Lab 2: IR Identification of Analgesics By: Alice Story

Purpose: To use Infared Spectroscopy to determine the functional groups of samples 2 and 7.
Introduction: Infared Spectroscopy is a forensic technique used to analyze organic compounds . Infared radiation identifies compounds when infared light strikes an object. The spectrum starts where the red region of visible light ends.
Materials and Methods: An unknown saturated solution of samples 2 and 7 were prepared. On one side of the IR cards one sample was placed on to the card. The card was placed into the spectroscopy on the side that did not contain any sample (background). Then the card was placed on the side containg sample 2 (repeated for sample 7) and the spectroscopy created a graph to later determine the functional groups.
Results: The readings from the spectroscopy graph identified the unknown samples 2 and 7. Sample 2 contained Aspirin and Tylenol PM. Sample 7 was Aspirin.
Discussion: The spectroscopy identified the unknown samples 2 and 7 by identifying specific functional groups. The determination of the specific functional groups determine the substance(s) in each sample.

Lab 2: IR Identification of Analgesics by Brittani Summers

Purpose: To identify drugs using Infrared Spectroscopy

Introduction: Infrared Spectrometers use radiation to identify certain substances. The radiation from the light strikes the substance and the spectrometer shows waves. The peaks from the waves show the different types of chemical bonds formed in the substance.

Materials:

• IR Cards
• IR Spectrometer
• Samples 2 & 5

Procedure:

1. Side A of one IR card was placed into the Spectrometer and served as the background/control of the experiment.
2. Side B of one of the IR Cards was placed into the Spectrometer containing Sample 2.
3. Side B of the other IR Card was placed into the Spectrometer containing Sample 5.
4. The graph of the the transmittance of the two substances was then printed.
5. Later on, the drugs within the substance was then discovered by the peaks of the waves transmitted through the Spectrometer. The use of table titled "Characteristic Infrared Absorption Frequencies" was used to discover the bonds featured in the structures of the possible drugs in the mixture.

Results/Discussion/Conclusion:

Sample 2 contained each of the following:

1750 absorbance: C=O ester

1300 absorbance: C--O alcohols, ethers, and esters

2900 absorbance: O--H acids

Sample 2 contained Aspirin as well as Tylenol

Sample 5 contained each of the following:

3300 absorbance: N--H amines

2900 absorbance: O--H acids

1300 absorbance: C--O alcohols, ethers, esters

Sample 5 contained Tylenol and Ibuprofen

Lab 2: IR Identification of Analgesics by Carla Scott

Objective: To use Infrared Spectroscopy to determine the purity of specific samples of analagesics and prescription drugs.

Introduction:
Infrared Spectroscopy is a tool commonly used in identifying chemical compounds by. This technique is used most often in forensic laboratories to determine whether analgesic or prescription drugs were used in criminal investigations.

Materials: Saturated solutions, IR Cards, and Spectroscometer

Procedures:
Saturated solutions 1 drop of sample 4 & 6 was placed on the film of IR cards and placed in the Spectrometer and read.

Results/Data: Based on the readings from the Infrared Spectroscometer the following findings were found:

Sample 4 was determined to be Ibuprofen

Sample 6 was determined to be Tylenol

Discusssion & Conclusion:

This laboratory experiment's goal was to use Infrared Spectroscopy to determine which analgesics were present. I found that my samples contained Ibuprofen (sample 4) and Tylenol (sample 6) which are both over-the-counter drugs.

By Carla Scott

Lab 2: IR Identification of Analgesics by Serina Lewis

Purpose: To proceed with the drug purification experiment using Infrared Spectroscopy

Introduction: The Fourier Transform Infrared Spectrophotometer is used by forensic labs to identify drugs and organic poisons in powders, urine and tablets. The instrument measures the frequencies at which a group of atoms in a sample rotates and vibrates in a molecule. IR spectroscopy, most often used in criminalistics, is used to determine what is present. Two regions of interest when measuring the absorption of infrared radiation are the functional group region and the fingerprint region. The functional group region shows the absorption patterns for each of the functional groups present. The fingerprint region shows a pattern of each molecule's absorption bands and is formed when the atoms in the molecule are vibrating. These regions contribute to the difficult mathematical procedure used to get the data that forms the IR spectroscopy chart.

Materials: Samples 4 and 7 (1% saturated solution), pipette, IR cards, and IR spectrophotometer

Procedures: A drop from a pipette of each sample were placed on separate IR cards. Then, the IR cards were left to dry. Once the sample on the IR card dried, the IR card was placed into the spectrophotometer and the spectrum was obtained.

Results

Chart 1, below, sample IR spectra for sample 4

Chart 2, below, sample IR spectra for sample 7

Sample 4- absorption of 3000-2500 cm

Sample 7-absorption of 1725-1705 cm

Discussion/Conclusion: The IR spectra chart was compared with the characteristic infrared absorption frequencies chart given from the instructor. It was concluded that Sample 4 is ibuprofen and Sample 7 is aspirin.

