228 Winter 2012 Manual

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Chemistry 228

General Chemistry Lab 2

Winter 2012

Lab Coordinators:

Dr. Eric Sheagley
sheagley@pdx.edu

Dr. Gwen Shusterman
shustermang@pdx.edu

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Chemistry 228
General Chemistry Laboratory
SYLLABUS Winter 2012

Lab Packet: All printed material for this lab will be available on Blackboard OR may be
purchased at Smart Copy (1915SW6
th
Avenue).

Prelab Exercises: Prelab instructions are included in the lab packet. You should
answer any questions presented and prepare for the weeks lab before your lab meeting.
Pre-labs are due at the beginning of the lab period.

Materials: You will need chemical splash safety goggles. These are available from the
chemistry stockroom (Room 280 SRTC) or at the campus bookstore. You will need a bound
carbonless copy notebook (not loose paper) for recording data. You are responsible for all
laboratory equipment checked out to you. If you break glassware, you will pay the replacement
cost of the glassware.

Dress for lab: You must wear shoes that cover your entire foot, including the heel.
They should fit up near your ankle; leather is preferred but any non-porous material is
okay. Short shorts and short skirts are not allowed. Your clothing must cover your
torso and legs down to your knees.

Grading: The laboratory is graded on a Pass/No Pass basis. An average of 75% of all
points available in the lab is required to pass.

Late Work: Laboratory reports are due at the beginning of the lab period following
completion of the experiment. Lab reports should be typed. Late reports will be
docked 5 points per day late.

Attendance: Attendance in this lab is mandatory.
YOU MUST ATTEND ALL SCHEDULED LABORATORY MEETINGS. If you are not
able to attend lab you must notify your laboratory instructor as soon as possible.
Students are responsible for completing the lab report for the missed lab. Data can be
obtained from a lab partner or the lab TA. The made up work should be clearly labeled
and indicate the origin of the data reported. Reports are due the class meeting
following the syllabus deadline. In addition to completing the make-up lab you must
make up the missed lab time. The make-up laboratory will not be the same lab you
missed but will be a unique activity that will take place during week 10 of the quarter,
during the regularly scheduled lab period. FAILURE TO DO BOTH WILL RESULT IN
A NO PASS GRADE. If you miss two or more labs your grade will be a NO PASS.

NOTE: If you are more than 15 minutes late to lab you will be marked late. Two late
arrivals during the term will be counted as a missed lab. In addition, late students may
be assigned to lab clean up duties at the conclusion of the lab period. If you are
chronically late you will be given a NO PASS.

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Plagiarism: Experiments will be done in groups sharing the computer for data analysis
and acquisition. You may compare data with other groups, but the content of your lab
reports MUST be written individually. It will be considered an act of plagiarism if you
borrow tables or graphs from another student (learning how to properly create a table
or graph is an important skill, learn how to do it on your own!). You cannot paraphrase
the internet, your book or any other source without the proper reference. Additionally,
it will be considered an act of plagiarism if you borrow data without prior approval
from your TA. There are additional resources online to help you avoid plagiarism.
Please be sure to check http://www.lib.pdx.edu/instruction/survivalguide/writeandcitemain.htm
or http://web.pdx.edu/~b5mg/plagweb.html, and feel free to discuss the issue with your TA or
the lab coordinator.

Depending on the severity of the offense(s), you will receive, at a minimum, a zero score for the
report. Additionally, a report may be made to the Office of Student Affairs.

Grading Criteria

Unless otherwise noted, every lab report is worth 90 points, including the prelab,
notebook and technique. Each lab report will be graded according to the following point
distribution:

Prelab: 10 points

Abstract: 10 points

Introduction: 10 points

Data: 10 points

Results: 15 points

Discussion: 15 points

In addition to the above points each lab meeting will have an additional 20 points
assigned on the following basis:

Notebook: 10 points
These points are awarded by the TA based upon the quality of your lab notebook. Your
TA will be looking to see that you are including a title, a statement of purpose, the
procedures, data tables and that all data is present.

Lab technique: 10 points
The basis for assigning these points includes (but is not limited to) general lab technique
and methods, safety, general mannerism in lab and cleanliness.

Both of these criteria will be evaluated by your TA during each lab meeting. At the end
of each lab you must check out with your TA so that he or she can assess your lab
notebook and verify that you have cleaned your work area

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Chemistry 228
Winter 2012 Schedule

Week 1
Check-in.
Announcements and registration adjustments and Lab Safety
View the Lab Safety Video. A link is available on D2L. Complete the quiz, also
available on D2L, before returning week 2 or you will not be able to participate in the
lab.
Enthalpy of Neutralization of Phosphoric Acid

Week 2
Monday is a holiday, the observance of Martin Luther King, Jr. Day.
All labs canceled for the week.

Week 3 (Enthalpy of Neutralization of Phosphoric Acid report due)
Enthalpy of Reaction and Hess's Law

Week 4 (Hesss Law report due. Please write your TAs name on the report and deposit it in the
mailbox located outside of the door to the chemistry office on the second floor of SRTC)
Gas Laws Online Lab. All lab sections do not meet.

Week 5 (Gas Laws online report due)
Decomposition of Hydrogen Peroxide

Week 6 (Decomposition of Hydrogen Peroxide report due)
Vapor Pressure and Heat of Vaporization

Week 7 (Vapor Pressure and Heat of Vaporization report due)
Using Freezing Point Depression to Find Molecular Weight

Week 8 (Molecular Weight by Freezing Point Depression Report Due)
Kinetics: Rate and Order of a Chemical Reaction

Week 9 (Kinetics: Rate and Order of a Chemical Reaction report due)
Chemical Equilibrium: Finding a Constant K
c

Week 10 (Chemical Equilibrium: Finding a Constant K
c
report due)
Make up Lab
Check Out and

Labs are graded on a Pass/No Pass basis.

In order to pass the lab you must turn in every lab report.

More than one absence will result in a No Pass for the class.

You must receive 75% or greater of all the points available to pass.

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Do not copy your partners, friends, old lab reports. That is plagiarism!
Laboratory Safety
Rules and
Procedures

Safety Rules
The guidelines below are established for your and your classmates personal
safety. Failure to adhere to the guidelines below will result in a loss of Lab
Technique points.

Personal Protective Equipment (PPE) is used to protect you from serious injuries or illnesses
resulting from contact with chemical hazards in the laboratory. Spills and other accidents can
occur when least expected. For this reason it is necessary to wear proper PPE. The PPE for
student labs consist of goggles, gloves and clothing. Proper PPE is required for all students or
they will be asked to leave the lab

Goggles Goggles must be worn whenever any experimental work is being done in the
laboratory to protect the eyes against splashes. Only indirect-vented goggles are
allowed in the student labs and should be worn at all times when any chemical is being
used in the lab. These are for sale in the bookstore and stockroom. You should not wear
contact lenses in a chemical laboratory. Chemical vapors may become trapped behind the
lenses and cause eye damage. Some chemicals may dissolve soft contact lenses. The
most important aspect of having the goggles fit comfortably is the proper
adjustment of the strap length. Adjust the strap length so that the goggles fit
comfortably securely and are not too tight. If you find that your goggles tend to fog,
you can pick-up anti-fog tissue from the stockroom.

Gloves Gloves should be worn to protect the hands from chemicals. Gloves are
provided through your student fees and are located in the student labs. For health and
safety reasons it is important to always remove at least one glove when leaving the
student laboratory, this prevents things such as door handles from getting contaminated.

Clothing Dress appropriately for laboratory work. You must wear shoes that cover
your entire foot, including the heel. They should fit up near your ankle; leather is
preferred but any non-porous material is okay. Your clothing must cover your torso and
legs down to your knees. Short shorts, short skirts, tank tops and halter tops are not
allowed.

Eating, drinking and smoking are prohibited in the laboratory at ALL times. Wash your hands
after finishing lab work and refrain from quick trips to the hall to drink or eat during lab. If
you take a break, be certain to remove gloves and wash hands before ingesting food or drink.

Never work alone in the laboratory or in the absence of the instructor.

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Headphones may not be worn in lab.

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Safety Procedures

Know location of safety equipment; fire extinguisher, fire blanket, first aid kit, safety
shower, eyewash fountain and all exits.

In case of fire or accident, call the instructor at once.

Small fires may be extinguished by wet towels.

If a persons clothing catches fire, roll the person in the fire blanket to extinguish the
flames.

In case of a chemical spill on the body or clothing, stand under the safety shower and
flood the affected area with water. Remove clothing to minimize contamination with the
chemical.

If evacuation of the lab is necessary, leave through any door that is safe, or not
obstructed; doors that lead to other labs may be the best choice. Leave the building by
the nearest exit and meet your TA on the field next to Hoffmann Hall. This would also
be the meeting place in the event of an earthquake or other emergency. It is good to know
the nearest exits of your lab on the first day of class.

Spilled chemicals must be cleaned up immediately. If the material is corrosive or
flammable, ask the instructor for assistance. If acids or bases are spilled on the floor or
bench, neutralize with sodium bicarbonate, then dilute with water. Most other chemicals
can be sponged off with water.

Avoid contact with blood or bodily fluids. Notify the instructor or stockroom personnel if
ANY blood is spilled in the lab so that proper clean up and disposal procedures may be
followed.

If a mercury thermometer is broken, do not attempt to clean up yourself. Notify students
around you, so that mercury is not spread, then notify your lab instructor or stockroom
personnel. The stockroom is equipped for proper clean up and disposal of mercury.

Laboratory Procedures and Protocol

General Etiquette:

Leave all equipment and work areas as you would wish to find them.

Keep your lab bench area neat and free of spilled chemicals. Your book bag, coat, etc.,
should be kept in the designated area at the entrance to the lab, not at your bench.

All chemical waste must be disposed of in proper containers. Proper disposal of chemicals
is important for student safety and proper disposal. Putting chemicals into the wrong
containers can lead to injury from unexpected chemical reactions. Mixing waste can also

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make it more difficult or expensive for PSU to dispose of them. Only chemicals should go
into waste jars. Waste jars for each experiment will be provided in the lab. They will be
labeled specifying which contents should be placed inside. It is important that you replace
the lids to the waste containers. When done with the waste jar, make sure it is placed in a
secondary container. Do not put anything down the sink unless you are explicitly told to
dispose of it this way. Your instructor will provide specific disposal guidelines when
needed. Following these guidelines assists us in lowering the environmental impact of the
labs.

There are several locations for very specific waste.
i. Chemical waste these containers are ONLY for chemical waste generated
in the lab. They are each specifically labeled for each lab and waste type.
READ THE LABELS.
ii. Contaminated paper waste this is ONLY for paper towels used for
clean-up of chemical spills.
iii. Broken glass this is ONLY for broken glassware.
iv. Gloves this is ONLY for used gloves.
v. Normal trash this is for all other trash that is not chemically
contaminated, glass, or gloves.

Clean your bench and equipment Clean all your glassware- dirty glassware is harder to
clean later. Wash with water and detergent scrubbing with a brush as necessary. Rinse well
with water. Do not dry glassware with compressed air, as it is frequently oily. The water
and gas should be turned off and your equipment drawer locked.

Clean the common areas before you leave the lab. Point deductions for the entire class
will be imposed if the instructor or stockroom is not satisfied.

Return any special equipment to its proper location or the stockroom.

Handling Chemicals:

Obtaining reagents:

Read the label CAREFULLY. The Chemicals are organized by experiment in secondary
containment bins. Make sure the chemical name and concentration match what is required
by the experiment!

