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CHM 151 LL Composition, Separation, & Measurement


Lab Notebook Composition and Separation
Chemistry is the study of the composition and properties of matter and the changes it undergoes.
When two or more substances that do not react chemically are blended, the result is a mixture in
which each of the component substances retains its identity and its fundamental properties. The
separation of the components of mixtures is a process frequently encountered in chemistry.
Physical processes are often used so as to retain the fundamental properties of the components in
the mixture. Physical techniques used to separate mixtures rely on differences in the properties
of the components in the mixture. These physical separation techniques include filtration,
distillation, sublimation, and extraction. You will apply these techniques in this experiment to
separate a sample containing a homogeneous mixture of ammonium chloride (NH4Cl), sodium
chloride (NaCl), and sand (silicon dioxide, SiO2) into their individual components.
Sublimation is the direct passage of a substance from the solid to the gas state. You will remove
ammonium chloride from the mixture of solids by subliming it, since it is the only component in
the mixture capable of subliming under normal experimental conditions in the chemistry
laboratory. As the ammonium chloride compound sublimes it will chemically react to release
ammonia gas and gaseous hydrochloric acid which are both harmful to breathe so this first part
of the procedure must be done in the chemical fume hood in the lab.
Extraction is a separation technique that involves transformation of a substance in the mixture
from one phase to another. Since sodium chloride is soluble in water you will extract the
sodium chloride out of the remaining solid sample by adding water to the solid sample. Once
the sodium chloride dissolves in the water the sand will remain in the solid phase to create a
solid-liquid heterogeneous mixture.
Filtration is a separation process for a solid-liquid mixture by passing the mixture through a
barrier, usually filter paper, with fine pores. The larger particles of sand will be trapped by the
filter paper allowing the liquid phase solution containing the water and dissolved sodium and
chloride ions to pass through.
Distillation is a process used to separate the components of a homogeneous solid-liquid mixture
(a solution containing dissolved solids). The liquid component vaporizes as is reaches its
boiling point, leaving a residue of the solid component in the bottom of the container. The
sodium chloride can be recovered from the sodium chloride homogeneous solution by
evaporation of the water.
Measurement
Chemistry is an experimental science studying matter and the changes it undergoes.
Measurements are fundamental in experimental science to determine whether change has
occurred and, if it has, how much change has occurred. In this experiment you will become
familiar with measuring mass and volume.
Scientific measurements must be as precise as possible. This means that every measurement
will include one uncertain or estimated digit. When making measurements we normally
estimate between the smallest scale divisions on the instrument being used. Then only the
uncertain digit should vary if the measurement is repeated using the same instrument, even if it
is repeated by someone else. The accuracy of a measurement or calculated quantity refers to its
agreement with some known value. For example in this experiment you will be trying to
determine the percent composition of each component in the mixture. Once the experiment is
completed and turned in your instructor will tell you the known composition and with this

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information you could then determine the accuracy of your lab work.
Because every measurement made in the laboratory is really an approximation, it is important
that the numbers you record reflect the precision of the device you are using to make the
measurement. The assumption is made in this course that an uncertainty of at least one unit
exists in the last digit. The uncertainty of the measurement should be given with the actual
measurement, for example:
Analytical Balance Mass example: 5.0988 +/- 0.0001 g
25 mL Graduated Cylinder Volume example: 10.5 +/- 0.1 mL
Each instrument has an inherent amount of uncertainty in its measurement. Even the most
precise measuring device cannot give the actual value because to do so would require an
infinitely precise instrument. A measure of the precision of an instrument is given by its
uncertainty. If you are unsure of the uncertainty of an instrument a good rule of thumb is to
assume the uncertainty of a measuring device is 20% of the least count. Recall that the least
count is the smallest subdivision given on the measuring device.
Significant Figures
When a measured value is determined to the highest precision of the measuring instrument, the
digits in the measurement are classed significant digits or significant figures. When reading data
measured by other scientists it is important to be able to determine the precision of any
measured value so a set of rules was established. The following rules will help you determine
the number of significant figures in any measurement.
1. All nonzero digits are significant. (3.467 cm = 4 significant figures)
2. Zeros between nonzero digits are significant. (2.07 mL = 3 significant figures)
3. Zeros beyond the decimal point at the end of a number are significant.
(6.00 mL= 3 significant figures)
4. Zeros preceding the first nonzero digit in a number are not significant.
(0.0341 g = 3 significant figures)
5. Zeros at the end of a number are significant if the number contains a decimal point.
0.0300 g (three significant figures) 3.0 cm (two significant figures)
A problem arises when a number ends with zeros but contains no decimal point. In such cases,
it is normally assumed the zeros are not significant. Scientific (exponential) notation can be
used to clearly indicate whether the zeros at the end of a number are significant. For example, a
mass of 11,500 g can be written in scientific notation showing three, four, or five significant
figures depending on how the measurement is obtained:
1.15 x 10
4
g (three significant figures)
1.150 x 10
4
g (four significant figures)
1.1500 x 10
4
g (five significant figures)
Significant Figures in Calculations
When carrying measured quantities through calculations, the least certain measurement limits
the certainty of the calculated quantity and thereby determines the number of significant figures
in the final answer. To keep track of significant figures in calculations, we will make frequent
use of two rules, one for addition and subtraction and another for multiplication and division.

