Assignment One

Tuesday September 29th 2015

Analytical Chemistry
Note:
This observation took place during a Quantitative Chemical Analysis Laboratory. This lab
ran for approximately two and a half hours, though this lab was not broken down into timed
increments. This lab observation will be broken down into three separate sections, as this lab
did involve the calibration of three different instruments used in the chemistry field.
Definitions:
Titration: The method of adding a solution with a known concentration to an unknown
solution in order to determine the concentration of the unknown. Burettes are generally used
during a titration.
Pipet: These instruments can be narrow tubes, some even having a larger bulb in the middle
of them. These can be used for measuring as well as transferring out smaller portions of
liquids.
Burette: Is a long narrow, generally glass tube with a stopcock at the end which allows you to
let the liquid flow and then to cut off the flow.
Volumetric Flask: This glassware is used for the diluting of solutions as well as the preparing
of a standard solution.
Bromocresol Green: An indicator which is put into an unknown solution, which, during
titrations will change colour as the pH of the solution begins to change.
Crucible: Glass bowl used to filter the remaining precipitate left in a solution, which will later
be weighed to determine composition of the precipitate.
Desiccator: A glass container, used to hold the crucibles containing precipitate I order to
remove any remaining moisture.
Relevant Background Information:
The observation was taken place during a CHEM 3111 Lab course, which is an undergraduate
Quantitative Chemical Analysis course where students are taught how to titrate samples as
well in this lab course they will be designing their own research project for the seconds half
of the semester. The purpose of this lab being observed was being able to calibrate the
glassware such as a volumetric flask, a pipet as well as a burette this is being done so that
the students readings will remain accurate throughout the course of the semester. Even
though these instruments are generally already marked with the maximum volume which it
can hold, this laboratory will go one step further in order to find the most accurate volumes
which these instruments can actually hold (which should not be far off from the labelled
volume). This is done so that the readings throughout the semester will be as accurate as
possible, leaving little to no room for systematic errors to occur.
Rules and Conventions:

In the laboratory all students must make sure to come prepared with lab goggles in hand as
well as a lab manual In order to record data throughout the experiments taking place. The lab
goggle are a necessity to have whilst in the laboratory as chemicals are being used throughout
the experiments conducted, and these chemicals can easily splash up into ones eye perhaps
causing serious damage. During laboratory practises the students must also be sure that they
are using their own clean and calibrated glassware, and failure to do so can really skew the
data points for the remainder of an experiment. This is why during laboratories it is crucial to
clean the glassware after each use so that the results remain accurate throughout each
experiment.
Significant People:
Lab Instructor (Dr. Murphy) Our instructor is a very important person to have throughout
our lab period as he is an expert in the field of Quantitative Analysis. The lab instructor
informs the students on how the experiments should be performed as well as going over
safety tips so that no errors or mistake will occur during the lab period. As well if there are
any questions or concerns which may come to mind throughout the experiment the lab
instructor will help the students through the difficulties helping them expand the mind on the
topic being taught as well as being able to learn from the Instructor. The Instructor plays a
crucial role in keeping the laboratory under control as well as making a safe environment for
the students to work in.
Lab Partner (Kristina) The lab partners are also a very important people to have during the
experiments, without them the experiment would become a lot more time consuming than
they already are. The significance of having a partner work on the experiments along ones
side, can actually help with the accuracy of data having someone to double check
calculations for an experiment so that that results are correct. As well with a lab partner they
can also look over volumetric readings to make sure that the readings are no more than +/0.01 off from the volume needed.
Artefacts:
Volumetric Flask Glassware used in a Chemistry Laboratory which must be held at a
specific temperature. This glassware is generally used for the diluting of solutions as well as
the preparing of a standard solution.
Pipet The pipet being used is only a 10mL pipet. These instruments can be narrow tubes,
some even having a larger bulb in the middle of them. These can be used for measuring as
well as transferring out smaller portions of liquids.
Burette Is a long narrow, generally glass tube with a stopcock at the end which allows you
to let the liquid flow and then to cut off the flow. The burettes are used for the titrations of
different liquids, the most common titration would be an acid (Hydrochloric acid) and bad
(Sodium Hydroxide).
Domain:
The focus of these Lab classes would primarily be on the instructor as he explains how the
calibrations should be done in the correct manor. As students we all rely on his teachings, so
when it comes to performing the actual calibrations we all get our correct results without our
data being altered. The students greatly value the knowledge the lab instructor has, as it

