Experiment for Identification of Paracetamol

• PATRICK ANTWI MANU

IDENTIFICATION OF PARACETAMOL THROUGH THE USE OF PHARMACOPIEA TEST

ABSTRACT

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Paracetamol is widely used (NHS Choice, 2012) for the relief of minor pain, toothache, headaches, symptoms of cold and reduces of patient’s temperature (control fever symptoms). It is classified as a mild analgesic agent.

The following procedures were used during the experiment of identification of paracetamol. TLC method is important for separation of mixture. This technique is commonly used to determine the presence of particular compound through comparison of Rf values of both unknown samples and the standard samples.

Melting point analysis is also useful for identification of compound. The melting point range can be indicated and recorded with the help of a thermometer. For instance, the melting point of paracetamol ranges from168 to172 degree Celsius

Infra-red spectroscopy is one of the most essentially useful methods for identification of compound. It is usually used to identify medicines that contain correct drug in most pharmaceutical industries. Structural information about the functional group of unknown compounds can be ascertained through the use of infra-red spectroscopy.

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Significantly, the results generated during this experiment attest the accuracy and importance of these methods for identification of compounds. For example, the Rf values of TLC method as well as infra-red spectroscopy analysis demonstrated the presence of paracetamol and cafeine in sample ‘B’ and ‘D’ respectively.

INTRODUCTION

Paracetamol is the best alternative choice for children and ulcer patients who have a minor pain such as headache and children. Consequently, too much it (NHS Choice 25/06/2012) can cause severe harm to the kidney and the liver.

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AIM OF THE EXPERIMENT

Identify paracetamol from various unknown samples through pharmacopeia test.

Hypothesis

The range of melting point of the samples that contain paracetamol would be (168 to 172) degree Celsius.

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Again, the samples that contain paracetamol only would turn into violet without changing to red after the experiment D.

The Rf values of unknown samples that contains paracetamol would be the same as the Rf value of the standard sample when compared.

Apparatus used for the experiment

Micro-spatula

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UV-light

Indicator

IR spectroscopy

Melting apparatus

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Pencil

Rule

Chromatography tank

TLC plate

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Thin capillary tube

Conical flask

Beaker

Micro-pipette

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Materials used

Ethyl acetate

Four unknown samples

Water

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Dichromate

METHODS

Melting point analysis

Melting point analysis was conducted for all the four unknown samples labelled A, B, C, and D. Small amount of crystals of each unknown samples was fetched into the melting point capillary tube. The capillary tube contained the sample was placed into the melting point apparatus. The samples temperature was measured with digital thermometer. Hence, both initial and final melting point of the samples was observed and recorded. This experiment was repeated twice to obtain the ranges of the melting point.

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INFRA-RED TECHNIQUE

During the experiment, the arm of IR spectroscopy was cleansed with (ethanol) alcohol. The background of IR spectroscopy was scanned. Hence, each sample was placed on the mouth of the IR spectroscopy and scanned. The wavelength detected the various bound in each compound. Copies of each compound scanned was printed out for observation and reading.

EXPERIMENT D FOR IDENTIFICATION TEST ANALYSIS

The experiment D was conducted for all the four unknown samples labelled A, B, C, and D. 0.1g of each unknown samples were measured with macro spatula and 1ml of concentrated hydrochloric acid was added to it. The solution was gently shake and heated to boil for about three minutes. 1ml of water was added to the boiling solution. After boiling, the solution was then placed in an ice bath to cool. Observation was made and there was no precipitation form. Therefore, 0.05m of 4.9/L solution of potassium dichromate was added to it and the colour developed for sample ‘B’ was violet without changing into red. However, the colour developed for sample ‘A’ was slightly red and changed to purpled whilst sample ‘C’ and ‘D’ developed yellow hint colour and diluted violet colour respectively.

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TLC METHOD

A solvent system of about 20ml of ammonia: methanol: chloroform (1:19:80) was placed into the chromatography tank. A filter paper was placed against the wall inside the chromatography tank. The tank lid was placed on to prevent the evaporation of the solvent. The tank was left for about twenty minutes to allow saturated atmosphere to be formed.

TLC method was conducted by using four unknown samples labelled A, B, C, D and ethyl acetate. During the experiment, a solution was made from each of the four unknown samples A, B, C, and D respectively. Thus, about 10mg of each sample was fetched with micro-spatula into the small beaker and dissolved with the small volume of ethyl acetate.

Moreover, TLC plate was prepared by measuring 1.5cm distance from the edge of the plate with a rule. A horizontal line was drawn and marked the intervals with a pencil. The distance in between each interval was about 1.5cm apart. The line was demarcated into six intervals for the four unknown samples as well as the standard samples, which comprises of paracetamol and caffeine solution.

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Each solution was fetched with the help of a micro-pipette and spotted on the TLC plate at different intervals. In addition, the standard sample solutions of paracetamol and caffeine were spotted on the same plate at different position. Thus, spot A, B, C, D, Par and Caff in that order. The TLC plate was placed into the chromatography tank and covered with the lid. The solvent then moved up gradually through capillary action. Hence, the solute spotted on the TLC plate moved up along with the solvent (thus, mobile phase). TLC plate was removed from tank when the solvent reached about 2cm distance to the edge and marked with a pencil.

Moreover, the plate was left to dry for about 20 minutes. After the evaporation of the solvent has taken place, TLC plate was then placed under the UV light for observation. A drawing was made with a pencil around the new spots formed on the plate. A measurement of the distance travelled by both solvent and substance were recorded. The Rf value was calculated for both unknown samples and the standard samples. Therefore, the Rf value was calculated base on the formula below.

Rf value = distance travelled by substance divided by the distance travelled by solvent. Finally, the Rf values of unknown samples were compared with Rf values of the standard samples.

