CHEMISTRY 59-241

PHYSICAL CHEMISTRY

LABORATORY MANUAL

WINTER 2007

2nd EditionDEPARTMENT OF CHEMISTRY & BIOCHEMISTRY

UNIVERSITY OF WINDSOR

TABLE OF CONTENTS

Emergency Procedures ................................................................................................... 2

Safety Regulations ............................................................................................................... 3

Policy on Plagiarism ............................................................................................................... 6

Marking Scheme and Outline ....................................................................................... 10

General Laboratory Outline ....................................................................................... 11

Attendance Policy ............................................................................................................... 12

Student Agreements ............................................................................................................... 13

EXPERIMENTS

Experiment 1: Solid – Liquid Phase Diagram ............................................................... 15

Experiment 2: Determination of Ka Using the Conductance Method ........................... 21

Experiment 3: The Iodine Clock ....................................................................................... 29

Experiment 4: Thermodynamic Functions of a Galvanic Cell ....................................... 37

Experiment 5: To be posted on the web later in the term

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EMERGENCY PROCEDURESFire Department 911 or pull wall alarm

Ambulance Dispatch 911

Medical Office 7002

Poison Control 9-800-268-9017

First Aid Kits Rooms 172-2, 175 and 274-2

Eye Baths are in each hallway

Safety Showers are in each laboratory

EMERGENCY EVACUATION PROCEDURES

Discovery of a Fire

1. Shout, “Fire” and advise TA a fire has been discovered.

2. Do not attempt to fight fires that cannot be easily handled; consult your TA.

3. If fire is too large to use a fire extinguisher, activate fire alarm pull station.

4. Follow TA’s instructions on fire evacuation.

Sounding of Evacuation Alarm

1. Place all flammable materials into safety cabinets.

2. Shut off all heat sources including lit Bunsen burners.

3. Close all doors and windows.

4. Ensure any handicapped persons are given assistance.

5. Evacuate the building quickly by walking out the nearest exit. DO NOT use the elevators.

(If smoke is encountered in a stairwell or corridor, use an alternate route.)

6. DO NOT re-enter the building until the Fire Department or Campus Police authorize it.

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SAFETY REGULATIONSSafety is a matter of the greatest importance to everyone in the Department. The principal dangeris fire, but others (toxic fumes, sharp objects, etc.) are also of concern. Graduate Students have adouble responsibility of concern as laboratory workers and teaching assistants. Most safetyprocedures derive from common sense. The basic rule of safety is “If you are unsure of theconsequences of an action, DON’T DO IT!” The following sets out regulations, which apply inteaching laboratories. Strict adherence to these is a MUST. Defaulters may be excluded from thelab and course.

One of the most common accidents to occur in the laboratory is a chemical spill. Any chemicalspilled on yourself or on your clothing must be washed off with LARGE AMOUNTS OF WATER.The incident MUST be reported to the TA. If acid is spilled on floors or laboratory benches, it mustbe neutralized immediately (solid sodium bicarbonate) and then cleaned up with water after thegeneration of all gas (carbon dioxide) ceases. Obtain the assistance of the TA.

The following rules are strictly enforced:

Cell phones or any other electronic devices are not permitted duringscheduled laboratory time. If a student is observed using any electronicdevice, the device will be confiscated until the laboratory session hasconcluded. “Turn it off or turn it over!”

• Safety glasses must be worn at all times in the laboratory. Students refusing to wearsafety glasses (or shatterproof spectacles) will be refused permission to perform theexperiment. Never wear contact lenses in the laboratory.

• Notify the TA of any accident, cut, or burn no matter how trivial it appears.

• Only those people directly involved in the laboratory experiment are allowed in thelaboratory. Visitors are not permitted to enter the laboratory.

• It is mandatory that a laboratory coat be worn in the laboratory.

• No open-toed shoes or sandals may be worn. Students not wearing the proper footwearwill not be permitted to enter the laboratory and perform the scheduled experiment.

• Keep working space clean and free of apparatus and/or other materials. This isparticularly important when flammable materials are in use.

• Laboratory work is only permitted on assigned laboratory periods in the assignedlaboratory room. Work is not permitted unless a TA is present. Experimental workconducted outside of stipulated laboratory hours is prohibited by departmentalregulations on grounds of safety.

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• Anyone attempting unauthorized experiments in the laboratory will be subject to severedisciplinary action.

• Smoking, eating, and drinking are not permitted in the laboratory.