Do not take the reagents to your bench.

We recommend always picking up bottles by the label. If all students do this, then any
unnoticed spills when pouring will not cause possible problems for the next user.
Remember to wear gloves while working with reagents.

Do not put stoppers or lids from reagents down on the lab bench. They may become
contaminated. Be sure that the lids or stoppers are replaced.

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Do not place your own pipet, dropper, or spatulas into the reagent jar. Pour a small amount
into a beaker and measure from that. Please pour on the conservative side to minimize
waste and cost of labs. You can always go back for more.

Do not put any excess reagent back in the reagent jar. Treat it as waste and dispose of it
properly.

When weighing chemicals on the balances, never weigh directly onto the weighing pan.
Weigh into a weighing boat or beaker. Any spills on the balances MUST be cleaned up
immediately. If you are unclear how to clean a spill, notify your instructor. The balances
you are using are precision pieces of equipment and costs up to $4000.

All chemicals should be treated as potentially hazardous and toxic. Never taste a chemical
or solution. When smelling a chemical, gently fan the vapors toward your nose.

Any chemicals that come in contact with your skin should be immediately washed with soap
and copious amounts of water.

Laboratory Procedures

Never pipet any liquid directly by mouth! Use a rubber bulb to draw liquid into the pipet.

Never weigh hot chemicals or equipment.

When heating a test tube, always use a test tube holder and be certain never to point the
open end of the test tube toward yourself or another person.

Handling glass tubing or thermometers: to insert glass tubing into a rubber stopper,
lubricate the glass tubing with a drop of glycerin, hold the tubing in your hand close to the
hole, and keep all glass pieces wrapped in a towel while applying gentle pressure with a
twisting motion.

To prepare a dilute acid solution from concentrated acid, acid should be added slowly to
water with continuous stirring. This process is strongly exothermic, and adding water to
acid may result in a dangerous, explosive spattering.

Use the fume hood for all procedures that involve poisonous or objectionable gases or
vapors.

Never use an open flame and flammable liquids at the same time.

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Keeping a Lab Notebook

In keeping a lab notebook, there are certain principles that should be followed. These boil down
to being clear and complete in your entries in your lab notebook. There are also certain
conventions for lab notebooks that are universally followed. High on this list are the following:

Use a notebook with pre-numbered pages
Record entries in ink
Keep entries reasonably neat and organized
Never tear pages out of your lab notebook (other than the carbonless copy pages)

What Kind of Notebook Should I Use?
For this class you must use a notebook with carbonless copy pages.

General Guidelines

Write your name on outside front of notebook
Use black ink, fine-tipped ball-point pen (this will photocopy clearly)
At the front of the notebook, leave a few pages for a Table of Contents
Each lab should have a brief introduction and description of procedure
Generally use only the right hand page for most text
Use facing left page for working graphs, manual calculation, and working notes
Prepare data tables in advance - with columns for calculated results and notes
Working graphs done in lab notebook to monitor progress

Usage and Structure

The overriding principle for a lab notebook is to record in it all the pertinent information about
your lab work. This boils down to clear descriptions of what you did and what you observed as
a result. It is a working tool, and a reference for other researchers who might want to read your
notebook and reproduce your work. (This applies to notebooks in learning laboratories: Your lab
instructor may want to look at what you did in order to understand your results. This is often the
case. So, it needs to be clear.)

The word clear here is crucial. In order to be clear, data must be recorded in well-thought-out
tables, clearly labeled. Descriptions of procedures must be clear and concise; to the point.

You should record all your work in your lab notebook. That is the proper place for all lab
planning and observations. Nothing should be recorded on odd scraps of paper, etc.

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Structure for your Lab Notebooks:

For each lab in this class you should have the following sections in your lab notebook:
Title
Purpose
Procedure and Observations
It is also often helpful to include a Result section

Note: When preparing your notebook for lab only write on the right hand page.

Title:
With your lab notebook laid open, on the right hand page write down the title of the
experiment, and the date. In general, you will use the right-hand page for all your writing. The
left-hand page is reserved for recording scratch work. Dont use this space until you need to.
One example of how to use the left-hand page: if your work requires simple calculations using
your measurements, use the left-hand page to do the calculations. If unexpected results occur
later, sometimes you can look back at your scratch work and discover the error. (Oh, I
subtracted wrong! We put in 10.5 grams of copper sulfate, not 9.5 like we thought!) Better to
discover the error after the fact than never to discover it at all.

Purpose:
Below the title, write the purpose of the experiment in one or two sentences. This section serves
to remind you and notify the reader what the experiment is about.

Procedure and Observations:
This next section will be labeled Procedure and Observations. As the name suggests, write
down what you actually do and what you observe. This section is where you should have pre-
prepared tables for data collection. Set up this section by dividing the page into a right and
left column. In the left hand column write your procedure and in the right column next to
the procedure, record observations and data or measurements.

Results and Discussion:
You might want to include a final section that is labeled Results and Discussion. In this section,
you would describe what results you got, what conclusions you have reached, ideas for
continuing work, etc.

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An example of a prepared notebook follows.

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Writing Style in the Lab Notebook

For certain entries in your lab notebook, such as the Introduction before each experiment, you
should strive to write as logically and clearly as possible. It is also a good idea to write in the
third person passive voice, to get into the habit, and so that in many cases you can copy entries
from your lab notebook into your reports without the need for major revisions/rewrite.

However, this is a working document. It is not expected that you write perfect prose in your
notebook it is a first draft. Just do the best you can.

Also, as a working document, with many entries being written while an experiment is in progress
(your observations) it is understood that many entries will be brief but still record crucial
observations.

Example

Notebook entry:
Added 10 mL of 1M HCl solution turned red instantly; pcpt. a few secs later clr soln.

When written into a lab report or journal article, this would be expanded a bit and made
grammatically correct.

10 mL of 1.0 M HCl were added to the clear reaction mixture. This immediately resulted in a
crimson solution, and a red precipitate formed a few seconds later, leaving a clear solution.

Adapted courtesy of Keith James

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Report Guidelines

For most experiments performed this term you will turn in a type written report (at the end of
each lab you will find a summary of which sections to include in the report for that lab). The
reports are due at the beginning of class the week following completion of the experiment.
Below is a description of what should be included in each section. The sections are presented
here in the order they should appear in your lab report.

It is expected that you will complete each experiment and do the necessary calculations and
analysis during the scheduled lab period each week. You may discuss the calculations and
analysis with your lab mates. Your written lab report should be your own individual work!! The
lab report sections should be complete but CONCISE. For most experiments this term, your
report should be 1-2 pages long.

Writing Style
You will write you reports using a formal scientific writing style. A lab report must be written in
the third person, passive voice. Also, it must be in the past tense. It should not contain personal
pronouns such as, I, we or he neither should it contain proper names of persons.

Good: 50 mL of 1.0 M HCl were poured into a 125 mL Erlenmeyer flask

Bad: I poured 50 mL of hydrochloric acid into a flask.

Also bad: Joe Shmoe poured 50 mL of hydrochloric acid into a flask. This is not the correct
form of 3
rd
person. It includes Joes name.

Also bad: We are going to put 50 mL of acid into the flask. Uses future tense; also, we.

After you write your report, there is one more thing to do before you print it and hand it in:
Proofread it! Read it out loud. If is doesnt sound right, it isnt. Fix it. Then do it again until it
is right. You will enjoy writing reports more if you take pride in what you hand in.

Abstract:
This is like a condensed version of your lab report. It is a stand-alone document. Abstracts are,
in fact, often published separately from the articles they describe. A library search of the
literature generally involves reading abstracts. This is done with the aim to identify articles that
need to be read in full, and eliminate many others whose abstract makes it clear that they are not
relevant to the study at hand. So, the abstract needs to be brief, but complete.

There are three questions that should be answered in any good abstract
1. What did you do?
2. How did you do it?
3. What did you find?

Even though it sequentially appears first, you should consider writing this part of the lab report
after you have finished the remaining sections.

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Introduction:
Here, you want to address WHY you did this experiment. Your introduction begins with a
statement of the purpose of the experiment. You will do this again in the abstract, but remember
the Abstract is a stand-alone document. What you say there will not count; you will find that as
you write the report that you will be repeating yourself a bit.

Next, provide any relevant background, to put the experiment into context. Include any key
concepts, mathematical equations or chemical equations needed by the reader to understand your
experiment. This means that your Introduction will often include some explanation of the
theory behind the experiment. Dont just write the equations, but provide information as to
why they are relevant. You may consider writing your introduction with a central theme, such as
density, types of chemical reactions..

Data:
This is section is where your experimental data belong. In this section you would also
include observations and descriptions of other pertinent events. This section is not where the
calculations, interpretation and discussion of your results belong. (In published papers, a data
section is usually not included, but, this is a class so this section will be included.)

Tables
Whenever possible, data should be presented in the clearest format possible, usually in the
form of a table. When you present your data in a table it is necessary to take the following
into account.
- Number tables sequentially as they appear (Table 1, Table 2.).
- Be sure to refer the reader to view the tables in the text.
- Construct a descriptive table caption and place it above the table.
- Tables should include descriptive column headings, including units.
- Tables should not be divided across page boundaries

For a simple example, see Table 1.

Table 3: Mass of Water as Determined by a Pan Balance (+/- 0.01g): Here
the volume of water delivered by a 10 mL volumetric pipet was determined
utilizing the mass of water delivered and waters density (0.9980 g/ml).
Run # mass water weighed (g) Volume water (ml)
1 9.95 -
2 9.94 -
3 9.98 -
Average 9.96 9.98
Error +/- 0.02 +/- 0.02

Graphs
When graphical presentation of data is necessary, please prepare graphs using the following
guidelines.
- Number figures sequentially as they appear (Figure 1, Figure 2.).
- In your writing, be sure to cite the tables in the text.

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- Insert a caption below he graph that indicates what is being plotted on the y-axis vs. what
is being plotted on the x-axis (always y vs. x)
- Each axis should be clearly labeled, including units.
- Figures should not be divided across page boundaries
- Remove gridlines, titles and equations from the graph. If this information is pertinent, it
should be included in the caption.
- If the slope or intercept is necessary for other parts of the experiment, then place the
values in the caption with proper units.

For a simple example, see Figure 1.

Figure 1. A calibration curve for the absorbance at 470 nm of aqueous Allura red solutions as a function of
the concentration. A best fit line was rendered resulting in a slope of 5.86 mM
-1
.

Results:
The results section is where you should show sample calculations and report all of your
results.

For every type of calculation you should show one sample calculation. Each calculation should
have a descriptive title, i.e. Calculating the density of Coca-Cola. The calculation section
should be annotated. The annotation is provided to describe why each calculation is useful and
relevant to the lab activity. The description should not be any longer than two or three sentences
and should help you describe your results in your discussion section. Sample calculations may be
written by hand attached as an appendix to your report. The results of all calculations should be
summarized in a table where appropriate.

Calculating the density of Coca-Cola
The volume (355 mL) and mass (394 g) of the contents of a can of coke had previously been
determined above. The density is determined utilizing the relationship d=m/v (equation 1) which
was explained in the introduction.
d = 394 g / 355 mL = 1.11 g/mL

Discussion:
In this section, you will discuss interpretations of the experimental results. This is where
you get to present your thinking process. For any labs that have questions to answer, this is also
where the answers get written up.