The Rf value for paracetamol

Rf = 3.90/6.1

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Rf value = 0.639 = 0.64

RESULTS

(b).

Melting point analysis results

SAMPLES How Do You Meet Prof Standards? We stick to your rubric like glue—nailing the structure, depth, and tone your professor wants—then polish it with edits for that extra shine. Our writers know what profs look for, and we double-check every detail to make sure it’s submission-ready and grade-worthy.	A	B	C	D What’s Your Editing Like? Send us your draft and tell us your goals—we’ll refine it, tightening arguments and boosting clarity while keeping your unique voice intact. Our editors work fast, delivering pro-level results that make your paper pop, whether it’s a light touch-up or a deeper rework.
MELTING POINT RANGE	171- 175	171 – 172	200 – 206	159 Can You Pick My Topic? Yes—we’ve got your back! We’ll brainstorm fresh, workable ideas tailored to your assignment, picking ones that spark interest and fit the scope. You choose the winner, and we’ll turn it into a standout paper that’s all yours.

The sample ‘A’ is a bit higher than the normal range of the standard paracetamol sample. Equally, sample ‘B’ indicated the presence of paracetamol as the ranges 171-172 degree Celsius

(c). & (d). EXPERIMENT D FOR IDENTIFICATION ANALYSIS results

		SAMPLES
	A	B	C	D Do You Do Quick Revisions? Yep—need changes fast? We’ll jump on your paper and polish it up in hours, fixing whatever needs tweaking so it’s ready to submit with zero stress. Just let us know what’s off, and we’ll make it right, pronto.
Colour of solution	Slightly red and turned to purple	Violet	Yellowish hint	Dilute violet

Sample ‘A’ developed purple colour which shows para-aminophenol

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The colour achieved for sample ‘B’ was violet which show positive result and it was therefore indicated the presence of paracetamol. The colour developed for sample ‘C’ was yellow hint which indicated the presence of caffeine. However, sample ‘D’ developed diluted violet colour which shows the presence of caffeine and paracetamol.

Infra-red analysis results

Sample A 

Sample B

Bond	Functional group	Frequency / wave number absorption cm-1 Can You Add Data or Graphs? Absolutely—we’ll weave in sharp analysis or eye-catching visuals like stats and charts to level up your paper. Whether it’s crunching numbers or designing a graph, our writers make it professional and impactful, tailored to your topic.	Intensity
v N-H	amine	3319.12 stretch	strong
v C-H		2794.94 stretch	strong/medium
v O-H	Hydrogen bond in alcohol, phenol How Do You Manage Big Projects? We tackle each chunk with precision, keeping quality consistent and deadlines on track from start to finish. Whether it’s a dissertation or a multi-part essay, we stay in sync with you, delivering top-notch work every step of the way.	3109.51 stretch	Strong
v C=C		1650.71 Aromatic stretch	s Do You Follow Global Academic Rules? Yes—we’ve got it down! Our writers switch seamlessly between UK, US, Australian, or any other standards, matching your school’s exact expectations. Your paper will feel native to your system, polished and ready for wherever you’re studying.
v C=O		1609.82 amide stretch
N-H delta	amide	1562.66 amide bend What is a progressive delivery and how does it work? Progressive delivery is a cool option where we send your paper in chunks—perfect for big projects like theses or dissertations. You can even pay for it in installments. It’s just 10% extra on your order price, but the perks are worth it. You’ll stay in closer touch with your writer and can give feedback on each part before they move to the next. That way, you’re in the driver’s seat, making sure everything lines up with what you need. It saves time too—your writer can tweak things based on your notes without having to redo huge sections later.
v C=C	Aromatic stretch	1504.96 aromatic stretch

The functional group obtained on sample ‘B’ indicated the presence of paracetamol.

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Sample C

Sample D

(g). Results for TLC analysis

STANDARD SAMPLES	Paracetamol	Caffeine
Rf values from TLC analysis	0.64	0.89

SAMPLES	A	B	C	D
Rf values from TLC analysis	0.74	0.64	0.89	0.73

The Rf values calculated for TLC analysis indicated that sample B is paracetamol when compare with the standard samples. Thus, 0.64

Compound A, C, and D are less polar since they travelled faster and further in the mobile phase and they are more attracted to the mobile phase than compound B.

However, compound B is more polar and travel slowly in the mobile phase. It is most attracted to the stationary phase.

Discussion

The experiment D of sample ‘B’ clearly showed positive outcome and indicated the presence of paracetamol as violet colour was achieved. In addition, TLC analysis also indicated that sample ‘B’ was paracetamol when Rf value of unknown samples ‘compared to the standard samples. Therefore, this shows the accuracy and precision of the positive outcomes of the experiment. Equally, the ranges obtained from melting analysis for sample ‘B’ also confirmed the presence of paracetamol.

Experiment D of sample ‘A’ showed deep purple colour and the infra-red analysis confirmed that, it is para-aminophenol. Moreover, both experiment D, TLC method and infra-red analysis confirmed the presence of caffeine in sample ‘C’.

However, sample ‘D’ developed dilute violet colour TLC analysis which shows a mixture of (two compounds) paracetamol and caffeine. The infra-red analysis also confirmed that, sample ‘D’ was a mixture of two compounds.

Time

SUMMARY

REFERENCE

Barber, J., Rostron, C.,(2013). Pharmaceutical Chemistry

Hill, G., Holman, J,. (2011) Chemistry in Context. 6^th edition

NHS Choice, (25/06/2012). Available at: http://www.nhs.uk/Conditions/Painkillers-paracetamol/Pages/Introduction.aspx

APPENDICES

Mobile phase:

Rf value: retention factor for thin layer chromatography.

Stationary phase:

TLC: thin layer chromatography

UV light: ultraviolet light

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