• Extraneous items (coats, books, etc.) should remain in the area designated for coats andschoolbags. These items are not permitted at the workbenches.

• Long hair is a fire hazard and must be tied back at all times.

• Perform all operations with poisonous or disagreeable materials in a fume hood.

• Never deliberately purposefully inhale (smell) or taste any chemical. The propertechnique to identify an odour is to fan across the top of the container with your hand towaft very dilute vapours toward you.

• Never place your face directly over the top of a container which is being heated or pointit at a neighbour. The contents may "bump" and be violently ejected from the container. This can happen even after the heat has been removed.

• Never dispose of ANY chemical into the sink. Use ONLY the properly labelled wastecontainers for disposal liquid and solid chemical waste.

• Never use a Bunsen burner for ANY purpose unless instructed to do so by the TA.

Accidents and Injuries

If a student's clothes catches on fire, lie down and roll over repeatedly to smother the flames. Donot run about, which includes running any distance for a safety shower. Use the safety showeror fire blanket if very close by.

Chemical spills on benchtops, fume hoods, etc., should be cleaned up with paper towels andwashed. Treatment with an appropriate neutralising reagent, if necessary, should be based onconsultation with the lab co-ordinator.

Dangerous chemicals that come into contact with skin or clothing should be washed off,followed by prolonged washing for 5 to 10 minutes. Do not be concerned with neutralization,just wash. If a sizable quantity of corrosive material is on the clothes, prevent skin contact byquickly removing the clothing.

Two eye baths are available in the laboratory for washing out eyes. Be sure to ask for help, nomatter how slight the eye injury is.

Internal contact with chemicals can occur through a cut from broken glass, or by inhalation or

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ingestion. Wash out cuts and allow free bleeding to occur for a few minutes. The laboratoryco-ordinator, who is trained in First Aid, can treat cuts. If shattered glass was involved, inspectfor fragments still in the wound before bandaging. Move into fresh air for inhalation problemsand do not exert oneself until breathing has become normal. Report at once if any chemicalsmay have entered the mouth, whether or not if any chemical has been swallowed. Delay will notmake any necessary treatment less unpleasant or less necessary.

Burns should be immersed in very cold water for about 5 minutes and, if necessary, dressingshould be applied afterwards.

In general, remember the locations of the alarm box, showers, hoses, and extinguishers in case ofemergencies.

Important: MSDS (Material Safety Data Sheets) for all chemicals used in the labs per course can be found in a binder at the TA stations within the labs.

Important: You must answer the questions and sign the Safety Questionnaire on page 12of this manual. Please hand this form in to your TA.

The University of Windsor has a Policy and Procedure on Sexual Harassment. The followingstatement is drawn from the policy:

"The University of Windsor is committed to providing an environment for study, teaching, research work, and play for all members of the University community that is supportive of professional and personal development and free from sexual harassment."

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POLICY ON PLAGIARISMBelow are the guidelines that outline the policy on plagiarism for the University of

Windsor. TA’s will address this issue with students during the first week of the laboratories anddiscuss the outcomes that are of a result of plagiarism.

ACADEMIC INFORMATIONUndergraduate Degree Regulations

2.4.22 POLICY ON PLAGIARISMPlagiarism is defined as: “The act of appropriating the literary composition of another, or

parts of passages of his or her writing, or the ideas or language of the same, and passing them offas the products of one’s own mind.” (Black’s Law Dictionary).

It is expected that all students will be evaluated and graded on their individual merit andall work submitted for evaluation should clearly indicate that it is the student's own contribution.

Students often have to use the ideas of others as expressed in written or published workin preparing essays, papers, reports, theses and publications. It is imperative that both the dataand ideas obtained from any and all published or unpublished material be properlyacknowledged and their sources disclosed. Failure to follow this practice constitutes plagiarismand is considered to be a serious offence. Thus, anyone who knowingly or recklessly uses thework of another person and creates an impression that it is his or her own, is guilty of plagiarism.

Plagiarism also includes submitting one’s own essay, paper, or thesis on more than oneoccasion. Accordingly, it is expected that a thesis, essay, paper or a report has not been and isnot concurrently being submitted for credit for any other course. In exceptional circumstancesand with the prior agreement of the instructor, a student may use research completed for onecourse as part of his or her written work for a second course.

A confirmed incident of plagiarism will result in a sanction ranging from a verbalwarning, to a loss of credit in the course, to expulsion.