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The discussion is one of the most important parts of the lab report! It is your chance to
show WHAT YOUR RESULTS ARE and that you UNDERSTAND what you did in the
lab. This DOES NOT mean to include detailed procedures or that you need to re-explain your
calculations in words. It DOES mean that a general description of the experiment can be useful
in explaining your results and putting them in context.

In this section you should also discuss error analysis. This does not necessarily mean trying to
explain what went wrong. (Maybe nothing did go wrong!) It means discussing the limitations of
your experiment. For example, if you are doing calorimetry in a coffee cup, and the cup feels
warm to your hand, it means that some heat is escaping. Also, if you are reading a 5 degree
temperature change with a thermometer that you can only read to the nearest 0.5 degree, there is
a significant uncertainty in the exact magnitude of the temperature change. You could easily
have a 10% error, or even more, and this needs to be taken into account. It at least needs to be
mentioned, to show that you were aware of the issue. This is a limitation of the apparatus, not an
error on your part.

And, yes, if something did go wrong (your lab partner forgot to write down the exact molarity of
your reagent), then that should go here, too, along with an explanation of how you attempted to
correct for the error. (In this case, you may have had to re-do the experiment.)

Adapted courtesy of Keith James.

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Example Lab Report
Following is an example of a lab report prepared according to the previous report guidelines.
Sample calculations can be written on a separate paper and attached to the report.

Calibration of a 10 ml Volumetric Pipette a 10

Abstract:
A 10 ml volumetric pipette was calibrated by determining the mass of water delivered by
a pipette. A pipet was used to precisely deliver 10 mL of water. The mass of water was then
converted to volume using the density of water. The volume of the pipette was determined to be
9.98 +/- 0.02 ml when the mass of water was determined on a pan balance and 9.998 +/- 0.002
ml when determined with an analytical balance.

Introduction:
A volumetric pipette is designed to deliver a stated volume of liquid; however, the actual
amount of liquid any individual pipette delivers may vary slightly from this ideal stated volume.
In order to determine the actual volume an individual pipette delivers, it will be calibrated. In
this case, calibration refers to the comparison of the actual amount of liquid delivered by the
pipette to the standard value of the pipette (10 ml).
Because delivered volume is being calculated, another measurable quantity must be used
to verify the volume delivered by the pipette. In this case, the relationship between mass and
volume (density) will be used. Mass is an easily measurable quantity that can be determined
with a high degree of accuracy due to the availability of electronic balances. Mass can then be
converted to volume by the use of density.

D (density) = m (mass)/ V (volume)

The density of water at a variety of temperatures is readily available and will be used here to
calibrate the volume of the pipette.

Data:
Diameter of beaker: 3.9 cm +/- 0.1 cm
Mass of water evaporated in 60 seconds: 0.0016g +/- 0.0002g
Temp of water: 20.5 C +/- 0.2 C
Density of water: 0.9980 g/ml

Table 1: Mass Determined by Pan Balance (+/- 0.01g)
Run # mass beaker (g) mass beaker + water (g)
1 27.88 37.83
2 27.88 37.82
3 27.88 37.86

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Table 2: Mass Determined by Analytical Balance (+/- 0.0001g)
Run # mass beaker (g) mass beaker + water (g) t(transfer) t(weigh)
1 27.2349 36.5618 2:29:00 2:30:30
2 27.2348 36.7813 2:32:00 2:33:20
3 27.2335 36.8251 2:41:20 2:42:30

Results:

Calculation of the volume of water: In this calculation, the average mass of water for the three
trials, shown in Table 1, as determined by the pan balance was divided by the know density
of water at 20.5 C. The data are summarized in Table 3.

Volume = 9.96 g / 0.9980 g/mL = 9.98 mL

Table 3: Mass of Water as Determined by a Pan Balance (+/-
0.01g): Here the volume of water delivered by a 10 mL
volumetric pipet was determined utilizing the mass of water
delivered and waters density (0.9980 g/ml).
Run # mass water weighed (g) Volume water (ml)
1 9.95 -
2 9.94 -
3 9.98 -
Average 9.96 9.98
Error +/- 0.02 +/- 0.02

Calculation for the mass evaporated: To correct for evaporation of water in the time it takes to
measure the mass of the water delivered by the volumetric pipet, the mass of water that
evaporated was estimated. The rate of evaporation of water in the 50 mL beaker in 60
seconds: 0.0016g. The data are summarized in Table 4.

Mass evaporated = rate of evaporation x time of evaporation
= (0.0016 g/ 60 s) x 90 s = 0.0024 g

Calculation of the mass transferred: The mass of water initially transferred was the sum of the
mass of water evaporated and the mass of water present at the time of weighing (Table 2). The
data are summarized in Table 4.

Mass transferred = mass water weighed + mass (transferred)
= 9.9769 + 0.0024 = 9.9793 g

21
Table 4: Mass of Water as Determined by an Analytical Balance (+/-0.0001 g): ): Here the volume of water
delivered by a 10 mL volumetric pipet was determined utilizing the mass of water delivered and the density
water (0.9980 g/ml). A correction was added to account for the water that evaporated during the
measurement.
Run # mass water weighed (g) t(evap) (s) mass (evap) (g) mass (transferred) (g) Volume (ml)
1 9.9769 90 0.0024 9.9793 -
2 9.9735 80 0.0021 9.9757 -
3 9.9756 70 0.0019 9.9775 -
Average 9.978 9.998
Error +/- 0.002 +/- 0.002

Discussion:
The mass of water delivered by a 10 ml volumetric pipette was determined on both a pan
balance and an analytical balance (Tables 1 and 2 respectively). The mass of water was then
converted to volume using the density of water. In the case of the analytical balance, the rate of
evaporation of water (which is a systematic error) was taken into consideration. In this case the
mass of water that evaporated from the time the water was delivered to the beaker to the time of
weighing was added to the weighed mass of water delivered by the pipette. This correction was
not necessary when the pan balance was used since the accuracy of the pan balance is +/- 0.01 g
and the evaporation rate of water under experimental conditions was found to be 2.7 x 10
-5
g/s.
The use of the analytical balance increased both the precision and the accuracy of the calculated
volume of the pipette (9.98 +/- 0.02 ml with the pan balance and 9.998 +/- 0.002 ml with the
analytical balance, see tables 3 and 4). The improvement in the results can easily be seen by the
percent error which was calculated to be 0.2 % with the pan balance and 0.02 % with the
analytical balance. The largest source of error in this experiment most likely came from the
difficulty in accurately filling the pipette to the mark with water which introduced random error
into the experiment.

22
General Chemistry Lab Report Checklist

General
_____ Have you listed your name, partner's name, a descriptive lab title and date?
_____ Did you use spellchecker?
_____ Is your report written in passive third person voice (you did not use the words I,
we, they, etc.)
_____ Is proper tense is maintained within sections?
_____ Have you correctly written your chemical formula and names correctly?
_____ Were correct subscripts, superscripts, and symbols are used?
_____ Did you separate the numbers from their units (0.25 mL was added. not 0.25mL
was added)?
_____ Did you check significant figures?
_____ Do your numbers include leading zeros (0.25 mL was added. not .25 mL was
added)?
_____ Did you make sure that you did not start a sentence with a number?
_____ Are your references cited in one official style?
_____ Have you made a citations whenever ideas from outside?
_____ All subjects and verbs are in agreement?
_____ Did you make sure that there are no run-on sentences or fragments?

Abstract
The abstract is a condensed summary of the report's findings. Abstracts are often written last.
They should be clear, concise, and self-contained and, in the context of this lab, approximately
three sentences long.
_____What did you do? (Identify the rationale behind the investigation)?
_____How did you do it (summarize the procedure, without using specific steps)?
_____Present the important findings numerically including error statistics?

Introduction
The introduction will provide the reader information on what you are doing why you did it and
critical background information necessary in understanding the methods and results of your
experiment.
_____Did you include a statement of purpose?
_____Is there sufficient background so that the reader can understand what you did?
_____Are necessary equations, chemical or mathematical, included?

23
Data
This section should give only the data and observations from the lab, without results
_____Are your data tables properly formatted?
_____Are your calculations, either attached as an appendix, or typed neatly into the data
section?
_____Are your figures and tables numbered sequentially and referred to in the text. Table
captions above and figure captions below. Tables and figures are not broken over
multiple pages
_____Are the axes on your graphs formatted properly with labels?
_____Are all graphs and tables accompanied by a written description relating the same
information to the reader?

Results:
We will be treating this section as a calculational section. This is where you will be showing all
calculations along with a written description as to how the calculations were carried out and what
the result of the calculation is and how it relates to the lab. Your readers must easily find your
results in order to evaluate and interpret them.
_____Are calculations accompanied by text explaining the both the method of calculation
and results of the calculation?
_____Units? Significant Figures?
_____Is a straight forward presentation of the results of your experiment included in
either a table or in text?
_____Can your key results be understood by a reader without reliance on figures and
tables?

Discussion:
In this section, you will discuss interpretations of the experimental results. It will be necessary to
describe your results, cite tables or figures. It should include a general description of the
experiment to put the results into context.
_____Can your key results and discussion be understood by a reader without reliance on
figures and tables?
_____Are key results highlighted and carefully explained?
_____Did you make logical deductions based on the results (usually questions are given
in the lab manual to help this)?
_____Have you discussed sources of error or ambiguities in the data?
_____Did you confirm all relationships that were stated in purpose or abstract?
_____Do your conclusions clearly contribute to the understanding of the overall
problem?

24
Chemistry 228

Pre-Lab: Enthalpy of Neutralization of Phosphoric Acid

Part A

Answer the following questions in your lab notebook (be sure to show work for
any calculations):

1. A neutralization reaction was carried out in a calorimeter. The temperature of the solution
rose from 20.0 C to 25.6 C. Is this reaction endothermic or exothermic?

2. A neutralization reaction was carried out in a calorimeter. The change in temperature (T)
of the solution was 5.6 C and the mass of the solution was 100.0 g. Calculate the amount
of heat energy gained by the solution (q
sol
). Use 4.18 J/(gC) as the specific heat, C
s
, of
the solution.

3. What is the value of q
reaction
for the neutralization reaction described in number 2?

4. How many moles of phosphoric acid are contained in 50.0 mL of 0.60 M H
3
PO
4
?

5. What is the value of AH
reaction
(in kJ/mol phosphoric acid) if 50.0 mL of 0.60 M H
3
PO
4
was
used in the reaction described in number 2?

Part B

Prepare your lab notebook for the lab. This includes stating the purpose of the
experiment, summarizing the procedure in a bulleted format (be sure to include
space for observations) and preparing any tables necessary for data collection.

At the start of your lab, remove the copies of the pages where you
completed the above work from your lab notebook and turn them into
your TA.

25
The Enthalpy of Neutralization
of Phosphoric Acid
OBJECTIVES
In this experiment, you will
- Measure the temperature change of the reaction between solutions of sodium hydroxide
and phosphoric acid.
- Calculate the enthalpy, H, of neutralization of phosphoric acid.
- Compare your calculated enthalpy of neutralization with the accepted value.
- Calculate the enthalpy, H, of neutralization per ionizable hydrogen for phosphoric acid.

