CEM 1610 Lab Manual Fall 2019
CEM 1610 Lab Manual Fall 2019
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Table of Contents
Laboratory Safety 3
Periodic Table 10
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Safety Agreement
Before you begin the lab experience for this semester you must sign a form indicating that you have read
and agree with the following laboratory safety statement. Be aware that the rules of the lab are for your
safety and the safety of others. These rules are based on the guidelines set forth by the EPA and OSHA.
Failure to abide by these rules violates Belmont, EPA and OSHA policies.
“I acknowledge that laboratory safety regulations and equipment have been explained to me. I agree to
abide by these regulations. I understand that my laboratory grade will be affected if these regulations are
violated and I may be asked to leave lab. I further agree that if I am injured while in violation of these
regulations, I absolve Belmont University and its employees of any liability for my injury.”
1. Know the exact location of all exits from the laboratory and building.
2. Determine the location and procedures to operate all safety equipment in the laboratory.
Available safety equipment may include: biological safety cabinets, eyewashes, fire
blankets, fire extinguishers, first aid kits, fume hoods, safety showers, or spill kits.
3. Notify my laboratory instructor or faculty advisor immediately if I might be pregnant, have
an allergy, or have any medical condition that could render me particularly susceptible to
chemical exposure.
4. Wear closed-toe shoes, appropriate clothing, and any required personal protective
equipment when working or observing in the laboratory. Clothing must fully cover the
torso and legs. Required personal protective equipment may include: face shields, gloves,
laboratory coats, rubber aprons, or safety glasses/goggles.
5. Secure long hair.
6. Keep the laboratory bench and floor around the work area uncluttered and free from book
bags, purses, coats, or other obstructions.
7. Not eat, drink, use tobacco, or apply cosmetics in the laboratory.
8. Not work in the laboratory unsupervised. Work may only be performed during times
assigned by your laboratory instructor or faculty advisor.
9. Come prepared and proceed with care when working in the laboratory. Only work
approved by your laboratory instructor or your faculty advisor may be performed.
10. Read reagent bottle and container labels carefully before use. All reagent bottles and
containers should be securely closed following use.
11. Exercise caution when working with Bunsen burners, hot plates, or hot water baths.
12. Immediately report chemical spills, damaged or malfunctioning equipment, and all injuries -
no matter how minor – to the laboratory instructor or faculty advisor.
13. Dispose of used or broken materials in proper waste containers according to my laboratory
instructor's or faculty advisor’s directions. Chemical waste containers must be
appropriately labeled and securely closed when not in use.
14. Clean work areas, common areas, glassware, reusable supplies, and equipment after use.
All items should be returned to their proper storage locations following use.
15. Wash hands thoroughly before leaving the laboratory.
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Keeping a Laboratory Notebook
In this course (and any future lab-based chemistry courses) you are required to keep an official laboratory
notebook. This notebook is will be your closest companion in lab. Everything you do in lab will be
recorded in your notebook. Below you will find everything you ever wanted to know about keeping your
notebook (probably more than you wanted to know).
The notebook must be bound so that pages cannot be ripped out and/or lost. Composition
notebooks with sewn pages work best.
Pages should be numbered starting with the very first page. Since composition books are not
usually numbered, you will need to do this yourself.
The first 2-4 pages should be left blank (initially) and filled in as the table of contents as you go.
Use PEN ONLY to write in your notebook. If you make a mistake draw a line through the mistake
and write the correct entry beside or above it.
DO NOT tear pages out of your notebook.
All data, observations, amounts used, etc. are entered in you notebook as you complete the
experiment. DO NOT write things down somewhere else to transfer into your notebook later.
Always write directly in your notebook.
ALWAYS write down all digits of numbers experimentally determined. Example: if you weigh out
exactly 6.100 g of something, write down 6.100 g…not 6.1 g; if you deliver 25 mL of a liquid using
a 25 mL volumetric pipet, write down 25.00 mL…not 25 mL.
Prepare for lab by making data tables in your lab notebook that you can fill in during lab.
Because you turn in pre-lab assignments before lab, you need to write any pertinent information
in your notebook. Example: did you calculate the concentration of a set of standards for pre-lab?
If so, you need to write those concentrations down in your notebook as well.
Your lab notebook must contain information about what was done and what was observed. It must also
be understandable (clear and legible) by someone else.
You absolutely should not be recording your data on a worksheet in real time. Always record data
in your lab notebook then transfer the pertinent information to the worksheet.
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Guidelines for Formal Chemistry Lab Reports
The primary goal of writing reports is to learn to communicate your lab findings in a clear, concise manner
so that others can understand what you have done and learned from the experience. Your reports should
be well-written scientific papers that guide the reader through your experiment from purpose to
conclusions and will be graded based on the format described below as well as adherence to rules of
English grammar, spelling, etc. These reports are typically 3-7 pages (single-spaced text) including
everything but the appendix. The key is to maximize your space by carefully choosing how to report your
data. You should have plenty of information to write about, so you should not be struggling to meet a
page minimum…you should be struggling to trim your report to include all of the relevant information and
not be too long. Keep reading for a more in-depth explanation of what should be in each section of your
report.
The Chemistry Lab Report format is based on the format of journal articles published in the Journal of the
American Chemical Society. Lab reports should contain the following sections and must be typed.
Reports are to be written in passive voice—you should be explaining what was done. Thus, terms like
“I, my, our, we,” etc. should not appear in your report.
1. Introduction: Your introduction should tell the reader why the experiment was completed. You must
explain the purpose of the experiment and the theory behind the experimental procedure. Background
information on the system (e.g. theory, reaction, or enzyme being studied) should be included and must
be properly cited. Figure(s) should be used where applicable (ChemDraw or equivalent figures are
expected for synthesis labs). Note that all figures should be labelled with a descriptive title and must
have a citation for the source if the author did not create the figure (eg: Figure 1. Reaction between A
and B. Drawn using ChemDraw). Most of your citation/references of source material will occur in the
Introduction.
How to write an introduction…determine the purpose of the experiment and write a thesis statement. Do
this before you do much research for your report. Once you have a thesis statement, you can build your
introduction. Find some sources (your textbook is usually a very good resource) and read different
passages that talk about what you have identified as the purpose. Think about it. Find any equations
(mathematical and/or chemical) that are necessary or helpful for explaining your results. Take some
notes. NOW write your intro so that, by the time the reader finishes reading your intro, (s)he knows the
purpose of the experiment, how you will conduct the experiment, why you are doing the experiment the
way that you are, and what kind of results you expect.
2. Experimental: The reader must be made aware of the step-by-step procedure followed during an
experiment. Sometimes it is necessary to write out (in paragraph form) the entire procedure. Often,
students can include only a brief narrative describing what the researcher actually did during the
experiment and refer the reader to the procedure in the lab book by referencing the lab book. Include
statements about the actual amounts of reagents (etc.) used in the experiment (eg 1.203 g of sodium
chloride...not ‘1 g’ as stated in the procedure). This section will NOT include a numbered or bulleted list
of steps. If no stepwise procedure was given for a particular experiment (i.e. you had to devise the
procedure yourself), include an explanation of the steps followed in paragraph form. Deviations from the
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referenced procedures should be noted in this section. Note that this section must be written in PAST
tense (because you are reporting what you already did) using PASSIVE VOICE (“the solution was
stirred”). Personal pronouns like ‘I’, ‘my’, ‘we’, etc should never appear in your experimental section.
3. Results: Report all lab data in tables and/or graphs as appropriate. The use of spreadsheet
software (such as Excel) will make this much easier to complete. Explanations of calculations, including
sample calculations, should be included when appropriate. Do NOT include repetitive calculations! You
may reference your lab notebook for sample calculations if necessary. Each table, graph and/or figure
should be placed in a logical location within or just before the discussion section and must be
discussed in the text of the report. Do NOT allow tables or figures to be split between pages if possible.
If a table, graph or figure is discussed in the text, then it is essential to the report and should be included.
If you have not referenced something in the body of your report, it should be moved to the Appendix. All
tables, graphs and figures must have a label and a descriptive title. [Example…Figure 1. Calibration
curve fit for determining copper concentration.]
4. Discussion: This is where you assign meaning to your data (from the results section). Include a
brief analysis of the results of the experiment in context of what you talked about in your introduction.
Comparison of experimentally obtained quantities with literature/accepted values should be made
whenever possible. The discussion should always include an error analysis and include suggestions for
how the results could be improved. Error analysis is more than identifying what went wrong or mistakes
that may have been made. In this context the error analysis should identify where/how a measurement or
piece of data may be incorrect and HOW that impacts your result. Example 1: Approximate volumes
were measured using beakers in the experiment. The accuracy of this experiment could be improved by
measuring solution volumes with a graduated cylinder instead which would allow the data to be recorded
to more significant figures. Example 2: The volume recorded from the graduated cylinder may not match
what was delivered because there were still droplets of liquid clearly visible after the liquid was
dispensed. This means that the amount of liquid delivered and massed is less than what was measured,
so the calculated density of the liquid would appear to be less than the true value.
5. References: You do not know everything there is to know about the topics discussed in the lab
experiments you will conduct. When using the ideas/information generated by others it is essential that
you give the appropriate credit for such work. Thus, you must include proper citations within your report.
