CHEM 307 - Faculty



CHEM 307.001,002 Laboratory syllabus

Coppin State College. Department of Natural Sciences

Organic Chemistry I Fall Semester, Dr. Amah

LABORARORY SYLLABUS

A. Safety Goggles Required

Maryland State Law, College regulations, and Departments policy require that safety goggles must be worn at all times in the lab. This applies to you when you are in the lab even though you may not be working at the time. It is recognized that wearing safety goggles may be uncomfortable, but keep in mind that being blinded or having impaired vision for life is likely to be less enjoyable. Unlike many chemical reactions, eye damage is irreversible! Please cooperate. This safety goggle requirement is for your own good. You may be and excellent, safety laboratory worker, but a student near you may be a disaster in lab. Students not wearing safety goggles when required to do so may, at the option of the instructor, be dismissed from lab and allowed to make up the missed work. As a consequence, such students will not be able to hand in the laboratory report on that experiment and thus fail the course.

B. Laboratory Safety, Equipment and Waste Disposal

Safety in working in the laboratory, in working with chemicals and equipment, and in working with other students is of great importance. Please reach the following very carefully.

I. Laboratory Safety: Safety work in the laboratory is vitally important to you and others working in the laboratory. Read Zubrick, Chapter 1. We emphasize and enforce laboratory safety. Lab lectures will provide detailed instructions for the proper and safe methods of conducting experiments.

II. Laboratory Equipment: Commonly used laboratory equipment and apparatus are shown and their use described in the lab text. Read Zubrick, Chapters 4, and 6. You will use many of these items during the semester. When experimental procedures require the use of equipment that is unfamiliar to you, refer to these chapters.

III. Cleaning Glassware: Use care in handling glassware. Check each piece of glassware for chips or cracks before using it. If in doubt, ask your instructor. Heating or using cracked glassware is dangerous. Even though we not charge for glassware that is broken, we do ask your cooperation in handling it with respect and care.

IV. Hazardous Waste Disposal: We place great emphasis on the proper disposal of all the waste generated by students taking organic chemistry. One hood in the lab is devoted to the storage of containers in which various types of waste are to be placed. You will be instructed about the proper disposal of waste that results from experiments you perform and which waste container to use for disposal of waste. If in doubt, consult your instructor. Please do your part to minimize the pollution of our environment.

V. Safety Equipment and Emergency Exits: Become familiar with the location of safety equipment (fire extinguishers and safety shower) in the laboratory. Your instructor will show these to you and will instruct you about exits from lab and building in case of emergency.

C. Pre-Lab Exercises

Pre-lab Exercises are contained in the CHEM 307 Supplements. Due date are given in the Semester Calendar. Pre-lab exercises are due at the beginning of lab period. Late pre-lab exercises will receive a grade of “0”. You will find the answers to these exercises in one or more of the following: (a) assigned reading for experiment; (b) experimental procedure(s); (C) section J in this syllabus; and (D) “For Your Safety” section of those experiments contained in the CHEM 307 Supplements.

D. How to Prepare for Laboratory Work

Successful completion of the assigned lab work requires study and preparation before coming to lab. This is essential so that you can be well-organized in your work. Have well in mind what you are going to do before coming to lab. Plan ahead.! It will save you lot of time and permit you to complete the lab work on the allotted time. It will also have added benefit of your understanding WHAT you are doing and WHY you are doing it. Material must be prepared and written in your lab notebook before coming to lab and is discussed in Section E of this syllabus. Your notebook may be checked at any unannounced time to ensure that you have prepared it in advance.

E. Advance Preparation and Lab Notebook

You must keep a notebook in lab and must use it to recall your data and other pertinent facts relating to your work. Two different “types” of experiments are done in CHEM 307 laboratory this semester: Investigative, and Preparative. The following indicates what to write in your notebook before coming to lab. You should also have a Table of Contents at the front of the notebook that you keep up to date. The Sec. J in this lab syllabus indicates which experiments are Preparative and which are Investigative. All data must be written in your lab notebook and therefore will be on the data sheets you hand in (Section F) The same data must be written in your lab Reports(Section H). State each new experiment on a new notebook page.

a) Investigative Experiments

For each investigative experiment, write the following in your notebook BEFORE coming to lab.