INTRODUCTION
A great deal can be learned by conducting an acid-base reaction as a titration. In addition, acid-
base reactions can be observed and measured thermodynamically. In this case, the reaction is
carried out in a calorimeter. If the temperature of the reaction is measured precisely, the enthalpy
of neutralization of an acid by a base (or vice versa) can be determined. In this experiment, you
will react phosphoric acid with sodium hydroxide.
You will use a Styrofoam cup nested in a beaker as a calorimeter, as shown in Figure 1. For
purposes of this experiment, you may assume that the heat loss to the calorimeter and the
surrounding air is negligible. Phosphoric acid will be the limiting reactant in this experiment, and
you will accordingly be determining the enthalpy, H, of neutralization of the acid. Selecting a
limiting reactant helps ensure that the temperature measurements and subsequent calculations are
as precise as possible.
Pages 246-248 and 257-258 in your text will provide background information.

Figure 1
MATERIALS NEEDED
Vernier computer interface
Temperature Probe

PROCEDURE
1. Obtain and wear goggles. It is best to conduct this experiment in a well-ventilated room.

26
2. Connect a Temperature Probe to Channel 1 of the Vernier computer interface.
3. Start the Logger Pro program on your computer. Open the file Lab 1 Phosphoric from the
Chemistry 228 folder.
4. Nest a Styrofoam cup in a 250 mL beaker as shown in Figure 1. Measure out 50.0 mL of
0.60 M H
3
PO
4
solution into the foam cup. CAUTION: Handle the phosphoric acid with
care. It can cause painful burns if it comes in contact with the skin.
5. Use a utility clamp to suspend the Temperature Probe from a ring stand (see Figure 1).
Lower the Temperature Probe into the phosphoric acid solution.
6. Measure out 50.0 mL of 1.85 M NaOH solution in a graduated cylinder and transfer it to a
250 mL beaker. CAUTION: Sodium hydroxide solution is caustic. Avoid spilling it on your
skin or clothing.
7. Conduct the experiment.
a. Click to begin the data collection and obtain the initial temperature of the H
3
PO
4

solution.
b. After you have recorded three or four readings at the same temperature, add the 50.0 mL
of NaOH solution to the Styrofoam cup all at once. Use a glass stirring rod to stir the
reaction mixture gently and thoroughly.
c. Data will be collected for 10 minutes. You may terminate the trial early by clicking
, if the temperature readings are no longer changing.
d. Click the Statistics button, . The minimum and maximum temperatures are listed in the
statistics box on the graph. If the minimum temperature is not a suitable initial
temperature, examine the graph and determine the initial temperature.
e. Record the initial and maximum temperatures for Trial 1.
f. Close the Statistics box by clicking the X in the corner of the box.
8. Rinse and dry the Temperature Probe, Styrofoam cup, and stirring rod. Dispose of the
solution as directed.
9. Repeat Steps 48 to conduct a second trial. If directed, conduct a third trial. Print a copy of
the graph of the second trial to include with your data and analysis.

27
DATA TABLE
Trial 1 Trial 2 Trial 3
Maximum temperature (C)
Initial temperature (C)
Temperature change (T)
DATA ANALYSIS
6. Write the balanced equation for the reaction of phosphoric acid and sodium hydroxide.

7. Use the equation below to calculate the amount of heat energy gained by the solution (q
sol
).
In determining the mass, m, of the solution use 1.11 g/mL for the density (be sure to use the
total volume of the solution after the acid and base are mixed). The change in temperature
(T) is a directional change where T = T
f
T
i
. Use 4.18 J/(gC) as the specific heat, C
s
,
of the solution.
q
sol
= C
s
m T

8. The heat calculated above represents the heat gained by the solution (the solution being
predominantly water). Since we are interested in the heat of neutralization of phosphoric
acid we need the heat transfer associated with the reaction (q
rxn
). If the solution gained
heat, the reaction must have given off heat. This relationship can be expressed by the
following equation:
q
sol
= -q
rxn

9. Determine the number of moles of phosphoric acid used in the reaction. Use the moles of
phosphoric acid along with q
rxn
to determine the enthalpy change, H, for the reaction in
terms of kJ/mol of phosphoric acid. This is your experimental value of H.
H = q
rxn
/moles H
3
PO
4

10. The accepted value for the H of neutralization for phosphoric acid is -156.44 kJ/mol.
Calculate the percent error in your experimental value.

28
The Enthalpy of Neutralization of Phosphoric Acid Lab Report

Your report for this lab should include the following sections:

Abstract:
Your abstract should be written individually

Introduction:
Include why you did this experiment, relevant background, and general equations.

Data:
Include your data table

Results:
Report your calculated value of H of neutralization for phosphoric acid and the
value of H of neutralization per ionizable hydrogen in phosphoric acid.
Include a results table with results from each trial and an average value for the H
of neutralization for phosphoric acid.
Report the percent error for the H of neutralization for phosphoric acid.
Be sure to attach hand written sample calculations to the back of your report.

Discussion:
Discuss the experiment and any possible sources of error

29

Chemistry 228

Pre-Lab: Hesss Law

Part A

any calculations):

1. What is the formula that relates the temperature change observed in a substance with the
energy released or absorbed?

2. When you measure a temperature rise during a chemical reaction, is the reaction endothermic
or exothermic?

3. The enthalpy of the reaction for the reaction of calcium oxide with hydrochloric acid is
exothermic. Will the reverse reaction have a positive or negative AH?

4. Hesss Law allows us to combine reactions to determine the heat of reaction for a net reaction
that has not been measured. For the reactions described in the lab, the second reaction is difficult
to measure as written. You will measure the heat of reaction for the reverse reaction. How will
you use the measurement in the Hesss Law calculation?

Part B


your TA.

30

Enthalpy of Reaction and Hess's Law

Introduction

In this experiment you will be finding the enthalpy of formation for MgO
(s)
using an
indirect method. Remember, according to Hess's Law (see your textbook for more
details), if two or more reactions can be added to give a net reaction, AH

for the net
reaction is simply the sum of the AH
'
's for the reactions which are added. Consider the
following three reactions:

1) Mg
(s)
+ 2 H
+
(aq)
---> Mg
2+
(aq)
+ H
2(g)
AH
1

2) Mg
2+
(aq)
+ H
2
O
(l)
---> MgO
(s)
+ 2 H
+
(aq)
AH
2

3) H
2(g)
+ 1/2 O
2(g)
---> H
2
O
(l)
AH
3

4) Mg
(s)
+ 1/2 O
2(g)
---> MgO
(s)
AH
4

You will determine the heat of reaction for reactions 1 and 2 experimentally, then use
the known value of the enthalpy of formation of water (AH
3
= -285.9 kJ) to calculate
AH
4
which is the enthalpy of formation of MgO. Be aware that equation (2) is the
reverse of the reaction you actually run and measure. (Note: the enthalpy of formation
of MgO cannot easily be measured.)

Experimental Procedure

Obtain a coffee cup calorimeter from the stockroom. Make sure the cup is clean and
dry.

a) Using a weighing boat, weigh out a sample containing between 0.45 - 0.55 grams
of magnesium. Put 50. mL of 1.0 M HCl into the calorimeter and measure the
temperature until it stabilizes. Record this reading as your initial temperature.
Then add the Mg and replace lid. Stir vigorously as the metal dissolves (use a stir
rod, not the thermometer), and record the temperature every 30 seconds until it is
approximately constant for two minutes. Record your data in your lab notebook.
Use a format that allows you to readily identify which experiment you are
recording.

Conduct another trial as above. Make sure the calorimeter is clean and mostly dry
before repeating the experiment.

31

b) Repeat the above procedure, this time replacing Mg with MgO. (Use a clean, dry
calorimeter.) You should use a molar equivalent of MgO (24.3 g Mg is the molar equivalent
of 40.3 g MgO, why?, your measurement should be within 5%) Be certain all the MgO
dissolves, this will require vigorous stirring!!

Conduct another trial as above.

Calculations
To relate heats of reactions (in energy units of Joules) with temperature differences we
use:
q = m x S x AT

For the reactions above, it is a good approximation to take specific heat of the solution
to be the specific heat of water, S = 4.184 J/g-C.

For mass, because you are using the specific heat of pure water, use the mass of the
water only, not the combined mass of water and solute.

Calculate q for reaction 1 and 2.

Report AH
rxn
for reaction 1 and 2, be certain to use units of kJ/mol.

Calculate AH
4

Caution: Wear your goggles at all times. HCl is a
strong acid. Hydrogen gas is flammable. Do not use
any open flames in the lab.

32

Hesss Law Lab Report:


Abstract:

Introduction:

Data:
Prepare a data table that includes the initial and final temperatures for each trial
Report the mass of Mg and MgO used in each trial

Results:
Prepare a results table showing the calculated AH
rxn
for each trial and averages
for reactions one and two and the value of AH

for reaction four
Be sure to attach hand written sample calculations to the back of your report

Discussion:
As part of your discussion, answer the following questions:
1. For an exothermic reaction, does the temperature observed rise or fall?
2. For an exothermic reaction, is AH
positive or negative?
3. Is reaction 1 endothermic or exothermic? reaction 2?
4. In this lab, you measure the quantity, q. How is this different
from AH
rxn
, (remember the definitions and units)?

Answer the following question and attach it to your report:
Further Analysis

An alloy (a metal mixture) containing magnesium and another metal, that does not
react with hydrochloric acid, needs to analyzed. You are asked to determine the
percent magnesium in the alloy. a) Describe the procedure you would use to
determine the percent magnesium in the alloy, and b) if the sample were 30%
magnesium calculate the heat evolved if a 5 gram sample were analyzed in that
manner.

33

Deriving the Gas Laws Using Computer Simulations

Introduction

According to the kinetic molecular theory, gases are in constant and random motion with enough
kinetic energy such that they rarely interact with one another. When gas particles collide with the
walls of a container, they rebound with no apparent loss of energy. These characteristics describe
an "Ideal Gas." Experimental evidence suggests that many common gases making up air behave
in this manner when studied at temperatures well above their boiling points.

We are constantly being exposed to the behavior of gases. Each time we pump up a tire, blow up
a balloon, use a spray can, or experience the cooling of gases as they escape from a gas storage
container, we are reminded of how gases behave with changes in temperature (T), volume (V),
pressure (P), or number of particles (n).

The behavior of gases has been scientifically investigated starting with Robert Boyle's work in
1662, followed by Jacques Charles' (1787) and Joseph Gay-Lussac's work (1802). Together these
studies led to the so called "Gas Laws" which relate volume (V), pressure (P), temperature (T)
and numbers of particles of gas (n).

In a scientific manner, one can derive the mathematical relationships that exist between these
variables by holding two of the variables constant, changing one and monitoring the effect on the
fourth variable. To derive the relationships, you will be using an interactive research-based
simulation produced by the PhET project at the University of Colorado.

PROCEDURE 1: Pressure Volume Relationship
1. Go to the Physics Education Technology from the University of Colorado at:

http://phet.colorado.edu/new/simulations/sims.php?sim=Gas_Properties

2. Click the RUN NOW button under the Gas Properties Simulation window (highlighted in
green).

3. Play around with the simulator and see what sorts of tools are available to you to analyze
the behaviors of gases. Qualitatively get a feel for the relationships that exist between the
four variables that describe gases: P, V, n and T. If you ever get to a point that you need
to reset the simulator, you can always hit the reset button at the bottom right of the
screen.

4. If you have not already done so, on the lower right side of the screen, click on the
RESET button.

5. On the right side of the screen, click on the MEASURMENT TOOLS button. Next,
click on the RULER option to activate the ruler.

34

CLICK

HERE

6. In the upper right hand corner, click on the TEMPERATURE button under the
Constant Parameter heading. This will hold temperature constant while allowing you to
observe the relationship between pressure and volume.

