Safety in an Organic Lab

1
 THE CHEMISTRY LABORATORY
INCLUDES HAZARDS AND RISKS.
This presentation summarizes some of the
safety rules for an organic laboratory. If some of
the material is unfamiliar, or you did not take
general chemistry at the College of Charleston,
you should review the information in the
attached link: General Chemistry Lab Safety

2
 1. PPE
Personal Protective Equipment: What must be worn when you work in
the laboratory.

Eye Protection

Lab Coat

Long Pants

Closed Toed Shoes – no exposed skin around feet

Lab gloves – when required

3
 Eye Protection
• Contact lenses are OK as long as glasses/goggles are worn
• Prescription glasses – you must wear goggles over them
• Safety goggles are provided in organic labs in UV irradiating
cabinets
• Eye wash stations are present in all labs

4
 Clothing and Foot Protection
• Clothing must cover all exposed
skin including legs/ankles
• Stockings or leggings do not
provide good coverage
• Sandals, flip-flops, Crocs, open-

toe and open-top (i.e. ballet flat)
shoes and canvas shoes (i.e.
Toms) are not appropriate.
These are not going to protect
your feet if you drop a piece of

glass with a liquid chemical
reagent in it.

5
Result of Improper Footwear in a Laboratory

Northwestern University, Evanston, IL July 2003

Your instructor will send you home to change if you do not

have appropriate shoes or other required PPE.
6
 Hand Protection: Chemically resistant Lab
Gloves

✓
• Wear gloves of a material known to be resistant to
permeation by the substances in use – nitrile is good for most
of our laboratory classes.
• Inspect each glove for small holes or tears before use.
• When you spill on your glove or tear it, change it
immediately. Throw gloves away any time you take them 7off.
 Karen Wetterhahn 
(October 16, 1948 – June 8, 1997)

Dartmouth College

The latex gloves she was wearing were

not resistant to methyl mercury – it
passed through the glove, through her
skin, entered her blood system and
resulted in her death weeks after the
exposure. 8
 Use of Gloves
Remove gloves before handling objects such as
doorknobs, telephones, pens, computer keyboards,
pH meter or other electronic buttons, or phones
while in lab. It might be convenient to have one
gloved hand and one ungloved hand to do
procedures where these kinds of things are used.
• Throw away gloves anytime you take them off.
• You should expect to use several pairs of gloves in
any given lab period.
• Glove video
9
 2.
Safety Equipment in the Lab
Eyewash and Safety Shower:
Know where these are in your lab.

10
 Eyewash / Safety Shower
The eyewash The safety shower is
is on the left. on the right. Pull the
Pull the handle and water will
handle and a start spraying from the
fountain of shower head on the
water will ceiling. There’s no
appear that drain in the floor – we
you can use only do this in
to bathe your emergencies, because
eyes. a flood of water will
have to be cleaned up.

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Eye Wash

12
Safety Shower

13
 3.
Chemical Fume Hoods: You must do your experiment in the hood if any of
your reagents are flammable, have harmful fumes or present a splash or
explosion hazard. This means pretty much at all times for organic chemists.

14
 Using the Fume Hoods properly
This
window/bar
is called
the sash.

If this is not saying NORMAL, then the hood

is not protecting you. Keeping the sash
and sliding panels in proper position keeps this
NORMAL, otherwise the alarm goes off.
If the alarm goes off, you need to reposition The sash should never be raised above
things to the correct positions, then press the the green “operation” level when you
“mute” button to reset the controller. are working in the hood. 15
 Closed, not in use In use, side-to-side panel
used as shield

✓ ✓
In use, sash (window) raised Don’t open side shields
to less than 18 inches to make one big window.

✓ × 16
• When using a laboratory hood, Check that the airflow is
in the normal range on the digital display
• Turn on the hood light
• Set the equipment and chemicals back at least 6 inches.
• Never lean in and/or put your head in the hood when
you are working. This is worse than doing the
experiment with no hood at all.
• It’s a good idea to put liquid reagent containers in trays
to catch all spills and drips

17
 4.
Know the risks of the chemical reagents you are
working with

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Labels are important

Even if it seems obvious.

