Chemistry 361:

Analytical Chemistry Laboratory

Spring 2012

Coordinator: S. Nichole Taylor
Office: ELL 334B
E-mail: nicholet@uvic.ca
Phone: 721-7158

updated April 19, 2012

Lab Marks (with final letter grades)are Here!

 

Labs will begin the week of January 9th, 2012. The location of the lab is ELL 328. Please attend your scheduled lab period. No experimental work will be performed during the first week, so there is no need for safety glasses. There will be an analytical chemistry and statistics exercise, so be prepared to stay for a couple of hours.

The goals of this course include :

  1. Develop analytical laboratory technique
  2. Critically evaluating data as it is collected in the lab, and fix possible problems
  3. Increase competence of data collection and presentation
  4. Make reasonable conclusions based on the data
  5. Assess reliability of results
  6. Enhance the ability to communicate all of the above in written form

The Prerequisite for Chem 361 is Chem 212.

Recommended Text Books (available as reference books for in lab use only, may also be available in the library):

Harvey, David. Modern Analytical Chemistry. Toronto: McGraw Hill. 2000.

Harris, Daniel C. Quantitative Chemical Analysis. New York; W.H. Freeman and Company. 2006.

Skoog, Douglas A., et al. Analytical Chemistry. Toronto; Saunders College Publishing. 2000.

There are copies of these books available in the lab and also some in the MacPherson library.

As well, Principles of Instrumental Analysis by Skoog, Holler and Nieman (5th Edition) is available in the lab. This is also a great resource for Chem 361.

Materials needed :

Laboratory manual:
A manual is available in the bookstore. This will be required for the lab.

Laboratory notebook :
Students will be required to purchase a notebook supplied for Chem 361. It is printed by Hayden and McNeil, and provides numbered, carbonless copy paper for recording results. The same notebook was used for Chem 212, and if there are blank pages in the Chem 212 notebook, the student can use this for Chem 361. There are several styles available, including flip-up, side bound, and side spiral bound. Any are acceptable in this course.

Safety Glasses and Lab Coats :
Safety glasses must be worn and can be purchased from Science Stores. Lab coats are recommended and can be purchased from the University Bookstore or Science Stores. Please note that starting this year lab glasses must be worn regardless of whether or not you have prescription glasses. Special lab glasses that fit over prescription glasses are available for purchase from Science Stores.

 

Experiment Specific Info

LC1:

The solutions are caffeine in an acetonitrile/water mix.

LC2/CE:

there will be no internal standard for these experiments.

Please note! For LC2 and CE reports you can have one extra day for a due date as you will not get your data until the day after the experiment. So your due date will be 8 days after your scheduled experiment date.

The QC concentration is: 50.8 mg/L methyparaben, 50.0 mg/L ethylparaben, 48.1 mg/L propylparaben.

LC2 - a new column is in use. Please use a flow rate of 1.0 mL/min.

If you are scheduled to do LC2 before LC1, do not fear! Simply answer questions 3.4 and 3.5 on page 39 before doing the LC2 experiment, and you will have all the info you need (presuming you come to lab prepared as per the manual).

LC1 - please use a flowrate of 1.0 mL/min. The column currently has been chenged so this is a necessary change in procedure.

PREP - you shouldgo ahead and prep your lotion samples on your LC2 or CE PREP days. The samples will be fine and this will save you valuable time on your analysis day.

CE:

BIG CHANGE: on page 52, in the table, instead of CE test mix, please use your highest paraben standard. Same in step 1 below the table, and any other reference to the CE test mix. In other words, you will NOT be using the CE test mix. You can therefore skip steps 21 and 22, as you have already run the highest paraben standard. You can therefore answer the questions for Part A for the runs with your highest standard (the first two questions of the report).

***on page 52, step 2 tells you that two of your buffer vials are for the separation. Please remember this when building your method later for step 12***. WRITE THIS DOWN IN YOUR FLOW CHART!

Also for CE:

  1. On p.54 under the table, it should say the FOURTH line of your method will be for the injection of the sample.
  2. Please make note of the following: For the INLET BUFFER TRAY, use column F first, E next, then D, etc. Same for the SAMPLE TRAy on the inlet side. For the OUTLET BUFFER TRAY, please use column A first, then B, then C, etc. Following this rule will avoid missed injections in your sequence due to incompatible tray positions (tray collision error).
  3. When you go to print your data the next day, the software is amazing at putting ALL data not in your folder but in C:\32Karat\Projects\Default\Data. Scroll through to find your initials.

 

AES:

sample ID serving size sodium per serving
Lays lightly salted potato chips 50 g 160 mg
Kettle Brand Sea Salt Potato chips 40 g 160 mg
Pringles Original Chips 28 g 150 mg

For AES you must rinse your syringe filters ten times with 10 mL deionized water for each of those rinses. The reason is that the filters are made with sodium boroscillicate glass, and there is tons of sodium in the filter. This has to be washed out before you use them for your samples.

ISE:

CHANGE-Use 50 mL (not 100 mL) for the volume of standards, samples, spikes, etc.

Crest has 0.243% sodium fluoride.

 

Result Report Forms:

  1. ISE
  2. CE
  3. LC2
  4. AES