Within the text of the report any information that cites an outside source should be denoted with a
superscript number3 that corresponds to the entry in the reference list at the end of the report. The list of
outside sources used in the report should appear as a numbered list in the order in which they are used in
the format listed below. Formal reports should have at least 2 sources in addition to the lab book (and
you must always include the lab book). Note: if you don’t know how to include super- or subscripted
numbers in your work, you must figure that out…ask!
6. Appendix: Any raw data, computer output, spectra, etc should be included in this section if not
already used as a figure in the report. You must report ALL data obtained during lab in your report in
some form. Not all reports will have an appendix.
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Glassware Reference Guide
Volumetric flask—used to contain exact volumes when filled so that the bottom
of the meniscus just touches the line
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Buret (and buret clamp)—used to deliver a specific volume…more accurate and
precise than a graduated cylinder; liquid is dispensed from mark to mark.
Volumetric pipet—used to deliver exact volumes when filled to the line and the liquid allowed to drain by
gravity out of the pipet…do not use the bulb to blow out the last drop of liquid. As a general rule of
thumb, a “Class B” pipet is precise to 4 significant figures while a “Class A” is precise to 5. In other
words, if you dispense 10 mL from a Class B pipet, you must record 10.00 mL, whereas if you use a
Class A, you must record 10.000 mL. While not strictly correct, this is a good place to start worrying
about significant figures in a practical way.
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Steps for Solving Problems About…
This is fantastic sheet to make a second copy of and carry around with you, it’s a good one page reference for lecture, too.
Reaction yield (to determine how much product using the balanced equation)
Step 1: convert from grams of reactant to moles of reactant
Step 2: convert moles of reactant to moles of product (multiply by the ratio of elements from the balanced equation)
Step 3: convert from moles of product to grams of product (this is the theoretical yield)
Percent yield
Take the actual yield and divide by the theoretical yield, then multiply by 100.
Limiting reactant (determining which is limiting and how much product you expect)
Step 1: convert from grams of reactant “A” to moles of reactant “A”
Step 2: convert moles of reactant “A” to moles of product (multiply by the ratio of elements from the balanced
equation)
Step 3: convert from moles of product to grams of product (this is the theoretical yield if reactant “A” is limiting)
Step 4: convert from grams of reactant “B” to moles of reactant “B”
Step 5: convert moles of reactant “B” to moles of product (multiply by the ratio of elements from the balanced
equation)
Step 6: convert from moles of product to grams of product (this is the theoretical yield if reactant “B” is limiting)
[repeat for any other reactants present]
Step 7: the limiting reactant produces the least amount of product.
Dilution Problems
Step 1: determine the moles of solute in original volume (M x volume in liters)
Step 2: divide moles of solute by new volume in liters
(Alternatively you can use M1V1 = M2V2)
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Laboratory Techniques and Things We Expect You to Know
Safety:
1. Refer to the Safety Agreement and the Rules of the Lab in the opening pages of this manual.
2. Many of the Rules of the Lab can be summarized in two basic guidelines:
a. Always wear approved eye protection in the lab, even if you are not “doing chemistry.”
b. Always think about what you are going to do before you start doing it. Most accidents
occur in the lab due to general carelessness or inattention. Interestingly, you are at
greatest risk in the lab during your 2nd – 4th semesters, not the first.
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viii. Volumetric flasks are calibrated to contain the printed amount at a specific
temperature (usually 20.0°C). If you need to deliver a specific amount, proceed
to the next set of instructions.
c. Volumetric flasks are used to make solutions in, but should not be used for storage,
despite what Dr. Stace may or may not do in his research lab. If you need to store a
solution, you should transfer what you just made to a clean glass or plastic bottle. If you
solution is alkaline (basic) do not store it in a glass bottle. Strong bases slowly dissolve
glass.
4. The buret
a. Inspect the buret for general cleanliness, if dirty, you can fix that with a bit of scrubbing
with soap and a buret brush (a very long glassware brush to clean the entire bore length).
Also take a close look at the tip, make sure no particles of junk are stuck in there and the
tip is not broken.
b. The buret should be hung from a buret clamp (ask your instructor), not from a 3 or 2 jaw
clamp.
c. Close the stopcock at the bottom. Use the small buret funnel or squirt bottle to fill the
buret about ¼ with your solvent (usually, DI water).
d. Remove the buret and empty it from the top into a waste beaker or sink. Roll the pipet as
you empty it so you rinse all the sides.
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e. You should now fill the buret to the top with RO water and let it drain, checking to make
sure it drains break-free, but if you already scrubbed it, this step is probably unnecessary.
f. Finally, fill the buret past the 0.00 mark with your titrant. If you use a funnel, be careful
that you do not overflow the buret (do you want to guess how I know about this?)
g. Open the stopcock all the way and allow sufficient titrant to drain into a waste beaker until
all the air is “blown out” of the buret tip. Sometimes, several blasts of titrant (open it all
the way, close it and open it again) is needed to dislodge all the air from the tip.
h. You do not need to get the titrant level to be 0.00 mL. You will determine added volumes
via difference Vfinal-Vinitial ([ending volume reading] – [starting volume reading]).
i. Three last tips:
i. When you are doing “colorimetric titrations” put a white paper towel behind your
flask. It makes the faint color changes much easier to see.
ii. Always read a buret to 2 decimal places, this will require you to estimate the last
place. To stay consistent with our significant figures rules, if you start at 1.22 mL
and end at 32.22 mL, you must record 31.00 mL as the added volume, not 31
mL. If you fail to record buret readings to two decimal places, your instruction will
hang you by your thumbs in the stock room. For hours. Or days.
iii. Make a quick “buret card:” make a dark, heavy mark (about 1 cm thick) with a
marker on a note card or even a folded paper towel. If you hold this behind the
buret, it makes the bottom of the meniscus much easier to see. You will actually
see three meniscus. Pick one (I like the really fine one) and keep using it
because you are measuring delivered liquid by difference.
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g. Do not use a paper towel to dry out the glassware when done. The paper towels are
quite filthy and will re-dirty your labware. Air-drying in the lab drawer is best.
h. Do not use compressed air jets to speed up drying. That air is contaminated with pump
oil, and is under enough pressure to blow the glassware out of your hand if you are not
expecting it.
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Experiment 1: Density, Precision & Significant Figures, oh my!
Purpose: In this experiment you will work to understand how different measurements result in different
numbers of significant figures. You will also practice using different types of glassware and learn to use
the laboratory balance. Ultimately, you will determine the density of a liquid and compare that value to
the accepted value.
Introduction: As you have (hopefully) learned from your textbook, density (mass of something per unit
volume) is a physical property of stuff (compounds, elements, substances, etc.) and can be used to help
in the identification of unknown things. Density is also an intrinsic property, meaning that the density for a
substance is the same regardless of the sample size. Density as a method of identification notably
appears in history in the story of Archimedes (and King Hieron of Syracuse, Sicily). In a nutshell, the king
was suspicious that subpar materials had been substituted for gold in his crown and employed
Archimedes to figure out if it was pure or not. Archimedes knew that if he could determine the density
that would tell him how pure the gold in crown was…but he needed to figure out the volume first.
(http://www.britannica.com/biography/Archimedes) [Curious about other contributions from Archimedes?
Google “Archimedes Screw”…it’s a pretty stunning idea]
Today’s experiment will lead you through determining the density of ethanol using two different types of
glassware ( that differ in how precise they can measure a volume). When calculating the density, you will
round your answer off to the lowest number of significant figures as is dictated by the marks on the
container you use to measure the liquid.
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Experimental Procedure
Part A: Using a graduated cylinder to determine density of a liquid
Note—the 50 mL graduated cylinder is marked every one mL. This means that you can determine the
volume to nearest mL and then estimate between the lines to record volumes to the 10th of a mL. Each
volume measured with these cylinders must contain one digit after the decimal place.
1. Find the things you need: The glassware you need for this experiment is located in your
workstation: one 50 mL graduated cylinder, one small beaker (150 mL), three 125 mL
Erlenmeyer flasks, 2 rubber stoppers that fit the flasks, one 250 mL Erlenmeyer flask, and
one 400 mL beaker with about 250 mL of ethanol in it.
2. Determine the mass of an empty flask with a stopper (because ethanol will evaporate
quickly): Place the empty Erlenmeyer flask on the balance and record the mass (trial 1
graduated cylinder). Make sure the balance shows “0” before you weigh anything and always
record all digits from the balance.
3. Measure the actual volume of ethanol: Measure about 30 mL of ethanol exactly using your
graduated cylinder (fill it to near the 30 mL line but don’t worry about getting it perfect, you will
read the exact volume from the cylinder) and pour it into the weighed flask. Record the
volume of ethanol dispensed using 3 significant figures.
4. Determine the mass of ethanol: Weigh the flask+stopper+ethanol and record the mass.
Subtract the mass of the flask and stopper from the total mass to get the actual mass of
ethanol. Be sure to use the appropriate number of significant figures. This is trial 1
graduated cylinder.
5. Collect the used ethanol in your 250 mL Erlenmeyer flask and allow the 125 mL flask to air
dry in preparation for part B.
7. Repeat steps 2-6 two more times so that you finish with three values for the density of
ethanol (graduated cylinder). Calculate the average and standard deviation of the density of
ethanol measured with a graduated cylinder.
Note—the 150 mL beaker is marked every 10 mL. This means you can determine the volume to nearest
10 mL and then estimate between the lines to record volumes to the one mL. Each volume measured
with a beaker should not contain a decimal place (since you are estimating to the closest mL).