In the chemistry lab, nothing is ever obvious.
19
NFPA Diamond

20
 MSDS (SDS)
• Provides procedures for handling or working with
that substance in a safe manner
• Includes physical data:
melting point, boiling point, flash point, etc.
• Includes safety data: incompatibilities, toxicity,
health effects, reactivity, storage, disposal:
protective equipment & spill-handling procedures
first aid

21
 How to find an MSDS
• There are on-line repositories of MSDS that can be searched
by the following methods:
• Common Name
• IUPAC (International Union of Pure and Applied Chemistry)
Name
• C.A.S. NUMBER – (Chemical Abstracts Service) a number
assigned to all commercialized chemicals available in the US
• The easiest to use is the CAS number, as it is a unique
identifier that isn’t subject to spelling errors
• MSDS for each experiment are posted on OAKS

22
 Incompatible materials
• Certain chemicals should not be stored and
cannot be safely mixed with certain other
chemicals due to severe reaction exotherm or
uncontrolled production of a toxic product.
Every lab has a
legible matrix that
lists the general
classes of
materials that
should not be
mixed together: 23
 Texas City Disaster of 1947
• Incompatible oxidizer and fuel source mixed
• Worst industrial accident in American history
• Freighter full of ammonium nitrate and fuel oil
(ANFO) exploded, igniting other ships
• 581 dead, entire city devastated

Ship anchor thrown

across city by
24
explosion
 Introductory toxicology
• AN MSDS contains valuable information on
the health dangers of the chemicals but often
use concepts and acronyms that are new to
students:
ID
RA C LH
RC AS

0
L NIOSH

LC5
PE #

nd
OSHA Righ

0a
TLV t to K
A

n ow

LD5
TW

acts
PR

STEL
O

Mutagenicity vs. TOSCA

P
65

teratogenicity

You need to know what is what to read an MSDS 25

 Regulatory agencies and standards
• Over the last 40 years the US and state governments and various international bodies have
developed regulations and standards that try to improve safety and industrial hygiene standards
including the following:
• EPA: Environmental Protection Agency, who have the primary responsibility to ensure chemicals
are used and disposed of in an environmentally sensitive manner
• TOSCA: the Toxic Substances Control Act of 1976 regulates which chemicals may be produced or
imported in the US
• OSHA: Occupational Safety and Health Administration is the US agency that assures safe and
healthful working conditions by setting and enforcing standards
• NIOSH: National Institute for Occupational Safety and Health is responsible for researching the
prevention of work-related injury and illness, and providing guidance to OSHA
• RCRA: the resource conservation and recovery act of 1976 that sets the standards for chemical
waste disposal in this country and overseesthe “superfund law” CERCLA
• California Proposition 65: The state of California passed a very rigorous law to protect drinking
and ground water from toxic chemicals. It is increasingly the standard for companies when
evaluating chemical safety

All of these regulations have been developed to make the use

and handling of chemical safer, so their impact on lab safety
has been profound 26
 Acute and chronic toxicology
• Acute toxin: rapid absorption of the substance and the
exposure is sudden and severe. Normally, a single large
exposure is involved.
– Examples are carbon monoxide, hydrofluoric acid, hydrogen
cyanide and nicotine
• Chronic toxin: prolonged or repeated exposures of a duration
measured in days, months or years. Symptoms may not be
immediately apparent.
– Examples of chemicals of high chronic toxicity include
dimethylmercury, nickel carbonyl, benzo-a-pyrene, N-
nitrosodiethylamine, and other human carcinogens or substances
with high carcinogenic potency in animals

27
 Carcinogens, mutagens and teratogens
• One of the most significant chronic risks associated with chemicals is
their potential to cause cell mutation and proliferation.
– Carcinogen: chemicals that can increase the incidence of cancer in the body
– Mutagen: chemicals that cause mutations in DNA that lead to hereditary
genetic defects in a fetus
• There are two other general classifications that you should be aware
of:
– Teratogen: chemicals that induce non-hereditary malformations of a fetus
– Sensitizer: chemicals that no reaction in a person during initial exposures,
but further exposures will cause an allergic response to the chemical

28
 Routes of Entry and Allowable Exposure Limits

• There are four main routes by which hazardous chemicals enter the
body:
– Inhalation: Absorption through the respiratory tract. Most important in terms of severity.
– Skin absorption.
– Ingestion: Absorption through the digestive tract. Can occur through eating or smoking
with contaminated hands or in contaminated work areas.
– Injection. Can occur by accidental needle stick or puncture of skin with a sharp object.