1) Title of Experiment and References

2) Introduction-one or two sentences is sufficient

3) Experiment to be Performed-List, in statement form (one or two lines is adequate), for each experiment to be performed. Leave adequate space or room to record your data and results.

b) Preparative Experiments

The information shown in “Preparative Experiments, Part I” in CHEM 307 Supplements must be written in your laboratory notebook BEFORE you come to lab.

F. Materials to Be Handed in From Laboratory Notebook

At the conclusion of each experiment, hand in the carbon copy from the laboratory notebook for the work you have done for the entire experiment. Staple the sheets together. Use your notebook to record data, and keep it in a logical order so that you and your instructor can identify it.

G. Before Leaving Lab Each Period

When you are ready to leave lab, clean all glassware and make sure you have all equipment and glassware in the correct locker. Remember to put all clamps, clamp holders, and iron rings in the correct locker. Glassware that you use in lab must be cleaned at all times. Your instructor will inspect your area of work check and initial your notebook before you leave. Failure to have your notebook initialed and checked out before you leave will reduce the grade on the laboratory report for that experiment.

H. Laboratory Reports

( Laboratory reports for each experiment must be handed in. One or more missing laboratory reports will result your getting a grade of “F” in the course.

( Laboratory reports must contain the data that you have recorded in your notebook and therefore be on the data sheets you handed in at the completion of each experiment. Laboratory reports will penalized if they contain data that is different from or missing from the data sheets.

( Laboratory reports are to be written in a clear, concise, readable form in ink on 8-1/2 – 11” paper. Write on ONE SIDE of paper only! Typed or word processed reports are required. The reports should contain the data you recorded in your notebook, even though you have handed in the data sheets. Late reports will be penalized at least by 10 points. Be sure that your final reports include the material requested in Section J. Keep the reports brief and to the point; please do not rewrite the material given in the lab text or handouts. Before writing the reports, see the “Laboratory Report” discussion for each type of experiment: Investigative or Preparative.

a) Investigative Experiments

1) Title of Experiment and References

2) Introduction: several sentences are sufficient.

3) Conclusion/Comments: State what you learned from the experiment an how it relates to the theories and techniques of organic chemistry. List three(3) experimental problems, including reasons, that may have been encountered in the experiment.

b) Preparative Experiments

See “Preparative Experiment, Part II” in CHEM 307 Supplements for a sample for laboratory reports for preparative experiments.

I. Laboratory Grading

To pass the course, you must pass the lecture and laboratory portions of the course with a grade of D or better. All laboratory work will be assigned numerical grades, whose letter grades translation is: A = 90-100; B = 80-89; C = 70-79; D = 60-69. All laboratory experiment must be performed, and you must submit a written laboratory report on each experiment. Failure to hand in one or more laboratory reports will result in your getting an “F” in the course.

J. Experiments and Comments

These section contain the information about the experiments that you will perform this semester. Included are the reading assignments from the lab text and/or the lecture text. Experiments are designed as being “Preparative” or “Investigative” to allow you to determine the format for your notebook and the laboratory report for each experiment. Please read these comments carefully before preparing for an experiment and writing the laboratory report.

Label Compound: When handling in liquids or solids from any experiment, label your sample vials with the following information:

Your Name

CHEM 307, Sec. #, Instructor

Name of Content

Yield: weight in g

Bp or mp of content

Hand in Compounds: Unless directed otherwise, compounds must be handed in. Failure to do so will result in a 10-point penalty on the laboratory report.

a) Recrystallization: Read Zubrick Chapters 13, and 17.

Experiment:

You will be given an unknown solid to purify by recrystallization from water. The unknown will be either benzamide (mp 130-131 0C) or 2-ethoxybenzamide (mp 132-134 0C) containing water-soluble impurity and carbon.

1) Dissolve the Solid: Place a 250-mL Erlenmeyer flask containing about 60-70 mL of water. Weigh 1-2 g of the unknown organic sample and put it in the water while it is cold. Place the Erlenmeyer flask on a hot plate and allow the water to boil. Constantly stir the solution with a stirring rod until all the unknown solid dissolves. Record in your notebook the exact volume of water you added.

2) Filter the Insoluble Impurities: Using hot, gravity filtration, add about 5 mL of hot solvent to the funnel containing the filter paper; this preheats the funnel but is not a substitute for boiling the solvent in flask before doing the filtration.

