CHM 2354 - Full Lab Manual 2024

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University of Ottawa *

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2354

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Chemistry

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Apr 3, 2024

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CHM 2354 LABORATORY OF ANALYTICAL CHEMISTRY LABORATORY MANUAL Winter 2024 Department of Chemistry and Biomolecular Sciences University of Ottawa

1 IMPORTANT NOTICE TO ALL STUDENTS. Safety glasses/goggles are mandatory in all Chemistry laboratories. Students will NOT be allowed to work in the laboratory without their safety glasses. Lab coats are mandatory. No contact lenses, sandals, or open shoes, short pants/skirts/short leggings may be worn in the laboratories. For all the laboratory sessions you will require: Safety glasses and Lab coat Access to lab protocol Good quality bound notebook (Hard cover preferred, but spiral bound accepted) Calculator Pen (no pencils permitted) Permanent marker Ruler A University computer account YOU WILL START THE LABORATORY WITH EXP. 1 ON THE VERY FIRST SESSION. BE PREPARED.

2 Contents Laboratory Schedule 3 General Information 2-6 Laboratory Notebooks 3-4 Calculations and Statistical Analysis in Analytical Chemistry 7-12 Experiment #1. Fundamental analytical techniques 13 Experiment #2. Analysis of Aspirin 21 Requirements for Formal Report for Experiment 2 Experiment #3 . The Determination of Sodium Carbonate in Soda Ash 31 Experiment #4 . The Determination of Chloride by the Volhard Method 35 Experiment #5. An investigation of interferences in the determination of Ca 2+ in water by Flame Atomic Absorption Spectrophotometry 39 Experiment #6 . Determination of iron in multi-vitamin tablets by colorimetry and verification of their consistency between two production batches. 47

Updated 2024 Lab Schedule You will be performing experiments throughout the semester by following the schedule provided below. Take note of what bay your lab bench is located in on the first day, and cycle through the experiments in this manual according to the schedule. It is possible that you will be performing experiments based on theory and material that has not yet been covered in class. All topics and techniques are nonetheless covered in your required textbook, and outlined in the Required Reading for every prelab. Week Bay A Bay B Bay C Bay D Bay E Bay F Jan 15 Expt 1 Jan 22 2 2 2 2 2 2 Jan 29 2 2 2 2 2 2 Feb 5 5 3 5 3 3 3 Feb 12 5 3 5 3 3 3 Feb 19 Study Break Feb 26 4 5 4 4 4 4 Mar 4 4 5 4 4 4 4 Mar 11 3 4 3 5 6 6 Mar 18 3 4 3 5 6 6 Mar 25 6 6 6 6 5 5 Apr.1 Easter holiday Apr 8 6 6 6 6 5 5 * Please write your final result for each experiment on the result sheets provided by your TA before leaving lab. Sign your name next to your result to testify to the following:  The result you are submitting is the same as that written in your notebook  You have not in any way falsified data or fudged calculations  You have double-checked your calculations for accuracy You must record the day and time of your submission on the result sheet. Late submission or changes/corrections to submitted results will result in a 10% decrease in your result mark. Such changes must be recorded on a new result sheet and signed by you. They may not been sent to your TA by email.

Updated 2024 General Information Absenteeism: Attendance is compulsory at all laboratory sessions. A student is required to produce a medical certificate from their doctor or campus health center if absent from any session. No other excuses will be accepted. Students who do not have a valid reason for missing a lab session will not be allowed to make up the time. Students who miss more than two lab sessions will not receive a grade for the course. Grading: 70% Accuracy and precision of results  The accuracy mark will be based on the closeness of your reported value to the actual value.  The precision mark is based on the standard deviation in your unknown value  If you miscalculate your final result, you will be allowed to recalculate it and hand it in for a re-grade (once!) with a 10% penalty to your mark . Resubmissions will only be accepted up to 2 weeks after handing in your result. No resubmissions will be accepted after that point. 15% Laboratory Notebook 5% Long Report for Experiment 2 2.5 % Short Reports for each of Experiment 5 and 6 5% TA evaluation Required Text:  Laboratory Manual Other suggested textbook: “ Quantitative Chemical Analysis ” by Daniel C. Harris & Charles A. Lucy, 10th edition Ensure that you read all relevant material in this manual and prepared any work required before attending a laboratory session.

Updated 2024 Format of Course: This course is designed to teach you skills in handling substances and apparatus in a quantitative manner. It may be necessary for two students to share the equipment contained in an assigned locker but each student performs the experiments independently unless otherwise stated. There are six experiments. The first is devoted mainly to calibration of glassware. The object of the remaining five experiments is to analyze "unknown" samples for various components. Each student will be given a coded sample for each analysis . Do not interchange samples or code numbers with the person who shares your locker. A failure for that analysis is likely to result if you are not careful about this. If you repeat an analysis, you must obtain a fresh sample and sample code. Also, if you spoil an analysis through spilling, etc., you should abandon it and start over with a fresh sample. Laboratory Notebooks: You are required to keep a bound, hardcover laboratory notebook . All experimental results and observations must be recorded in the notebook. All modifications, even minor, to the protocol in the lab manual, must be recorded. Notebooks should be kept according to the standards of a research laboratory notebook, given below. Adherer to them strictly or you will be harshly penalized! An example of a good notebook entry can be found on page 6. DO the following:  Each experiment should start on a new page.  Each time you record a new experiment, write the experiment title, date at the top of the page.  Number the pages of the notebook.  Recorded all data, notes, and observations directly into your notebook in ink .  If you make an error in a notebook entry, cross through the error with a single line so that the information underneath the line is still legible.  All work in your notebook should be legible and set out in a way that someone who has not performed the lab will be able to understand your results. DO NOT do the following:  Write data or calculations on loose-leaf sheets of paper then copy them into your notebook later.  Record data in pencil  Scribble through errors, erase errors, or use whiteout in your notebook. (In a research lab, such practices could result in the loss of a patent!)

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