CLICK

HERE

7. Using the mouse and the right button, drag the ruler into a position that will allow you to
measure the length of the container.

8. Using the mouse and the right button, grab hold of the man pushing against the container
and expand the length of the container so that it measures 9.0 cm. Record this as your
initial length (the height of the box will remain 5.0 cm and the width of the box will
remain 5.0 cm)

35

GRAB
AND
DRAG

9. Using the mouse and the right button, grab hold of the pump handle and inject one cycles
worth of gas into the chamber by pulling the handle up then pushing it back down.

MOVE UP THEN DOWN

10. Once the pressure has somewhat stabilized, record your pressure value for the chamber
length of 9.0 cm. This will represent your initial pressure in atmospheres.

36

PRESSURE (ATM)

11. Using the mouse and right button, grab hold of the man pushing on the container and
decrease the length of the container to approximately 8.0 cm. Once the pressure has
stabilized (again, this may take a short period of time to happen), record the new pressure
for a length of 8.0 cm.

PUSH IN

12. Repeat step 9 for approximate lengths of 7.0 cm, 6.0 cm, 5.0 cm, 4.0 cm, 3.0 cm, and 2.0
cm (you will probably not get to exactly 2 cm). For each trial, record the length value
and resulting pressure value in a properly labeled data table.

37
13. Record any qualitative observations on the behavior of the gas molecules as the volume
decreases.

14. Click the RESET button to remove all the gas particles from the chamber before moving
on to the next section.

PROCEDURE 2: Volume Temperature Relationship
Devise an experiment using the simulator in which you can elucidate the relationship between
Temperature and the Volume of a gas. Collect and record your data over a wide range of
temperatures, 0-600 K, in a properly labeled table

Procedure 3: Temperature Pressure Relationship
Temperature and the Pressure of a gas. Collect and record your data over a wide range of
temperatures, 0-600 K, in a properly labeled table

Procedure 4: Pressure Quantity Relationship
Quantity and the Pressure of a gas. Collect and record your data over a wide range of number of
molecules in a properly labeled table

Analysis:
For this lab, you will need to submit neat labeled data tables for each procedure. You must also
submit a graphical representation for each relationship. Be sure to label each axis and include a
title for each graph (Please see the information on pages 15 and 16 of this lab manual). I
suggest that you utilize Microsoft Excel or some other comparable spreadsheet software to
produce your tables and graphs. Along with the graphs and tables for each procedure, answer
completely the questions below that correlate with each section.

Analysis: Procedure 1: Pressure Volume Relationship
1. Graphically represent the Pressure (atm) Volume (cm
3
) relationship with volume on the
x-axis.
2. Graphically represent the Pressure (atm) and Inverse Volume, 1/V (cm
-3
) relationship
with 1/V on the x axis
3. Identify the mathematical relationship that exists between pressure and volume, when
temperature and quantity are held constant, as being directly proportional or inversely
proportional. Explain your answer and write an equation that relates pressure and volume
to a constant.
4. Why were you asked to graph pressure and the inverse of volume?
5. Calculate the slope of the line for your pressure vs. 1/volume graph. What does this
number represent? Would you expect it to be the same for all gases? Explain your
answer.

38
Analysis Questions: Procedure 2: Volume Temperature Relationship
6. Graphically represent the Temperature (K) Volume (cm
3
) relationship.
7. Identify the mathematical relationship that exists between volume and temperature, when
pressure and quantity are held constant, as being directly proportional or inversely
proportional. Explain your answer and write an equation that relates volume and
temperature to a constant.
8. Calculate the slope of the line for your temperature vs. volume graph. What does this
answer.

Analysis Questions: Procedure 3: Temperature Pressure Relationship
9. Graphically represent the Temperature (K) Pressure (atm) relationship. Make sure the
axis that represents temperature includes a range from 0 K to 600 K.
10. Identify the mathematical relationship that exists between pressure and temperature,
when volume and quantity are held constant, as being directly proportional or
inversely proportional. Explain your answer and write an equation that relates pressure
and temperature to a constant.
11. Calculate the slope of the line for your temperature vs. pressure graph. What does this
answer.
12. Explain the effects of temperature on molecular motion. Using this explanation, explain
why both pressure and volume can decrease with decreasing temperature.
13. Absolute zero is theorized to be the temperature that all molecular motion stops. Based
on this, what would you predict to be the pressure and volume of a gas sample whose
temperature is decreased to absolute zero? Explain.

Analysis Questions: Procedure 4: Pressure Quantity Relationship
14. Graphically represent the Quantity (number of molecules) Pressure (atm) relationship
15. Describe the impact of increasing the number of molecules (or moles) of a gas on the
pressure of a gas sample. Would you expect this trend to be the same for all gases?
Explain your answer.
16. Based on your previous observations, predict the impact of changing the number of moles
of a gas sample on the volume of the gas sample (if pressure and temperature are held
constant) and on the temperature of a gas sample (if pressure and volume are held
constant). Explain your answer.

39

Chemistry 228

Pre-Lab: Decomposition of Hydrogen Peroxide

Part A

any calculations):

1. What is Daltons law of partial pressure?

2. A mixture of three gasses (A, B and C) has a total pressure of 849 torr and the partial
pressure of A is 57 torr and the partial pressure of B is 573 torr. What is the partial
pressure of C?

3. A gas has a volume of 94 mL, a pressure of 743 torr and a temperature of 20 C.
Calculate the number of moles of gas present. Assume ideal behavior of the gas.

4. If 0.00946 moles of O
2
gas is collected from the decomposition of hydrogen peroxide,
how many moles of hydrogen peroxide were reacted?

Part B


your TA.

40
Decomposition of Hydrogen Peroxide

OBJECTIVES

Decompose hydrogen peroxide using KI as a catalyst
Measure the volume of oxygen gas generated through the decomposition reaction
Illustrate Daltons Law of partial pressure
Determine the number of moles of oxygen gas produced using the ideal gas law
Determine the percent hydrogen peroxide in an aqueous solution

INTRODUCTION

Hydrogen peroxide spontaneously decomposes to form oxygen gas according to the
following equation:

2 H
2
O
2
(aq) 2H
2
O (l) + O
2
(g)

This process usually occurs very slowly. Many different compounds or ions are capable of
acting as catalysts increasing the rate of the reaction. Here, potassium iodide (KI) will be used as
a catalyst to make the reaction produce products rapidly enough to study the reaction in the lab.
The apparatus we will use to collect oxygen gas in this experiment is shown in figure 1.
Hydrogen peroxide will be placed in the Erlenmyer flask. The catalyst (KI) is located in the
syringe and can be added to the Erlenmyer flask to initiate the reaction. As the reaction proceeds
oxygen gas will be produced in the Erlenmyer flask and travel through the tubing. The gas will
be collected in the graduated cylinder. The graduated cylinder is initially filled with water. As
the gas enters the cylinder it displaces water allowing the volume of the gas to be measured.

Figure 1

41
MATERIALS NEEDED
125 mL Erlenmyer flask
100 mL graduated cylinder
Rubber stopper with adaptors, tubing and syringe

PROCEEDURE

1. Place an 125 mL Erlenmyer flask on a balance and tare the scale. Add approximately 5 g
of hydrogen peroxide solution into the Erlenmyer flask. Record the actual mass used.
Obtain a ring stand and clamp the flask as shown in figure 1. Place the rubber stopper
tightly in the flask (this should be air tight).
2. Place approximately 400 mL of water in an 800 mL beaker.
3. Completely fill a 100 mL graduated cylinder with water. Cover the cylinder with
parafilm and invert the cylinder in the 800 mL beaker. Carefully clamp the cylinder in
place such that the opening of the cylinder is below the surface of the water in the beaker.
Remove the parafilm and carefully place the end of the tubing just inside the graduated
cylinder as shown in figure 1. The graduated cylinder should be completely filled with
water. If there is a small amount of air present in the cylinder record the volume. If there
is more than 10 mL of air in the cylinder, you will need to redo the setup.
4. In a small beaker obtain a small amount (approximately 10 mL) of 0.5 M KI. Draw up 3
mL of the KI solution into the syringe. Attach the syringe to the adaptor in the rubber
stopper.
5. Initiate the reaction by depressing the stopper on the syringe and adding the KI to the
hydrogen peroxide.
6. Allow the reaction to proceed until no further production of oxygen gas is observed
(around 10 to 15 minutes).
7. Measure and record the temperature of the water.
8. Record the final level of the water in the graduated cylinder. Be sure to record your
measurement to 2 decimal places.
9. Repeat the above procedure two more times for a total of three trials. At least two of
your trials should agree well with one another.

DATA ANALYSIS

1. Determine the pressure of the oxygen gas:
Because the oxygen gas was collected over water some of the gas collected is water
vapor. The gas collected is therefore a mixture of both oxygen and water. The total
pressure of the gas is the sum of the pressures exerted by the oxygen gas and water vapor.
To determine the pressure of oxygen gas we must apply Daltons law of partial pressure.

P
Tot
= p
O
2

+ p
H
2
O

In other words, you can find the pressure of oxygen gas by subtracting the partial
pressure of water at the temperature of the water (also known as the vapor pressure of
water) from the total pressure (or atmospheric pressure). Your TA will provide the

42
current barometric pressure. A table of the vapor pressure of water at various
temperatures follows.

Table 1: Vapor pressure of water at various temperatures
Temperature
Vapor
Pressure Temperature
Vapor
Pressure Temperature
Vapor
Pressure
(
o
C) (torr) (
o
C) (torr) (
o
C) (torr)
15 12.8 21 18.6 27 26.7
16 13.6 22 19.8 28 28.3
17 14.5 23 21.1 29 30
18 15.5 24 22.4 30 31.8
19 16.5 25 23.8 31 33.7
20 17.5 26 25.2 32 35.7

2. Determine the volume of the oxygen gas:
When the reaction was initiated, 3 mL of KI solution was added. This volume needs to
be subtracted from the volume of gas collected. If your initial volume of gas was not
zero, this must also be taken into consideration.

V
O
2
= V
final
V
initial
3 mL

3. Calculate the number of moles of oxygen gas generated:
Now that the pressure, volume and temperature of the gas are known, the moles of gas
can be calculated using the ideal gas law. The temperature of the gas will be considered
to be the same temperature as the water temperature measured during the experiment.

PV = nRT

4. Calculate the amount of H
2
O
2
:
Using the balanced equation, calculate the number of moles of H
2
O
2
present in the initial
solution. Calculate the molar mass of H
2
O
2
and determine the grams of H
2
O
2
present in
the initial solution.

5. Calculate the mass percent of hydrogen peroxide:
Using the mass of H
2
O
2
calculated above and the initial mass of the H
2
O
2
solution,
calculate the mass percent H
2
O
2
in the initial solution.

43
Hydrogen Peroxide Lab Report:


Abstract:

Introduction:

Data:
Include a data table with data from all 3 trials

Results:
Include a results table with the mass percent of hydrogen peroxide from each trial

Discussion:

44

Chemistry 228

Pre-Lab: Vapor Pressure and Heat of Vaporization

Part A

any calculations):

1. When using the equation P
1
/T
1
= P
2
/T
2
to relate temperature and pressure of a gas, what
must be held constant?

2. A sample of gas is held in a capped flask. At 25 C the pressure is 693 mmHg. What is
the pressure of the gas at 37 C?

3. If the heat of vaporization of water is 40.7 kJ/mol, how much energy is required to
vaporize 5.0 g of liquid water at 100 C?

