Thin Layer Chromatography of Spinach Leaves Extract & Synthesis of Acetylsalicylic Acid Through Acetylation Reaction Report Hello this lab report is for or

Thin Layer Chromatography of Spinach Leaves Extract & Synthesis of Acetylsalicylic Acid Through Acetylation Reaction Report Hello this lab report is for organic chemistry 1

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INSTRUCTIONS

Author: (You)

Instructor: (Me)

Section: 691

Date:

(Write your own scientific title)

Introduction

Stick to the main topics: esterification, Fisher esterification, synthesis of acetylsalicylic acid, thin layer chromatography, TLC uses, polarity – don’t get into the medicinal history of acetylsalicylic acid. Keep it simple. There should be citations in this paragraph since this is where background information lives.

There are two parts of this experiment that overlap a little, but aren’t directly connected. If you prefer to use a 3 paragraph structure in order to keep the experimental specifics organized, that is fine. Write a separate hypothesis to end P2 and P3. If you combine both parts of the experiment into a single “In this experiment” paragraph, that’s fine too, just stay organized – clear and concise – you can write two hypotheses at the end of the paragraph, one right after the other.

In the spinach experiment, the main idea is to observe the separation of the spinach pigments and to evaluate the extracted ?-carotene to see if it was properly isolated from the other spinach pigments when prepared. In the acetylsalicylic acid synthesis, the main idea is to use TLC, MP, and %yield to determine if the synthesis goes to completion and judge its success.

Terms to include: esterification, mobile phase, stationary phase, salicylic acid, acetylsalicylic acid, retention factor, catalyst (any form of that word), polarity (any form of that word), adsorb (any form of that word).

Materials

Make a list from the lab handout, but also jot down items in your lab notebook while watching the experiment. Everything used should be on this list, including volumes and masses.

Procedures

Numbered list of instructions of how the experiment will be performed. Focus on writing in your own words. Part A and Part B would be appropriate here (or whatever you want to call them).

Data

Photo of experiment notes (name, experiment, date at top of page). Requirements for notes will be discussed during Blackboard meeting. You will need a flow scheme for the ASA synthesis.

Remember that I’m looking for the actual notes you take while watching the experiment, not a fancy rewritten version — the purpose of this is so I can see how you are taking notes and give suggestions for improvement (we’re trying to have you start taking notes like a professional). You only lose points in this section if you don’t follow the instructions given in the lab manual (if there’s a table or flow scheme required) or if you leave out instructions discussed in the Blackboard session.

Results and Calculations

Table 1. Rf values for spinach plate – the number of Rf values in this table should match the number of spots visible on the plate in the experiment video. Details will be discussed in the Blackboard session.

Table 2. Rf values for ASA synthesis plate (1 spot before heating and 1 after heating)

Table 3. Percent yield of ASA (include theoretical yield in grams, actual yield in grams, and percent yield). Salicylic acid is being esterified in a reaction with excess acetic anhydride; SA is the limiting reagent, and it’s a 1:1 reaction.

Table 4. Melting Point (literature MP of ASA, literature MP of SA, experiment MP of product, cite literature values)

Include Rf equation and percent yield equation somewhere in Results and Calculations section (not inside tables; list equations on a separate line).

Remember units (and remember that Rf is a ratio, so it’s unitless).

Discussion

Discuss results from spinach TLC plate. Was the experimental ?-carotene pigment (first yellow vial, Lane 3) properly extracted as compared to the ?-carotene lab standard (Lane 4), or did it show traces of other spinach pigments? Was there a ?-carotene spot in the extracted chlorophyll (Lane 2) or the whole spinach extract (Lane 1)? Based on polarity, where is a ?-carotene spot expected to finish on the TLC plate compared to other spinach pigments, and did the results show as expected? If ?-carotene was seen in the spinach extracts (Lanes 1 and 2), did it have the same Rf as the isolated ?-carotene spots (Lanes 3 and 4)? If not the same, suggest reasons why ?-carotene might have traveled differently when isolated compared to when it’s being separated from a mixed spot.

