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Chemistry 1020 Laboratory Manual Winter, 2014 Senior Laboratory Instructor: Richard Bartholomew UA 3071 [email protected] Table of Contents...

All needed data is provided on attached files. All equations and constants needed are provided on the chem manual on pages 96-98, 106-107.

Please show all calculations and steps.

Calculations, Part I
1. Write a balanced, net ionic equation for the titration reaction. Use this equation to perform
the subsequent calculations.

2. Calculate the [OH ] in the saturated Ca(OH)2 solution. -

3. Determine the experimental solubility of the Ca(OH)2 at your experimental temperature.

4. Determine the experimental Ksp of Ca(OH)2 at the observed temperature.

*Please record the Results of Calculations, Part I on the first table on page 106

Calculations, Part II

1. Calculate the total [OH ] in the saturated solution of Ca(OH)2 in sodium hydroxide for the -
solution assigned to you.

2. Calculate the [OH ] that comes from the dissolution of Ca(OH)2. The total [OH ] (calculated - -
above) is the sum of the [OH ] from the NaOH and the [OH ] from Ca(OH)2. - -

3. Calculate the solubility of Ca(OH)2 in the NaOH solution.

4. Calculate the experimental Ksp of Ca(OH)2 for the saturated solution of Ca(OH)2 in NaOH.

Please record the Results of Calculations, Part II on the second table on page 106

Final Questions:
1. During the filtration of the saturated Ca(OH)2 the funnel is covered with a watchglass and
afterwards the flask is stoppered. This is to minimize contact with the atmosphere. Why is
this necessary? How would the observed Ksp and solubility of Ca(OH)2 be affected if contact
with the air were not minimized?

2. The saturated solutions of Ca(OH)2 contain a white solid which was removed by filtering.
What is this solid? If it were not removed, how would it affect the calculated (observed)
values for Ksp and solubility of Ca(OH)2?

3. Given below are data from a previous year. The Ksp is independent of [NaOH] while the
solubility of Ca(OH)2 decreases as the [NaOH] increases. Explain why this is the case. (for this question the table on page 107 will help).