Source: 2004/2006 Undergraduate Academic Calendar, Paragraph 2.4.22

For additional information on this topic, please visit the University of Windsor’s websitededicated to student integrity at http://www.uwindsor.ca/aio

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SENATE BY-LAW 31UNIVERSITY POLICY IN RESPECT TO JUDICIAL PROCEDURESARTICLE I. SANCTIONS AND DEFINITIONSProscriptions Stated

University discipline is limited to student misconduct which adversely affects theUniversity community’s pursuit of its educational objectives. Students are expected to conductthemselves in a manner compatible with the objectives and purposes of the University ofWindsor. Any student at the University of Windsor whose conduct is improper in that it exhibitsa lack of integrity touching upon the educational objectives and requirements of the Universitymust be disciplined appropriately in the interest of safeguarding and upholding these standards.

It is desirable to define and identify further the standards demanded of each student at theUniversity of Windsor in the interest of educational integrity. Enumerated below are illustrationsof improper conduct which would lead to an inference of lack of integrity. These are illustrativeonly and shall not be taken as in any way limiting the generality of the high standards of conductrequired by the objectives and purposes of the University of Windsor.

Examples of misconduct for which students are subject to university discipline aredefined as follows:

a. Dishonesty, such as cheating, plagiarism, impersonation at an examination, or knowinglyfurnishing false information to the University.

b. Forgery, alteration, or use of University documents, records, or instruments ofidentification with intent to defraud.

c. Intentional obstruction or disruption of teaching, research, administration, disciplinaryproceedings, or other University activities, including public service functions, and otherauthorized activities on University premises.

d. Malicious abuse of any person on University premises or at University sponsored orUniversity supervised functions or malicious conduct which threatens, endangers orharasses any such person.

e. Theft from or deliberate damage to University premises or theft of or deliberate damageto property of a member of the University community on University premises.

f. Failure to comply with directions of members of the University administration or of the

teaching staff acting in the proper performance of their particular duties. g. Violation of published University regulations, including regulations relating to entry and

use of University facilities.

h. Violation of published rules governing University residence halls.

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i. Deliberate alteration or misappropriation of computer records, data, software, etc. of theUniversity or member of the University community.

j. Breach or misuse of the Code of Computing Practice for the University of WindsorComputer Centre user.

Sanctions Defined

a. Admonition. Notice to the student, orally or in writing, that s/he has violated studentrules and that continuation or repetition of the conduct found wrongful, within a period oftime stated in the warning, may be cause for more severe disciplinary action.

b. Censure. Written reprimand for violation of a specified regulation, including thepossibility of more severe disciplinary sanction in the event of conviction for theviolation of any University regulation within a period of time stated in the letter ofreprimand.

c. Disciplinary Probation. Exclusion from participation in privileges or extracurricularUniversity activities as set forth in the notice of disciplinary probation for a specifiedperiod of time.

d. Restitution. Reimbursement for damage or misappropriation of property. Reimbursementmay take the form of appropriate service to repair or otherwise compensate for damages.

e. Suspension. Exclusion from classes and other privileges or activities as set forth in thenotice of suspension for a definite period of time.

f. Expulsion. Termination of student status for an indefinite period. The conditions ofreadmission, if any is permitted, shall be stated in the order of expulsion.

g. Exclusion from Campus. Denial of access to the campus for an indefinite period fornon-academic misconduct. The conditions for removing this ban, if any, shall be includedin the exclusion order.

Source: http://athena.uwindsor.ca/units/senate/senate.nsf/Bylaws?OpenView

Important: You must read all plagiarism guidelines in this manual and sign the form onp. 14 of this manual. Please hand in this form to your TA.

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Department of Chemistry and Biochemistry at the University of WindsorGuidelines for Examinations, Assignments and Laboratory Reports

Cheating and Plagiarism1. During an examination, students must not have in their possession any unauthorized books,

notes, or extraneous material, unless permitted by the instructor. 2. All incidents of cheating and plagiarism will be reported by the instructor directly and

immediately to the Departmental Head for consideration of disciplinary action as delineated in Senate By-law 31.

Calculators1. Students may only use calculators approved by the Faculty of Science and/or their instructors.

Programmable calculators and calculators with infra-red transmission capability are not permitted.

Absence1. Attendance of laboratories and mid-term examinations is MANDATORY.2. Students who miss a mid-term examination or laboratory must provide written documentation

to justify an absence. Unexcused absences or incomplete laboratory reports will result in a grade ofincomplete, which in turn will result in a grade of incomplete for the course.

