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Assignment One

Tuesday September 29 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.
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 labeled 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
goggles 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 one's 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 ultimately 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 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 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.
Artifacts:
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.
th

Commented [LB1]: Explain what a titration problem is.


Maybe include an example or a vocabulary list before
the paper. Why were only titrate samples used rather
than other samples?
-KM
Commented [LB2R1]:

Commented [LB3]: Maybe mention the name of your


lab instructor. You could give information about who
they are and why they are significant. Also, if you want
to interview him to go above and beyond that could also
help the paper become stronger.This can also be the
same with the Lab Partner-add more about who you
worked with and how they impacted you.
-KM

Commented [LB4]: I would suggest that you add the


definitions of these key terms. This way you won't lose
major points off your grade. It will also help better
prepare the reader for the section.
-GB
Commented [LB5R4]:

Pipet The pipet being used is only a 10 mL 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 manner. 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:
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
of 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?

Commented [LB6]: Tell us about who you interviewed


and maybe add a photo of the professor. The questions
are very straight forward and easy to understand even
though they are about a difficult topic. Maybe include
interview with the lab instructor or lab partner to go
above and beyond.
-KM
Commented [LB7]: I really enjoy the format of your
interview questions. They really probe the interviewee
to answer them in depth. I feel like I better understand
the interviewee related to your area of study.
-GB

Commented [LB8]: Overall, the information provided in


the assignment is very interesting. However, for the
observations, it would benefit if you mark time in a
different format. For example, mention the time that the
lab began and provide a time stamp throughout the
observation on the side.
-GB

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:
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. For her to get the most accurate results she was to repeat the calibration in
five different trials. Prior to the calibration she first got the weight in grams of the volumetric
flask. 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. 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). 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.
Pipet During this observation, I watched as my lab partner calibrate her pipet during 10
different trials. For the calibration of the pipet she was to sit by the scale which, was boxed in,
so that the airflow 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. Once
she had the scale at zero, she began to pull up distilled water through the pipet until it was at
its maximum capacity. 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. 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. This measurement of the pipet will to be used throughout the remainder of
the semester, to ensure accuracy with all of her measurements.
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. 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. 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:
A weighing 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. 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. 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. To prevent any of the hydrochloric acid from evaporation, we covered the

Commented [LB9]: I would like to suggest that you


bold some of the titles so that the reader does not get
lost looking down the page. Without the bold words its
dry easy to lose your place in the reading causing a bit
of confusion of structure. With the bold titles not only will
this add a an easier flow but a more structured
presentation.
-GB

Commented [LB10]: A suggestion to go above and


beyond would be to include your calculations for each
experiment. Also before each observation it could help
the reader understand the experiment by adding
objectives. The overall layout of the experiment is very
straight forward and uses correct tenses for Chemistry
Lab (as far as I know).
-KM

beaker with a watch glass. We then had to rinse out the burette with the hydrochloric acid in
order to get more accurate results. 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. 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. Next we
began adding the hydrochloric acid from the burette into the Erlenmeyer flask until the colour
of the solution begins to change. Once we hit the green colour, 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. 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. 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. 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. Following this step we began to boil the solution, to get rid of any
dissolved carbon dioxide the remained in our solution. 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. 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.
Observation Three:
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. 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. We then had use our three 250 mL
beakers and pipet 10 mL of the unknown solution into each one. 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. 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. 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. 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. Following this step we added 20 mL of ammonium
oxalate to each of the beakers, as well as adding 15g of urea. 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. 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. 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. Once all three of the beaker solutions have been suction filtered, the crucibles were
then placed back in our labelled 1000 mL beaker. We had to cover our beaker with aluminium
foil, and then the beaker was placed into an oven to dry for the next week.

Commented [LB11]: I like how the observations are


very detailed and explain what is going on at each step.
I think it would b interesting to add the conclusion. It
would also be helpful to see a picture of the lab
procedure/worksheet.
-KM

Commented [LB12]: Here would be a good place to


add a concluding sentence. The last sentence ends
your observation well but doesn't really end the paper in
the same manner. This will help with the "drop off"
feeling of just stopping at the end of the observation.
Gabriel Bryant