3) Crystallize the Compound: Allow the flask to cool to room temperature, a process that may be hastened by first cooling in a beaker of cold tap water before placing it in an ice-water bath.

4) Isolate the Crystals: Collect the recrystallized solid on a Buchner funnel attached to the filtration flask that must be clamped. Connect the filter directly to the house vacuum line using a heavy-walled tubing provided(do not use condensed hose as it will collapse under vacuum).

5) Dry the Crystals: Place the top part of the Buchner funnel containing the solid in a beaker so it won’t fall over when you open your locker and store it in you locker of hood to dry. Do not cover the funnel or the beaker. During the next lab period, transfer the crystals from the funnel to a clean dry sample vial. Wash the vial with water and then with acetone, followed by drying on a laboratory dryer or oven before putting the sample in it. Determine the weight of pure sample solid in grams and percent recovery, which is defined as:

Percent recovery = weight of pure sample, g/weight of impure sample, g x 100.

Determine the mp of the solid and identify the unknown using the mixed mp technique, as described in part (b) below.

Melting Points: Read Zubrick, Chapter 12.

Experiment: Determine the melting points of:

a) Your recrystallized unknown

b) Your unknown mixed with benzamide (50:50)

(c) Your unknown mixed with 2-ethoxybenzamide (50:50)

Melting point will be determined using the MelTemp melting point apparatus which will be demonstrated in the laboratory. On the basis of this mixed melting data, identify your unknown.

1) Data sheets for both parts

Put the recrystallized sample in a properly labeled sample vial. Return any unused unknown to your instructor

2) Waste Disposal and Clean UP

Used capillary tubes-place in “used capillary tube” beaker on the bench. Place all used filter paper in the trash-can. Put all solutions in the sink.

3) Laboratory Report

This two-part investigative experiment is to be written up as a single laboratory report-see Section H(a). The report will receive a single grade that will be determined by the quality of the written report and to a lesser extent by the yield and purity of the recrystallized solid. As a guide, see “Laboratory Report on Recrystallization and Melting Point” in CHEM 307 Supplements.

3. DISTILLATION AND GAS CHROMATOGRAPHY

a) Distillation: Read Zubrick Chapters 13, 17, 18(heating mantle), 19, 20.

Experiment:

Do experiment in Zubrick, chapter 20”Class 3: Fractional” This experiment will be done in pairs. All equipment must be clean and dry. Each student must record the data in his/her laboratory notebook. Each student will perform fractional distillation on a 50-50 mixture of ethyl acetate and butyl acetate. Place a 35-mL sample of this mixture in a 100 mL round bottom flask containing several boiling chips. Use Rashing rings as the column packing. Place the thermometer so that the top of the mercury bulb is just slightly below the bottom of the sidearm of the distillation head. Collect three (3) 10-mL fractions in clean, dry large sample vials clamped just below the take off adapter. Calibrate each sample vial by placing 10-mL of water in another vial and marking the 10-mL level of the three clean dry vials with a marking pen. Label each vial to identify the fraction number A heating mantle will be used for heating. Start with the VARIAC set at 90, When you start to collect the 10-mL fractions increase the setting on the VARIAC to 125 for the remainder of the distillation. Record the distillation data in your notebook in a table with the following heading:

Fraction number bp range volume collected

Other observations: (1) Color of original mixture and color of each fraction must be recorded in your notebook. (2) At the completion of the distillation, turn off VARIAC , remove the heating mantle, and allow the apparatus to cool. Submit a sample of each fraction for gas chromatographic analysis-see part(b) bellow. The method of sample submission will be demonstrated. Tightly cap each of the original vials and place them ina beaker to keep them from tipping over. Keep them in your personal drawer until the gas chromatography results are returned to you.

Hand in: The data sheets from the distillation should be handed in.

Waste Disposal and Clean UP:

1) Pot residue-place in “organic waste” bottle in the hood after determining the volume remaining in the flask.

2) Column packing-place in the “used column packing” beaker in the hood.

3) Clean and put all glassware and equipment in proper locker. Clean and dry your work area.

b) Gas Chromatography: Read Zubrick Chapter 31.

Experiment

Cap each sample vial and shake each one to ensure complete mixing. Submit a sample of each fraction obtained by each pair of students for analysis using auto-injection gas chromatography.