8. Determine the mass of an empty flask with a stopper (because ethanol will evaporate
quickly): Place the empty Erlenmeyer flask on the balance and record the mass on the data
sheet trial 1 beaker. Make sure the balance shows “0” before you weigh anything and always
record all digits from the balance.
9. Measure the actual volume of ethanol: Measure about 20 mL of ethanol exactly using your
beaker, record the actual volume, and pour it into the weighed flask. Record the volume of
ethanol dispensed using 3 significant figures.
10. Determine the mass of ethanol: Weigh the flask+stopper+ethanol and record the mass.
Subtract the mass of the flask and stopper from the total mass to get the actual mass of
ethanol. Be sure to use the appropriate number of significant figures. This is trial 1 beaker.
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11. Collect the used ethanol in your 250 mL Erlenmeyer flask.
13. Repeat steps 8-12 two more times so that you finish with three values for the density of
ethanol (beaker). Calculate the average and standard deviation of the density of ethanol
measured with a beaker.
14. Cleaning up: pour your collected ethanol into the designated “ethanol waste” bottles located
in the hood. Because ethanol evaporates quickly and cleanly, you do not need to further
wash your glassware. Place the glassware back into your workstation.
You will complete and turn in the worksheet at the end of this experiment AND your instructor will grade
your notebook. You must record your data in your notebook BEFORE recording anything on the
worksheet.
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Experiment 2: Atomic Spectra
Purpose: In this experiment you will practice taking measurement and recording observations. You will
also practice calculating values associated with light and comparing your calculated values to
experimental values for some of the specific electronic transitions you observe in the hydrogen atom.
You will also use your observations to identify the metal ion in an unknown solution.
Introduction: One of the most amazing and telling properties of the elements is the fact that their gas-
phase atoms will only emit certain wavelengths of light when burned in a flame or exposed to an electrical
charge. Eventually, through many interesting twists and turns, chemists came to know that each element,
as a gas-phase atom, has its own characteristic line spectrum. An atom’s spectrum results from its
electrons making specific transitions between energy levels (in the case of emission the electrons start
at one energy level and move to a lower level while in absorption the electrons move to a higher energy
level), and therefore is like a “fingerprint” for each element. You will make observations about both the
composite (or overall) color that particular atoms emit as well as look for the specific lines of color for
each element that may be helpful in identifying that element. The measurements in this experiment will
be made using a spectroscope. A spectroscope contains a prism which separates light into its
component wavelengths. The metal spectroscopes you will use are marked with a scale in nanometers
while the handheld plastic spectroscopes are marked in an arbitrary scale.
In the first part of this experiment, you will observe the spectral emission lines from the hydrogen atom
through a spectroscope and determine which electronic transition each line you observe represents. You
will also make qualitative observations about the emission spectra of helium and another element. In the
second part of the experiment you will use a flame to excite the metal atoms in several salt solutions and
note the composite flame color for each element as well as the major spectral lines when observing the
flame through the spectroscope.
Experimental Procedure
Hydrogen: record the composite (overall) color of the light from the tube and the wavelength and
color of each line observed. Compare the wavelengths of light from the pre-lab exercise to the
wavelengths of light that you observe. Assign a transition to each of the lines.
Helium: record the composite color of the tube and the color and wavelength of each of the
lines. Note which of the lines seem brightest and dimmest. (you will likely see 6 lines)
Neon: record the composite color of the tube, the color of the dominant lines and estimate the
number of lines observed.
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Calculate the energy (in joules) and wavelength (in nanometers) of light emitted for each of the following
electronic transitions (n initial n final) in the hydrogen atom. Please refer to section 3.4 in your
textbook for more guidance and additional equations. (these can be done before lab)
1 1
∆𝐸𝑡𝑟𝑎𝑛𝑠𝑖𝑡𝑖𝑜𝑛 = −2.18 𝑥 10−18 𝐽 ( 2 − 2 )
𝑛𝑓 𝑛𝑖
a) n=2 n=1
b) n=3 n=1
c) n=4 n=1
d) n=5 n=1
e) n=6 n=1
f) n=3 n=2
g) n=4 n=2
h) n=5 n=2
i) n=6 n=2
j) n=7 n=2
Part B. Fire
You will work in pairs for this part of the experiment. Set up a gas burner so that the flame is several
inches tall and has no yellow in it (ask your instructor for help adjusting the flame, if needed). There are
several bottles labeled with metal ions that may include (but may not be limited to): Li +, K+, Ca 2+, Cu2+,
Zn2+, Sr2+, Ba2+.
Obtain a wire loop and dip it in the metal ion solution. Carefully place the wet loop in the flame and
observe the composite color for that metal ion (typically the first flash of color that you notice—the wire
itself will cause a yellow flame if left in the flame too long). Some ions will be more difficult to see and
may require several attempts before a composite color is observed. Record the composite color of each
of the metal ions in the flame. If metals are presented as solid salts—dip the wire in water then in the salt
and shake off any excess particles before placing the loop in the flame. Your instructor may ask you to
make a small amount of a concentrated solution by adding a few salt crystals to a couple of drops of
water to make the metal ion solution. [Between each metal ion you need to clean the wire loop so that it
does not contaminate the flame giving you false results. To clean the wire dip it in the acid cleaning
solution provided, dip it in water, dip it in the acid solution again, then place it in the flame. Repeat until
the ion color is no longer obvious in the flame.] Record your observations for each of the metal ions.
Next you will try to observe individual lines for each element by looking at the flame through one of the
plastic handheld spectroscopes. One person should produce the colored flame as above while the other
observes through the spectroscope. Record any general observations about the spectrum and the
wavelengths of the dominant lines. Complete this procedure for the Li+, Ca 2+, Cu2+, and Sr2+.
The unknown solutions contain Li+, Ca 2+, or Sr2+ (they all burn “red”). Use the spectroscope to identify
the dominant lines and determine which metal ion is contained in each unknown solution. There is a
yellow line that appears in most (if not all) of the solutions…this line cannot be used for identification
purposes.
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Experiment 3: Periodic Trends and Pattern Recognition
Purpose: You will work in pairs to identify patterns and make sense of seemingly random information.
You will also practice making and recording experimental observations and using those observations to
identify chemical trends.
Introduction: In the beginning, Chemistry focused on the search for the elements and understanding
why the elements have the properties they do. The development of the periodic table was actually a giant
leap forward in standardizing how scientists discuss and understand the elements. As you have already
seen, the periodic table is not a random listing of the elements, but a carefully constructed array of
elements grouped by various properties. The periodic table is to a chemist what a palette and paintbrush
is to an artist and what a chisel and mallet is to a sculptor: The tool(s) through which they build their
creations. If a chemist wants to make a new kind of plastic or an alloy with unique characteristics, s/he
looks to the periodic table for guidance. While you will not necessarily be expected to use the periodic
table quite this skillfully, you will be expected to gain an understanding of how all of this useful information
is stored in its deceptively simple form.
Pattern recognition is a skill that is essential for just about anyone in a science-related field. Because you
are in the introductory chemistry course intended to prepare students for careers in the sciences, it is
essential that you sharpen this skill of pattern recognition as quickly as possible. It is extremely difficult to
hone this skill while trying to learn some abstract concept at the same time. Because of this, your first
‘exercise’ in pattern recognition will involve something that has nothing to do with chemistry (or so it will
seem). Your instructor will give you a set of drawings and ask you – in the comfort of your lab group – to
group those drawings according to whatever pattern you think exists within them.
Each group will be given a set of 30 drawings in a Ziploc bag (please check to see that you have that
number). Your task is to look through the drawings and find some criterion (or, perhaps, criteria) with
which to place them into appropriate groups and periods. Once these have been identified, then the
drawings should be organized into a table. Take a picture/sketch your table. Explain your trends (groups
and periods).
Repeat the exercise but identify a different pattern by which you can organize your “elements” and
draw/explain this set of trends.
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Part B: Graphical Analysis of Atomic Radius and Ionization Energy
Open the Excel file: CEM 1610_Exp 2_Periodic Trends_Graphing Data. In this file, you will find data for
the atomic radius (pm), first ionization energy (kJ/mol) and second ionization energy (kJ/mol) for the first
36 elements on the periodic table.
By graphing and analyzing this data, you will begin to understand and interpret periodic trends.
Atomic Radius
1. Highlight rows 1-37 in Column A (Atomic Symbol).
2. While holding down the ctrl key, highlight rows 1-37 in Column B (Atomic Radius).
3. Select the Insert tab.
4. Select a 2-D line with markers.
5. Right click on the y-axis, and select “format axis.”
6. Change the maximum bound setting to 250, the minimum bound setting to 0, and the major unit
setting to 10.
7. Stretch the graph until you can clearly see both all the numbers on the y-axis and all the atomic
symbols on the x-axis.
8. After lab, print the graph. Click on the graph (so that the graph is selected) and print. The graph
should appear full size on the print preview.
Ionization Energy
1. Highlight rows 1-37 in Column A (Atomic Symbol).
2. While holding down the ctrl key, highlight rows 1-37 in Column C (First Ionization Energy) and in
Column D (Second Ionization Energy).
3. Select the Insert tab.
4. Select a 2-D line with markers.
5. Right click on the y-axis, and select “format axis.”
6. Change the maximum bound setting to 7500, the minimum bound setting to 0, and the major unit
setting to 200.
7. Stretch the graph until you can clearly see both all the numbers on the y-axis and all the atomic
symbols on the x-axis.