• Most exposure standards, Threshold Limit Values (TLVs) and Permissible Exposure
Limits(PELs), are based on the inhalation route of exposure. expressed in terms of either
parts per million (ppm) or milligrams per cubic meter (mg/m3) concentration in air.
• Other measures of chemical exposure:
• Lethal dose or concentration for 50% of the exposed population (LD50 or LC50)
expressed in mg contaminant per kg of body weight
• Short term exposure limit (STEL or TLV-STEL) is the amount of a substance you can
be exposed to for 15 minutes four times a day

29
 5.
Fire Safety

30
 Fire Alarms –
know the location of one close to your lab

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Fire Extinguishers – we have several in the
labs and in the hallways.

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33
 Types of Fire Extinguishers

This is a special
fire extinguisher
for combustible
metal fires. It is a
type D fire
extinguisher. You
won’t need to
use this unless
you work in a
research lab with
combustible
metals.

Most of our fire extinguishers are ABC.

It contains a dry powder to put out the
kinds of fires we might encounter in the 34
chemistry labs where we have class.
• http://www.youtube.com/watch?v=HCVRZuup
cFw

35
 Student Reaction in a Fire
Although we want you to be informed on the operation of a fire
extinguisher, we do not expect you to use it. If a fire is ignited in
your area, the proper STUDENT response is to:

1) Notify everyone in the room

2) If possible shutdown any reaction in progress by removing
heat/energy source and/or pulling plug on power cord
3) Proceed to the nearest exit and pull the nearest fire alarm
4) Evacuate the building
5) Assemble in front of the library or in the YWCA parking lot for
a positive headcount

36
 Flammables, combustibles, and potentially
explosive materials
• There are different ways of designating that a chemical is a fire risk:
• Flashpoint - minimum temperature at which a liquid gives off a
vapor in sufficient concentration to ignite in the presence of an
ignition source
• Combustible liquid - Any liquid having a flashpoint at or above 37.8
oC (100 F) but below 93.3 oC (200 F)

• Flammable liquid - any liquid having a flashpoint below 37.8 oC

• Autoignition temperature - the lowest temperature at which it will
spontaneously ignite in a normal atmosphere without an external
source of ignition, such as a flame or spark
• Explosive - A chemical that causes a sudden, almost instantaneous
release of pressure, gas, and heat temperature.

37
 Synthesis of explosive material
• In organic lab we often do reactions to add functional groups to benzene
rings. A simple reaction is shown below:
2 equiv. HONO2, H2SO4 NO2
70 oC, 1 hour

NO2

• If a student overcharged the amount nitric acid and overheats the reaction
the following chemical is isolated:

O2N NO2
Trinitrotoluene
If this is not handled carefully
there are serious
NO2 repercussions:

• Another risk is the formation of Peroxides – Explosives that can be

generated in lab when organic ethers are heated for a prolonged period in
the presence of air. 38
 Working with flames
• Never leave experiments unattended unless you take
special precautions to avoid accidents and you notify the
responsible individuals.
• Flames are never allowed when flammable gases or
liquids are in use.
• Always alert others before lighting a flame.
• Never leave a flame unattended under any circumstances.
• Turn off the natural gas at the valve when you are finished
with your work Closed valve is
Perpendicular to hose
• In the organic lab, Bunsen burners are rarely used to
either (1) to pull TLC spotting tubes; or (2) to conduct
flame or combustion tests.

39
 UCLA Lab Fire: December 29, 2008
Sheri Sangji was using this plastic syringe
to transfer tert-butyllithium. This was not
the correct procedure, because this
compound is well-known to ignite if it is
comes in contact with air. The syringe
plunger dropped out of the syringe and
the reagent ignited. Sheri died January 16,
2009 of severe burns. She was wearing
nitrile gloves but no lab coat. The students
assisting her did not remember to put her
under the safety shower.

40
 Lessons from UCLA accident
Lessons: Know the proper procedures for
transferring dangerous reagents. Wear your lab
coat at all times in the lab. Know where safety
shower and other emergency equipment is –
you may need to be the one who needs to be
ready to act when your lab mate is unable to
help himself/herself.