-Serina Lewis

Lab 1: Identification of Analgesics using Thin Layer Chromatography by Carla Scott

Objective: To identify the purity of analgesics/prescription drugs using TLC.

Introduction:

The purpose of this laboratory experiment was to identify the purity of certain analgesic products and/or prescription drugs. This technique is commonly used during Crime Scene Investigations to examine and verify the presence of drugs that may have played a role in the crime. Crime scene investigators often use tests similar to this to determine whether an analgesic or prescription drug was used in foul play. In this particular experimental protocol 7 samples of analgesics were used along with thin layer chromatography plates to determine the presence and purity of the samples. A UV lamp was later used to verify their presence.

Materials: Samples 4 & 6 (1 % solution) ethyl acetate and acetic acid were used as solvents. Iodine and and UV lamp were used to identify spots placed by capillary tube. TLC plates made up of Si, were cut into 25 x 5 cm plates (using a ruler) and placed inside a beaker with a watch glass on top.

Procedure: Using a pencil, a line was drawn about 1 cm from the bottom portion of the chromatorgraphy plate. A capillary tube was then used to place spots on the TLC plate above the line previously drawn. Next, the plate was place in a beaker containing ethly acetate or acetic acid (dependent upon the trial) and a piece of filter paper and covered witha watch glass Once the TLC plate was placed into the beaker the solvent vapors completely saturated the plate it was removed and placed on a piece of wax paper to dry. After the plate dried it was placed under a UV lamp and observed. The plate was then placed into a beaker containing iodine.

Results/Data: Figure 1. TLC of Samples 4 & 6

Our results are indicated as follows:

In Figure 1, sample 4 had an R/f value of 0.60

In Figure 1, sample 6 had an R/f value of 0.61

Discussion & Conclusion:

In this experiment the goal was to use Thin Layer Chromatography to determine the presence of analgesic materials and how pure it is. The Rf value calculated from sample 4 it is determined that the substance was pure. The Rf value calculated for sample 6 was 0.61. This value concludes that the substance in this sample was pure as well.

By: Carla Scott

Lab 1: Identification of Analgesics using TLC by Alice Story

Purpose: To identify the purity of analgesics/ prescription drugs using TLC.

Introduction: Drug identification is determined by TLC, which is a analytical technique used to analyze the purity of chemical compounds.

Materials and Method: An unknown sample labeled number 2 and 7 (1% solution) was prepared in ethyl acetate and acetic acid . Iodine and a UV lamp were used to identify the spots of the samples. The TLC plates were made of Si and cut into 25x5 cm plates. The plates were placed inside a beaker containing filter paper and a watch glass was placed on top.

Procedure: A 1cm line was drawn at one end of the TLC plate and at the other end a 1in line was drawn. Above the 1cm line a capillary tube was used to spot the sample on to the plate. Once the sample was applied, the plate was placed into the beaker until the solvent reached the 1in line. The plate was removed from the beaker and placed on to a Kimwipe to dry. When the plate dried the samples 2 and 7 were viewed using a UV lamp and/or iodine.

Results: The Rf values were determine from figure 1. The Rf value for sample 2 was 0.50 and sample 7 value was 0.53.

Figure 1. TLC Samples 2 and 7

Discussion: This experiment allowed the determination of purity of samples 2 and 7. The results determined that sample 2 spotting resulted in a streak. Sample 2 streaking was due to an overload or many components ran together creating a streak. Sample 7 resulted in a pure substance since there was no abnormality to the spot.

By: Alice Story

Lab 1: Identification of Analgesics by Kaneshia Newell

Objective: To learn the structure and properties of organic molecules.

Introduction: In Crime Scene Investigations, delicate instruments such as an ultraviolet lamp and TLC plates are used to analyze the the purity of chemical compounds: drugs and organic poisons. In this lab course, we used these instruments to determine the purity of analegesics found in traditional phramacies.

Materials and Methods: We weighed 1 mg of Sample 3 and Sample 6 into a valve and mixed it with ethyl acetate and acetic acid. We drew a line 1 cm from the bottom of the verticle TLC plate with a pencil. Using a capillary tube, placed a few spots on the the TLC plate. Place a filter paper in a 400 mL beaker with the solvent. Once the TLC plate dries, placed it in the solvent of ethanol and acetic acid until the product diffuses 1 inch from the top. Observe data and record results using the UV lamp for detailed observations. To make results more visible, we used iodide in a beaker as seen in Figure 1.1.

Results and Discussion: Performing a TLC analysis of the unknown analgesics, the number of components that were observed were 3 out of 3 in Sample 3 and 3 out of 3 in Sample 6. The results in Sample 3 were more faint compared to the results in Sample 6 as seen in Figure 1.2.

The R(f) value was 0.55 cm in each sample.