Analysis of gas chromatography

The GC data you will get back contains the GC traces for each fraction and a copy of the GC of the standards. The standards are ethyl acetate and butyl acetate so that the peaks in the GC traces for the three fractions can be identified. The retention times are provided at the top of each peak and also in the data summary at the bottom of the sheet. If an area given as 100e2 this represents 100%.

Waste Disposal

1. After getting back the gas chromatographs, place the rest of each sample in “organic waste” container in the hood

2. Wash sample vials and place them in your personal drawer.

Laboratory Report

Write one report covering fractional distillation and gas chromatography as an investigative experiment-see Section H(a). For each pair of students performing fractional distillation, one set of GCs of the three fractions and of the standards will be provided. Each student must submit a report for this experiment and each report must contain the GC traces for the three fractions and the standards. One student may submit he original GC data and the other may submit photocopies of it. In addition to the normal report format (Name, course number, and section in the upper right hand corner, followed by Experiment Title and References in the Center and the Introduction in few sentences) use the following format for the rest of the report

Data: The data for fractional distillation and gas chromatography must be presented in a table, per the following example. Scientific data routinely presented in tables in the literature.

Fraction volume(mL) bp or bp range Ethyl acetate Ethyl acetate Butyl acetate Butyl acetate

Number Retention time % in fraction Retention time % in fraction

Questions

Answer the following question by number, following the table of data.

1. What is the purpose of fractionally distilling a mixture of two compounds whose boiling points are fairly close, as is the case of ethyl acetate and butyl acetate?

2. What is the purpose of performing chromatography on each fraction?

3. Ideally fraction 1 should contain what pure compound? Did it?

4. Ideally fraction 3 should have contained what pure substance? Did it?

5. Should fraction 2 contain only 1 compound? If not, what should it contain?

6. If fraction 1 and/or 3 were a mixture, what do you think may have caused it? What might you do experimentally to get pure compounds in fraction 1 and 3?

7. What effects would the following changes in the experimental procedure have on the separation of the mixture(improve it make it worse, have no effect?)

a) Increase the temperature (VARIAC setting) at the beginning of the distillation.

b) Use a fractional distillation column that was twice as long.

8. You start with 35 mL of a mixture of 25% ethyl acetate and 75%butyl acetate and collect 10 mL fractions. Assuming perfect separation, what compound(s) should be contained in (a) fraction a, (b) fraction 2 and (c) fraction 3?

9. Based on your data, what is the boiling point of ethyl acetate and butyl acetate?

Attach the gc traces of each fraction and of the standard at the end of the report.

3. PREPARATION OF CYCLOHEXENE (Preparative)

Read: “Preparation of Cyclohexene” in CHEM 307 Supplements; Zubrick Chapter 15, McMurry, see 17.7

Experiment: “Preparation of cyclohexene” in CHEM 307 Supplements. Run infrared soectrum of your cyclohexene product. The “IR Spectrum of cyclohexanol” is in the CHEM 307 Supplements.

Hand In: Data sheets. Properly labeled the product after running its IR spectrum. No product handed in -10 points from the final report.

Laboratory Report for Preparation of cyclohexene. See section H(b) in this lab syllabus and “Preparative Experiments” in the CHEM 307 Supplements. Include the mechanism for this reaction. In your Results and Conclusions, also analyze the IR that you ran on your product and that of cyclohexanol and hand both IR spectra in with the report.

4&5. Preparation of 1-Bromobutane and Infrared Spectroscopy

a) Preparation of 1-Bromobutane(Preparative)

Read: McMurry, Secs. 10.7, 11.16. Zubrick, Chapters 15, 18,19, 20, 22. “Preparation of 1-Bromobutane” in CHEM 307 Supplements. Omit mechanism.

Experiment: “Preparation of 1-Bromobutane” in CHEM 307 Supplements. Run infrared soectrum of your final product.

Hand In: Data sheets. Properly labeled the product after running its IR spectrum. No product handed in -10 points from the final report.

Laboratory Report for Preparation of cyclohexene. See section H(b) in this lab syllabus and “Preparative Experiments” Part II in the CHEM 307 Supplements. Omit the mechanism for the reaction.

b) Infrared Spectroscopy (Investigative)

Read: Zubrick Chapter 33. McMurry, Secs. 12.5-12.9

Experiment:

1. 1-Bromobutane Run infrared spectrum of your 1-bromobutane product from the experiment(a) above. The “IR Spectrum of 1–Butanol” is in the CHEM 307 Supplements

2. Unknown Obtain the IR spectrum of the unknown liquid provided you. On the basis of the IR spectrum, use the “List of Possible IR Unknowns” in CHEM 307 Supplements to determine the structure of the unknown.

