The Nature of Analytical Chemistry

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1 The Nature of Analytical Chemistry Chapter 1 Slide 1 Analytical Chemistry is a measurement science consisting of a set of powerful ideas and methods that are useful in all fields of science and medecine. This is Analytical Chemistry in Action!!! We are on Mars, sent by NASA in the spacecraft Pathfinder Pathfinder has landed on Ares Vallis. Sojourner rover is collecting data on marsian rocks using an APXS (Alpha proton X-ray spectrophotometer). APXS is an instrumental analytical techniques which combines Rutherford Backscattering spectroscopy, proton emission spectroscopy, and X-ray fluorescence. Slide 2 01-CO 1

2 Type of Information QUALITATIVE QUANTITATIVE Data collected by sojourner was sent to Earth and analyzed to determine the identity and concentration of most elements of the periodic table. The results were compared to analogous data of earth samples. Separation was not necessary which is the case in most analysis processes Slide 3 Homework Assignment What killed the deers? Feature 1-1, page 12 It is analytical chemistry in action, too. Not as sophisticated as that applied to samples on Mars But useful Slide 4 p.12 2

3 A. ROLE OF ANALYTICAL CHEMISTRY Slide 5 Fig 1-1, p. 5 ANALYTICAL CHEMISTRY Method Development Types of Methods Chemical, Biochemical, Biological, etc Instrumental Types of Analysis Qualitative analysis Quantitative analysis Characterization analysis Slide 6 3

4 Analytical Chemistry (CHE322) Course Application of Quantitative Methods of Analysis Learning Principles of their operation Special Focus Precision Accuracy Errors Statistical analysis Slide 7 B. Classification of Quantitative Analytical Methods Typically two measurements are performed in a quantitative analysis The first is a property that can be measured by the tools at hand The second is a quantity that is proportional to the first and is an indirect measure of the property sought for. Analytical methods are classified according to the nature of the second measurement Slide 8 4

5 Quantitative Analytical Methods Gravimetric methods Mass is measured to Volumetric methods Volume is measured Electroanalytical methods Electrical property: potential, current, resistance, charge, etc. Spectroscopic methods Property of radiation: intensity, wavelength/ frequency, phase, etc. Slide 9 C. Typical Quantitative Analysis Process I Method Selection Criteria 1) Base on Nature of Sample and Goals -accuracy -sensitivity -relialibility 2) Based on Practical considerations -cost -time -expertise Slide 10 Fig 1-2, p. 6 5

6 Acquiring Sample Is the sample representative? Challenge: select a small sample of composition that accurately represents the bulk Challenge: population size and heterogeneity Slide 11 Processing Sample: To preserve sample integrity Dry Keep under inert atmosphere To convert to a form suitable for measurements Grind Dissolve Oxidize, reduce, etc. Slide 12 6

7 Eliminate interferences Interferents/ interferences: species other than the analyte that affect the measurement. Matrix: all components in the sample containing the analyte. Solutions: remove or mask Slide 13 Calibrating and Measuring Calibration: process of determining the exact relationship between the property measured and the property sought for (Determination of k). C A = kx Generally, standards are used to calibrate a method. Slide 14 7

8 Calculating and Evaluating Results Calculation 1mol. HCl mol. Tris C HCl = = M 1mol. Tris vol. HCl Evaluating result = estimate reliability What is the uncertainty of the computed result? An analytical result without an ESTIMATE of RELIABILITY is of no value. Skoog et al., p. 10 Slide 15 Buffer and Blood ph Buffer is used to calibrate ph meter ph of a human blood sample is measured ph = /-??? (confident? How confident?) What is the uncertainty The accuracy of this result depends on the accuracy of the ph of the buffer. Assume that a ph lower than 7.35 is indicative of a physiological problem Slide 16 8

9 D. Feedback ControL Role Is a control quantity within acceptable boundaries? Example: is the blood glucose level within acceptable limits of concentration? (60-95 mg/ml) Feedback system: process of continuous measurement and control (cycle). Feedback loop: cycle of measurement, comparison, and control. Establish threshold levels/ upper and lower limits Slide 17 Slide 18 Fig 1-3, p.11 9

10 Slide 19 p.12 Slide 20 Homework #1- Overall Analytical Process Due date: 9/12 Read on page 12 Dear Kill: A Case Study Illustrating the Use of Analytical Chemistry to Solve a Problem in Toxicology. Summarize the nature of the problem and how it was solved? What is the analytical problem? What type of information is needed to solve the problem? How will the solution to this problem be used? What criteria were considered in selecting the method and designing the experimental procedure? Were there any potential interferences that had to be eliminated? If so, how were they treated? Is there a plan for validating the experimental method? How were the samples collected? Is there evidence that any of the steps of the analytical approach on page 6 were repeated? Was there a successful conclusion to the problem? Use SciFinder Scholar* to get the article by Oguma et al. from Analytical Biochemistry 368, (2007), pp Make a copy that you will submit with your homework. Summarize the nature of the analytical problem and how it was solved. Answer questions 1 to 9. *Literature Search strategies will be presented in Penfield library instruction room 1 on September 28th at 3 pm. You are required to attend. 10

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