Lab 2- TLC
docx
keyboard_arrow_up
School
Northeastern University *
*We aren’t endorsed by this school
Course
2312
Subject
Chemistry
Date
Feb 20, 2024
Type
docx
Pages
5
Uploaded by AgentCrownHummingbird43
Experiment #2
Thin Layer Chromatography
Lab Partner – Teaching Assistant – Date Performed – October 5, 2023
Date Due - October 12, 2023
Experimental Objective
Thin layer chromatography (TLC) is performed in the first stage of the experiment to determine which solvent is best for separating aspirin, acetaminophen, and caffeine. Subsequently, the components of a combination are identified using TLC and the specified solvent.
Procedure
Setting up the TLC plates and determining the better solvent
One centimeter down from the TLC plate's bottom, a horizontal line was drawn. From this line, vertical lines were drawn to show the locations of the samples (aspirin, acetaminophen, and caffeine). After that, the samples were moved via the capillary tubes onto the TLC plate. The sample size was intended to be as small as a tiny dot because any larger or smaller would have distorted the findings. For comparison, two solvents were used: 1:1 Hexanes:Ethyl Acetate and 95% ethyl acetate with 5% acetic acid. The TLC jars received around 3 mL of solvent poured to them. Subsequently, the plates were inserted into their corresponding jars, with the upper part of each plate resting on the jar. The solvent was about 1 cm from the top when the plate was taken out. Where the solvent ceased was marked on the plate.
The spots on the TLC plate were visible using the short wave UV section. To find the Rf values, the spots were lightly drawn with a pencil. We compared the two plates to see which solvent would produce the best outcomes. Since the samples separated, 95% ethyl acetate and 5% acetic acid seemed to be the best solvent. Working unknown sample #247
In a test tube, about 28 mg of unknown #247 were dissolved in 1 milliliter of 95% ethanol. The unknown solution was made and spotted on a second TLC plate. A ruler was used to measure from the beginning line to the center of each sample dot after all of the plates had been produced.
The sample's Rf values were ascertained using the dots. To ascertain which compounds made up unknown #247, the values of the unknown and the known substances were compared.
Results
Figure 1:
Drawn depictions of all 3 TLC plates involved
The below equation was used to calculate the Rf values for all spots on all plates, given the dimensions and measurements of the observed plates which are pictured above. The measurements and calculated data are shown in the below tables.
Table 1:
Data from TLC plates in 1:1 Hexanes:Ethyl acetate
Your preview ends here
Eager to read complete document? Join bartleby learn and gain access to the full version
- Access to all documents
- Unlimited textbook solutions
- 24/7 expert homework help
Solvent distance (cm)
6.1
Caffeine spot (cm)
0.5
Caffeine Rf
0.082
Acetaminophen spot (cm)
1.2
Acetaminophen Rf
0.197
Aspirin spot (cm)
3.2
Aspirin spot Rf
0.525
Table 2:
Data from the TLC plate in 95:5 ethyl acetate:acetic acid
Solvent distance (cm)
6.1
Caffeine spot (cm)
1.3
Caffeine Rf
0.213
Acetaminophen spot (cm)
3.9
Acetaminophen Rf
0.639
Aspirin spot (cm)
4.9
Aspirin spot Rf
0.803
Table 3:
Data from TLC plate of unknown #247 in 95:5 ethyl acetate:acetic acid
Solvent distance (cm)
6.2
Spot #1 (cm)
4.9
Spot #1 Rf
0.790
Spot #2 (cm)
2.0
Spot #2 Rf
0.328
Conclusion
Most likely, a mistake in the capillary tube transfer process was the cause of the absence of movement in the last two samples. The reason the sample sizes didn't move with the solvent was probably because they
were too small. The 95:5 ethyl acetate:acetic acid solvent would have been the better solvent if these
mistakes hadn't happened because it is more polar and has a larger separation than the selected 1:1 hexanes: ethyl acetate. The Rf values obtained with the selected TLC solvent were similar to the compounds in the unidentified sample, mistakes notwithstanding. The unknown's values matched those of
the solvent's aspirin and caffeine. Consequently, it was found that unknown #247 contained both caffeine and aspirin.
Related Documents
Related Questions
Column Chromatography
Alumina
Chromatography Mixture
9:1 Hexanes:Ether
8:2 Hexanes:Ether
1:1 Hexanes:Acetone
Amount Used
3.962 g
0.143 g
9.50 mL
9.50 mL
11.00 mL
Additional Observations (Color, etc.)
BIU X₂ X² →
BI IU X₂ X² →
BI IU X₂ X² →
BI IU X₂ X² →
BIU X₂ X² →
arrow_forward
Use a suitable model to explain how separation and identification of a mixture of organic compounds can be achieved with a thin layer chromatographic (TLC) technique.
arrow_forward
anch of the following components cannot be detected by gas chromatography?