4. Would you expect most of the components in a perfume to have a low or high vapor
pressure? Explain.

Part B


your TA.

45
Vapor Pressure and
Heat of Vaporization
When a volatile liquid is placed in a container, and the container is sealed tightly, a portion of the
liquid will evaporate. The newly formed gas molecules exert pressure in the container, while
some of the gas condenses back into the liquid state. If the temperature inside the container is
held constant, then at some point a physical equilibrium will be reached. At this equilibrium, the
rate of condensation is equal to the rate of evaporation. The pressure at equilibrium is called
vapor pressure, and will remain constant as long as the temperature in the container does not
change.
In mathematical terms, the relationship between the vapor pressure of a liquid and temperature is
described in the Clausius-Clayperon equation,
C
T R
H
P
vap
+ |
.
|
\
|
A
=
1
ln
where ln P is the natural logarithm of the vapor pressure, H
vap
is the heat of vaporization, R is
the universal gas constant (8.31 J/molK), T is the temperature (in Kelvin) and C is a constant not
related to heat capacity. Thus, the Clausius-Clayperon equation not only describes how vapor
pressure is affected by temperature, but it relates these factors to the heat of vaporization of a
liquid. H
vap
is the amount of energy required to cause the vaporization of one mole of liquid at
constant pressure.
In this experiment, you will introduce a specific volume of a volatile liquid into a closed vessel,
and measure the pressure in the vessel at several different temperatures. By analyzing your
measurements, you will be able to calculate the H
vap
of the liquid.
OBJECTIVES
- Measure the pressure inside a sealed vessel containing a volatile liquid over a range of
temperatures.
- Determine the relationship between pressure and temperature of the volatile liquid.
- Calculate the heat of vaporization of the liquid.

Figure 1

46
MATERIALS
Vernier Gas Pressure Sensor
Temperature Probe
rubber stopper assembly
plastic tubing with two connectors
PROCEDURE
1. Obtain and wear goggles. CAUTION: The alcohol used in this experiment is flammable and
poisonous. Avoid inhaling the vapors. Avoid contact with your skin or clothing. Be sure that
there are no open flames in the room during the experiment. Notify your teacher immediately
if an accident occurs.
2. Use a hot plate to heat ~200 mL of water in a 400 mL beaker.
3. Prepare a room temperature water bath in an 800 mL beaker. The bath should be deep
enough to completely cover the gas level in the 125 mL Erlenmeyer flask.
4. Connect a Gas Pressure Sensor to Channel 1 of the Vernier computer interface. Connect a
Temperature Probe to Channel 2 of the interface.
5. Start the Logger Pro program on your computer. Open the file Lab 4 Vapor Pressure from
the Chemistry 228 folder.
6. Use the clear tubing to connect the white rubber stopper to the Gas Pressure Sensor. (About
one-half turn of the fittings will secure the tubing tightly.) Twist the white stopper snugly
into the neck of the Erlenmeyer flask to avoid losing any of the gas that will be produced as
the liquid evaporates (see Figure 1). Important: Open the valve on the white stopper.
7. Your first measurement will be of the pressure of the air in the flask and the room
temperature. Place the Temperature Probe near the flask. When the pressure and temperature
readings stabilize, record these values.
8. Condition the Erlenmeyer flask and the sensors to the water bath.
a. Place the Temperature Probe in the room temperature water bath.
b. Place the Erlenmeyer flask in the water bath. Hold the flask down into the water bath to
the bottom of the white stopper.
c. After 30 seconds, close the valve on the white stopper.
9. Obtain a small amount of ethanol. Draw 3 mL of ethanol into the 20 mL syringe that is part
of the Gas Pressure Sensor accessories. Thread the syringe onto the valve on the white
stopper (see Figure 1).
10. Add ethanol to the flask.
a. Open the valve below the syringe containing the 3 mL of ethanol.
b. Push down on the plunger of the syringe to inject the ethanol.
c. Quickly pull the plunger back to the 3-mL mark. Close the valve below the syringe.
d. Carefully remove the syringe from the stopper so that the stopper is not moved.
11. Gently rotate the flask in the water bath for a few seconds, using a motion similar to slowly
stirring a cup of coffee or tea, to accelerate the evaporation of the ethanol.

47
12. Monitor and collect temperature and pressure data.
a. Click to begin data collection.
b. Hold the flask steady once again.
c. Monitor the pressure and temperature readings.
d. When the readings stabilize, click .
e. Record these values in your notebook.

13. Add a small amount of hot water, from the beaker on the hot plate, to warm the water bath by
35C. Use a spoon or a dipper to transfer the hot water. Stir the water bath slowly with the
Temperature Probe. Monitor the pressure and temperature readings. When the readings
stabilize, click . Record these values in your notebook.
14. Repeat Step 13 until you have completed five total trials. Add enough hot water for each trial
so that the temperature of the water bath increases by 3-5C, but do not warm the water bath
beyond 40C because the pressure increase may pop the stopper out of the flask. If you must
remove some of the water in the bath, do it carefully so as not to disturb the flask.
15. After you have recorded the fifth set of readings, open the valve to release the pressure in the
flask. Remove the flask from the water bath and take the stopper off the flask. Dispose of the
ethanol as directed.
16. Click to end the data collection. Record the pressure readings, as P
total
, and the
temperature readings in your data table.
17. Do not exit the Logger Pro program until you have completed 14 of the Data Analysis
section.
DATA TABLE

Initial Trial 1 Trial 2 Trial 3 Trial 4 Trial 5
P
total
(kPa)
P
air
(kPa)
P
vap
(kPa)
Temperature (C)

48
DATA ANALYSIS

1. The P
air
for Trials 2-5 must be calculated because the temperatures were increased. As you
warmed the flask, the air in the flask exerted pressure that you must calculate. Use the gas
law relationship shown below to complete the calculations. Remember that all gas law
calculations require Kelvin temperature. Use the P
air
from Trial 1 as P
1
and the Kelvin
temperature of Trial 1 as T
1
.
2
2
1
1
T
P
T
P
=
3. Calculate and record the P
vap
for each trial by subtracting P
air
from P
total
.
4. Prepare and print a graph of P
vap
(y-axis) vs. Celsius temperature (x-axis).
a. Disconnect your Gas Pressure Sensor and Temperature Probe from the interface.
b. Choose New from the File menu. An empty graph and table will be created in Logger Pro.
c. Double-click on the x-axis heading in the table, enter a name and unit, then enter the five
values for temperature (C) from your data table above.
d. Double-click on the y-axis heading in the table, enter a name and unit, then enter the five
values for vapor pressure from your data table above.
e. Does the plot follow the expected trend of the effect of temperature on vapor pressure?
Explain.
5. In order to determine the heat of vaporization, H
vap
, you will first need to plot the natural
log of P
vap
vs. the reciprocal of absolute temperature.
a. Choose New Calculated Column from the Data menu.
b. Create a column ln vapor pressure.
c. Create a second column, reciprocal of absolute temperature, 1/(Temperature (C) + 273).
d. On the displayed graph, click on the respective axes, and then select ln vapor pressure to
plot on the y-axis, and reciprocal of absolute temperature to plot on the x-axis. Autoscale
the graph, if necessary.
e. Calculate the linear regression (best-fit line) equation for this graph. Calculate H
vap
from
the slope of the linear regression.
f. Prepare and print a second graph.
6. The accepted value of the H
vap
of ethanol is 42.32 kJ/mol. Compare your experimentally
determined value of H
vap
with the accepted value.

49

Vapor Pressure and Heat of Vaporization Lab Report:


Abstract:

Introduction:

Data:
Include your data table

Results:
Include a copy of your graph of P
vap
vs. T (C)
Include a copy of your graph of ln P
vap
vs. 1/T (K)
Report your value for AH
vap
of ethanol
Report the percent error in your calculated value of AH
vap
for ethanol

Discussion:

50

Chemistry 228

Pre-Lab: Freezing Point Depression

Part A

any calculations):

1. What is a colligative property?

2. Give the equation for freezing point depression and indicate the units for each term in the
expression.

3. A measurement of the freezing temperature of a solution allows you to calculate the
concentration of the solution. What else do you need to measure to determine the molar mass of
the solid added to the solvent?

4. A student adds 1.504 g of a solid to 25.0 mL of water. The freezing temperature is measured
to be -1.20 C. What is the molality of the solution?

5. What is the molar mass of the solid above?

Part B


your TA.

51
Using Freezing-Point Depression
to Find Molecular Weight
When a solute is dissolved in a solvent, the freezing temperature is lowered in proportion to the
number of moles of solute added. This property, known as freezing-point depression, is a
colligative property; that is, it depends on the ratio of solute and solvent particles, not on the
nature of the substance itself. The equation that shows this relationship is:
AT = K
f
m
where AT is the freezing point depression, K
f
is the freezing point depression constant for a
particular solvent (8.28C-kg/mol for t-butanol in this experiment
1
), and m is the molality of the
solution (in mol solute/kg solvent).
In this experiment, you will first find the freezing temperature of the pure solvent, t-butanol,
C
4
H
10
O. You will then add a known mass of aspirin, to a known mass of t-butanol, and
determine the lowering of the freezing temperature of the solution. By measuring the freezing
point depression, AT, and the mass of aspirin, you can use the formula above to find the molar
mass of the aspirin solute, in g/mol.
OBJECTIVES
- Determine the freezing temperature of pure t-butanol.
- Determine the freezing temperature of a solution of aspirin and t-butanol.
- Examine the freezing curves for each.
- Calculate the experimental molar mass of aspirin.
- Compare it to the accepted molar mass for aspirin.

Figure 1
MATERIALS
Temperature Probe Copper stirrer

1
The Computer-Based Laboratory, Journal of Chemical Education: Software, 1988, Vol. 1A, No. 2, p. 73.

52

PROCEDURE
1. Obtain and wear goggles.
2. Connect the Temperature Probe to the computer interface. Prepare the computer for data
collection by opening the file 15 Freezing Pt Depression from the Chemistry with
Computers folder.
Part I Freezing Temperature of Pure T-butanol
3. Add about 175 mL of tap water 250 mL beaker. Using a hot plate warm the water to a
temperature of about 35 C. The t-butanol used in this experiment is flammable. Do not
use Bunsen burners during this lab.
4. Weigh a CLEAN, DRY test tube. It can be propped in a plastic 250 mL beaker to facilitate
measuring; this is useful when the tube is not empty. Add 3 mL of t-butanol to your test tube
using a dry Pasteur pipette. Do this carefully so that you do not get any t-butanol on the
upper portion of the test tube. Warm the t-butanol to 35 C for three minutes.
5. Insert the Temperature Probe into the hot t-butanol. About 30 seconds are required for the
probe to warm up to the temperature of its surroundings and give correct temperature
readings. During this time, fasten the utility clamp to the ring stand so the test tube is above
the water bath. Then click

to begin data collection.
6. Prepare a large beaker, 400-600 mL with an ice water bath. Fill beaker 2/3 full with tap
water. Lower the test tube into the water bath. Add ice to your water bath to bring the
temperature down. Make sure the water level outside the test tube is higher than the t-
butanol level inside the test tube.
7. With a very slight up and down motion with the copper stirrer, continuously stir the t-butanol
during the cooling.
8. Continue with the experiment until data collection has stopped (10 minute run). Use the hot
water bath to melt the probe out of the solid t-butanol. Do not attempt to pull the probe out
this might damage it. Carefully wipe any excess t-butanol liquid from the probe with a paper
towel or tissue. Weigh the test tube and t- butanol.
9. To determine the freezing temperature of pure t-butanol, you need to determine the mean (or
average) temperature in the portion of graph with nearly constant temperature. Move the
mouse pointer to the beginning of the graphs flat part. Press the mouse button and hold it
down as you drag across the flat part of the curve, selecting only the points in the plateau.
Click on the Statistics button, . The mean temperature value for the selected data is listed
in the statistics box on the graph. Record this value as the freezing temperature of t-butanol.
Close the statistics box.
Part II Freezing Temperature of a Solution of Aspirin and T-butanol
10. Store your data by choosing Store Latest Run from the Experiment menu. Hide the curve
from your first run by clicking on the vertical axis label and unchecking the appropriate box.
Click . Repeat steps 5-10 so that you have two trials of the freezing point t-butanol.
11. Measure out approximately 0.3 grams of aspirin into a weighing boat. Using a funnel, add
the aspirin to the t- butanol already in the 4 test tube. The purpose of the funnel is to
prevent aspirin from sticking to the inside wall of the test tube where it would be difficult (or
impossible) to get into solution. Be careful not to get the funnel stem into the solvent! If you
do, you will have to dump the solvent, clean and dry your apparatus, and start all over by
weighing out a new portion of t-butanol. Determine the mass of the aspirin by weighing the
test tube, solvent and aspirin. It may take several minutes for the aspirin to dissolve. Heat the

