Chapter 0 The Analytical Process As an illustration of how the analytical process works, the books starts with an example of the steps taken by a pair of analytical chemists who want to determine the caffeine content in a chocolate bar. This is a nice example, and you should read through it. Rather than recap their story here, I want to point out several key terms that appear in the narrative that you need to be aware of. 0-1 Analytical Chemist’s Job Sampling Real analysis usually starts with an ugly sample that really isn’t well suited for analysis. Thus while this course will concentrate on the nice clean analysis of a simple neat sample, real analytical chemists usually spend a great deal of time getting their sample ready for the analysis and making sure that their preparation hasn’t actually ruined their sample The material of interest may be Homogenous- the material has one uniform composition Heterogenous - The composition varies form one part to another If the material is homogenous then getting a sample is easy, and any old piece will do (Maybe - see example in book about analyzing chocolate). If, however, the material is heterogeneous, then care must be taken to make sure the sample obtained truly represents the entire material Sample Preparation Once you have a sample, you need to quantitatively get it into a form that you can analyze. The steps taken here will vary from sample to sample and method to method. Decanting - Pouring an upper layer off of a 2 phase mixture. (Best done in a Separatory Funnel) Analytes - The substance you wish to measure. Quantitative transfer – Complete transfer of a material from one vessel or form to another. Slurry - Suspension of a solid in a liquid Supernatant liquid - A liquid above a packed solid. Chemical Analysis Chromatography - any method that separates different components in a mixture. Qualitative Analysis - Identification of what the unknown is Quantitative Analysis - Identifying how much of the unknown is present. 2 3 Calibration curves One tool that is used frequently is plot the response of some instrument vs the amount of one of the chemicals we are analyzing When we use a set of standards to calibrate the response of the machine, this plot is called the Calibration curve or standard curve. Interpreting Results Your final result is a number, and some measure of that number’s uncertainty. Will spend a chapter on statistics for this. Quality Assurance Now you have a set of results, how reliable are you? In an industrial or commercial setting you need to follow a set of practices called Quality Assurance to prove and document that the results you obtain are reliable. 0-2 Steps in a chemical analysis The analysis of a sample contains many steps: 1. Formulating the questions 2. Searching the literature 3. Sampling - obtaining a representative sample -extracting the smaller lab sample from the bulk sample 4. Sample Preparation - converting the lab sample into something suitable for analysis -May include concentration, dilution, or chemical reaction of analyte -Removing or masking other things that can interfere with the analysis 5. Actually performing the analysis on several samples 6. Final interpretation of the results 7. Drawing a conclusion The bulk of this book deals with step 5. You can see that it is a small part of an analytical chemist’s job. Now go back to the example given in 0-1 and see if you can see where each of these steps were performed.