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Addition and subtraction the result of a calculation has the same number of decimal places as
the measurement with the fewest decimal places (the least precise measurement). When the
result of the calculation implies more precision than could be possible, due to the measurements
taken on the centigram and decigram balances, it must be rounded off.
For example: Add the mass measurements taken from three different balances, each having a
different degree of precision.
Centigram balance 20.42 g Two decimal places

Analytical balance 1.3220 g Four decimal places Most precise
measurement
Decigram balance + 83.1 g One decimal place Least precise
measurement
Final calculated
answer
104.8420 Implies more precision than could be possible
so it must be rounded to the least precise
measurement, the tenths place (0.0)
Correct answer 104.8 g Four significant figures after rounding


Multiplication or division the result of a calculation contains the same number of significant
figures as the measurement with the fewest significant figures. When the result contains more
than the correct number of significant figures it must be rounded off. For example, if we have
5.098 g of sodium chloride and 30.5 mL of solution and we wanted to determine the density
(mass/volume) of the salt solution in this experiment:
(5.098 g) / (30.5 mL) = 0.167147541 is the answer on the calculator
However, this answer describes a precision of 9 significant figures which is far beyond the
precision of the original measurements. Although the mass of sodium chloride has four
significant figures (5.098 g), the volume of the solution has only three significant figures (30.5
mL) so the density of the solution can only be recorded as 0.167 g/mL, with three significant
figures.
Note that for addition and subtraction, decimal places are counted; whereas for multiplication
and division, significant figures are counted.
Rounding of Numbers
When rounding off numbers, look at the leftmost digit to be removed to determine whether you
will round the number up or down.
If the leftmost digit to be removed is less than 5, the preceding number is left unchanged.
Rounding 6.248 to two significant figures gives 6.2
If the leftmost digit to be removed is 5 or greater, the preceding number is increased by
1. Rounding 5.735 to three significant figures gives 5.74 and rounding 3.376 to two
significant figures gives 3.4.



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Mass
The directions in this experiment are written for use with an analytical balance. These milligram
balances are extremely precise giving a mass measurement to the ten-thousandth place (0.0001
g). This is considered the precision (or an uncertainty of +/- 0.0001 g) of the balance. Even
though this is a digital instrument, the balance is making an estimate at the ten-thousandths
place. All measurements of mass taken on the analytical balance recorded in your data sheet
should reflect this degree of precision. When using the analytical balance please be gentle with
these sensitive instruments and use the following procedures:
1. Before placing your item to be massed on the balance check the display to make sure it is
reading zero. If not press the tare bar once to zero out the balance.
2. Carefully open a side door and place the item on the pan and close the door.
3. Allow sufficient time for the mass to be measured.
4. Record the mass, remove the item and close the door.
5. Never place chemicals directly on the balance pan; first place the weighing boat or container
on the balance pan, tare the balance and then mass the chemicals by placing them onto the
weighing boat or into the container (beaker, for example)
6. Please be sure to clean up any materials you spill on or around the balance and close all the
glass doors on the balance once you are done with you measurement.
7. Never make any adjustments to the balance. If it seems out of order tell your instructor.
8. Make sure items to be weighed on the balance are at room temperature, never put a hot
object on the balance pan.

Volume
The graduated cylinder is the device you will be using in lab to measure liquid volumes.
Graduated cylinders are tall, cylindrical vessels with graduations scribed along the side of the
cylinder. Since volumes are measured in these cylinders by measuring the height of liquid, it is
crucial that the cylinder have a uniform diameter along its entire height, which is the case with
the glass cylinders you are using in lab. Beakers and flasks are marked to indicate only
approximate volumes and should not be used to measure volumes during experiments. When
observing a volume in a graduated cylinder, read the point on the graduated scale that coincides
with the bottom of the curved surface called the meniscus of the liquid. Most volumes
measured in the graduated cylinder should be estimated and recorded to the nearest 0.1 mL but
check with your instructor if you are not sure.








