Enzymatic Determination of Glucose in Blood, Serum or Plasma (page 785)
(B-12) Team Experiments
Experiment 39 Method Validation and Quality Control Study (page 793)
The Gas-Chromatographic Determination of Ethanol in Beverages
Experiment 40 Proficiency Testing: Determination of Z Values of Class Experiments (page
795)
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C. Instrument Calibration Procedures
(C-1) pH Electrodes and Chloride Electrodes
(C-2) LABPRO +Calculators (Vernier + Texas Instruments)
(C-3) Spectrophotometer (Flinn or Spectronic 20)
(C-4) Ultraviolet Spectrophotometer (HachDR4000/Genesys 2)
(C-5) Infrared Spectrophotometer (Avatar 360 FTIR)
(C-6) Voltammetric Analyzer (OMNI 101 Potentiostat)
(C-7) Gas Chromatograph (Gow Mac 350)
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