Chemistry 1020 lab manual W14.pdf

Chemistry 1020 Laboratory Manual
Winter, 2014
Senior Laboratory Instructor:
Richard Bartholomew
UA 3071
[email protected] Table of Contents
DEDICATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . iii
LABORATORY CALENDAR . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 1
SAFETY RULES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 2
SAFETY PROCEDURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 5
GOOD LABORATORY PRACTICE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 9
LABORATORY REPORTS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 12
PROCESS FOR RE-SCHEDULING MISSED LABORATORIES . . . . . . . . . . . . . . . . . . . . . . 16
WEIGHING TECHNIQUES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 18
VOLUMETRIC TECHNIQUES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 22
OPERATION OF THE BUNSEN BURNER . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 29
SUCTION FILTRATION . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 31
SIGNIFICANT FIGURES . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 33
LABORATORY REPORT RECEIPT SHEET . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 39
SAFETY ACKNOWLEDGEMENT . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 40
LOCKER EQUIPMENT LIST . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 41
i 1. THERMOCHEMISTRY AND THE MEASUREMENT OF THE ENTHALPY OF
DISSOCIATION FOR ACETIC ACID . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 44
2. EFFECT OF CONCENTRATION AND TEMPERATURE ON REACTION RATE . . . . . 67
3. pH TITRATIONS AND BUFFERS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 80
4. DETERMINATION OF THE SOLUBILITY PRODUCT CONSTANT OF CALCIUM
HYDROXIDE . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 97
5. SYNTHESIS OF MALEIC ACID AND CONVERSION TO FUMARIC ACID. . . . . . . . . 109 ii DEDICATION
For the “Tigers”
(They know who they are!) iii LABORATORY CALENDAR Winter, 2014 Laboratories begin the week of January 13 and you will do one experiment every two weeks
for a total of 5 during the semester. Dates Experiment January 15 - 24 1 - Thermochemistry January 29 - February 7 2 - Effect of Concentration and Temperature on
Reaction Rate February 12 - 15 3 - pH Titrations and Buffers February 17 - 21 Reading Week - no labs February 24 - 28 3 - pH Titrations and Buffers March 5 - 14 4 - Determination of the Solubility Product
Constant for Calcium Hydroxide March 19 - 28 5 - Synthesis of Maleic Acid and Conversion to
Fumaric Acid 1 U OIT Chem. 1020U, W14; Introduction - 11.20 SAFETY RULES Safety in the laboratory is of the utmost importance to your instructors and also must be to
you, the student. Everybody’s safety depends on each student adhering to the safety rules and
procedures outlined in this manual. The following rules must be obeyed and will be rigorously
enforced. 1. Students arriving more than 10 minutes late to a laboratory period will not be allowed access
to the laboratory. Students must arrive promptly to receive instructions about the safe
conduct of the experiments. 2. ALL students must wear eye protection. For people with eyeglasses it must be worn over
regular glasses. This rule will be vigorously enforced. 3. Contact lenses should not be worn in the chemistry laboratory. 4. All students must wear a lab coat. A 100% cotton lab coat is best. Lab coats protect skin
and clothing from chemicals. The front of the lab coat should be buttoned while working in
the laboratory. 5. Open shoes or sandals are forbidden. They expose the feet to spilled chemicals. Footwear
must enclose the entire foot from ankle to toes. 6. Loose or bulky clothing presents a hazard and should not be worn in the laboratory. 7. Clothing that exposes large areas of the body (e.g. shorts, tank tops) must not be worn in the
laboratory. 2 U OIT Chem. 1020U, W14; Introduction - 11.20 8. Long hair must be tied back. The simple rule: if it can be tied back, it must be tied back! 9. Aisles must be kept clear of boots, coats, knapsacks, etc. 10. Students must know the locations of: a) fire extinguishers b) eye wash stations c) emergency showers d) emergency exits e) fire blanket f) fire alarms 11. Eyewash stations, shower, fire blanket and fire extinguishers must not be obstructed. 12. Absolutely no smoking, eating or drinking in the laboratory. Neither food nor drink may be
brought to the laboratory. 13. No laboratory may be started without an instructor present. Unauthorized experiments are
strictly forbidden. Experiments must not be left unattended. 14. Never put broken glass in the regular garbage. To do so presents risks to janitors and
cleaning staff. Broken glass should be swept up with a dust pan and brush and disposed in
the receptacle for broken glass. ONLY broken glass should be placed in this container. 15. When diluting acid be sure to add the acid to the water. Add the acid slowly and with plenty
of stirring. Diluting acids generates huge amounts of heat (it is a very exothermic process).
Keeping the water in excess allows this heat to be more effectively dissipated. If the heat is
3 U OIT Chem. 1020U, W14; Introduction - 11.20 not adequately dissipated the rapid heating may cause the solution to be ejected from the
beaker, injuring the experimenter. If the acid is added to the water, the ejected solution will
be comparatively dilute and therefore less dangerous. 16. NEVER, EVER pipette by mouth. Safety bulbs are provided for pipetting. When pipetting
by mouth it is very easy to lift the tip of the pipette above the level of the liquid being
pipetted As a result, solution will enter the mouth. 17. Never point the mouth of a test tube at yourself or others. This is especially true if the test
tube is being heated. 18. NEVER taste chemicals or solutions. Should you get any chemicals in your mouth, do not
swallow. Rinse your mouth thoroughly and then consult an instructor. 19. If you must smell a chemical, waft the vapours toward your face with your hand. Do not