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Brief Review of Metric Systems more information available in your textbook
In science the metric system is used almost exclusively. The basic unit of length is the meter
(m); of mass, the gram (g); of volume, the liter (L). The meter, the gram, and the liter are related
to larger and smaller units by multiples of 10. Prefixes are used for the unit of measure
expressing these multiples of 10.
Prefix Abbreviation Value x basic unit Some Conversion Factors
Kilo- k 1000 1 km = 1000 m
Deci- d 0.1 1 m = 10 dm
Centi- c 0.01 1 m = 100 cm
Milli- m 0.001 1 m = 1000 mm
How does 1 kilometer compare to the other units in the metric system?
1 km = 1000 meters = 10,000 dm = 100,000 cm = 1,000,000 mm
Safety
You must wear goggles and an apron whenever you are working in the lab.
Before coming to lab class for this experiment you are required to go to the Flinn Scientific
MSDS web page (http://www.flinnsci.com/search_MSDS.asp) and read the MSDS
information required for your pre-lab assignment. Refer to the syllabus and additional
materials for more details regarding the pre-lab.
Disposal of Chemicals
Place the sand remaining at the end of the experiment in the waste crock. Rinse the sodium
chloride in the second evaporating dish down the sink.
Objectives
1. Experiment with physical processes used to separate the components of mixtures. Be able to
identify characteristics of physical processes as compared to chemical processes.
2. Use Bunsen Burner properly and safely.
3. Apply techniques of filtration, extraction, and sublimation for separating the components of
mixtures.
4. Correctly measure and record the mass and volume in this experiment. Be sure to record
measurements with the correct number of significant figures and the uncertainty of each
measurement.
5. Determine the % Composition of your sample.







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Procedure
Part A. Percentage of ammonium chloride, NH4Cl
In this step ammonium chloride is removed from the mixture by sublimation and its mass is
found by difference.
#1. Weigh a clean, dry evaporating dish and record the mass of the evaporating dish in Table I of
the Report Sheet (B).
#2. Check out an unknown sample from your instructor and record the number or letter of your
unknown sample on the Report Sheet.
#3. Add approximately 1.00 g of the sample into the evaporating dish and reweigh. Record the
actual mass of your sample in the appropriate place in Table I of the Report Sheet (A).
#3. Place the evaporating dish with the sample on wire gauze supported by a ring on a ring stand
IN THE FUME HOOD as shown in the picture below:

The gas valve is the lower of the two knobs (blue label) located on the side of the hood and the
gas outlet is the lower of the two outlets in the hood (color coded blue). Heat the evaporating
dish containing the solid sample with a burner for about seven minutes. Remove the flame and
gently stir the mixture with a stirring rod (being careful to wipe any solid on the lip of the
evaporating dish as you finish stirring), then apply heat again for at least five minutes.
#4. Let the evaporating dish cool. Use the metal crucible tongs to carefully remove the
evaporating dish and place it on a clean, dry watch glass for transport to the balance area. Weigh
the evaporating dish and remaining solid, recording the mass measurement Table I (C).
I would suggest you take a couple of minutes to complete questions 1 and 2 at this point since
they are asking about the sublimation portion of the experiment.
Part B. Percentages of sodium chloride, NaCl, and of sand
In this step the solid remaining from the previous step is mixed with water in order to dissolve
the sodium chloride. The solution is filtered away from the sand and the mass of sodium chloride
is found by evaporating the water from the solution. The sand remaining on the filter paper is
dried and its mass determined.
#1. Measure approximately 20 mL of deionized water using a 25 mL graduated cylinder and
record the volume in Table II. Add this water to the solid in the evaporating dish and stir gently.
Record the volume of water in Table II (D).
#2. Obtain a second clean, dry evaporating dish and weigh it. Record the mass in Table II (E).

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#3. Obtain a piece of filter paper and fold it as illustrated below, and weigh it. Record the filter
paper mass in Table II (F)
#4. Place the filter paper in a funnel supported by a clay triangle on a ring attached to a ring
stand, and wet it gently to make the paper stick to the funnel. Place the second weighed
evaporating dish under the funnel with the end of the stem of the funnel lightly touching the
inside of the evaporating dish.




#5. Slowly pour the sand-water heterogeneous mixture into the funnel and filter paper. Add a
small amount of distilled water from your wash bottle to rinse out any remaining solid (sand)
from the original evaporating dish and pour it through the filter. (Add only enough water to
remove any solids. Excess water will have to be evaporated.)
#6. After the liquid has drained through the filter, carefully remove the paper from the funnel,
open it out and place it on a watch glass. Place the glass and paper under a heating lamp to dry.
Check the drying progress of the filter paper as it may burn if it becomes overheated. You need
to weigh the dried paper to find the mass of the sand, which is in step 7 however, you can
proceed to step 8 while the filter paper is drying.
#7. Weigh the dried sand and filter paper and record this mass data in Table II (F).
I would suggest you take a couple of minutes to complete questions 3 and 4 at this point since
they are asking about the sand portion of the experiment.
#8. Clamp a ring on the ring stand and adjust its height so that the hottest part of the Bunsen
burner will reach the ring. Place wire gauze on the ring.