Laboratory Report for Infrared Spectroscopy

See Section H(b) of this syllabus. Specific comments are provided here.

1. For the spectra of 1-butanol and your 1-bromobutane product, interpret each by marking key absorption peaks on each spectrum and write what causes each peak. Write a paragraph concerning the changes that were observed in the spectra of the starting material and the product, and state how the spectra showed that the reaction had in fact occurred.

2. For the Unknown, mark key absorption peaks directly on the spectrum and write what causes each peak. On the basis provide the structure of the unknown from the “List of Possible IR Unknowns” in the CHEM 307 Supplements. Start by identifying structural features and functional group(s) in the compound whose IR you have run. Each unknown will contain at least two structural features and/or functional groups. Mark directly on the key absorption peaks that provide information about structural features and functional group(s). Table 3.1 (pages 70-71) McMurry provides a table of the family names, examples and the structure of commonly encountered functional groups. Limit your consideration to the following. It may help you to write the functional group structure by each name using Table 3.1

Aliphatic groups(hydrogens attached to sp3 hybridized carbon atoms)

Aromatic ring( aromatic hydrogens and carbon-carbon bonds associated with ringsalcohol

Aldehyde

Ketones

Alkene( vinyl hydrogens and c=c stretching)

Alkynes (terminal hydrogen and c-c triple bond streching)

Amines ( 10, 20, and 30)

Carboxylic acid

Esters

Nitrile

Nitro

Amides( 10, 20, and 30)

As a hint, eliminate compounds on the list that you know your unknown can’t be; for example the absence of a peak due to –OH stretch allows you to eliminate alcohols, carboxylic acids, and phenols.

3. Attach the three IR spectra to your report.

6. MOLECULAR MODELS (Investigative)

Read: McMurry, Secs. 3.2, 3.3. Chapters 4 and 9.

Experiment: “Directions for Molecular Model Experiment” in CHEM 307 Supplements. This experiment will be “in lab” practical concerning stereochemistry of organic molecules. You may use any materials or books you desire and may discuss it with other students and your instructor.

Hand In: the answer sheet at the conclusion of the experiment.

7. Compound Identification; Infrared Spectroscopy (IR), Proton Magnetic Resonance Spectroscopy (PMR) and Mass Spectrometry (MS) (Investigative)

The lecture and laboratory will be devoted to: (a) discussion of IR; (b)discussion of MS; (c) discussion of PMR and (d) compound identification using IF, PMR and MS.

Reading and Study Problems

IR Spectroscopy: McMurry Secs. 12.5-12.8. “Spectra Data”, “Sample IR Spectra”, and “Structure Determination Problems Using IR Spectroscopy” in CHEM307 Supplements.

PMR Spectroscopy: McMurry : Secs. 13.1-13.3 and secs. 13.8-13.13. “Spectra Data”, “Sample PMR Spectra; Structure Determination Using IR, MS and PMR Data” and “Structure Determination Problems using IR and PMR Data” in CHEM 307 Supplements.

Mass Spectrometry: McMurry, Secs 12.1-12.4. “Sample Mass Spectra” in CHEM 307 Supplements. Answers to these problems: “Answers to Spectral Problems Sets” in CHEM 307 Supplements. Ignore any references to CMR and CMR problems.

a) Infrared Spectroscopy (IR)

The interpretation of IR spectra will be discussed for compounds containing all commonly encountered functional groups. This technique will be used (a) on the product obtained from dehydration of cyclohexanol, (b) to identify the IR unknown [Expt. 4(b) and (c) in the compound identification experiment (Expt. 6) described below.

b) Proton Magnetic Resonance (PMR)

The interpretation of PMR spectra will be discussed for compounds containing some commonly encountered functional groups. This technique will be used in the compound identification experiment, part (d) below.

c) Mass Spectrometry (MS)

The interpretation of mass spectra will be discussed to learn how it may be used to determine (1) the presence or absence of Cl or Br in a compound and (2) the molecular weight of the compound. This technique will be used in the compound identification experiment, part (d) below

d) Compound Identification (Investigative)

This experiment combines IR, MS, and PMR to deduce the structure of an unknown organic compound.