4 Essential oils
Alcohols
b) Volatile compounds
d) Non-volatile compounds
13-
is measured as time elapsed from the point of injection to the peak maximum?
a)-Column efficiency d)- Delectability
c)-Retention time
14- Which of the following can be used to detect the components in gas chromatography
a) non-volatile compounds b) volatile compounds
c) Salts
d) b&c
15-Which of the following methods is often referred to as mechanical separation processes.
a)-Gas Chromatography b)-column chromatography c)- Sedimentation
16- For obtaining better resolution in TLC.
and then developed with a second solvent at right angles to the first
a) Stepwise b) Descending e) Ascending
17- This is defined as transport of electrically charged particles in a direct-current electric field
a) ion exchange chromatography b) Electrophoresis c) ultracentrifuge
d) exclusion
18-This figure indicates to schematic Diagram of
a) Gas chromatography…
arrow_forward
19. What is thin layer chromatography (TLC) LEAST
useful for from the list below?
A) To determine if crystallization or distillation may be
more effective for a separation
B) To determine the number of components in a mixture
C) To determine the appropriate solvent for column-
chromatographic separation
D) To monitor the progress of an organic synthesis
reaction
14. The solubility of salicylic acid in water is 7.8g/100ml
at 100°C and 0.25g/100ml at 25°. Estimate how much
water is needed to recrystallize a 19g sample of
salicylic acid?
A) 150ml B) 250ml
C) 300ml D) 400ml
arrow_forward
A young researcher set out to develop a method for quantifying the polycyclic aromatic hydrocarbon (PAH) content in a
contaminated soil sample using open tubular gas chromatography. During the initial stages of method development, the
researcher was unable to separate the early eluting compounds, anthracene and naphthalene, with baseline resolution.
Select the possible modifications the researcher could make to improve the resolution.
use a column with a smaller inner diameter
decrease the column length
increase the stationary phase thickness
increase the temperature
choose a different stationary phase
arrow_forward
Look up the boiling point for each of the following compounds then determine
the order that they will elute from the column. Use this elution order to
identify the compound in each of the 6 standard chromatograms. Once you
have identified the compound in each chromatogram, record its retention
time.
Compound Structure
Compound
Name
Elution Order (1-6)
Non polar → Polar
Boiling
Retention Time
(From Chromatograms)
Point
Propyl
acetate
H
H.
H.
Butyl
acetate
H.
H.
H
H.
H
H.
H.
H.
Methanol
H
O-
Ethanol
2-butanone
H H
H.
H.
4-methyl-2-
pentanone
H.
H.
HH
H.
arrow_forward
Three students did a chromatography experiment, where Rf = distance of solute / distance of solvent.
What could be the possible errors why student 3 had results that are quite far from that of students A and B?
arrow_forward
use the following chromatogram and table as your data.
What is the %composition of the Vitamin A peak in the sample?
78.43%
77.73%
7.867%
72.74%
arrow_forward
Q1: The following are relative peak areas for chromatograms of standard solutions of methyl
vinyl ketone (MVK)
MVK concentration
mmol/L
0.5
Relative peak area
3.76
1.5
9.16
2.5
15.03
3.5
20.42
4.5
25.33
5.5
31.97
A sample containing MVK yielded relative peak area of 21.3. Calculate the concentration of
MVK in the sample.(use excel)
arrow_forward
1a) Hexane, CH3(CH2)4CH3, is found to have a long retention time when separated from a mixture. A column with a C18 (18-carbon chain) stationary phase and a methanol-water modal phase is used for the separation. Explain why hexane has a long retention time.
1b)You wish to chromatographically seperate a mixtureof the follwing compunds. Which of the two compounds will be most difficult to seperatate from one another? Why?
arrow_forward
The uses of thin layer chromatography are:
1) To identify unknown compounds
2) Determine purity of products
3) Analyze reaction mixtures
4) To waste time in lab
5) Determine the melting point of the product
U 6) Put an astronaut on the moon.