8. Click on the text “Chart Title” on the graph and type in the title Ionization Energy (kJ/mol).
9. Click on the graph and print. The graph should appear full size on the print preview.
10. After lab, print the graph. Click on the graph (so that the graph is selected) and print. The graph
should appear full size on the print preview.
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Part C: Investigating Reactivity
Now that you understand a little more about how the periodic table was developed and pattern
recognition, it’s time to put your skills to the test. Your goal for this section of the exercise is to develop a
statement about the periodic trend for reactivity. To do this you will be observing the behavior of a few
metals in water and/or dilute hydrochloric acid. If your metal samples appear to be dull/matte, use a
paper towel to wipe/clean the surface (this will be especially helpful for lead and zinc).
1) Place a small amount (1-2 pellets or a few granules) of each of the following into small, labeled
test tubes: zinc, tin, magnesium, calcium, lead. You need just enough to be able to observe a
reaction.
2) Add a 4-5 drops of water to each test tube and record your immediate observations. Wait 1-2
minutes and look again. Do you see any additional bubbles on the surface of the metals? If so,
this is consider a positive reaction (though less reactive than the first round of observations).
3) Add 4-5 drops of the 6M hydrochloric acid solution to each test tube and record your immediate
observations. Again, wait 1-2 minutes and look again. Note: things that react well with water
may not react much more with the acid, but the metals that didn’t react with water might show a
more obvious reaction now that you have introduced the acid.
4) Compare your data with data from another student. Use this information to write a statement
about the general trend for reactivity and the periodic table. Find the elements you have been
given on the periodic table and note their position relative to each other (in the same row? In the
same column?
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Experiment 4: Fun with Excel!
Purpose: As a student in the sciences you are expected to computer programs to work with your data to
produce reports and graphs. Excel is a widely used spreadsheet program that can be used to organize
data and perform a wide variety of calculations. The key to using Excel (or any other similar program) is
to know how to tell it what you want it to do. The purpose of this exercise is to help you figure this out.
Introduction: For this exercise, you will be constructing a calibration curve from data collected from a
series of Cu(NO3)2 solutions of increasing concentrations (Molarity) (x-value) and their corresponding
absorbance values (unitless) (y-value). You will learn more about solution concentration and absorbance
later in the semester. The point of this particular exercise is to learn how to utilize Excel to generate plots
and make simple calculations using the provided data. It is advisable to make notes for future use. If you
have a laptop computer that you expect to be using for most of your data analysis this semester, you may
want to bring it with you for this experiment. There will be computers available for you to use during the
lab period, but if you use a different program or operating system you can use this time in lab to figure out
how to make graphs on your own computer.
There are several methods available to determine the concentration of a solution. In this exercise we will
be using the absorption of light to determine concentration. Many molecules absorb certain wavelengths
(types) of light. Thus, the amount of light absorbed by a solution is directly proportional to the
concentration of molecules in the solution. By measuring the absorbance of a series of solutions of
known concentration, you can plot the absorbance (y-axis) vs. concentration (x-axis) of the solutions and
draw a line of best fit. This is known as a calibration curve, though it is actually a straight line. The
equation of this line relates the absorbance to the concentration. Once you have determined the line of
best fit, you can measure the absorbance of an unknown solution and solve the equation for the
concentration.
y = mx + b
Go to Excel…(if you have never used Excel for calculations, ask your instructor to explain it)
2) Enter 16.575 into cell A1
3) Enter the equation for #1 into cell B1. Begin your equation with “=” so that Excel knows you are
entering an equation. Instead of entering “16.575” into your equation, click on cell A1. This tells
Excel that you want to use the value in A1 in your equation.
4) Hit enter. This should give you the same answer you calculated. If you get no answer, your
equation isn’t quite right. If you get a number but it doesn’t match, check both calculations and
figure out where you went wrong.
5) Use excel to calculate the moles of carbon in the following amounts of benzene: 4.226g, 7.801g,
10.025g, 22.210g, 68.775g, 105.47g, 152.05g, 215.25g, additional values assigned by your
instructor.
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Part B. Constructing and Using a Calibration Curve
Experimental Data: Cu(NO3)2 concentrations (x-value) and corresponding absorbance values (y-value)
Absorbance values for unknown Cu(NO3)2 solutions: 0.36, 0.45, 0.19, 0.53, 0.62, 0.78
6) Use Excel to make a graph of the experimental data given for Cu(NO3)2 (instructions below).
7) Use Excel to calculate the concentrations of the unknown Cu(NO3)2 solutions listed.
Though it is called a curve, the calibration data provided should lie along a straight line with the equation
y = mx + b. This is because at low concentrations (under 1) the relationship between absorbance and
concentration is linear. Each of the four standard solutions has a known concentration and a measured
absorbance. Note that when the concentration doubles, the absorbance also doubles (with some room
for experimental errors). Use Excel to make a graph of the absorbance (y-value) vs. concentration (x-
value). Below are some general guidelines for using Excel to make graphs. Almost every graph that you
will make for your chemistry classes will be a “scatter” plot. This means that you will be plotting simple
coordinates. Excel has several other options for graph types so be sure to choose “scatter” when given
the opportunity.
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Your line of best fit and the corresponding equation should appear on the graph. There is an option to set
the y-intercept equal to zero. For this experiment you may do this, but you need to know that it includes
the origin as a point and forces your line through that point. A better representation of your data is to
allow your curve to have a value for the y-intercept (b in your equation) since you did not actually
measure a solution of zero concentration for this experiment. Your instructor will tell you their preference
for this exercise.
To determine the concentration of an unknown solution, substitute the measured absorbance into the
equation of the line and solve for the concentration. Try this using the formula option in Excel and by
hand using the y = mx + b equation that you generated with your plot. Be sure that your chart is
appropriately labeled and email your spreadsheet to your instructor as indicated above. The file you send
must be a .xls file and you must include the equations (not just filling in the answers in the calculated
cells). Your instructor may accept a hardcopy, please ask for clarification.
Every student needs to complete this exercise on their own and turn in their work. You do not learn how
to use Excel if you don’t actually use it. It gets easier to understand and figure out every time you use it.
Your instructor will give you specific instructions for submitting your work.
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Experiment 5: Separating a mixture
Purpose: During this experiment you will use the property of solubility to make a simple separation easy
and efficient to perform. You will learn how to set up and use a vacuum filtration system that will be used
later in the semester. Finally, at the end of this experiment you will investigate error and how that error
impacts your results.
Introduction: Mixtures are an important part of chemistry. Many of the substances we run into during
our studies, and life in general, are mixtures or solutions. A mixture contains two or more components
that have been physically combined and can be physically separated. A solution is a type of
homogenous mixture made by dissolving a solute in a solvent. During this experiment you will prepare a
mixture of salt and sand by measuring known quantities of each substance. Once mixed, it will be your
job to “unmix” the components and recover the sand. There is more than one way to separate this
mixture…which will be the easiest? Let’s look a little more closely at the components and figure that out.
The salt in this experiment is average table salt…sodium chloride (NaCl). The sand is just normal
sand…silicon dioxide (SiO2). Both components consist of very small particles. Though it is possible to
distinguish the particles from each other, the small size makes it a tedious process to separate them
physically. In order to be more efficient (and learn more stuff), you will use the difference in solubility of
each component to separate them. For this experiment you may work in pairs (you may only be a group
of 3 if we have an odd number of students in lab).
Weighing: In this experiment you will record the mass after each step you complete. Why? This will
allow you to calculate the amount substance that you add to the container…and how much is left at the
end. Though it can be a little tedious, this method helps reduce errors in your data and allows you to
compare data from different days and different experiments with more confidence. The things you will
need to know in this experiment include how much sand and salt is in your mixture. To know this you will
need the mass of the container empty as well as the mass after you add each component. As you step
up to the balance for each measurement, be sure that it reads zero. Once the mass is displayed, record
all digits given on the balance.
Percent: Often overlooked, the concept of calculating a percent comes in quite handy in life. Here you
will be calculating the percent of sand that you recover. In general, percent means parts of something
“per 100” (cent = 100). For exams your score is often reported in percent (the number you got right
divided by the number possible times 100). Percent is used every day when reporting statistics…63% of
voters were in favor of something means that for every 100 people, 63 of them voted yes. How will this
help you determine the percent of sand recovered? What is the “part” and what is the “whole”? If you
don’t recover 100% of the sand, where did it go? What are the errors that might have occurred during the
experiment?
2. Add about 5mL (you can estimate the amount, this is about a teaspoon) of sand to the 150 mL
beaker and record the mass (beaker + sand).
3. Add 2-3 grams of salt directly to the sand in the beaker and record the total mass (beaker + sand
+ salt)…then make sure they are mixed together.
4. Label your watchglasses 1-4 with a permanent marker. Record the mass of 3 of your
watchglasses…you’re going to need this mass at the end (a watchglass is the glass circle that
looks like a large lens in your drawer).
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5. Determine and record the mass of sand and salt in your mixture.
6. Repeat 2 more times so that you have 3 mixtures to separate and analyze in part 2.
7. Set up a steam bath by filling a 250 mL beaker 2/3 full with water and placing it on a hotplate set
to med-high (300-350°C). While you continue with the rest of the experiment, this should reach
boiling. You may set the hotplate higher until it boils, but you must keep a close eye on it.