place the container directly under your nose - you may be overcome by the gas. NOTE: Students who arrive for laboratories inappropriately addressed may be forbidden from
performing the experiment. Students who violate the safety rules may be dismissed from the
laboratory period. In such cases the student will be given a grade of zero for the laboratory report. 4 U OIT Chem. 1020U, W14; Introduction - 11.20 SAFETY PROCEDURES Fire Fire is one of the most serious problems that may be faced in the chemistry laboratory. For
no other safety issue is the adage “an ounce of prevention is worth a pound of cure” more applicable. In the event of a small fire, use the fire extinguisher. Remove the pin by twisting and pulling
it out. Direct the nozzle of the extinguisher at the base of the fire and squeeze the trigger. Ensure
that at all times you are between the fire and your escape route. Small fires can rapidly and easily
become large fires. If the fire cannot be safely extinguished in 30 s, leave the room. For large fires pull the fire alarm. If in doubt, pull the fire alarm and leave the building. The
more time people have to escape the more likely they will be successful. Turn off all services
(burners, hot plates, water, etc.); leave the room The last person out of the room must close the door
– this is the single most effective way to slow the spread of fire. Leave the building by the nearest
exit and move well away from the doors. The laboratory demonstrator (or teaching assistant) should
call emergency services and give all necessary details to the fire crews. Clothing on Fire DO NOT RUN! Wrap the victim in the fire blanket or use a lab coat to smother the flames.
“Drop and Roll” is effective. The emergency shower can be used. Have someone call the
emergency number and get medical assistance. 5 U OIT Chem. 1020U, W14; Introduction - 11.20 Fire Alarm UOIT uses a “two stage” fire alarm system. The first stage is a warning that there may be
an emergency in the building. In the first stage the fire alarm rings at a rate of 30 rings per minute.
At the first stage of the alarm, stop all your experiments when it is safe and convenient to do so and
prepare to leave the building. Await further instructions. If the fire alarm progresses to the second
stage (louder, more frequent alarm), immediately stop all experiments. Turn off all services (gas,
electricity, water, etc.). Before leaving the laboratory make sure the hallway is free of smoke and
fire. If it is, leave the laboratory and exit the building by the quickest route. Close the door to the
laboratory. Once outside, move away from the building and assemble at the western end of the first
floor atrium of UB. If UB is closed, meet in the car park immediately to the east of UA. Your TA
will do a headcount to ensure everyone is out. Do NOT wander away without telling your TA!
Under no circumstances should you return to the building until told by the fire department that it is
safe. Escape Routes for First-year Laboratories Room Primary Escape Secondary Escape UA 3420 Turn left, descend staircase at Turn right, then left along southern northwest corner of atrium. Exit corridor. Descend staircase at southeast building by north doors. corner of building. Exit building by doors
at southeast corner. UA 3480 Turn left, descend staircase at Go straight along southern corridor. northwest corner of atrium. Exit Descend staircase at southeast corner of building by north doors. building. Exit building by doors at
southeast corner. 6 U OIT Chem. 1020U, W14; Introduction - 11.20 Medical Situations UOIT maintains a service called the Campus Emergency Response Team (CERT). The
CERT is staffed by volunteers who have had extensive first aid training. If CERT assistance is
required, the CERT team can be contacted at x-2400. Pregnancy If you are, think you may be or are planning to become pregnant, you should be aware that
the risks to a mother and a developing foetus from the chemicals used in these laboratories are
generally unknown. You may wish to consider deferring taking this course until after your baby has
been born. If you decide to take this course, consultation with your family doctor is strongly
encouraged. If you would like the Material Safety Data Sheets for the chemicals in this course, they
will be provided. Fainting If at any time you feel light headed, dizzy or that you may faint, immediately sit down on the
floor. Fainting itself is rarely harmful; falling because of it may cause injury. Call for medical
assistance. If someone should faint, try to assess whether they have been injured by the fall. Make
them as comfortable as possible and call for medical assistance. Cuts Minor cuts should be treated with plenty of cool water. Ensure no foreign objects are present
(such as glass) and apply an appropriate dressing. Seek medical attention at student services. For more serious cuts the victim should sit or lie down and keep the cut elevated. Bleeding
7 U OIT Chem. 1020U, W14; Introduction - 11.20 should be kept to a minimum by applying direct pressure (assuming no foreign objects are present
in the wound). Call for emergency medical assistance. Burns Burns can be either thermal (caused by heat) or chemical. In both cases the first step is to
apply plenty of cool water. If the chemical reacts with water, remove it by brushing it from the skin.
If necessary, seek medical attention. Allergies and Other Pre-existing Conditions If you suffer from severe allergies or other pre-existing medical conditions such as epilepsy,
diabetes, etc., it may be helpful (although not required) to alert your instructor(s) and to advise them
of any necessary precautions or first-aid treatment. 8 U OIT Chem. 1020U, W14; Introduction - 11.20 GOOD LABORATORY PRACTICE 1. Use clean equipment. Dirty apparatus can lead to poor results (and therefore, poor grades!)
or to unexpected and potentially dangerous reactions. Beakers and flasks can be cleaned with
soap and water followed by thorough rinsing with tap water and deionized water. Soap
should be avoided when cleaning volumetric glassware such as pipettes, burettes and
