CHM 3105 INTRO.

TO CHEMICAL RESEARCH TECHNIQUES Fall 2013 Syllabus

Dr. Roy Keyer Beury 344A Tel 215-204-7186 Dr. Vassil Boiadjiev Beury 200 Tel 215-204-0471 Pre/Corequisites: Course Description: Book: Attendance: keyer@temple.edu Office Hours vboiadj@temple.edu Office Hours

Grading:

Lab Technique:

Notebook:

One of the following: Chemistry 1032, 1042 or 1952 as well as one of the following: Chemistry 1034, 1044, or 1954. Math 1042.Co-Requisite: Chemistry 3103. Introduction to the application of instrumental analytical methods, with particular emphasis on equilibria and acid-base techniques. Written scientific reports will require a quantitative analysis of collected data, including statistics and error analyses. The lecture book (Harris 8E) is required. Lab procedures are available online in Blackboard. Attendance is mandatory. There will be NO make-up labs. Missing a lab will result in a zero for the experiment. You are expected to come to lab fully prepared prelab written in notebook, amounts of reagents listed, calculator and safety glasses on hand. This is not your first lab course. We should not have to remind you about the basics, nor should we have to tolerate unprepared students. As such, those who come unprepared will be dismissed and receive a zero score for the day. Each lab is worth 100 points: 15% Notebook, 15% Lab Technique, and 70% Lab Report. The lab reports will be 75% of your course grade. The final exam will be 25% of your grade. Course grades will be based on a standard curve of >95% A, >90% A-, >87% B+, etc. Your use of the proper laboratory techniques will be monitored for every experiment and will be reflected in your grade. The technique grade for the entire class will suffer if cleanliness of common areas is not maintained. A record of every experiment performed in the lab must be kept in your laboratory notebook. The laboratory notebook will be signed by your TA at the end of each lab session and a copy of the pertinent pages should be attached to your lab report. ALL data and notes must be recorded first in the notebook using ink. Writing data on a scrap piece of paper and copying it to your notebook is unacceptable and a penalty will be assessed. You are expected to write a pre-lab and procedure in your notebook.

Course Schedule:

Dates Aug 26 Sep 03 Sep 10 Sep 17 Sep 24 Oct 01 Oct 08 Oct 15 Oct 22 Oct 29 Nov 05 Nov 12 Nov 19 Nov 26 Aug 30 Sep 09 Sep 16 Sep 23 Sep 30 Oct 07 Oct 14 Oct 21 Oct 28 Nov 04 Nov 11 Nov 18 Nov 25 Dec 04

Experiment 1 - Take Home Assignment and Check-in 2 - Statistics Computer Assignment 3 - Preparing and Standardizing NaOH 4 - Preparing and Standardizing Acetic Acid 5 - Determination of unknown acid concentration 6 - Following Titrations with pH Electrode 7 - Preparation and Behavior of Buffer Solutions 8 - Titration Calculations & Simulations 9 - Spectrophotometric Determination of Fe 10 - Spectrophotometric Determination of glucose 11 - Determination of pKa of Bromothymol Blue 12 - GC analysis of hydrocarbons Final Exam Special Topic

Lab Report:

The outline is typical for reports in analytical chemistry, but the reports depth should be greater in this advanced course. Lab reports are due at the start of the following period. Late reports will lose 10 points per day (even if it is 5 minutes late, you will lose 10 points). Lab reports must be typed. Name Title of Experiment Date of Experiment Unknown Number (if applicable) Date of Report Purpose: One or two sentences stating purpose of experiment and how the purpose was accomplished (Procedure: Usually the procedure is included in the report. However, in this course the procedure is placed in the laboratory notebook and is not repeated in the report.) Sample Calculations: This section consists of a single sample calculation for each process in the experiment. Calculations must be labeled. If replicate determinations of the same quantity are performed, only one sample calculation should appear for that determination. In the sample calculation all units and mole conversions are clearly shown. Calibrated glassware volumes are used whenever available. An extra significant figure is carried through intermediate calculations and the final result is rounded according to the usual rules. Data and Results: The necessary raw data and calculated results for each replicate determination are presented here in tabular form. A properly constructed data table has the following features: 1) The table has a title 2) It contains all data necessary for to verify calculations 3) Data which is common to all measurements (e.g., concentration of NaOH) is presented only once. 4) Each column is labeled with the name of the variable and the units in parentheses 5) The average calculated result and pertinent statistical information are presented at the bottom Discussion: Here the results of the experiment are summarized and the sources of random and systematic error are discussed. Any questions or discussions that are listed in the Experimental Write-up are to be address. You need to discuss your results, and if possible, compare them to expected results. Do not blame any mistakes (known or unknown) on human error. No scientist would ever report that. Instead, determine which steps have the greatest uncertainty and comment on that. For instance, comment on the ease or difficulty in obtaining a reproducible endpoint in a titration using phenolphthalein. Section 1 2 Day MW TR Time 1:00-3:50 8:00-10:50 Instructor Dr. Roy Keyer Dr. Vassil Boiadjiev Email Office

Instructor contact information

Example Discussion Section The goal of this experiment was to standardize a solution of KOH using glycine HCl (primary standard) and bromocresol green as the indicator. The aqueous reaction is

Measurement mass Glycine HCl (g) V initial (mL) V final (mL) [KOH] (M) average [KOH] sd [KOH]

Trial 1 0.4875 0.05 26.83 26.78 0.1632 0.1707 0.0071

Trial 2 0.4925 0.12 25.01 24.89 0.1774

Trial 3 0.4851 0.08 25.43 25.35 0.1716

error 0.0002 0.05 0.05 0.07 0.0005

and the endpoint was detected when the color changed from yellow to pale green.

rsd [KOH] 4.2% The result is an average concentration of 0.1707M with a standard deviation of 0.0071 (4.2%). A solution of approximately 0.2 M was desired, so the concentration of the standardized solution is lower than expected. Future experiments will need to take this into account. The error analysis is given below. For the error in :

( ) (

( ) (

The error in the concentration of KOH is based on the equation [ [ ] ] [ ]

The averages of [

and ]

will be used to calculate the error in [KOH]. ( ) ( ) ) ( ) ( )

The error in the KOH concentration is 0.0005M which is 0.3% relative error. From the calculation, the error in the volume measurements is more than 40 greater than that of the mass measurements. Therefore, methods to reduce the error in the volume measurements should improve the quality of the results. The color change for this indicator was from yellow to green, a difficult change to observe. Visually detecting and halting the titration at the same color was challenging and was likely the largest source of random error. In trials 1 and 3, the titrations were both stopped at a pale green endpoint. The endpoint for trial 2 was darker, which may explain why the concentration value for this trial is the largest. This difficulty in achieving reproducible endpoint colors also explains the large relative standard deviation (4.2%) compared to the relative error (0.3%). Calculation of the relative error does not include any term for the color measurement. For improved data, additional trials should be performed and those with darker colored endpoints should be discarded.