8. Locate the squeeze bottle in your drawer or cabinet and fill it with RO water.
9. Also fill your largest glass beaker with RO water. You will use this in the next step rather than
making frequent trips to a water source.
10. Use water to dissolve the salt but not the sand. You will end up with a mixture of salt water with
sand in the bottom. Your goal is recover all of the sand by filtering the sand out of the saltwater…
a. Add water from step 9 to the mixture of salt and sand until the beaker is about 2/3 full and
stir until the salt dissolves, then let the sand settle to the bottom.
b. Pour off most of the salt water solution into your large plastic beaker (it’s probably in the
cabinet under the long drawer) leaving the wet sand in your glass beaker.
c. Add water to the wet sand in the glass beaker (again) until the beaker is about 2/3 full
and stir.
d. Repeat steps b & c two more times to make sure there is no salt left on the sand.
11. Assemble your filtering apparatus using a side-arm flask, the plastic filter (with the grey rubber
cone adapter), a vacuum hose (heavy red/orange rubber tube—NOT the green and black braided
tubing, that’s for gas), and a piece of filter paper. Connect the other end of the vacuum hose to
the vacuum nozzle on the benchtop.
12. Turn on the vacuum, wet the filter paper with your squeeze bottle, and pour the water/sand
mixture into the plastic filter (try to transfer as much as possible on the first try). Rinse out the
beaker with water from your squeeze bottle being careful to add the liquid from each rinse to the
filter. Your goal is to transfer all of the sand to the filter. You may need to turn the beaker upside-
down and spray water into it (over the filter apparatus) to get all of the sand out.
13. Carefully remove the filter paper and sand using a small metal spatula and place the filter paper
with the sand on a labeled watchglass.
14. Place the watchglass on a steam bath until you can easily remove the filter paper. (about 5-7
minutes)
15. Scrape the sand off the filter paper onto the watchglass and return to the steam bath until the
sand is dry (an additional 8-10 minutes).
16. Using tongs carefully remove the watch glass and set it on a paper towel to cool for 3 minutes.
17. Dry the bottom of the watchglass and record the mass of the sand + watchglass.
18. Repeat part 2 with each of the mixture you made in part 1. You should have 3 trials of data.
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19. Clean up: place clean, dry sand back in original container. Put all things used during this
experiment back in your workstation after you have washed them (beakers, watchglasses,
squeeze bottle, etc.)
1. Did you get all of the sand back? Why or why not? Where did it go?
3. What errors could lead to you recovering more than 100% of the sand?
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Experiment 6: Gravimetric Analysis and Popcorn
Purpose: Determine the water content of various things using gravimetric techniques. You will also
practice applying concepts and calculations that you already know to different situations.
Introduction
Chemical Hydrates—water as part of the chemical structure: Many ionic compounds incorporate
water in stoichiometric amounts when they form crystals. If this is the case, the compound is said to be a
hydrate. On the other hand, a compound that has no water associated with it is said to be anhydrous.
For example, anhydrous copper (II) sulfate contains only Cu2+ and SO42- ions in the crystal. The usual
hydrated form of copper sulfate has the formula CuSO45H2O and is named copper (II) sulfate
pentahydrate. Note that the ratio of ions and water molecules are whole numbers just like regular
compounds, 1:1:5 in this case. Some compounds can exist in more than one hydrated form. For
example, iron (II) chloride, besides existing in the anhydrous compound, can
form iron (II) chloride dihydrate (FeCl22H2O) and iron (II) chloride tetrahydrate (FeCl24H2O). Each of
these compounds has different physical properties including density, color and crystal structure. Which
compound exists depends upon the environmental conditions. It is possible to have mixtures of more
than one hydrate so that the overall composition appears to be non-stoichiometric. You may have a
sample of iron chloride that has 25% of the sample existing as the dihydrate and 75% of the sample
existing as the tetrahydrate. The overall stoichiometry of the water will be 0.25(2) + 0.75(4) = 3.5, which
would then yield a formula of FeCl23.5H2O.
In order to determine the formula of a chemical hydrate you need to determine the “empirical” formula or
the lowest whole number ratio of water molecules to formula units of the rest of the compound. First,
determine the moles of each part (the water and the anhydrous compound), then divide by the moles of
the anhydrous compound to determine the ratio. Once you have the ratio you need to round to the
nearest 0.5 (or multiply through to get whole numbers). Unknown hydrates are typically written with an
“n” in the formula: CuSO4nH2O, where you are trying to determine the value of “n.”
Your lab group (up to four people) will use gravimetric techniques to analyze two different types of sample
for water content. The first sample is a commonly used chemical that is normally hydrated. Each student
will collect data to determine the formula of the compound and figure out if it is “appropriately” hydrated.
As chemicals sit on storage shelves, they may incorporate additional molecules of water or lose
molecules of water over time. This is an important piece of information as it affects the molar mass of the
solid compound. Each member of your lab group needs to analyze one sample of the hydrate (about 0.5
grams) using the method described below and you will compile your results into a single average value.
The second sample is commercially available popcorn. Each member of your lab group will analyze four
kernels of popcorn.
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Pre-lab Assignment
1) Write out the list of steps you will follow during this experiment in your lab notebook for both parts of
the experiment. [note: you will be analyzing ~0.5g of hydrate]
30
Experimental Procedure
Each student will complete 1 trial for the “hydrates” portion and pop 4 “good” kernels during this
experiment. Data from 4 students working in a group will be combined to determine averages.
Gravimetric Analysis: The amount of water in hydrates can be found using gravimetric techniques. The
first step is to determine the mass of the empty crucible. A crucible is cleaned, heated for about 10
minutes in a Bunsen burner flame, cooled for about 3 minutes, and weighed. The crucible should be
placed on your wire gauze for cooling. The heating, cooling and weighing steps are repeated for a
maximum of 3 times (heat only 5 minutes and cool for 3 minutes for these repetitions), or until
consecutive measurements of the mass are within ±0.005g. If the crucible weighed 20.465g after the first
heating, cooling and weighing and 20.423g after the second heating, cooling and weighing then the cycle
needs to be repeated because the difference is 0.032g. The mass after the third cycle is 20.420g which
is only 0.003g different than the second mass…so you are finished. Always use the last value obtained
as the mass of the empty crucible. Care must be taken to handle the crucible with tongs and to make sure
the crucible is cool before weighing or errors will be introduced.
Next you will need to determine the mass of sample that you place into the crucible. Add the appropriate
amount of sample the crucible and record the new mass. The difference in mass between the empty
crucible and the filled crucible gives the mass of the sample. The crucible is heated gently with a Bunsen
burner for several minutes. In order to “heat gently” the flame of the burner should be approximately 2-3
inches high, with no yellow, and the sample needs to be suspended 4-6 inches above that flame. This
heating drives off the water but the sample stays cool enough to prevent the anhydrous sample from
decomposing (many metal-containing ionic salts convert to the metal oxide if heated too strongly) or
combust (in the case of a combustible sample, like paper or corn). Allow the sample cool to room
temperature by placing the hot crucible on your wire gauze and record the mass while the sample is still
in the crucible (do not throw away the contents of the crucible at this time). Following the same heating-
cooling-weighing procedure you used for the empty crucible, repeat the cycle until the sample comes to
constant mass (you should have no more than three masses). Once your sample reaches constant mass
you may discard the solid inside the crucible in the designate waste container in the fume hood.
Hydrates: The stoichiometry of hydrates can be calculated from the gravimetric data obtained from the
above procedures. The mass of water lost is converted to moles of water and the mass of the anhydrous
salt is converted to moles of anhydrous salt (the chemical formula for the anhydrous salt must be known).
The molar ratio of anhydrous salt to water gives the stoichiometry and hence the formula of the hydrated
salt. If, within experimental error, the molar quantities are whole numbers, then you can assume the
original sample was a single hydrate. If not, the environmental conditions may be such that a mixture of
hydrates is present. You need to report the average experimentally determined formula of your hydrate.
Popcorn: Each member will analyze the water content in a sample of 4 corn kernels. Determine the
mass of the corn kernels separately by placing them on weighing paper on the balance. Keep track of the
individual corn kernels by placing them in your labeled well plate or on labeled weighing papers. Then
pop each kernel individually in an Erlenmeyer flask by passing it over a Bunsen burner. Repeat for all
four kernels. Kernels that do not pop or are burned must be discarded. Record observations on each of
the kernels that you pop (including color, relative amount of fluffiness, whether the shell is intact, and
anything else that seems remotely relevant). Use a glass stirring rod to quickly dislodge kernels that stick
to the walls of the flask. Determine the mass of each popped kernel separately. Handle kernels with
forceps or tongs to keep the mass of dirt/oils from your fingers off the kernels before and after popping.
Tips to prevent burning: keep the flask moving and turn flask over immediately after kernel pops. The
glass will stay hot enough to burn the kernel for about a minute after you take it out of the heat…get the
kernel out as fast as possible. Place the hot flask on your wire gauze to prevent breakage. You will report
your individual results on the provided worksheet, but you will need to collect the information from your
entire group to complete your data set. You need to report the average % by mass water in your kernels.
**** To get your analyses finished in a timely manner, work on the popcorn analysis during the times you
are waiting for the crucible to cool in the hydrate analysis.****
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Experiment 7: Molecular Structure & Bonding Theories
Purpose: In this laboratory activity you will gain additional practice predicting the three-dimensional
structure of molecules and ions without the use of models. You will also use your knowledge of geometry
and bond angles to predict the relative stability of several cyclic compounds, and will compare the
structures of some larger drug molecules. Model kits should be used to check the validity of your
proposed molecular structures. In this exercise you will begin by predicting the geometry of several
molecules and ions. You will then be able to check your work by viewing a computer generated 3–D
model of the molecule or ion.