allows the calibrations of the glassware to run smoothly giving us a better understanding of
the topic.
Literacy Practises:
During the calibration of the glassware it was important to record all data in the lab manual,
then we later turn in all of our notes with all of the calculations and measurements on them to
the lab instructor. For each instrument being calibrated, there are a number of trials which
much be done so it is important to have all of the trials recorded. This is because when it
comes the writing out your calculations, the mean must be calculated from all the trials so
that the volume of the glassware can be as accurate as possible for the future labs.
Interview:
Interview with Dr. Brian Cooper, Professor of Quantitative Analysis
1. Describe why you decided to be a Professor in the Chemistry field?
A: I have a strong personal need for novelty, I like to learn new things. The biggest
advantage if being a professor is that you are expected to stay abreast in your field to
keep track of new developments in your field. The research is interesting, and an
intellectual challenge, I enjoy it. Though it is not necessarily my strength, but my
number one reason I chose this job is because I do enjoy learning.
2. Tell me what first got you interested in the study of Chemistry?
A: My father is a chemical engineer, my grandfather is a chemist, and my maternal
grandfather is a biochemist. The reason I got interested in science is because the
environment I grew up in, anytime I would ask a question about something technical
they were usually answered with technical answers. So being in that environment
got me interested in Science. Originally in high school I was more interested in
Physics, until I had a good Chemistry teacher, and a not so good Physics teacher
which tipped me over more to Chemistry.
3. What is your interest in Quantitative Chemical Analysis?
A: The teaching is whatever the department needs from me, but I put a lot of effort
into this course over the last couple of years to redesign the lab. I chose Analytical
Chemistry when I was going to graduate school, so after I graduated from
undergraduate institutions I was looking at graduate schools all over the country. I got
interest in instrumentation from a research group that I was in. I chose a graduate
school based on their program strengths and their Analytical Chemistry offerings.
4. Can you think of a time which has challenged you the most whilst being in the
Chemistry field?
A: The most difficult analytical problems come from Biological samples. A good
example of this is trying to detect protein markers in blood and serum. It is a
challenge because serum there are a handful of protein present in very high
concentrations, and virtually every protein in serum is present at a low level of
concentration. The ratio of the highest concentrations to the lowest concentrations is
about 10^12.
5. Discuss the importance of knowing the uncertainty in a value?
A: Uncertainty is important because when you measure something, the measured
quantity is not infinitely precise. There is always a limit to how well you know the
number that you measured, and you need to be able to express that limit somehow.
Any measured quantity has three parts, the value, the units and the uncertainty.

Observation One:
1. Volumetric Flask Whilst observing my lab partner calibrate the volumetric flask,
they had to be sure that the flask had no residue left on it that the flask was
completely clean before the calibration began.
2. For her to get the most accurate results she was to repeat the calibration in five
different trials. Prior to the calibration she first go the weight in grams of the
volumetric flask.
3. Following that, for each trial she would fill up the volumetric flask to the marked line
on the neck of the flask with distilled water, then would weigh the flask again and
record its weight.
4. She repeated this step four more times to have a total of five calibrations. Now that
the weight of the water was known she found the mean of the of the mass of the water
in the volumetric flasks, and with this and the known density of water (approx. 1.00
g/mL) she was then able to solve for the volume of the water (Mass of Water / Density
of Water).
5. From this she is was given the approximate volume of her volumetric flask which is
now to be used throughout the remainder of the semester for any future measurements
and calculations.
6. Pipet During this observation, I watched as my lab partner calibrated her pipet
during 10 different trials.
7. For the calibration of the pipet she was to sit by the scale which, was boxed in, so that
the air flow would not be able to affect the weight of water. In order for my partner to
perform the calibrations she was to put a beaker onto the scale then zero the scale out.
8. Once she had the scale at zero, she began to pull up distilled water through the pipet
until it was at its maximum capacity.
9. Once the pipet was filled the water in the pipet would then be released into the beaker
on the scale, and then being sure to shut the lid on the scale so the air drafts didnt
skew the reading.
10. This process of filling up the pipet and measuring the weight of the water held was
repeated nine other times leaving my partner with a total of ten trials completed. Such
as in the previous calibration she then found the mean of the mass of the water from
the ten different trials, then from there she was able to calculate the volume with the
known density.
11. This measurement of the pipet will to be used throughout the remainder of the
semester, to ensure accuracy with all of her measurements.
12. Burette During this portion of the laboratory my lab partner was actually not to
calibrate the burette, but to determine what the water level (meniscus) was at in each
burette and the readings must be +/- 0.01 mL to the answer for each (6) of the
burettes.
13. For her first trial reading the burettes, she missed two readings which were off more
than +/- 0.01 mL so she was to repeat the six readings again, though the instructor
does not inform us of which two readings were incorrect.
14. My lab partner begins the read the burettes in order to see where the meniscus lay, but
her answers had not seem too far off from her first trial. My lab partner then brought
her answers to the instructor as she seemed fairly confident in her readings, so the
instructor took a look at the water levels in the burettes. Once he was done examining
the water levels, he looked over my lab partners readings and she had gotten all six of