41
 7.
Disposal Procedures

42
 Broken Glassware
• Always check your glassware and discard any
with chips, breaks, or obvious flaws.
• Throw away broken glassware into special
glass waste containers, NOT the trash. YES

NO

43
 Waste Disposal
• Waste containers are provided for chemical waste
generated in laboratories
• Some things can go down the sink, some can’t.
Always check with your instructor.
• Care must be used to avoid mixing incompatible
chemicals such as
– Acids with Bases
– Oxidizers and Flammables
– Water reactive and aqueous solutions
– Cyanides and acids

44
 University of Maryland
September 26, 2011
• Students were conducting an experiment
with nitric acid and sulfuric acid was
added into a chemical waste container,
causing a violent chemical reaction
sparked a small fire in and near the
laboratory chemical ventilation hood.
• Two female students were injured as a
result
• Sustained first- and second-degree
chemical burns and superficial cuts.
45
 Handling Waste in Organic Labs
• Organic liquids like CH2Cl2 (aka methylene chloride, dichloromethane) &
acetone, & TBME & liquid reagents PUT IN ORGANIC (HALOGENATED)
LIQUID WASTE CONTAINER IN WASTE HOOD
• Aqueous – neutral (not basic or acidic) containing trace organics PUT IN
AQUEOUS WASTE CONTAINER IN WASTE HOOD
• Aqueous – neutral (not basic or acidic) containing NONTOXIC salts with
no trace organics CAN GO IN PUBLIC SEWAR, DOWN THE DRAIN (Use the
“Would I want to swim it rule?”. Yes? Then put it down the drain. NO?
Then put it in the aqueous waste container.)
• Solid chemical – old products, left over starting materials, includes
organic and inorganic PUT IN SOLID WASTE CONTAINER IN WASTE HOOD
• Solid, non toxic waste (paper towels, notebook pages) PUT IN TRASH
ONLY IF SAFE TO TOUCH WITH BARE HANDS

46
 Think First, Dispose Second
 PAPER, WITHOUT
CHEMICAL RESIDUE X PAPER, WITHOUT CHEMICAL
X CLEAN BROKEN GLASS RESIDUE
X CLEAN BROKEN GLASS
X CHEMICAL WASTE
X PAPER, WITHOUT CHEMICAL  CHEMICAL WASTE
RESIDUE
 CLEAN BROKEN GLASS

X CHEMICAL WASTE

47
 8.
How to be a good lab citizen

48
SEVEN must-have habits for lab-work

1. Be prepared before walking into the lab.

2. Think about the how and why before doing anything.
3. Begin with a clean, neat work area; make it so.
4. Minimize clutter; store book bags, equipment, etc.
5. Have instructions, pen and notebook available.
6. Return materials and equipment to proper places.
7. Make it clean and neat and orderly before leaving.

49
 Keep your lab area clean.

× eyewash/shower
station.
×
Don’t block the floor
in front of the Don’t leave cords
dangling because
someone will trip

×
over them.

Throw away used

paper towels and
used gloves,
immediately.
the floor because
someone will trip
over it. ×
Don’t leave things in

50
 Don’t put anything on your face or in your
mouth while you’re in lab.
• Take care not to ingest anything in the
laboratory!
• Food, gum, beverages, candy, and tobacco
products are never allowed in the laboratory.
• Don’t apply makeup, chap-stick, lotion, or
anything to your face or hands during lab. Wash
your hands with soap then leave the lab before
touching your face or other exposed skin.

× 51
Stay aware of what’s happening around you while
you’re working in the lab.

• Don’t use any distracting electronic devices

while in laboratory. If you touch your phone
during lab, you’re contaminating it with
whatever chemicals you’ve been working with.
• Do not wear earbuds in the lab. You need to be
able to hear important announcements,
especially in an emergency or when a safety
concern is addressed.

× 52
 Chemical storage

• Flammables/combustibles
• Acids
• Bases
• Oxidizers
• Nonreactive (e.g., brine)

53
 Mineral Acids – inorganic acids
Mineral Acids can be stored together except for Nitric Acid, which
must be stored by itself because it is also strong oxidizer.
Strong Mineral Acids Weak Mineral Acids
• Hydrochloric Acid • Phosphoric Acid
• Hydrobromic Acid • Boric Acid
• Hydroiodic Acid • Hydrofluoric Acid
• Nitric Acid
• Perchloric Acid
• Sulfuric Acid

54
 Organic Acids
• Organic Acids can be stored together, but they
must be stored separately from both mineral
acids and nitric acid.