Introduction: In General Chemistry we study two bonding theories—Valence Bond Theory and
Molecular Orbital Theory. Central to these theories is the idea that adjacent atoms in molecules share
electrons. In this experiment you will be using Valence Bond (VB) Theory to determine the shapes of
several different molecules. Read the section in your textbook that describes VB Theory.
The first step towards assigning molecular geometries is to draw out the Lewis structure. The Lewis
structure is a visual representation of where electrons are located within a molecule. The Lewis structure
shows whether electrons are participating in bonding or not, it does not depict the spatial orientation of
these electron domains. When drawing a Lewis structure there are a few rules to follow:
Once you have an acceptable Lewis structure, the electron domain (ED) geometry (often referred to as
the electron group geometry) can be determined. There are five ED geometries that are commonly
observed: linear, trigonal planar, tetrahedral, trigonal bipyramidal, and octahedral. Each molecule that
you will encounter during this exercise will fit one of these ED geometries.
After determining the ED geometry, you can assign the molecular geometry. Recall that electron
domains take up space and affect the molecular geometry but are not considered to be “part” of the
molecule. The molecular geometry is determined by counting the number of bonding domains and
assigning the appropriate geometry.
32
If there are 2 electron domains:
ED geometry is linear
If both ED are bonding domains, the molecular geometry is linear.
33
Name:__________________________________
Part A – VB Theory drawings: In your lab notebook, draw the Lewis structures for each of the
molecules or ions listed below. (There is no pre-lab assignment due)
H2O, XeF2, PBr3, NH3, SF6, SF4, BH3, XeF4, NH4+, N2H4, PCl5
For each of the Lewis structures you just drew, determine the number of electron domains (and the
number of those domains that are bonding pairs and are love pairs), assign the electron domain
geometry, assign the molecular geometry, and determine the hybridization of the central atoms (note: in
N2H4 both Ns are the same and both can be considered the central atom)
Part B - Cyclic Organic Compounds: The following compounds are all cyclic, with the atoms arranged
in a ring. Draw the cyclic Lewis structure for each of the following and determine the molecular geometry
around each of the carbon atoms.
1. C3H6
2. C4H8
3. C6H12
Analysis Questions: Given what you know about the possible geometries around carbon, what are the
bond angles around the carbons in each of these? Which of these compounds do you think is the most
stable? The least stable?
Analysis Question: Consider the following drugs. Two of them have very similar 3–D structures and hence
have similar biological effects. Which two are they? Look up the structures on the internet.
To find out, go to the Main Index at http://www.molecularmodels.ca/, and then click “Molecular Models,”
and then click “Drugs.” The drugs are listed in order of the number of carbon atoms in the compound—
from fewest to the greatest number of carbon atoms in the compound. It’s easiest to compare structures
by opening up different “windows” and viewing the structures side by side. Each structure will first appear
in a “wire frame” representation. You will probably prefer to view the models in the “ball and stick” view.
To change the way the molecule is displayed, right–click on the model and choose the desired
representation from the “Display” pop-up menu. Compare the structures and try to find the two that are
most alike.
34
Experiment 8: Qualitative Analysis of a known solution and an unknown solution
(2 weeks)
Purpose: Use chemical behavior to determine which ions are present in a solution. You will also
practice following a complex set of direction and making/recording observations which you will refer to
during week two of the experiment. This experiment will also present a few new lab techniques that will
be helpful for any young scientist to know.
Introduction: Two of the most common questions chemists set out to answer are 1) what is in the
sample? And 2) how much is in the sample? Gravimetric analysis (the popcorn lab) is often used to
answer the second question, as you have already done this semester. Now, as we dig a little deeper into
the laboratory experience, you will attempt to answer the first question. In the “old days” before chemists
had access to modern (and expensive) instrumentation, the techniques of qualitative analysis were
utilized to answer the question: “what do I have in this sample.” These so-called “wet chemistry”
techniques have been largely shelved as the instruments are easier to use, often also give quantitative
data (how much do I have), and generate less waste. However, learning how to do qualitative analysis
helps us learn chemical insight, and still gets used when a particular instrument is not readily available
(plus, it’s kind of fun).
You will perform a series of chemical tests that will serve to isolate and identify ions in aqueous solution.
During the first week you will analyze a solution that contains ALL of the cations in question. This means
that ALL of the tests will give you a “positive” result during the first week. After you have learned some of
the common techniques, you will be given an unknown solution and asked to identify the cations. It is
extremely important to record your observations during the first week since the unknown that you will
analyze during the second week will only contain 3 of the cations and you need to be certain you
understand what a “positive” test looks like for each of the cations. Also in the second week (only) you
will analyze a solid salt to determine which anion is present.
Safety:
As always, wear goggles. Of special concern are the “concentrated mineral acids:” 12 M HCl, 16 M HNO3
and 18 M H2SO4. They are exceedingly corrosive (especially the nitric and sulfuric acids) and can cause
near-instantaneous, very painful and often permanent eye injury. Not wearing eye protection in this
lab is grounds for immediate dismissal, regardless of the number of “warnings” you may have
received. Even if you are your lab partner are not actually working at the time, the knuckle head across
the room is working with a reaction and has the test tube pointed directly at you. A lifetime of blindness is
a high price to pay to avoid 3 hours of annoyance.
When working with the chemicals in red, below, you must work in a fume hood. Avoid breathing the
vapors from those chemicals. Know the locations of the sinks. If you spill a reagent on you, calmly but
quickly proceed to the sink and rinse the affected area with copious amounts (gallons) of water and notify
the instructor. When performing a reaction, make sure the mouth of the test tube in always pointed in a
safe direction (not at yourself, your lab partner, or mortal enemy). Never look down the muzzle of a test
tube to see what is going on, they are made of glass so you can look in sideways. Chemical aerosolize
and get on your hands, even if you “never touched anything”, so before you leave, you must wash your
hands with soap and water (it won’t hurt to wash up the arms a bit too).
35
Provided Reagents:
6M H2SO4 18M H2SO4 6M HCl 12M HCl
NH4NO3 AgNO3
Procedure:
The following is a procedure for separation and detection of each cation. You will work with a lab partner
for this experiment unless told otherwise by your instructor. During week #1 you will analyze a known
solution containing each of the cations so that you can see what positive tests look like. You need to take
very careful and detailed notes during the first week because this is how you will know what to look for in
the second week. Part of the notebook grade for this week will include how well you have recorded
observations in your notebook. During week #2 you will analyze an unknown solution that will contain 3
different cations from the unknown AND you will be analyzing a solid salt to determine the anion. Please
notice that each of the numbered tests in the procedure include steps for identification followed by steps
to confirm the presence of the cation in question. During week 2, if a test is negative there is no need to
conduct the confirmation test for a particular cation.
Centrifugation (you will need to share…always see if anyone else is ready for this step)
1. You will be centrifuging in a small test tube.
2. You need to balance the centrifuge rotor (have equal masses opposite each other). If the rotor is
unbalanced the centrifuge will “walk” right off the table or cause severe internal damage.
i. In addition to your sample, fill a test tube with water to equal volume as your sample.
ii. You might be able to pair your sample with another student, if you both have exactly the
same volume of “stuff”
iii. Make sure if you are centrifuging multiple samples that you mark yours with a “sharpie”
marker or something similar.
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3. Close the lid and turn the centrifuge on. If it has a speed adjustment, crank it up so it’s going pretty fast.
i. If the centrifuge starts to vibrate, shake, dance or shimmy, turn it off immediately,
ii. Please refer to step 3 again!
4. Once the rotor has reached full speed, let it run 2 – 5 minutes.
5. Turn off the power, but let the rotor slow down on its own. Don’t try to slow it down faster with your finger
(you might lose your finger!) or otherwise disturb it. If you slow it down faster, it might upset the pellet
formed at the bottom.
6. Carefully remove your test tubes. Visually check to ensure the sediment is packed at the bottom.
7. You can now “decant” the supernatant (the liquid on the top) into a separate test tube.
8. You should wash the pellet with some water, mix the washing & centrifuge again.
Litmus Paper
1. Any true litmus (a simple acid/base indicator) will turn blue in the presence of base, and red in the presence
of acid…you will be using “neutral litmus” which starts out purple and becomes more blue in the presence of
a base and more red in the presence of an acid. You might want to do a quick test with a known acid and a
known base so you know what to look for.
2. The litmus paper should be slightly moistened with a drop or two of RO water.
3. You will need to expose the paper to your analyte.
a. If it is a gas (e.g. NH3(g)), you should stick the paper to the end of glass stirring rod. Then lower
the rod into the headspace of the test tube. Be careful, don’t let the paper touch the inner wall of
the test tube or the liquid below
b. If the analyte is a liquid, you should dip your [clean] stirring rod into the liquid, and then touch the
paper with the end of the stirring rod.