volumetric flasks. 2. Once a chemical has been removed from its original container it must NEVER be returned
to the container. To do so risks contaminating the entire stock and thereby ruining the
experiments of others. If you have excess, it is cheaper to throw it away (appropriately) than
to risk contaminating the stock. 3. Chemicals are expensive and solutions can be time consuming to prepare. DO NOT
WASTE CHEMICALS. Read the manual very carefully and take only what you need. 4. Carefully read the labels of reagent bottles to ensure you are getting the right chemicals. Be
sure to properly label apparatus containing chemicals or solutions. Accidents may result
from the mistaken mixing of chemicals. 5. Remember to re-cap reagent bottles immediately after use. This prevents wastage of
chemicals by contamination and spillage. Do not allow caps to become contaminated
through contact with the bench top or other chemicals. 6. Do not remove reagent bottles to your benches. This causes frustration and unnecessary
delay for other students. 9 U OIT Chem. 1020U, W14; Introduction - 11.20 7. Certain chemicals used in these laboratories are hazardous or present an environmental risk.
Dispose of these chemicals in the appropriate waste dumps provided. 8. Set-up apparatus so that it is well back from the edge of the bench. All services (gas taps,
water taps, electrical outlets, etc.) should be readily accessible. 9. Keep your work area clean, tidy and well-organized. Cluttered work areas can lead to
accidents. Clean up all spills quickly. At the end of the lab period clean your work area. 10. Do not dispose of solid or insoluble materials in the sinks. To do so will inevitably lead to
clogs of the plumbing and to floods. 11. Large spills of acids and bases can be treated with the appropriate spill kit. Afterwards the
bench should be washed with plenty of cold water. 12. Mercury spills should be cleaned up immediately. The vapour from mercury is quite toxic.
Mercury spills are generally treated with powdered sulphur which reacts with the mercury
to form mercury sulphide. The resulting solid is collected and treated as chemical waste. 13. Do not wander aimlessly in the laboratory. 14. Never interfere with the work of other students unless that work presents an immediate
hazard to yourself or to others. 15. At the end of the laboratory period clean all equipment and return it to its appropriate place. 10 U OIT Chem. 1020U, W14; Introduction - 11.20 Handling Glassware 1. Apparatus that can roll (such as thermometers, etc). should be placed on the bench at right
angles to the bench to prevent it rolling onto the floor. 2. Suction flasks (or Büchner flasks) may collapse violently under vacuum if cracked or
otherwise weakened. Inspect suction flasks before using. Do not strike or tap a suction flask
while it is under vacuum. 3. Chipped, broken or cracked glassware should be discarded. Heating cracked glassware is
very dangerous - the glassware may shatter. Inspect glassware before using. 4. When inserting glass tubing into a stopper match the tubing to the size of the hole.
Sometimes the tube can be lubricated with water or glycerol. To protect hands from being
cut, wrap tube in a towel before inserting into the stopper. Apply force to the tube lengthwise while slowly twisting the tube. 5. To break glass tubing, use a triangular file to scratch the tubing at the point of the break.
Moisten the scratch and wrap the tube with a towel. Place thumbs against the glass tubing
on the opposite side of the scratch. Press against the tube while pulling hands apart. Fire
polish the ends of the tubing before using. 11 U OIT Chem. 1020U, W14; Introduction - 11.20 LABORATORY REPORTS 1. Attendance at laboratories and submission of a laboratory report are compulsory. Failure to
attend a laboratory or to submit the report may result in a grade of zero. A student may be
excused from a laboratory only by providing appropriate documentation. 2. Documentation for missed laboratories should be submitted to the senior laboratory
instructor . 3. In exceptional circumstances it may be possible to re-schedule an experiment. When
possible, requests for re-scheduling should be made in advance (in the case, for example, of
religious holidays). Laboratories may only be re-scheduled with the permission of the senior
laboratory instructor. See below for the process for re-scheduling laboratories. 4. A student who fails to submit more than TWO (2) laboratory reports will not receive credit
for the laboratory portion of the course. This may result in failure of the course. 5. With the exception of the last experiment laboratory reports are due at the beginning of the
next period. The report for the last experiment is due at the end of the last laboratory period. 6. Marks will be deducted from late lab reports at a rate of 2 marks per day. No report will be
accepted if it is more than 4 days late. 7. The laboratory report must be typewritten or written in ink - the choice is yours. Two (2)
marks will be deducted if the report is not typewritten or written in ink. 8. All original experimental data must be recorded in ink. Before leaving the laboratory have 12 U OIT Chem. 1020U, W14; Introduction - 11.20 your data signed by an instructor. The signed data must be submitted with the laboratory
report. If no signed data are submitted with the report or if data are not recorded in ink, two
(2) marks will be deducted. 9. Any errors in recorded data should be corrected by drawing a single line through the
erroneous data and writing the corrected data close by. The original data should remain
legible. 10. White-out must never be used on laboratory reports. 11. Laboratory reports should be legible and well-organized. The grammar, style, and spelling
will be assessed. Persistently poor spelling or grammar will be penalized. 12. Sample calculations must always be shown. In some cases the same calculation will be
repeated (in titrations, for example) - it is not necessary to show every individual calculation.
