PRAKTIKUM KIMIA ORGANIK

GENERAL RULES AND PRACTICES

By: Dr. Deana Wahyuningrum

GENERAL INFORMATION

GENERAL RULES: TASKS AND OBLIGATIONS OF STUDENTS

1ST WEEK

Experiment-01: THE SEPARATION AND PURIFICATION OF LIQUID MATERIALS: Distillation and Boiling Points

Experiment-02: THE SEPARATION AND PURIFICATION OF SOLID MATERIALS: Recrystallization and Melting Points

2ND WEEKExperiment -03: EXTRACTION: The Isolation of Caffeine

from Tea and Tests for Alkaloid Identification

3RD WEEKExperiment–04: COLUMN CHROMATOGRAPHY AND THIN

LAYER CHROMATOGRAPHY: The Isolation of Curcumin from Turmeric (Kunyit, Curcuma longa)

4TH WEEK

Experiment-05: ALCOHOL AND PHENOL: Properties and Chemical Reactions

Experiment-06: ALDEHYDE AND KETONE: Properties and Chemical Reactions

5TH WEEK Experiment-07: ESTERIFICATION OF PHENOL: The Synthesis of Aspirin

6TH WEEK

Experiment-08: THE ISOLATION OF ETHYL-p-METHOXYCINNAMATE FROM KENCUR (Kaempferia galanga L.) AND THE SYNTHESIS OF p-METHOXYCINNAMIC ACID

Several things you have to remember and understand:

Generally, organic chemistry reactions proceed slowly, how to speed up the reactions?

In order to gain more products and to have a more completed reaction, usually require more reactants used, how would the excess of reactants affect the products? And how to eliminate the remaining excess of reactants from products?

Every reaction require certain conditions, such as temperature, that would determine the completion of reaction, how do those conditions could be achieved?

There are some specific technic used in organic laboratory works, such as extractions, distillation, chromatography, etc., those technics should be well performed during the works, how do those technics could be mastered skillfully?

Understand and aware how to deal with the danger and hazard while working in the place where many toxic, flammable and unstable reagents stored.

You have to keep working in tidiness, calmness, careful and you should ready to learn more from every experience you had during laboratory works using the theory that you have been learnt from class.

IMPORTANT THINGS YOU HAVE TO KEEP IN MIND:

No additional laboratory works! If you absence at one of the laboratory sessions, then there won’t be any replacements of laboratory sessions. If you got sick, then you have to submit the doctor or your parents notification letter to your laboratory supervisor in charge as soon as possible.

It is forbidden to eat, drink, smoking, chattering during the works in laboratory

Laboratory is a place to do the experiments according to the procedures explained by the laboratory works supervisor

YOU HAVE TO REPLACE THE BROKEN OR MISSING APPARATUS/EQUIPMENTS AS SOON AS POSSIBLE. IF YOU DO NOT REPLACE THEM ON THE DUE DATE THAT HAVE BEEN DETERMINED, THEN YOUR MARK WILL BECOME T OR E.

SAFETY PROCEDURES

Awareness - CommunicationBE FAMILIAR with the locations and

operation of safety and emergency facilities such as fire extinguishers, first aid kits, spill kits, emergency wash facilities, fire alarm pull stations, telephones, and emergency exits.

BE ALERT to unsafe conditions.PROMPTLY REPORT unsafe conditions and

accidents to your supervisor.

SAFETY PROCEDURES Personal Protective Equipment - Proper Attire

Wear clothing appropriate for the level of hazard. Lab coats (knee-length) and proper footwear are required for work involving chemicals, biohazards or radioisotopes. Gloves and safety glasses or safety goggles must be worn as required by the work being performed.

NEVER WEAR CONTACT LENSES when working with hazardous chemicals, unless wearing safety goggles.

Open and/or high-heeled shoes must NEVER be worn in laboratories. Long hair must be tied back or otherwise restrained when working

with chemicals, biohazards, open flames or moving machinery. Leave behind protective equipment (lab coats, gloves, etc.) when

leaving the work area, except when going directly from one laboratory to another.

Wash hands and arms with soap and water before leaving the work area.

SAFETY PROCEDURES

SAFETY PROCEDURES Conducting Experiments

NEVER perform unauthorized work, preparations or experiments. Consider safety issues BEFORE beginning work. Refer to Material Safety

Data Sheets (MSDS) prior to using a product. Check all equipment for damage prior to setting up experimental

apparatus. Select a suitable location. Experiments involving hazardous materials

should be done in a vented fume hood. ADVISE assistants or supervisors of experiments in progress. DO NOT leaves an experiment unattended if it represents a potentially

hazardous situation. If necessary, POST SUITABLE WARNING SIGNS if hazardous situation is

present and left unattended. Include your name and the extension where you can be reached. Perform a safety check at the end of each experiment. Make sure that gas,

water, electricity, vacuum lines, air and heaters have been turned off unless required.