Use TLC and MP results to support a conclusion of whether salicylic acid was converted to acetylsalicylic acid or not. Did the before-heating and after-heating TLC spots have the same Rf values? Does this support any conclusion about synthesis of ASA being successful? What do the Rf values indicate about the polarities of SA and ASA compared to each other (higher polarity vs lower polarity). Evaluate the percent yield of the product (yield over 100% indicates error; low yield indicates mass loss — discuss possible reasons). Compare experimental MP to literature MP of ASA. How do the MP results support your conclusion about whether or not ASA was synthesized? Was there melting point depression, and if so, what does this suggest about the purity of the product? Draw an overall conclusion about the success of this acetylsalicylic acid synthesis.

Terms to include: mobile phase, stationary phase, salicylic acid, acetylsalicylic acid, polarity (any form of that word), retention factor, literature melting point, percent yield

Note: partial conversion from SA to ASA is possible (reaction must get enough heat energy for a sustained period of time to go to completion).

Remember to refer to tables containing the information rather than restating numbers.

Note: the questions I list in Discussion are prompts to help you form an analysis – they should not be addressed in a “question and answer” style in your report. Don’t restate the question and answer it like it’s a question on a test…weave the concepts into your discussion, and write like it’s an essay.

Postlab Questions

What compound will you have if acetylsalicylic acid is NOT successfully synthesized, and how would you confirm that identify using techniques from this lab?