All steps should be shown so the marker can understand how the calculation was done and
locate any errors in the method or arithmetic. Failure to show calculations will result in
substantial loss of marks even if the final answers are correct. 13. Academic misconduct is a serious offence and will be punished. Academic misconduct
includes (but is not limited to): plagiarism (copying) of lab reports, submitting false data,
misrepresenting data or using data from other students without the permission of the
instructor. Details about academic misconduct, punishments and appeals procedures are
given in the university calendar. It is the student’s responsibility to read and understand
these regulations. 14. Teaching assistants are provided with uniform marking schemes for all the experiments.
However, within the context of these marking schemes teaching assistants will exercise their
13 U OIT Chem. 1020U, W14; Introduction - 11.20 own judgement. At the end of the semester laboratory grades will be adjusted to account for
variation between individual teaching assistants. This may result in an increase or a decrease
in your laboratory grade. For semesters in which there is more than one teaching assistant, an overall class average for
the laboratory marks will be calculated and the marks for each individual teaching assistant
will be scaled to this value. No correction will be applied if the correction would be less than
two marks in thirty in the final laboratory grade. 15. A “performance evaluation” (worth 5 marks in 30) is part of your assessment in the
laboratory. This is an assessment of your general conduct, preparation, safety, attitude etc. Graphs for First Year Laboratories Graphs may be drawn by hand or by computer - the choice is yours. If doing by hand, you
must use graph paper that uses at least ten divisions per centimetre and each data point should be
circled. Whether drawn by hand or by computer follow these guidelines: 1. Unless instructed otherwise, the independent variable should be on the x-axis and the
dependent variable should be on the y-axis. 2. Use appropriate scales for the axes. Scales should be chosen so that the data fill the available
space. When plotting by hand, the scale should also be chosen to allow easy plotting and
reading of values; a scale in which 10 divisions represents 2/3 of a unit is not convenient!
The intersection of the axes does not have to take place at the origin (0,0).
14 U OIT Chem. 1020U, W14; Introduction - 11.20 3. The axes must be labelled. The name of the quantity and the units in which it is measured
should be written beside the axis, e.g.: “temperature / 0C” or “concentration / mol L-1". 4. Major divisions on the axes should be labelled. 5. A title must be added to each graph. Enough information must be in the title to make it clear
what the data represent. For example:
Experiment 5: Determination of the Order of Reaction for the Reaction between
Hydrochloric Acid and Thiosulphate Ion (2HCl(aq) + Na2S2O3(aq) ÿ S(s) + SO2(aq) +
H2O(l)) at 200C 6. Do not play “connect-a-dot” with the data. When appropriate, draw a smooth curve to “best
fit” the points. In many cases the curve may be a line. When using the computer, the line
or curve may be calculated by regression analysis. If this is the case, the function used for
the regression should be shown with the graph. The values of the adjustable parameters
should also be included. 7. DO NOT use data points for the calculation of the slope. If the slope is calculated “by hand”
the points used for the calculation must be clearly indicated on the graph. Clearly label the
points with ‘x’ and ‘y’ co-ordinates. Format for First-Year Chemistry Laboratory Reports Laboratory reports in first-year chemistry are not “formal” reports. That is, you do not need
to submit reports with “Introduction”, “Method”, “Results and Discussion” sections. You need to
submit your original data (signed by the TA), your sample calculations (including graphs) and the
answers to any questions posed in the laboratory manual.
15 U OIT Chem. 1020U, W14; Introduction - 11.20 PROCESS FOR RE-SCHEDULING MISSED LABORATORIES If miss your laboratory period (for whatever reason), you should complete the “Request for
Re-Scheduled Laboratory” form available in the “Laboratories” section of the Blackboard site for
the course. If missing the laboratory period is foreseeable (for religious observance, varsity athletics,
etc.), the request should be submitted in advance. To complete the form, you must suggest an
alternative time to attend a laboratory period. It is solely the responsibility of the student to find a laboratory period when they can attend.
A list of scheduled laboratory periods is available on the “Preview of Available Courses” at
MyCampus: http://www.uoit.ca/mycampus/avail_courses.html There must be sufficient space in the laboratory period. In other words, the number of students
enrolled in the section must be less than the maximum number of students (usually 23 or 24) allowed
in the section. Note, re-scheduling is done on a first-come, first-served basis; a laboratory period
may be full because of re-scheduling even if MyCampus indicates a vacancy. Once completed, the form should be submitted via e-mail to the senior laboratory instructor
([email protected]) for the course for approval. Do NOT submit the form through
Blackboard. You should use your “uoit.net” email account to submit the form. Your request should
be submitted at least three days in advance of the laboratory period you wish to attend. You should
use the following subject line in your e-mail: <Chem XXXX> - request for lab re-schedule, <your name> 16 U OIT Chem. 1020U, W14; Introduction - 11.20 If your request is approved, the senior laboratory instructor will sign and return the form to you by
e-mail. Approval is solely at the discretion of the senior laboratory instructor and not all requests
will necessarily be approved. If your request is approved, you mus...

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