SAFETY PROCEDURES Proper Handling of Hazardous Materials

Work with materials only when you know their flammability, reactivity, toxicity, and the emergency procedures associated with these materials. Refer to MSDS.

Transport hazardous chemicals (eg. solvents) and chemical waste in approved bottle carriers or on special waste cart, if available.

NEVER pipette by mouth. Clean up spills immediately if trained and able to do so. NEVER taste anything in the lab, never eat anything in the lab, and always wash your

hands when you leave the lab for the day. Always turn the fume hoods on when you are working in the lab. If you are carrying

out an operation in which vapors (other than those of water or ethyl alcohol) will be released into the air, do it under a hood.

If you spill a volatile material wipe it up with paper towels and deposit the towels in a fume hood, not in a wastebasket.

If you get a chemical on you, wash it off immediately with lots of water (and soap, if it is not readily water-soluble), EXCEPT IRRITANT/CORROSIVE CHEMICALS SUCH AS: CONCENTRATED H2SO4, PHENOL, BROMINE (IN ONE OF THESE CASES: DO NOT WASH WITH WATER!!!).

DO NOT WORK WITH ETHER (Diethyl ether) UNLESS THE WORKPLACE IS FREE FROM ANY FLAMES OR FIRE!!

SAFETY PROCEDURES INJURIES

If you are injured in the laboratory, inform your instructor or supervisor. If the injury is not trivial, seek medical attention. If you are ambulatory and otherwise feel OK, get someone to accompany you to the infirmary. If you do not feel well, get someone to call Public Safety Emergency.

BE PREPARED Know the location of the fire extinguishers, showers, fire blanket

and eye wash facilities. Read and understand the experimental procedure before you

arrive in lab. If you don’t understand, ask. Executing each step of the procedure without being aware of what could or should happen next, or being unaware of what you should do next, is likely to cause poor results and perhaps an accident.

SAFETY PROCEDURES SPECIFIC RULES: All students have to enter the laboratory on time (at 1 AM for afternoon session). All students have to wear laboratory coat before enter the laboratory. All students have to sign the admitance form directly while entering the laboratory. Report and submit the results, either data or products resulted from experiments,

that have been assesed by assistants. All apparatus or equipments that has been used should be returned or kept in

place in clean and dry condition. The laborans will check the properness and numbers of apparatus and equipments used by students.

The experiments have to be terminated before 5 AM (for afternoon session). All students have to check:

Whether all the apparatus or equipments borrowed have been returned to the stockroom? Whether the laboratory desk and floor have been cleaned? Whether the laboratory journal has been signed by assistants? Whether the gas and water faucets have been closed tightly? Wheter the electricity sources have been plug out?

If everything have been checked well, then all of students may leave the laboratory.

INDIVIDUAL ASSIGNMENTS OF STUDENTS

DO NOT FORGET TO PREPARE: The laboratory journal or laboratory workbook:

The book should be coverd y coloured wrapping paper (same colour per group)

The student’s identities must be written on the front cover of laboratory journal (name, NIM, group, no.laboratory desk or locker.

Pre-Lab Assignments have to be submitted at each laboratory session. This assignments have to be handwritten. Do not forget to write your name, NIM and group.

and bring the following equipments that might be needed during the laboratory works: stationary, matches or lighter, handkerchief, napkin, tissue, scissors, cutter.

THE LABORATORY JOURNAL OR WORKBOOK

The title and number of experiment The aims or objectives of experiment Short description of theory or basic concepts of each experiments. This

description should not more than 200 words. Physical and chemical properties data of each reagent used in experiments.

Students have to search the data from handbook, textbook or internet. List the reagents and equipments needed in experiment (draw the equipments

setup if needed). Experiment flowchart to help student understand each step of procedures well. The table of procedures and results, which contain short descriptions of

procedures and results. The calculation section List of references used

EXPERIMENT FLOWCHART

TABLE OF PROCEDURES AND RESULTS

LABORATORY WORKS REPORT The report should be written well and readable on A4 HVS paper. The report consists of the similar lists as laboratory journal with some

additional notes: - More comphrehensive theory - Discussion - Conclusion

Discussion and the truthfulness of data is the most being valued in report grading, therefore you have to be more focus in writing the discussion.

You have to submit the report on the next laboratory session. Do not be late, otherwise your report will not be graded.

The data form that has been signed by laboratory assistant have to be submitted directly at the end of each of your laboratory session.

SOME GENERAL BASIC PRACTICES

Setting up distillation apparatus. Performing Recrystallization. Performing Extraction. Preparing column chromatography. Setting up reflux (continuous reaction)

apparatus.

SELAMAT BEKERJA!!