the water levels correct to +/- 0.01 mL. During the time the water had been put in the
burette to the time my lab partner read the water levels, some of the water had
evaporated causing the original data to be skewed.
Observation Two:
1. A weighting bottle was used order to obtain approximately 0.8 to 1.0 grams of sodium
carbonate, following this the bottle then had to be closed tightly so no other particles
got into the salt.
2. At the balance, we then weighed out just over 0.13g of sodium carbonate, which was
then transferred into the Erlenmeyer flask rinsed down by deionised water.
3. We then had to obtain no more than 200 mL of hydrochloric acid in our 250 mL
beaker, which will be used for the titration.
4. To prevent any of the hydrochloric acid from evaporation, we covered the beaker with
a watch glass.
5. We then had to rinse out the burette with the hydrochloric acid in order to get more
accurate results.
6. Following this, we had to perform a scout titration to get the approximate volume to
mass ratio that should be taking place throughout the four titrations.
7. We added approximately 25 mL to the sodium carbonate in the Erlenmeyer flask,
which should then help to dissolve the salt, then added three drops of Bromocresol
green which, is an indicator telling us when the endpoint has been reached. This is
due to a colour change which takes places, turning the solution green when the
endpoint had been reached.
8. Next we began adding the hydrochloric acid from the burette into the Erlenmeyer
flask until the colour of the solution begins to change.
9. Once we hit the green colour we, we recorded the volume of hydrochloric acid used
with the amount of sodium carbonate used so we knew approximately how much
hydrochloric acid should be used throughout the next four titrations.
10. We then set up four 125 mL Erlenmeyer flask for our four experimental titrations, and
we weighed out approximately 0.13g of sodium carbonate for each of the Erlenmeyer
flasks.
11. Each sample had to be dissolved in 25 mL of water, just like in the scout titration, as
well as adding the three drops of the Bromocrescol green indicator.
12. We then began the titration and knew the stop the addition of hydrochloric acid when
we were in about 1 mL away from the measured volume of the scout titration.
13. Following this step we began to boil the solution, to get rid of any dissolved carbon
dioxide the remained in our solution.
14. After boiling the solution for 30 seconds, we added a few more drops of the
hydrochloric acid which then should have allowed the end point to have been
reached.
15. We then repeated this same titration three more times, and after the four trials had
been complete we calculated the volume to mass ratio for each titration to check for
precision seeing if our four results accurately matched up.
Conclusion and Formal Report for Observation 2
Experiment 1: HCl Standardisation

Abstract:
The laboratory of HCl standardisation is an experiment designed to see if ones
ability to perform a titration is as accurate and precise as possible, this is done in
order to find the correct concentration of the HCl. In order for to determine the
concentration of the HCl, sodium carbonate will be used this must be dissolved
in water prior to the titration, then will be titrated using the 0.1M of HCl which
should have a balanced equation such as the one below:
2HCl (aq) + Na2CO3 (aq) H2O (l) + CO2 (g) + 2NaCl (aq)
Though the carbon dioxide is in the gaseous form, it is still present whilst the
titration has reached equilibrium though the presence of the carbon dioxide will
remain dissolved until the end point has been reached. In order to detect when
the titration is at the equivalence point, bromocresol green will be use this
indicator detects pH changes by the changing of colour. If the pH is above 5.4
the colour of the solution will remain blue, if the pH is below 3.8 the colour of the
solution will turn yellow. In this laboratory, the end point to be met is around a
pH of 4.6 which will be more of a green colour before the end point is met the
solution will reach the equivalence point when there is the first sign of a green
colour change. After the first sight of the green colour change, the solution must
be brought to a boil to rid of any carbon dioxide for more accurate and precise
results. Following the boiling add more titrant, drop by drop, until the end point
has been reach the solution should then be a faint green colour with a pH of
approximately 4.6.
During the experiment I ran four titrations, with more than one titration this
allowed my concentration of HCl to be more accurate value. The concentration
for the HCl was obtained by averaging out the corrected concentration of HCl
from all four of the titration trials, which gave me a concentration of
approximately 0.104 mol/L.
With the result of 0.104 mol/L, the uncertainty of this value then had to be
calculated in order to make the concentration as accurate as possible with a
calculated value of 0.000328. The equation used is shown below:
0.0104 ts n
Data and Results Table:
Trials