3. Such a student should call the departmental office 253-3000 x3521 to report his/her name andthe examination missed within 24 hours of the exam.

4. Written documentation justifying the absence must be presented within 48 hours of theexamination or as soon as possible.

5. Excuses will not be accepted after a student has taken an examination.

Midterm examination1. Only examinations written in non-erasable ink will be considered for a grade appeal.2. All grade appeals must be accompanied with a written rationale for the grade appeal. Requests

such as "see question xx" contain insufficient information and will not be considered for a grade appeal.3. All grade appeals must be made either within five working days after the examination is

returned to the class, or by a date designated by the professor.

Laboratory Reports/Assignments1. Plagiarism is defined in section 2.4.22 of the University Calendar. Students are reminded that

copying laboratory reports and assignments constitutes plagiarism. When two or more laboratoryreports/assignments containing substantially identical material are submitted, a grade of 0 will be assignedto each student, and the incident will be reported to the Department Head.

Final Examinations1. A student may inspect his/her own corrected final examination.2. All posted final grades are unofficial, and non-negotiable.3. Students who wish a formal appeal of their final examination/grade as described in section 2.6

of the Calendar may complete the appropriate paperwork at the registrar's office. In general, successfulappeals will be based solely on academic merit. Grade appeals to satisfy admission or scholarshiprequirements or other program prerequisites will be rejected.

(These guidelines were approved by the Departmental Council on 19 Dec. 1996; updated Sep. 2003)

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MARKING SCHEME AND OUTLINEAll labs are marked out of 20.Abstract (3 marks)

The abstract is a crucial part of your laboratory report. It is a clear written paragraphwhich briefly conveys the intent of the laboratory exercise, mentions the methodology utilizedduring the laboratory period, summarizes important experimental observations, findings andconclusions. The abstract length must be between 200 to 300 words.

Procedure (0 marks)No marks are given for this section. You may indicate “as outlined in the 59–241 lab

manual”, quoting the relevant pages. However, if there is a major deviation from experimentalprocedure or significant problem with the data arising from experimental error, you must statethese differences in this section, as these deviations could influence the marks you receive inlater sections (i.e., see Results and Calculations below).

Results and Calculations (8 marks)Present your data in neatly laid out tables. Always include units and estimated errors

arising from experimental errors, instrumental readings, etc. Include a comparison of yourexperimental data with literature values where appropriate. Show a sample calculation for eachtype of calculation required, including the equation used, the numbers substituted into theequation, unit analysis and the final answer.

Discussion (7 marks)This section is meant to convey your understanding of the experiment. Discuss all

important results, where trends and anomalies are discussed with reference to the underlyingtheory of the experiment. Important results should be compared with those found in theliterature, and reasons for difference between experimental and literature data should bediscussed. When there are several sources of possible error, indicate to what extent each mayhave affected the final results. You may also choose to include in your discussion possibleapplications of the experiment, suggested improvements or extensions to the experiment, and/oralternative methods of measurement.

Be sure to answer the lab questions at the end of each experiment in this section as well.

Conclusions (1 mark)Write a brief statement summarizing the most important results of the experiment,

including numerical final results and per cent errors (if applicable).

References (1 mark)Make a list of all reference material, using the same format as the lab manual.

References should appear in the order they appear in the text. References in the text shouldappear as super-scripted arabic numerals. For example: The boiling point of benzene is 80.1 oC.3

References:3. Atkins, P.W. “Physical Chemistry, 7th Edition”, Oxford University Press, Oxford, 2001.

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GENERAL LABORATORY OUTLINE1. Lab attendance is compulsory.2. Laboratory reports must be turned in at the start of the next lab period. In the final week,

reports must be handed in exactly one week after the completion of the lab.3. Each laboratory report is marked out of 20, and accounts for a maximum possible 3

marks towards your final grade (the five laboratories have a total weight of 15 % in thiscourse).

4. Laboratories which are not completed receive a grade of zero. A completed laboratoryrefers to both attendance and performance in the lab, as well as handing in a completedreport.

5. If the laboratory is not completed due to illness or family tragedy, the student maypresent a doctor’s note or some other documentation to the upper year lab coordinator inorder to be excused from the laboratory. In this case, the student will receive a mark onthis “excused laboratory” equal to the average mark on all other laboratory reports.