53
test tube gently with hot water and agitate very gently (be careful not to splash) until
dissolution is complete. Repeat Steps 3-8 to determine the freezing point of this mixture.
12. When you have completed Step 8, click on the Examine button, . To determine the
freezing point of the aspirin-t-butanol solution, you need to
determine the temperature at which the mixture initially started
to freeze. Unlike pure t-butanol, cooling a mixture of aspirin and
t-butanol results in a gradual linear decrease in temperature
during the time period when freezing takes place. As you move
the mouse cursor across the graph, the temperature (y) and time
(x) data points are displayed in the examine box on the graph.
Locate the initial freezing temperature of the solution, as shown
here. Record the freezing point in your data table.
13. Discard your solution and repeat from step 11 with a new sample of t-butanol and aspirin.
14. To print a graph of temperature vs. time showing all data runs:
a. Click on the vertical-axis label of the graph. To display both temperature runs, click More,
and check the Run 1 and Latest Temperature boxes. Click .
b. Label both curves by choosing Text Annotation from the Insert menu, and typing T-
butanol (or Aspirin-t-butanol mixture) in the edit box. Then drag each box to a position
on or near its respective curve.
c. Print the graph.

PROCESSING THE DATA (METHOD 1)
1. Determine the difference in freezing temperatures, At, between the pure t-butanol (t
1
) and the
mixture of t-butanol and aspirin (t
2
). Use the formula, At = t
1
- t
2
.
2. Calculate molality (m), in mol/kg, using the formula, At = K
f
m (K
f
= 8.28C-kg/mol for t-
butanol).
3. Calculate moles of aspirin solute, using the answer in Step 2 (in mol/kg) and the mass (in kg)
of t-butanol solvent.
4. Calculate the experimental molar mass of aspirin, in g/mol. Use the original mass of aspirin
from your data table, and the moles of aspirin you found in the previous step.
5. Compare your experimentally determined molar mass of aspirin with the known value.
6. Calculate the percent error.

Time
Freezing Point

54

PROCESSING THE DATA (METHOD 2)

Here is another method that can be used to determine the freezing temperature from your data in
Part II. With a graph of the Part II data displayed, use this procedure:
1. Move the mouse pointer to the initial part of the cooling curve, where the temperature has an
initial rapid decrease (before freezing occurred). Press the mouse button and hold it down as
you drag across the linear region of this steep temperature decrease.
2. Click on the Linear Fit button, .
3. Now press the mouse button and drag over the next linear region of the curve (the gently
sloping section of the curve where freezing took place). Press the mouse button and hold it
down as you drag only this linear region of the curve.
4. Click again. The graph should now have two regression lines displayed.
5. Choose Interpolate from the Analyze menu. Move the mouse pointer left to the point where
the two regression lines intersect. When the small circles on each cursor line overlap each
other at the intersection, the temperatures shown in either examine box should be equal to the
freezing temperature for the aspirin-t-butanol mixture.
6. Use the temperature to calculate AT and your molar mass for aspirin. Compare your results
from the two methods.

55

Freezing Point Depression Lab Report:


Abstract:

Introduction:

Data:
Include a data table with all necessary mass measurements
Include graphs for the freezing of t-butanol and t-butanol-aspirin solution

Results:
Report the freezing point of pure t-butanol
Report your calculated molar mass of aspirin
Determine the percent error in your calculated molar mass (the actual molar mass
of aspirin is 180.2 g/mol)
Calculate the percent error in your determined molar mass of aspirin

Discussion:

56

Chemistry 228

Pre-Lab: Kinetics

Part A

any calculations):

1. Write the general form of the rate law for the reaction you will be studying this week.

2. A first order reaction has a rate constant of 2.90 x 10
-4
s
-1
. Calculate the half-life for this
reaction.

3. What is the overall order of a reaction that has the following rate law? Rate = [A]
2
[B]

4. For a reaction where the general form of the rate law is rate = [A]
m
[B]
n
, the following
data were collected. What is the order of the reaction with respect to A? What is the
order of the reaction with respect to B?

Initial Rate [A] [B]
0.01 M/s 0.025 M 0.025 M
0.01 M/s 0.025 M 0.050 M
0.09 M/s 0.075 M 0.025 M

Part B


your TA.

57
The Rate and Order of
a Chemical Reaction
OBJECTIVES
- Conduct the reaction of KI and FeCl
3
using various concentrations of reactants.
- Determine the order of the reaction in KI and FeCl
3
.
- Determine the rate law expression for the reaction.

INTRODUCTION
A basic kinetic study of a chemical reaction often involves conducting the reaction at varying
concentrations of reactants. In this way, you can determine the order of the reaction in each
species, and determine a rate law expression. Once you select a reaction to examine, you must
decide how to follow the reaction by measuring some parameter that changes regularly as time
passes, such as temperature, pH, pressure, conductance, or absorbance of light.
In this experiment you will conduct the reaction between solutions of potassium iodide and iron
(III) chloride. The reaction equation is shown below, in ionic form.
2 I
(aq) + 2 Fe
3+
(aq) I
2
(aq) + 2 Fe
2+
(aq)
As this reaction proceeds, it undergoes a color change that can be precisely measured by a
Colorimeter (see Figure 1). By carefully varying the concentrations of the reactants, you will
determine the effect each reactant has on the rate of the reaction, and consequently the order of
the reaction. From this information, you will write a rate law expression for the reaction.

Figure 1
MATERIALS
computer
Vernier Colorimeter
plastic cuvettes

58
PROCEDURE
2. Connect a Colorimeter to Channel 1 of the Vernier computer interface.
3. Start the Logger Pro program on your computer. Open the file 30b. Crystal Violet from the
Chemistry with Computers folder.
4. Set up and calibrate the Colorimeter.
f. Prepare a blank by filling an empty cuvette full with distilled water. Place the blank in
the cuvette slot of the Colorimeter and close the lid.
g. If your Colorimeter has a CAL button, set the wavelength on the Colorimeter to 430 nm,
press the CAL button, and proceed directly to Step 5. If your Colorimeter does not have a
CAL button, continue with this step to calibrate your Colorimeter.
h. Choose Calibrate CH1: Colorimeter from the Experiment menu, then click .
i. Turn the wavelength knob on the Colorimeter to the 0% T position.
j. Type 0 in the edit box.
k. When the displayed voltage reading for Reading 1 stabilizes, click .
l. Turn the knob of the Colorimeter to the Blue LED position (470 nm).
m. Type 100 in the edit box.
n. When the voltage reading for Reading 2 stabilizes, click , then click .
5. Obtain the materials you will need to conduct this experiment.
- Three 25 mL graduated cylinders.
- Approximately 100 mL of 0.020 M KI solution in a 100 mL beaker.
- Approximately 100 mL of 0.020 M FeCl
3
solution in a separate 100 mL beaker.
CAUTION: The FeCl
3
solution in this experiment is prepared in 0.1 M HCl and should
be handled with care.
- Approximately 60 mL of distilled water in a third 100 mL beaker.
6. During this experiment you will conduct 5 trials. This step describes the process for
conducting the trials using the Trial 1 volumes. When you repeat this process, use the correct
volume for each trial based on the table below.
Trial FeCl
3
(mL) KI (mL) H
2
O (mL)
1 10.0 10.0 0.0
2 10.0 5.0 5.0
3 5.0 10.0 5.0
4 7.5 5.0 7.5
5 5.0 7.5 7.5

o. Measure 10.0 mL of FeCl
3
solution using a graduated cylinder and pour it into a large test
tube.
p. Measure 10.0 mL of KI solution using a graduated cylinder.
q. Prepare a clean cuvette.
r. Add the 10.0 mL of KI solution to the test tube containing 10.0 mL of FeCl
3
solution.
Cover the end of the test tube with your thumb and quickly invert to mix.
s. Within 15 seconds of mixing the two solutions, fill the cuvette full with the mixture.
Wipe the outside of the cuvette with a tissue, place it in the Colorimeter, and close the lid
and begin collecting absorbance data. The timing of this step is imperative to receiving

59
useful data; practice several times with water before attempting with the KI and FeCl
3

solutions.

7. Click to begin collecting absorbance data. Data will be gathered for 2 minutes.
Observe the progress of the reaction in the beaker.
8. When the data collection is complete, carefully remove the cuvette from the Colorimeter.
Dispose of the contents of the beaker and cuvette as directed. Rinse and clean the beakers
and the cuvette for the next trial.
9. Examine the graph of the first trial. On the toolbar, select the Slope button. Slide the
cursor to the initial time point. This tool will determine the initial slope and thus approximate
the initial rate of the reaction. Record the slope as the initial rate of the Trial 1 reaction.
10. Repeat Steps 69 to conduct Trials 25. When you complete Step 9, use the same technique
to analyze Trials 25 that you used to analyze Trial 1. Note: You will skip Step 6c in Trials
25.

DATA ANALYSIS
1. Calculate the initial molar concentration of FeCl
3
and KI for each reaction and
prepare a data table containing the concentrations of each reaction and the initial
reaction rate.
2. What is the order of the reaction in FeCl
3
and KI?
3. Write the rate law expression for the reaction.

60

Kinetics Lab Report:


Abstract:

Introduction:

Data:
Include your data table with the initial concentrations of each reactant and the
initial rate of each reaction
Include graphs for each of your kinetic trials

Results:
Report the order of the reaction with respect to each reactant
State the rate law for the reaction

Discussion:
Explain how you determined the order of each reactant
As part of your discussion, answer the following question:
1. Is it possible to calculate the rate constant, k, from your data? If so,
calculate the rate constant. If not, explain why not.

61

Chemistry 228

Pre-Lab: Chemical Equilibrium

Part A

any calculations):

1. Write the equilibrium constant expression for the experiment you will be studying this
week.

2. If the equilibrium values of Fe
3+
, SCN
-
and FeSCN
2+
are 9.5 x 10
-4
M, 3.6 x 10
-4
M and
5.7 x 10
-5
M respectively, what is the value of K
c
?