Experiment: You will be given a liquid unknown to identify using spectral methods. Run an IR spectrum of your unknown. Analyze your IR spectrum and identify important structural features by marking the appropriate peaks on the spectrum. The unknown will be drawn from he following families of compounds: alkanes and cycloalkanes, alkenes and cycloalkenes, alkynes, alcohols, alkylhalides and aromatic compounds(aryl halides and aromatic hydrocarbons) You will be provided a copy of the mass spectrum and of the PMR of youar unknown. Analyze the mass spectrum to determine the presence or absence of Br or Cl and to obtain the molecular weight of the compound. Use the PMR spectrum as much as possible to determine structural features of the unknown.

Complete and hand in the preliminary Report form that is attached to the MS and PMR spectra provided for your unknown. Follow the directions on the orm. Attached the IR, PMR and MS of your unknown. The corrected Preliminary Report will be returned to you along with the percent (%) composition by weight for the unknown.

Laboratory Report

Use the following format for this report. Please keep it brief and to the point. Please do NOT include any information that is not relevant.

Name, Date Lab Section (in the upper right corner)

1. Introduction

2. Calculate empirical formula from the % composition and determine the molecular formula from the empirical formula weight.

3. Interpret PMR spectrum. Your interpretation must account for the chemical shift(indicate which hydrogens are responsible for which peaks), the peak areas, and the splitting pattern. To calculate peak areas, see “PMR Peak Area Calculation” in CHEM 307 Supplements.

4. Identify the unknown (Name and structure).

5. At the end of the report, attach graded Preliminary Report and interpreted PMR, MS, and IR spectra.

K. Study Guide for Laboratory Exams

The following is provided as study guide for the laboratory examination as follows:

First Laboratory Exam: Parts 1-7 below (no spectroscopy)

Second Laboratory Exam: Parts 8-12 below

Review Pre-lab Exercises and Lab Reports

1. General Comments You are not expected to remember weights or volumes of various materials and reagents that you used in lab. The emphasis will be on your understanding of the principles, concepts, and techniques used in laboratory work.

2. Equipment and Apparatus You should be able to identify all of the lab equipment that were used in lab this semester. Review each equipment.

3. Laboratory Safety, Equipment and Waste Disposal Review the comments and reading assignments. See section B of this syllabus.

4. Recrystallization and Melting Point Understand the concept of melting points and effect of impurities on them Know the terms from the reading, as for example: mixed mp, eutetic points, etc. Understand the use of mixed mp and compound identificaion. For recrystallization, know: purpose, experimental steps, and rationale of allowing crystals to form and leave impurities behind.

5. Distillation Understand the concept of fractional distillation. Knw eqipment for fractional distillation. Know about azeotrope mixture.

6. Gas Chromatography Know the general principles of method: how and why it works. Know how to read and interpret GC chart—retention times, % composition, and use of standards to identify compounds.

7. Preparation of 1-Bromobutane Know names and strucutres of reactants. Know how to calculate limiting reagents, theoretical yield and percent yield. Understand the purification method and why various steps were done, use of drying agents, the apparatus that was used(including reflux and simple distilation). Review the discussion and experimental procedure in the handout.

8. Infrared Spectroscopy Understand the use of IR. Tablesof IR absorption values will be supplied for your use.

9. PMR Know how to interpret PMR spectra and be able to account for chemical shift, peak areas, and splitting patterns. Tables of PMR chemical shifts will be provided for your use.

10. MS Know how MS work and how to interpret MS spectra for the presence of Br and Cl: fragments whose masses are 2 mass units apart with abundance of (a) 3:1 indicate presence of Cl or (b) 1:1 indicate presence of Br. Know parent peaks , base peaks, and how to determine molecular weight.

11. PMR, IR, MS and Compound Identification Know how to derive empirical formula from percent composition by weight. Know how to derive molecular formula from empirical formula. Know how to combine spectral information (IR, MS, and PMR) to get the structure of an unknown compound.

12. Preparation of Cyclohexene Know how to determine limiting reagent and theoretical yield and % yield. Understand purification scheme and procedure. Why various steps were performed ,use of drying agents, etc. Know why fractional distillation apparatus was used for the dehydration reaction. Review the discussion and experimental procedure in the handout.

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