Weeks 1 AND 2:
Cations: Na+, NH4+, Ag+, Fe3+, Ca2+, Ni2+
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Test #2: Identification of iron ions
Many metal hydroxide salts (“salt” is synonymous with “ionic compound”) are insoluble. Thus, if a
solution is made alkaline, many of the salts will precipitate out and can be separated. In our
current case, we are interested in:
Fe3+ + 3NH3 + 3H2O Fe(OH)3(s) + 3NH4+
(Fe(OH)3: Rust Colored)
Unfortunately, if you get the solution too basic, then other metal ions might also precipitate. We will use a
buffer to keep the concentration of OH-(aq) low enough that other ions won’t come out of solution too.
6) To test tube #2: add 2 drops of NH4Cl and then 6 M NH3 until the solution is basic to litmus.
7) Centrifuge and pour the decantate into test tube #3. Again wash the precipitate with ten
drops of RO water, centrifuge and discard the washing. The precipitate will now contain Fe 3+
ions, if they were originally present.
10) To test tube #3: Add three drops of (NH4)2C2O4. If a precipitate forms the solution
contained calcium ions.
11) Centrifuge and pour the decantate into test tube #4. Again wash the precipitate with ten
drops of RO water, centrifuge and discard the washing. The precipitate will now contain Ca 2+
ions, if they were originally present.
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Test #4: Identification of nickel ions
Nickel will precipitate as a hydroxide in strongly basic media. However, to get our solution to a high
enough pH we need to get rid of any NH3 around since ammonia and ammonium act as a buffer solution.
So we will first acidify the solution with nitric acid, then evaporate the solution to dryness. Acidification
converts the NH3 to NH4Cl, heat decomposes NH4Cl to NH3(g) and HCl(g). Once the ammonia is gone,
the nickel can be redissolved in a slightly basic media, wherein it forms the hexaamminenickel(II)
complex:
Ni(OH)2(s) + 6NH3(aq) [Ni(NH3)6]2+(aq) + 2OH-(aq)
The [Ni(NH3)6]2+ can be reacted with “dimethylglyoxime” to produce a strawberry red precipitate.
13) Transfer the decantate from above (test tube #4) to an evaporating dish and reduce it to
dryness over a low flame.
14) Add five to six drops of 16 M HNO3. Again evaporate until no more fumes are evolved.
Concentrated nitric acid is corrosive!
15) Dissolve the residue in five or six drops of 6 M HCl. Add 10 drops of RO water and transfer
the solution to a small test tube (test tube #4). Wash the evaporating dish with 10 more
drops of RO water and add that to the solution in the test tube. Add 3 M NaOH until the
solution is basic to litmus. If nickel ions are present, a precipitate will form. If a precipitate
does not form initially, add a few more drops of NaOH to be sure the pH is high enough for
precipitation.
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Identification of sodium ions:
(this test can be performed at any time)
Almost all sodium salts are soluble, so attempting to detect them by precipitation is a difficult. However,
sodium ions will impart a bright yellow emission to a flame test. If your solution yields a yellow flame, it
probably contains sodium ions.
sodium 1. Dip a wire with a loop at the end in a beaker of dilute hydrochloric acid (1.0 M), heat it
to red heat in a burner flame.
sodium 2. Then dip the wire loop into a beaker of RO water and again heat to a red heat.
sodium 3. Repeat this processes until the wire no longer imparts a color to the flame.
sodium 4. Dip the wire into your sample, place the wire in the flame, a bright yellow flame
indicates the presence of sodium ions.
sodium 5. You should compare the results of this test with a test of a known sodium solution: try
the test with 0.2 M NaCl(aq). Several different contaminants will also yield a yellow
flame, but with a different color of yellow.
The evolved ammonia will yield a characteristic order, and to save our olfactory nerves, it will also
turn red litmus paper blue. You are looking for evolved ammonia gas.
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Week 2 (only):
Anions: NO3-, CO32-, Cl-, Br-, I-
This is a single test (yea!). You will react a solid salt (not a solution) with concentrated sulfuric acid
(H2SO4(aq)) at room temperature in a small test tube. You will observe one of the following reactions:
I- (Iodide) Solid turns dark brown instantly. Slight formation of violet vapor. H2S is also
liberated, so you may detect the odor or rotten eggs.
You will need to identify the three cations in your unknown solution. You also need to identify the
unknown anion present in your solid salt sample.
2. What would be one potential drawback to using city tap water rather than DI throughout this
experiment? Be specific.
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Experiment 9: Limiting Reactant, Let’s Make Chalk!
Purpose: Carry out a common reaction and use stoichiometric calculations to compare the theoretical
amount of product to the amount of product that you actually recover. You will practice setting up and
using a filtration apparatus as well as a steam bath for drying your product.
Introduction:
Precipitation Reactions: In this lab we are going to use a common precipitation reaction to explore the
concept of limiting reactants. This reaction uses two aqueous salt solutions that are added together and
result in the precipitation of a single product (chalk) while the other (spectator) ions remain in solution. For
this experiment you just need to know the basics.
The main idea of a precipitation reaction is relatively straightforward. When the cations (+ ions) and
anions (- ions) of two aqueous solutions are exchanged and a salt that is insoluble in water is produced,
then a precipitation reaction has occurred. This is exactly what happens in the reaction that you will be
using to make chalk (calcium carbonate):
The products are simply the result of exchanging the cations and anions of the reactants. As a general
rule, metal carbonates are insoluble in water except for those made with group 1A metals (like sodium
and potassium).
Limiting Reagents: For this experiment, you may have a large quantity of Na2CO3 but you cannot
produce any chalk unless you also have CaCl2 (in this case CaCl2 is limiting). Stoichiometry allows us to
compare the amounts of various species involved in a reaction. If we know the balanced chemical
equation and the quantity of one of the reactants added or of a product produced, we can evaluate the
quantities of the other species produced or needed. In this procedure you are mixing two solutions so
you will need to use the concentrations and volumes of each solution to determine moles. In order to
determine which of the reactants is limiting, we must take into account both the amounts present and how
they are related by stoichiometry in the balanced equation. There are many “methods” for going about
this…the one that we find most useful is given below.
Limiting reactant (determining which is limiting and how much product you expect)
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The above may sound confusing. In this experiment you know the concentration and the volume of the
two solutions that you mix. Therefore you know the moles of Na2CO3 and the moles of CaCl2 that are
present. You only need one to predict the amount of CaCO3 that could be produced. Go ahead and
evaluate that for each reactant independently. If both give the same amount of product, then neither is a
limiting reagent. If there is a discrepancy, then the reagent that gives the smaller amount of product is
the limiting one.
Why use an excess of one reactant? If you produce no more product, then it just does not make
economic sense to use an excess of one reagent. The in-depth answer to this lies a little later this
semester. Here is a glimpse into the future: not all reactions go 100% to completion, in fact the majority
of really interesting ones do not. One trick employed to make them “go to completion” is to start with an
excess of one of the reactants. This essentially makes the other the limiting reagents. Getting back to
economics, it makes sense to choose the less expensive reagent as one to use in excess.
In this experiment, you and your lab partner will need to choose how much of the sodium carbonate
solution you will use. For reaction #1, calcium chloride will be the limiting reactant. You are instructed to
use 25 mL of the calcium chloride solution. How much sodium carbonate solution should you use?
Recall that the stoichiometry of the chalk reaction is 1:1, so you just need to deliver less moles of sodium
carbonate than calcium chloride. If you can determine the volume of sodium carbonate that contains the
same moles as 25 mL of calcium chloride, then you can just use less sodium carbonate. The amount you
choose should also be easily and reliably measured (so maybe you don’t choose a fraction of a milliliter).
Now, for reaction #2 you must make the calcium chloride limiting. How do you do that? Consider what
you just read about reaction #1 and work in the opposite direction. You will calculate the theoretical
yields for both reactions as part of your pre-lab assignment—be sure to write this in your lab notebook.
Percent Yield: Even with a reaction that is expected to go to completion, it is a completely different matter
when you get into the lab and perform it. Experimental procedures typically require several different
manipulations and transfers that tend to lead to loss of product. Some of these losses are due to human
error that can be eliminated with experience and improved technique. However, more often it is due to the
actual procedure involved. Percent (%) Yield is a measure of the actual product recovered in relation to
the amount of product you would get if everything proceeded perfectly:
% Yield (Efficiency) = (Mass of product obtained/Calculated mass of the product expected) × 100
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Experimental Procedure
While the actual work involved in this experiment is not great, there is a lot of time spent drying the
sample over a steam bath.
Reaction ~0.5M CaCl2 ~1.5M Na2CO3
#1 25mL
#2 25mL
1. (pre-lab exercise) Determine the amount of Na2CO3 you will use for each reaction.
- For reaction #1 CaCl2 should be limiting and for reaction #2 Na2CO3 should be limiting.
2. Record the mass of two watchglasses (make sure you can identify which is which).
3. Set up a steam bath, using your 400 or 600 mL beaker. Fill your beaker ~2/3 full of water and
bring to a boil on a hot plate. Once the water has started boiling turn the heat down. (You can
move on to the next step before the water boils.) Always be sure that the beaker is at least half-
full of water. You can add more as needed.
4. Using the appropriate graduated cylinders, dispense each reagent for reaction 1 into a 125 mL
Erlenmeyer flask (~1.5M Na2CO3 and ~0.5M CaCl2). Use a dedicated cylinder for each reactant.
5. Swirl the flask to mix the solutions and complete the precipitation reaction. Allow 5 minutes or so
for the reaction to run all the way to completion.