References

Include 1 reference other than lab manual. Thin Layer Chromatography and its Application in
the Synthesis of Aspirin
I.
Thin Layer Chromatography
Chromatography is the separation of two or more compounds or ions caused by their molecular
interactions with two phases – on moving phase and one stationary phase. These phases can be
a solid and a liquid, a liquid and a liquid, a gas and a solid, or a gas and a liquid. Three types of
chromatography are used extensively in organic chemistry: Thin Layer Chromatography (TLC),
Gas Liquid Chromatography (GC) and Column Chromatography (CC).
In chromatography, the sample partitions itself between mobile and stationary phases. If it has a
greater affinity for the mobile phase, it will move faster. If it has a greater affinity for the
stationary phase, it will move slower. If the sample is a mixture and the stationary phase and
mobile phases are well-chosen, various mixture components will have different affinities for the
phases, thus, will move at different rates, causing the mixture components to separate.
Successful separation depends on the different polarities of 3 components: the adsorbent, the
compounds, and the solvent. The adsorbent is always the most polar compound; common
adsorbents are silica gel and alumina. The compounds in the sample mixture differ in polarity
based on compound structure and functional groups. Solvents also differ in polarity. Appropriate
solvents for good separation should be selected based on the polarities of the sample compound.
Thin-Layer Chromatography (TLC) is a fast, simple, inexpensive, and sensitive analytical technique
that will be used repeatedly to carry out organic experiments. A plastic or glass plate coated with
a thin layer of silica (the adsorbent) is in general used. A small spot of solution containing the
sample compound is applied to a plate, about 1 cm from the base. The plate is dipped into solvent
in a covered chamber. The solvent moves up the plate by capillary action and meets the sample,
which is dissolved and carried up the plate by the solvent. Compounds in the sample mixture
travel at different rates due to different levels of attraction to the stationary phase. Results can
also vary depending on solvent choice; solubility influences the sample’s affinity for the mobile
phase (the solvent) during TLC.
Appropriate TLC mobile phase (solvent) differs from the stationary phase material in polarity. If
a polar solvent is used to dissolve the sample and the spot is applied to a polar stationary phase,
the sample spot will grow radically due to capillary action, which is not advisable as spots may
mix. To restrict growth of sample-spots, the carrier solvent (for dissolving samples and
application to plates) should be as non-polar or semi-polar as possible.
There are many applications for TLC. TLC can determine the number and relative amount of
components in a mixture. It can determine identity of unknown substances – if two compounds
on the same TLC plate give spots in identical locations, the compounds may be identical, but if
the spot positions differ, the substances cannot be the same. TLC can be used to monitor progress
of a reaction. Effectiveness of purification processes and appropriate conditions for a column
chromatographic separation can be determined.
In TLC, the retention factor (Rf) is a way to quantify spot results for comparison. The Rf is defined
as the ratio of the distance traveled by the compound to the distance traveled by the solvent.
Rf =
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A representation of TLC is shown here:
Experimental Procedure
Disposal of waste: All organic waste must be disposed into the organic waste container, all
aqueous waste to the aqueous waste container, and all solid waste to the solid waste container.
Nothing is disposed in the sink or trash can.
Obtain a TLC silica plate with fluorescent indicator. Draw a light pencil line about 1 cm from the
end of the plate. Mark the plate with four equidistant hash marks. Spot the plate with the four
pigments provided: spinach extract, chlorophyll extract, ?-carotene extract, and ?-carotene
standard solution using an open-ended capillary tube. Exert care not to overspot pigments.
Examine the plate under UV light to see if the compound was applied, if not, add more. DO NOT
look directly into the UV lamp. UV light can damage your eyes!
Add a mixture of 70% hexane/30% acetone in a tall beaker and place the TLC plate vertically in
the chamber, being careful not to touch the surface of the plate. When the solvent front has
traveled up the plate (2-3 cm from the top edge), remove the plate and gently draw a pencil line
to mark where the solvent stopped (quickly, before the solvent on the plate dries). After the plate
has dried, examine it under UV light. Using a pencil, mark the spots. Note the color of the spots
and record the distance travelled by each spot and the distance travelled by the solvent front
(the line marked after removing the plate from the solvent). Place the plate in an iodine chamber
for about 2 minutes. Do not breathe or get iodine on skin. Calculate all Rf values.
II.
Synthesis of Aspirin
In this part of the experiment acetylsalicylic acid (aspirin, ASA) will be synthesized from salicylic
acid (SA) and acetic anhydride. TLC will be used to determine whether the reaction has gone to
completion.
The ester group is an important functional group that can be synthesized in a variety of ways.
The low molecular weight esters have very pleasant odors and indeed comprise the major
flavor and odor components of a number of fruits.
Esters can be prepared by reacting a carboxylic acid with an alcohol in the presence of a catalyst
such as concentrated sulfuric acid, hydrogen chloride, p-toluenesulfonic acid, or the acid form
of an ion exchange resin. This way of ester preparation is called Fischer esterification.
Other methods are available for synthesizing esters, most of which are more expensive but
readily carried out on a small scale. For example, alcohols react with anhydrides and with acid
chlorides.
Aspirin is among the most versatile drugs in medicine; it is also among the oldest. Aspirin is an
analgesic, an antipyretic (fever reducer), and an anti-inflammatory agent. It is the premier drug
for reducing fever, a role for which it is uniquely suited. As an anti-inflammatory, it has become
the most widely effective treatment for arthritis. Aspirin is made commercially employing the
same synthesis presented above.
Experimental Procedure
Disposal of waste: All organic waste must be disposed into the organic waste container, all
aqueous waste to the aqueous waste container, and all solid waste to the solid waste
container. Nothing is disposed in the sink or trash can.
Place 1 g of salicylic acid, 2.5 ml of acetic anhydride, and 5 drops of concentrated sulfuric acid in
a 50 ml Erlenmeyer flask containing a spin bar. Swirl to dissolve. Prepare a TLC plate for 2 spots.
Take a TLC spot of the mixture using EtOAc:Hexane (1:1) as a solvent. Label the spot t=0. Heat
the reaction mixture with stirring on a warm sand bath or hot plate for 10 minutes. After 10
minutes, spot the heated mixture on the TLC plate and label the spot t=10. Taking a TLC at this
stage can verify that all salicylic acid was converted to product. Once it has been determined that
salicylic acid was converted to product, cool solution to room temperature, then cool in an ice
bath to crystallize the aspirin.
Add 20 ml of cold water to the flask and stir carefully. Vacuum filter the crystals using a Buchner
funnel. Wash the crystals with several small portions of ice-cold water. Crude aspirin can be
recrystallized with ethyl acetate. Dissolve the crude product in a minimum amount of hot ethyl
acetate (perform hot gravity filtration if it is necessary to separate the hot solution from insoluble
impurities). Allow the solution to cool to room temperature and then place in an ice bath to
complete recrystallization. Vacuum filter using a Buchner funnel. Find mass of dried crystals and
determine melting point.
2 3
12
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This is for number one
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Drison
6
6
Number two … The distance is between 2-2.7
or 2.8
10
0 1 2 3 4
12.
In number 3 we do the same thing as number
for which is recording the distance. The
distance as it shown in the pic is form 3 to 6

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