1
2
3
4

Mas
s (g)

Corrected
Mass (g)

Volum
e (mL)

0.13
4
0.13
2
0.13
3
0.13
0

0.13454364
0
0.13174273
2
0.13314318
6
0.13054234
2

24.33

Correc
ted
Volum
e (mL)
24.23

23.88

23.78

24.12

24.02

23.72

23.62

95%

Confidenc

Interva

[HCl]
(mol/L)

Correcte
d
[HCl]
(mol/L)

0.1043501
34
0.1041032
50
0.1041630
26
0.1038505
17

0.104388
513
0.104141
539
0.104201
337
0.103888
713

Average
[HCl]
(mol/L)

0.01
04

l
0.00032
8

*The common values used in the experiment were the molar mass of Na2CO3: 105.98833 0.00156 g/mol,
with a density of 2.53 g/mL. The blank volume was around 0.1 mL, which was used to calculate the corrected
volume. The average temperature was at 21.7 C, which was used to calculate the interpolated water density
of 0.09978401.

Observation Three:
1. During this observation we had to turn our hotplates on as soon as lab began, so once
our solution was made we could boil it immediately after then let it boil for 30
minutes.
2. We then chose a plastic vial containing an unknown calcium solution which was used
throughout the experiment. We had to use our pipet for this experiment, but before
we could use it, it had to be rinsed with a few millilitres of the unknown solution.
3. We then had use our three 250 mL beakers and pipet 10 mL of the unknown solution
into each one.
4. Following the addition of the unknown solution, we had to head over to the balance
stations with crucible tongs, and our desiccator containing three crucibles.
5. We then had to weigh all three of the crucibles, but in order to weigh them we had to
pick up the crucibles with the crucible tongs as we are not to touch the crucibles with
our hands.
6. Once all three of the crucibles have been weighed, they were then placed in a 1000
mL beaker and brought back to the lab bench.
7. We then began the precipitation by adding 50 mL of hydrochloric acid to each of the
250 mL beakers, as well as adding 4 drops of the methyl red indicator.
8. Following this step we added 20 mL of ammonium oxalate to each of the beakers, as
well as adding 15g of urea.
9. Once the urea has been added the solution in the beakers must be boiled for about 30
minutes until the solution has gone from the original pink colour to a more yellow
colour.
10.
Following the boiling of the three solutions we had the suction filter the heated
solution through our weighed crucibles, leaving only the precipitate left in the
crucible.
11.
If any of the precipitate remains in the beaker, it is to be washed out with
deionised water and poured into the suction filter until all precipitate lay in the
crucible.
12.
Once all three of the beaker solutions have been suction filtered, the crucibles
were then placed back in our labelled 1000 mL beaker.
13.
We had to cover our beaker with aluminium foil, and then the beaker was
placed into an oven to dry for the next week.

Conclusion and Data for Observation 3

Experiment 2: Gravimetric Analysis of Calcium
CHEM 3111
Lindsay Bulger

Abstract:
In the laboratory an unknown Calcium solution was obtained (2-34) and the
calcium present in the solution was approximately 27.43 0.002 % Ca as
stated in the Experiment 2 handout. Three replicated were then created with
HCl, acidified ammonium oxalate, solid urea as well as the addition of the
unknown sample being used in order to precipitate our sample into calcium
oxalate (CaC2O4H2O). At the 95% confidence interval the concentration of the
Ca was approximately 6.486 0.046. This uncertainty was calculated by the
uncertainty propagation involving the measured volume of the pipet, the mass
percent of Ca in the calcium oxalate as well as the mass of the calcium oxalate.
Replicate Number
Uncorr. Mass
CaC2O4H2O (g)
Buoyancy Corrected
Mass (g)
Average Corrected
Mass
CaC2O4H2O

1
0.2353

2
0.2366

3
0.2357

0.235393
101

0.2366936
16

0.2357932
60

0.0016

0.2360

*The density of the CaC2O4H2O used was 2.2 g / mL, as well the measured temperature during the laboratory
was approximately 21.6, and from this the interpolated density was calculated at 0.9978623 g / mL.

Quantity
Buoy. Corr. Mass of ppt (g)
Calibrated Vol. of 10 mL
Pipet (mL)
Mass % Ca in CaC2O4H2O
Calcium Concentration @
20

0.2359
9.9821

95% C.I.
source / value
0.0016
0.0041

27.429
6.4861

0.0020
0.0455

% Relative
Uncertainty
0.6783
0.0411
0.0073
0.7015