7. Allow the vacuum to run for about 1-2 minutes after the liquid has been pulled through to the filter
flask. Carefully remove the filter paper (it will still be moist) and place it on a pre-weighed watch
glass. Place the watchglass with the filter paper and product on the steam bath and leave it there
until the paper has dried (~10 minutes)
- Note: This is a good time to start the procedure over for the next reaction.
8. When the paper is dry remove the watch glass from the water bath. Allow it to cool to the touch
and very carefully using a glass rod (or a metal spatula), scrape the CaCO 3 from the filter paper
onto the watch glass. Try and get as much as you can off without tearing or scraping off some of
the filter paper. Discard the filter paper and return the watch glass to the steam bath for another
ten minutes or until the product appears completely dry…whatever comes first.
9. Remove from steam bath and allow it to cool to room temperature. Dry off the watch glass. This is
critical. Record the weight of the watch glass and CaCO 3.
Post-lab Assignment
Prepare a formal report based on the guidelines presented on page 5 of this manual and your instructor’s
directions. Be careful to follow the correct format and include appropriate references.
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Experiment 10: Using the Ideal Gas Law – Displacement of a Liquid by a Gas
Purpose: Using the behavior of gases and the ideal gas law to measure the amount (moles) of gaseous
product of a reaction. You will compare the amount of gas produced to the theoretical amount you
expected to produce and consider why those answers do not match. You will also practice making sure
units match in experimental calculations.
Introduction: Until now we have focused on measuring the mass of various chemical components of a
reaction. In the gravimetric analysis experiment you determined the mass before and after a reaction
occurred in order to determine how much of the substance was water. For the hydrate this allowed you to
calculate the formula for the hydrate. In the limiting reactant experiment where you made chalk, you
measured the mass of the product to determine the percent yield of that reaction. Measuring mass is
often a goal of chemical analysis because mass measurements themselves typically contain the least
amount of error. This brings us to the current experiment and a new situation—measuring the amount of
a gas produced. To begin to understand why the procedure is set up the way it is, you need to read
Chapter 11: Gases (in your textbook).
The reaction (above) occurs when a piece of magnesium ribbon makes contact with hydrochloric acid.
What will you observe that indicates the reaction is taking place? The hydrogen gas will appear as
bubbles in the solution. If you can collect the gas and measure the volume, you can use the ideal gas law
(along with the known conditions in the laboratory) to calculate the number of moles of the gas. The way
we collect the gas in this experiment (and in most situations) is generally very accurate, but it requires an
additional step in the calculation. The hydrogen produced in this reaction is collected by forcing it to
displace the water from a vessel with volume markings. This means that the hydrogen travels through
the water and the surface of the water remains in contact with the hydrogen gas that is collected. The
space in the vessel that appears when the gas displaces the water is called the “headspace” and the
pressure in this space is referred to as “Phead” in this experiment. To determine the true amount of
hydrogen produced, you must also account for both gases that enter the headspace: hydrogen produced
in the reaction AND water vapor. In other words, the pressure in the headspace is a combination of
hydrogen gas and water vapor (see equation below). Once you know any two of the quantities, you can
calculate the third. More about the calculations for this experiment is revealed in the “analysis” section.
Phead = P H2 + PH2O
Experimental Procedure:
Read this procedure through carefully before you begin.
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11. Slowly place the magnesium and mesh bag into
the top of the buret as shown in figure 10-1. Be
sure the magnesium is not touching the liquid.
Leave the top part of the mesh bag (that you
twisted) hanging outside the buret. Use a
square of parafilm to secure the top part of the
mesh bag to the top of the buret. Be sure you
don’t stretch the parafilm enough to make a hole
in it. If you do make a hole, get a new piece of
parafilm.
Figure 10-1. Mesh “bag” 13. With a glove on, use your finger to cover the top
of the buret. Quickly flip the buret over and
placed in buret. insert it into the water-filled beaker. (figure 10-2)
14. Quickly lower the buret so it is located just above the bottom of the beaker.
17. As the HCl and water mix, you will see the HCl start Figure 10-2. Invert
producing hydrogen gas as it reacts with the
magnesium. The gas will bubble up to the top of the buret.
the buret and force water out the bottom.
19. After the bubbling has stopped, raise the buret about 1 cm off the bottom
of the beaker. Read and record the volume (to the hundredths place).
This is your final volume. Remember, you will be reading the volume
backwards.
20. Measure the height of the water column (in cm) in the buret above the
water line in the beaker.
Figure 10-3. Reading the 21. Open the stopcock and release the hydrogen gas. Be sure to release
buret. the gas away from your face and be sure there are no open flames
when this is being done.
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27. Once you have completed the experiment, wash all glassware thoroughly with soap and water. Be
sure to rinse out the buret very well with RO water. Return all glassware and equipment to the
appropriate drawers/cabinets.
Here are a few definitions of pressures in this experiment that will be helpful:
Patm is the atmospheric pressure (convert to atm)
Pcolumn is the pressure exerted by the column of water inside the buret (see Analysis 2a)
Phead is the total pressure inside the headspace of the buret (the gas inside the buret is
both water vapor and hydrogen—see Analysis 2b)
PH2O is the partial pressure of water in the headspace. (see Analysis 4)
PH2 is the partial pressure of hydrogen in the headspace. (see Analysis 4)
Useful conversions: 1 atm = 760 mmHg = 101325 Pa, 1 in = 2.54 cm, 1 m3 = 1000000 cm3
Analysis 1. When the buret was full there was no gas thus no headspace was formed. The column
of water was “supported” by atmospheric pressure pushing down on the water in the trough. The
gas formed during the reaction displaced that water, pushing against atmospheric pressure.
a. You can calculate the Pcolumn if you know the height of the column and the density of the
water in the column: Pcolumn = hdg (the answer calculated from this equation is Pascals)
i. h = height of the water column in m (convert from cm to m)
ii. d = density of water in kg/m3 (see figure 10-4; convert from g/cm 3 to kg/m3)
iii. g = acceleration due to gravity in m/s2
iv. to get atm you will need to convert from Pa
Analysis 2. If the water level inside the buret is even with the water level in the trough the pressure
of the gas (Phead) is exactly equal to the atmospheric pressure (Patm). In this case, the water level
inside the buret should be a little bit higher than the level in the trough, so the pressure of the gas
inside the buret (Phead) is a little bit less than the atmospheric pressure. Another way to show this
is to say that Patm = Pcolumn + Phead.
Analysis 3. Remember that there are actually 2 gases in the headspace, hydrogen and water. To get
just PH2, you need to subtract out the partial pressure of water, PH2O, from Phead.
Phead = PH2 + PH2O
i. The vapor pressure for water (PH2O) for the temperature you recorded in the
water trough is in Figure 10-5
ii. The pressure is reported in Torr, which is equivalent to mmHg…you need to
convert to atm
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Analysis 4. To solve the ideal gas equation for n, you need to know the volume and temperature of
hydrogen in addition to the moles of hydrogen. You also need to make sure all of your measured
units match the units in R. (liters, atmospheres, moles, and kelvin)
VH2 = │Vfinal - Vinitial│ (use the absolute value because you read the buret backwards)
TH2 = temperature of the water in the trough
PH2 = calculated in Analysis 4
Calculate % error:
1. Subtract the actual value from the theoretical value (this is the “difference”)
2. Divide the absolute value of the “difference” by the theoretical (or accepted) value.
3. Multiply by 100.
Questions: Think about your results. Which quantity was greater…actual or theoretical? Which did
you think would be greater? What could account for this difference?
Figure 10-4. Density of water (g/cm 3) at different temperatures (whole degrees are listed on the left while
tenths are listed across the top.
http://jupiter.plymouth.edu/~jsduncan/courses/2012_Spring/Techniques/Exams/DensityOfWater-vs-Temp.pdf
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Figure 10-5. Vapor pressure of water at different temperatures. https://wattsupwiththat.com/2015/09/17/how-
reliable-are-the-climate-models/
49
Extra Practice with Lewis Dot Structures, Molecular Geometry & Nomenclature:
For each species below, write out the name and the correct Lewis Structure.
C2H4 C2H2
1. Obtain a model kit from the front table and look over the instructions. Note the colors that correspond
to carbon and hydrogen.
2. Examine each atom (C, H). Each sphere contains a defined number of holes. Record the number for
each atom in the table. What does the number correspond to?
3. First we will build the simplest alkane, methane. Place four connectors in the carbon atom. Attach 4
hydrogens to the carbon. Sketch this molecule in the table.
4. Detach one hydrogen from the carbon and connect a second carbon to the original carbon. Add
hydrogens (and connectors) as needed to fill all the available spots on carbon. You just made a model of
ethane! Sketch this molecule in the table.
Repeat the steps as in 4 to build propane and hexane in the table (the indicated number of carbon atoms
is shown in the table). Sketch each molecule.
Next, you will build corresponding models for the alkenes. Alkenes differ from alkanes in that (at least)
one of the carbon-carbon single bonds has been replaced with a carbon-carbon double bond. Starting
with ethene, make a model representing this alkene. You will need to use the springs to represent the
double bond (2 springs = 1 double bond) and adjust the number of hydrogens accordingly.
Finally, you will build two models of alkynes. Alkynes have (at least) one triple bond.Construct two
different molecules (ethyne and hexyne) using 3 springs to represent a triple bond where necessary.
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Further Lewis Structure Practice: See answer sheet for compounds.
ICl NH3 MgS H2O PCl3 MgCl2 CO2NaCl Na2O CH4 (methane)
PCl5
NO3- SO32-
SO42- PO43-
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