arrow_forward
SEE MORE QUESTIONS
Recommended textbooks for you
![Text book image](https://www.bartleby.com/isbn_cover_images/9781305446021/9781305446021_smallCoverImage.jpg)
EBK A SMALL SCALE APPROACH TO ORGANIC L
Chemistry
ISBN:9781305446021
Author:Lampman
Publisher:CENGAGE LEARNING - CONSIGNMENT
Related Questions
- Column Chromatography Alumina Chromatography Mixture 9:1 Hexanes:Ether 8:2 Hexanes:Ether 1:1 Hexanes:Acetone Amount Used 3.962 g 0.143 g 9.50 mL 9.50 mL 11.00 mL Additional Observations (Color, etc.) BIU X₂ X² → BI IU X₂ X² → BI IU X₂ X² → BI IU X₂ X² → BIU X₂ X² →arrow_forwardUse a suitable model to explain how separation and identification of a mixture of organic compounds can be achieved with a thin layer chromatographic (TLC) technique.arrow_forwardanch of the following components cannot be detected by gas chromatography? 4 Essential oils Alcohols b) Volatile compounds d) Non-volatile compounds 13- is measured as time elapsed from the point of injection to the peak maximum? a)-Column efficiency d)- Delectability c)-Retention time 14- Which of the following can be used to detect the components in gas chromatography a) non-volatile compounds b) volatile compounds c) Salts d) b&c 15-Which of the following methods is often referred to as mechanical separation processes. a)-Gas Chromatography b)-column chromatography c)- Sedimentation 16- For obtaining better resolution in TLC. and then developed with a second solvent at right angles to the first a) Stepwise b) Descending e) Ascending 17- This is defined as transport of electrically charged particles in a direct-current electric field a) ion exchange chromatography b) Electrophoresis c) ultracentrifuge d) exclusion 18-This figure indicates to schematic Diagram of a) Gas chromatography…arrow_forward
- 19. What is thin layer chromatography (TLC) LEAST useful for from the list below? A) To determine if crystallization or distillation may be more effective for a separation B) To determine the number of components in a mixture C) To determine the appropriate solvent for column- chromatographic separation D) To monitor the progress of an organic synthesis reaction 14. The solubility of salicylic acid in water is 7.8g/100ml at 100°C and 0.25g/100ml at 25°. Estimate how much water is needed to recrystallize a 19g sample of salicylic acid? A) 150ml B) 250ml C) 300ml D) 400mlarrow_forwardA young researcher set out to develop a method for quantifying the polycyclic aromatic hydrocarbon (PAH) content in a contaminated soil sample using open tubular gas chromatography. During the initial stages of method development, the researcher was unable to separate the early eluting compounds, anthracene and naphthalene, with baseline resolution. Select the possible modifications the researcher could make to improve the resolution. use a column with a smaller inner diameter decrease the column length increase the stationary phase thickness increase the temperature choose a different stationary phasearrow_forwardLook up the boiling point for each of the following compounds then determine the order that they will elute from the column. Use this elution order to identify the compound in each of the 6 standard chromatograms. Once you have identified the compound in each chromatogram, record its retention time. Compound Structure Compound Name Elution Order (1-6) Non polar → Polar Boiling Retention Time (From Chromatograms) Point Propyl acetate H H. H. Butyl acetate H. H. H H. H H. H. H. Methanol H O- Ethanol 2-butanone H H H. H. 4-methyl-2- pentanone H. H. HH H.arrow_forward
- Three students did a chromatography experiment, where Rf = distance of solute / distance of solvent. What could be the possible errors why student 3 had results that are quite far from that of students A and B?arrow_forwarduse the following chromatogram and table as your data. What is the %composition of the Vitamin A peak in the sample? 78.43% 77.73% 7.867% 72.74%arrow_forwardQ1: The following are relative peak areas for chromatograms of standard solutions of methyl vinyl ketone (MVK) MVK concentration mmol/L 0.5 Relative peak area 3.76 1.5 9.16 2.5 15.03 3.5 20.42 4.5 25.33 5.5 31.97 A sample containing MVK yielded relative peak area of 21.3. Calculate the concentration of MVK in the sample.(use excel)arrow_forward
- 1a) Hexane, CH3(CH2)4CH3, is found to have a long retention time when separated from a mixture. A column with a C18 (18-carbon chain) stationary phase and a methanol-water modal phase is used for the separation. Explain why hexane has a long retention time. 1b)You wish to chromatographically seperate a mixtureof the follwing compunds. Which of the two compounds will be most difficult to seperatate from one another? Why?arrow_forwardThe uses of thin layer chromatography are: 1) To identify unknown compounds 2) Determine purity of products 3) Analyze reaction mixtures 4) To waste time in lab 5) Determine the melting point of the product U 6) Put an astronaut on the moon.arrow_forward
arrow_back_ios
arrow_forward_ios
Recommended textbooks for you
- EBK A SMALL SCALE APPROACH TO ORGANIC LChemistryISBN:9781305446021Author:LampmanPublisher:CENGAGE LEARNING - CONSIGNMENT
![Text book image](https://www.bartleby.com/isbn_cover_images/9781305446021/9781305446021_smallCoverImage.jpg)
EBK A SMALL SCALE APPROACH TO ORGANIC L
Chemistry
ISBN:9781305446021
Author:Lampman
Publisher:CENGAGE LEARNING - CONSIGNMENT