Conclusion: The purpose of this procedure was to learn how to determine the purity of traditional drugs similar to the methods that the CSI use when determining the purity of poisons and illegal drugs since many chemical compound are similar. In Sample 6, the spots are in a linear pattern as they were when the experiement began. Therefore, the drug in Sample 6 is pure. Because of the amount of uncertainiy in Sample 3 (due to lack of a higher magnification), the assumption is that this drug was also pure. The observations were faint but the trace up the TLC plate was not. Within this experiment, we learned the how to determine the purity of a substance using instruments that the CSI use.

by: Kanieshia N.

Lab 1: Identification of Analgesics by Serina Lewis

Purpose: To learn why drug purification is important and how to purify drugs.

Introduction: This experiment will provide a positive identification of a drug and possibly will determine how much the drug is present. Thin-layer chromatography (TLC) is a sensitive, fast, simple, and inexpensive analytical technique used in carrying out organic experiments, and also widely used in crime labs. TLC is used by criminalist for drug identification to determine the number of components in a mixture, to determine the identity of two substances, to monitor the progress of the reaction, and to determine the degree of purity.

Materials and Methods: Sample 4 and 7 (1%solution), ethyl acetate and acetic acid were the solvents in the experiment.Iodine & a UV lamp were used to identify the spots. TLC plates, made of silica, were cut into 25 x 5 cm plates (used a ruler) , and a beaker with a watch glass on top.

Procedure: A 1 cm line was drawn from the bottom of the TLC plate using a pencil and a ruler. A capillary tube was used to spot the sample onto the TLC plate at the 1 cm line. The TLC plate and filter paper was placed in a beaker that contained ethyl acetate or ethyl acetate and acetic acid and then covered with a watch glass. Once placed into the beaker, the TLC plate became saturated with the solvent vapors. The wet TLC plate was removed from the beaker after the solvent and allowed to dry on a Kim wipe. In order to view the spots, the dried TLC plate was viewed by a UV lamp then placed into a beaker with iodine.

Results

The results indicated as follows:

Figure 1, on the right, the TLC plate with sample 4 and 7

Sample 4 had an Rf value of 0.45

Sample 7 had an Rf value of 0.53

Discussion/Conclusion: Based on the results, sample 4 is purified, while sample 7 is not.

-Serina Lewis

Biology Class of 2011

Lab 1 Identification of Analgesics Using TLC by: Brittani Summers

Purpose: To perform thin layer chromatography (TLC) analysis of unknown analgesics and determine: 1) the number of components in a mixture; 2) identify substances using Rf values; 3) determine the purity of the unknown analgesics

Introduction: This experiment will show the presence of certain drugs in a crime scene. The purity of the drugs is identified through the use of Thin Layer Chromatography by showing the possible presence of other substances in the mixture.

Materials:

• Unknown Sample 2 (1 % solution) prepared in ethanol, ethyl acetate and acetic acid



• Unknown Sample 5 (1 % solution) prepared in ethanol, ethyl acetate and acetic acid



• Iodine



• UV lamp



• TLC Plates



• Beaker with watch glass



• Ruler



• Calculator

Procedure:

1. A line was drawn 1 centimeter from the bottome of the TLC plate



2. A capillary tube was used to spot the TLC plate at the 1 centimeter line.



3. The TLC plate was then placed inside the beaker containing ethyl acetate and acetic acid and covered with a watch glass.



4. The mixture of ethyl acetate and acetic acid then began to absorb through the TLC plate. The TLC plate were then removed once the solvent reached approximately 1 inch from the top of the TLC plate.



5. The wet TLC plates were then left to dry.



6. The dried TLC plates were then observed under the UV lamp.



7. The plates were then placed in a beaker with solid iodine and the vapors from the iodine left more distinct marks on the TLC plates.



8. The TLC plates were then viewed again under the UV lamp and marks were made where the solution stopped flowing on the TLC plate.



9. With the ruler, measurements of where the solvent stopped and where the substance stopped were taken note of in centimeters.



10. The Rf values were then calculated by dividing the distance the substance traveled by the distance the solvent traveled.
    
    

• Rf= distance substance traveled/ distance solvent traveled

Results/Discussion/Conclusion:

Substance 2 had a Rf value of .613 Figures 1: Samples 2 & 5

Substance 5 had a Rf value of .565

The TLC plates showed several different spots in one line. Because there were several different spots in one line, it comes to a conclusion that the substance is not pure. Both substances 2 and 5 revealed several different spots so the conclusion was made that these two substances were not pure, therefore being mixed with something else.

Figure 2: Samples 2 & 5

Lecture One: The Role of Organic Chemistry in Crime Scence Investigations

Objective: To learn why drug purification is important and how to purify drugs using thin layer chromatography (TLC).

Welcome to the Spelman CSI Minicourse Blog

This is a blog created by Dr. Juana Mendenhall for MBRS RISE Spelman mini-course. The objective of this blog is to create an online course and lab notebook for the summer students enrolled in this course. We will use this blog to post class lecture topics, asks questions, and post lab experiment results.