6. No make-up labs are offered.7. If there is any evidence of plagiarism or duplication in lab reports among lab partners,

friends or other students, all parties will receive a grade of zero and be subject toacademic discipline, as per the University of Windsor Undergraduate Calendar.

Prelab PreparationRead your laboratory manual carefully. You must be prepared to answer questions asked

by your TA about the experiment and for surprise quizzes. You must know, or have writtendown, the physical constants of the chemicals you will be using. MSDS sheets are readilyavailable for those who wish to consult them. You must also know how to prepare solutionsrelevant to your experiment (e.g. 4M HCl from concentrated HCl) before you come to the lab. Ifthere is any procedure, or equipment operation, with which you are not familiar, PLEASE ASKYOUR TA FOR HELP. This will help to prevent accidents and waste of valuable time.

DISPUTES, COMPLAINTS, AND POLICYAny disputes or complaints arising from the laboratory course should, in the first

instance, be drawn to the attention of the TA. Should his/her decision be deemed unjust,representations may be made, in turn, to the Professor instructing the course, the Head of theDepartment of Chemistry and Biochemistry, and the Dean of Students.

ACKNOWLEDGEMENTSThe current edition of this manual was prepared by Robert W. Schurko. Previous

editions of this manual, as well as development and refinement of the experiments are credited to Cory Widdifield and Robert W. Schurko.

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LABORATORY ATTENDANCE POLICY

Attendance is mandatory for those registered in the laboratory portion of the course. Students mustattend each laboratory session, except outlined in the schedule. The following rules apply:

1. Students must arrive on time. Doors close five minutes after the start of the lab. Studentsarriving after the lab starts and/or when doors close will be reminded to arrive on time fromthat moment on.

2. Any student arriving more than 15 minutes late receives a warning the first time. A 10%penalty is applied for submitting a lab report 15 minutes after the beginning of the lab.

3. Any student who repeatedly arrives (more than 15 minutes) late will not be allowed into thelab, will not be given an opportunity to make up the lab, and will receive zero for thatexperiment. They will, however, be able to submit the lab report they were suppose to handin, but a 10% penalty will be applied.

4. If a student is absent from a lab, the student must inform you as well as the lab co-ordinatorof his/her absence within 2 or 3 days of the missed lab. If the student provides a validexcuse (i.e. medical certificate), the student will be excused from the experiment takingplace that day or may be allowed to repeat the missed experiment if time and availability areallotted. The student must make a photocopy of the, i.e. certificate, and submit a copy eachto you and the lab co-ordinator. Otherwise, if a student has missed a lab without a validreason, the student is entitled to a grade of zero.

Missed Labs

Students who cannot make it to their lab section must contact the lab coordinator to rescheduleanother time to perform the missed experiment. Students will not be admitted to another lab sectionwithout the permission from the lab coordinator. The lab coordinator will assign a lab section andstudents will be given an admission slip to attend the alternate lab section. It will be the students’responsibilities to inform their TA they will not be attending their regular scheduled lab sectionwithin a reasonable amount of time (± 2-3 days from the day they missed lab).

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Safety Questionnaire Please take a few moments to answer these questions.Where is the location of the fire alarm pull?

______________________________________________________________________________

How many fire extinguishers are in the lab? Where is its/their location(s)?

______________________________________________________________________________

Where is the nearest eyewash?

______________________________________________________________________________

Where is the safety shower in the lab?

______________________________________________________________________________

Where is the fire blanket in the lab?

______________________________________________________________________________

Student Safety AgreementI have read and understand the safety regulations and emergency procedures outlined in this manual.I will abide by these rules.

COURSE NO. 59-241 SECTION _______________ DATE ______________

TA’S NAME _______________________________________________________________

NAME (please print) _________________________________________________________

STUDENT ID # _________________ SIGNATURE _______________________________

This form must be signed and handed in to a teaching assistant before the student proceeds with the59-241 laboratory.

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Agreement on Plagiarism Guidelines and Policy

I, _______________________________________, have read and understood the policies onplagiarism outlined in this manual. I also understand the serious consequences that are to betaken if I have been caught with plagiarism and I will take full responsibility for my actions.

* * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * * *

COURSE NO. 59-241 SECTION _______________ DATE ______________

TA’S NAME _______________________________________________________________

STUDENT ID # _________________ SIGNATURE _______________________________

This form must be signed and handed in to a teaching assistant before the student proceeds with the59-241 laboratory.