3. Write the general form of the dilution equation.

4. A solution is prepared by adding 18 mL of 0.200 M Fe(NO
3
)
3
and 2 mL of 0.0020 M
KSCN. Calculate the initial concentrations of Fe
3+
and SCN
-
in the solution.

Part B


your TA.

62
Chemical Equilibrium:
Finding a Constant, K
c
The purpose of this lab is to experimentally determine the equilibrium constant, K
c
, for the
following chemical reaction:
Fe
3
+
(aq) + SCN
(aq) FeSCN
2
+
(aq)
iron(III) thiocyanate thiocyanoiron(III)
When Fe
3
+
and SCN
-
are combined, a dynamic equilibrium is established between these two
ions and the FeSCN
2
+
ion. In order to calculate the equilibrium constant, K
eq,
for the reaction, it
is necessary to know the concentrations of all the ions at equilibrium. In this experiment four
separate equilibrium systems, or trials, containing different concentrations of these three ions
(Fe
3+
, SCN
-
, and FeSCN
2+
) will be determined experimentally. The values for these equilibrium
concentrations will be substituted into the equilibrium constant expression to see if K
eq
is indeed
constant despite varied initial concentrations for the reactants. The K
eq
, is determined by using
the Law of Mass Action.

aA + bB cC + dD

This equation gives the equilibrium constant expression of:

K
eq
= [C]
c
[D]
d
/[A]
a
[B]
b
In order to determine the equilibrium concentrations for the three ions a standard solution needs
to be prepared. To prepare the standard solution, a very large concentration of Fe
3
+
will be
added to a small initial concentration of SCN

(hereafter referred to as [SCN
-
]
i
. The initial
[Fe
3
+
] in the standard solution is 900 times larger than [SCN
-
]
i
. According to LeChatelier's
principle, which states that when a system in dynamic equilibrium is disturbed, the system
responds so as to minimize the disturbance and return the system to a state of equilibrium. This
high initial concentration Fe
3+
ions on the left side of the equation forces the reaction far to the
right, using up nearly 100% of the initial SCN

ions. Using stoichiometry and the balanced
equation, it is assumed that for every mole of FeSCN
2
+
produced, one mole of SCN
is used up.
Thus since nearly all of the SCN
-
ions are consumed in order to minimize the disturbance, the
products concentration, [FeSCN
2
+
]
std,
at equilibrium is assumed to be equal to the [SCN
]
i.

Since the reaction produces the FeSCN
2
+
ions and this ion transmits the color red, the solutions
absorbance of blue light can be measured through the use of a colorimeter (see Figure 1).
Because the red solutions absorb blue light very well, the blue LED setting on the Colorimeter is
used. The computer-interfaced Colorimeter measures the amount of blue light absorbed by the
colored solutions (absorbance, A).

63
Figure1 Figure 2
According to Beers Law, there is a direct relationship between a solutions concentration and its
absorbance. In this case the concentration is the FeSCN
2+
ion and the absorbance is blue light
(470 nm). In other words, as the concentration of FeSCN
2+
increases so will the absorbance of
blue light (see Figure 2). The concentration of FeSCN
2
+
for any of the equilibrium systems,
trials 1-4, can be found by comparing the absorbance of each equilibrium system, A
eq
, to the
absorbance of the standard solution, A
std
, according to the following equation:

[FeSCN
2
+
]
std/Astd

= [FeSCN
2
+
]
eq/ Aeq

Since the concentration of [FeSCN
2
+
]
std
is known and the all of the absorbances for the
equilibrium solutions and the standard are measured and recorded all that needs to be done is to
solve for the unknown.
[FeSCN
2
+
]
eq
=
A
eq
A
std
X [FeSCN
2
+
]
std

Knowing the [FeSCN
2
+
]
eq
allows you to determine the concentrations of the other two ions at
equilibrium. For each mole of FeSCN
2
+
ions produced, one less mole of Fe
3
+
and SCN
-
ions
will be found in the solution (see the 1:1 ratio of coefficients in the equation on the previous
page). At equilibrium the [Fe
3
+
] and [SCN
-
] can be determined according to the following
equations:
[Fe
3
+
]
eq
= [Fe
3
+
]
i
[FeSCN
2
+
]
eq

[SCN
]
eq
= [SCN
]
i
[FeSCN
2
+
]
eq
Knowing the values of [Fe

3
+
]
eq
, [SCN
]
eq
, and [FeSCN
2
+
]
eq
, you can now calculate the value
of K
c
, the equilibrium constant.

64
OBJECTIVE
In this experiment, you will determine the equilibrium constant, K
c
, for the following chemical
reaction:
Fe
3
+
(aq) + SCN
(aq) FeSCN
2
+
(aq)
iron(III) thiocyanate thiocyanoiron(III)

MATERIALS
Vernier Colorimeter
1 plastic cuvette
five 20 150 mm test tubes
pipet bulb or pipet pump
Serological pipet

PROCEDURE
2. Label four 20 150 mm test tubes 1-4. Pour about 30 mL of 0.0020 M Fe(NO
3
)
3
into a
clean, dry 100 mL beaker. Pipet 5.0 mL of this solution into each of the four labeled test
tubes. Use a pipet pump or bulb to pipet all solutions. CAUTION: Fe(NO
3
)
3
solutions in this
experiment are prepared in 1.0 M HNO
3
and should be handled with care. Pour about 25 mL
of the 0.0020 M KSCN into another clean, dry 100 mL beaker. Pipet 2, 3, 4 and 5 mL of this
solution into Test Tubes 1-4, respectively. Obtain about 25 mL of distilled water in a 100 mL
beaker. Then pipet 3, 2, 1 and 0 mL of distilled water into Test Tubes 1-4, respectively, to
bring the total volume of each test tube to 10 mL. Mix each solution thoroughly with a
stirring rod. Be sure to clean and dry the stirring rod after each mixing. Measure and record
the temperature of one of the above solutions to use as the temperature for the equilibrium
constant, K
c
. Volumes added to each test tube are summarized below:

Test Tube
Number
Fe(NO
3
)
3

(mL)
KSCN
(mL)
H
2
O
(mL)
1 5 2 3
2 5 3 2
3 5 4 1
4 5 5 0

3. Prepare a standard solution of FeSCN
2
+
by pipetting 18 mL of 0.200 M Fe(NO
3
)
3
into a
20 150 mm test tube labeled 5. Pipet 2 mL of 0.0020 M KSCN into the same test tube.
Stir thoroughly.
4. Connect the Colorimeter to the computer interface. Prepare the computer for data collection
by opening the file Lab 8 Equilibrium from the Chemistry 228 folder of Logger Pro
5. Prepare a blank by filling a cuvette 3/4 full with distilled water. To correctly use a
Colorimeter cuvette, remember:
- All cuvettes should be wiped clean and dry on the outside with a tissue.
- Handle cuvettes only by the top edge of the ribbed sides.

65
- All solutions should be free of bubbles.
- Always position the cuvette with its reference mark facing toward the white reference mark
at the top of the cuvette slot on the Colorimeter.

6. Calibrate the Colorimeter.
a. Open the Colorimeter lid.
b. Holding the cuvette by the upper edges, place it in the cuvette slot of the Colorimeter.
Close the lid.
c. If your Colorimeter has a CAL button, Press the < or > button on the Colorimeter to select
a wavelength of 470 nm (Blue) for this experiment. Press the CAL button until the red
LED begins to flash. Then release the CAL button. When the LED stops flashing, the
calibration is complete. Proceed directly to Step 7. If your Colorimeter does not have a
CAL button, continue with this step to calibrate your Colorimeter.

First Calibration Point
d. Choose Calibrate CH1: Colorimeter (%T) from the Experiment menu and then click
.
e. Turn the wavelength knob on the Colorimeter to the 0% T position.
f. Type 0 in the edit box.
g. When the displayed voltage reading for Reading 1 stabilizes, click .

Second Calibration Point
h. Turn the knob of the Colorimeter to the Blue LED position (470 nm).
i. Type 100 in the edit box.
j. When the displayed voltage reading for Reading 2 stabilizes, click , then click
.

7. You are now ready to collect absorbance data for the four equilibrium systems and the
standard solution.
a. Click to begin data collection.
b. Empty the water from the cuvette. Rinse it twice with ~1 mL portions of the Test Tube 1
solution.
c. Wipe the outside of the cuvette with a tissue and then place the cuvette in the Colorimeter.
After closing the lid, wait for the absorbance value displayed in the meter to stabilize.
Then click , type 1 (the trial number) in edit box, and press the ENTER key.
d. Discard the cuvette contents as directed by your teacher. Rinse the cuvette twice with the
Test Tube 2 solution and fill the cuvette 3/4 full. Follow the Step-c procedure to find the
absorbance of this solution. Type 2 in the edit box and press ENTER.
e. Repeat the Step-d procedure to find the absorbance of the solutions in Test Tubes 3, 4,
and 5 (the standard solution).
f. From the table, record the absorbance values for each of the five trials in your data table.
g. Dispose of all solutions as directed by your instructor.

66
PROCESSING THE DATA
1. Write the K
c
expression for the reaction in the Data and Calculation table.
2. Calculate the initial concentration of Fe
3+
, based on the dilution that results from adding
KSCN solution and water to the original 0.0020 M Fe(NO
3
)
3
solution. See Step 2 of the
procedure for the volume of each substance used in Trials 1-4. Calculate [Fe
3+
]
i
using the
equation:
[Fe
3+
]
i
=
Fe(NO
3
)
3
mL
total mL
(0.0020 M)

This should be the same for all four test tubes.
3. Calculate the initial concentration of SCN
, based on its dilution by Fe(NO

3
)
3
and water:
[SCN
]
i
=
KSCN mL
total mL
(0.0020 M)
In Test Tube 1, [SCN
]
i
= (2 mL / 10 mL)(0.0020 M) = 0.00040 M. Calculate this for the
other three test tubes.
4. [FeSCN
2+
]
eq
is calculated using the formula:
[FeSCN
2+
]
eq
=
A
eq
A
std
[FeSCN
2+
]
std

where A
eq
and A
std
are the absorbance values for the equilibrium and standard test tubes,
respectively, and [FeSCN
2+
]
std
= (1/10)(0.0020) = 0.00020 M. Calculate [FeSCN
2+
]
eq
for
each of the four trials.
5. [Fe
3+
]
eq
: Calculate the concentration of Fe
3+
at equilibrium for Trials 1-4 using the equation:
[Fe
3+
]
eq
= [Fe
3+
]
i
[FeSCN
2+
]
eq

6. [SCN
]
eq
: Calculate the concentration of SCN
-
at equilibrium for Trials 1-4 using the
equation:
[SCN
]
eq
= [SCN
]
i
[FeSCN
2+
]
eq
7. Calculate K
c
for Trials 1-4. Be sure to show the K
c
expression and the values substituted in
for each of these calculations.
8. Using your four calculated K
c
values, determine an average value for K
c
. How constant were
your K
c
values?

67
Equilibrium Lab Report:


Abstract:

Introduction:

Data:
Include your data table with initial concentrations of each reactant for each trial

Results:
Include a results table with calculated K
eq
values for each trial and an average
value for K
eq


Discussion:
In addition, answer the following question as part of your report:
1. How are you K
eq
values to each other? Are they close enough
to justify the assertion that an equilibrium constant is constant?
2. What factors could have led to variations in K
eq
between trials.

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Knowing the values of [Fe

, based on its dilution by Fe(NO

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