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# 9. Fill 250-mL beaker about two-thirds full with
deionized water (use the deionized water faucet at the
instructors station) and set it on top of the wire gauze. Use
the crucible tongs to carefully put the evaporating dish on
the beaker.
# 10. Light the Bunsen burner, adjust the burner to
maximum flame height, and heat the water to a fast boil.
At this point, the flame height may be lowered slightly.
Add water to the beaker if necessary by using a wash-
bottle. DO NOT let the beaker boil dry.
#11. Evaporate the solution until only dry solid remains in
the evaporating dish.
#12. Turn off the Bunsen burner, and when the water in the
bath has cooled down slightly, remove the evaporating dish
from the bath with a tong and set it on the bench top to
cool. Weigh the cooled dish plus solid and record it in
Table II.
I would suggest you take a couple of minutes to complete
questions 5 and 6 at this point since they are asking about
the sodium chloride portion of the experiment.

Data Section of you lab notebook should contain the following information:
(1) Unknown Number (or Letter) __________________________________
(2) Data table below:
Table I Sublimation Data of ammonium chloride, NH4Cl
Item Measured Measurement (include uncertainty and unit) # sig figs
(A) Mass of evaporating dish
with sample before heating

(B) Mass of empty
evaporating dish

Mass of sample (A B)

(C) Mass of evaporating dish
with sample after heating






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Table II Percentages of sodium chloride, NaCl, and of sand
Item Measured Measurement (include uncertainty and unit) # sig figs
(D) Volume of water used

(E) Mass of 2
nd
evaporating
dish

(F) Mass of filter paper

(G) Mass of dry filter paper
with sand

(H) Mass of 2
nd
evaporating
dish with remaining solid



Questions
For each of the following questions involving calculations you must show the mathematical set
up required to answer the question in your lab notebook and have the correct number of
significant figures in order to receive credit for your response.
Question #1: Determine the mass loss due the sublimation of ammonium chloride (NH4Cl).
This mass loss is the mass of ammonium chloride that was originally present in the mixture.
Question #2: What is the percentage of ammonium chloride present in the original solid
sample?
Question #3: Determine the mass of the solid substance in the filter paper. This is the mass of
sand (silicon dioxide, SiO2) that was originally present in the mixture.
Question #4: What is the percentage of sand (silicon dioxide, SiO2) present in the original solid
sample?
Question #5: Determine the mass of the solid substance in the 2
nd
evaporating dish. This is the
mass of sodium chloride (NaCl) that was originally present in the mixture.
Question #6: What is the percentage of sodium chloride (NaCl) present in the original solid
sample?






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Question #7: Complete the following table in you lab notebook:

Theoretically, what should be the
total percentage?



Question #8: Percent error is a calculation done after an experiment that gives the experimenter
an idea of how the accuracy of their work in lab. Use the following mathematical equation to
determine the percent error for the total percentage of the substances you have separated in the
experiment.
Percent error = |experimental percent theoretical percent| / [theoretical percent]
Question #9: Using your own words in a complete sentence give a definition and one common
example of each of the four types of separation techniques used in this experiment.
(a) sublimation (b) extraction (c) filtration (d) distillation
Question #10: A 4.00 gram sample of a solution of sodium chloride in water was heated until all
the water had evaporated. The sodium chloride that remained weighed 1.22 grams. Calculate
the percentage of water in the original solution.
Question #11: A laboratory technician wants to prepare 80.0 grams of a mixture containing 50.0
% sand, 30.0 % sodium chloride, and 20.0 % ammonium chloride by mass. Calculate the mass
of each substance that the technician would need to mix.
Question #12: What are the possible sources of experimental errors in this experiment?
Question #13: During dental work or minor surgery, a local anesthetic, such as procaine or
lidocaine, is used to deaden the pain in a small area of the body. Although both are about
equally effective in numbing the pain, procaine is eight times more toxic than lidocaine. With
which anesthetic is it more important to be precise and accurate in administering a dose? Use a
sentence or two to explain your choice.
Question #14: When cutting the legs of a table to make it lower, precision is usually far more
important than accuracy. Use a sentence or two to explain your choice
Question #15: Determine the density of the sodium chloride solution that was collected after the
filtration was completed in part B. Assume the volume of the sodium chloride solution is the
same as the volume of water used in the experiment.
Conclusion Write a short paragraph summarizing your work in this experiment and describe
what you have learned after completing this experiment.
Please note: Your conclusion should always include a sentence or two reporting the actual
results of your experiment - in this case, it should include the % composition of the unknown
sample you analyzed in lab. Please be sure to include this information - do NOT leave your
results out of your conclusion - you are guaranteed to lose at least 1-2 points (or more).
Substance Percentage found
Ammonium chloride, NH4Cl
Sand, SiO2
Sodium chloride, NaCl
Total

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