55
 Storing Acids and Bases
• Mineral Acids can be stored in the same cabinet
as Bases, as long as they are physically isolated
from each other.
• If your lab contains some of each of these
categories of acids, you should have the following
separate cabinets:
1. Mineral Acids + Bases
2. Organic Acids
3. Nitric Acid (Strong Oxidizer)
56
The color of the bottle cap has a meaning.
Cap color corresponds to
concentrated solution of:
• Red: Nitric Acid
• Blue: Hydrochloric Acid
• Yellow: Sulfuric Acid
• Brown: Acetic Acid
• White: Phosphoric Acid

Also one base:

• Green: Ammonium Hydroxide

57
 Acid bottles (+ ammonium hydroxide)

• If you prepare an aqueous solution and store it in a

glass or plastic bottle, you shouldn’t use one of these
cap colors. Instead, try to use clear, black, orange, or
purple caps.

58
 Nitric Acid
• If nitric acid is mixed with a flammable organic
compound, such as acetic acid, the heat from the
oxidation and neutralization reactions is enough to
ignite the flammable material.
• Nitric acid also slowly destroys its red plastic bottle
cap. Always replace with a new red cap.
• Nitric acid may turn yellow over time because of the
release of nitrogen dioxide on exposure to light. The
yellow color does not affect the product’s usefulness
in the school laboratory.
59
 Sulfuric Acid
• Concentrated sulfuric acid is a strong
dehydrating agent. Because of its strong ability
to remove water, it reacts violently with many
organic materials such as sugar, wood, and
paper.
• If sulfuric acid has turned brown, it has
probably been contaminated with an organic
material and its purity should be in question.

60
 Hydrochloric Acid
• Concentrated hydrochloric acid fumes continuously
and cannot be stored without releasing hydrochloric
acid vapor. These fumes are responsible for most of
the corrosion damage in your chemical storeroom.
Storing hydrochloric acid in a wood or plastic-lined
acid cabinet is a must. Hydrochloric acid fumes will
quickly corrode metal cabinets.
• Hydrochloric acid fumes mixed with ammonia fumes
will react to form ammonium chloride clouds and
possibly toxic chloramines. Open containers of these
two reagents should not be in the same hood.
61
 Chemical Spills
• Notify your instructor and your neighbors if
you spill chemicals on the floor or bench.
• Don’t try to clean it up yourself. Your
instructor may need to use a specially
designed chemical spill kit.

http://www.youtube.com/watch?v=Dtp9vT15qIs

62
 Texas Tech January 7, 2010
• Conducting research funded by the U.S. Department of
Homeland Security on energetic / explosive compounds
• Attempting to produce 100 times more of an explosive
compound than the informal lab limit (100mg)

Lesson:
Follow instructions
in the lab.

63
 8.
Procedures and Practices

64
 Students must report any injuries,
big or small.

• Report all injuries to the instructor. We will

not call emergency services unless the
instructor determines it is a serious injury.
• An incident report will be filled out whether it
is small or serious.

65
 Injury procedure, continued

• First Aid kits are available in the lab with band

aids and other items for treating small cuts
and burns.
• If it is a serious injury, your instructor will call
campus emergency services, 843-953-5611.
Our campus officers will work with the
instructor and/or injured student to determine
whether or not 911 EMS should be called in.

66
 Process safety
When performing an experiment always consider the
following:
– Is the material flammable, explosive, corrosive, or reactive?
– Is the material toxic, and if so, how exposure to the material occur
– What kind of personal protective equipment or ventilation is needed to
protect myself?
– Will the process generate other toxic compounds, or could it result in a
fire, explosion, etc.?
– Are storage facilities appropriate for the type of materials used? Can
incompatible materials be properly segregated?
– What possible accidents can occur and what steps can be taken to
minimize the likelihood and impact of an accident?
– What are the proper procedures for disposal of the chemical(s)?
• As an example of process safety consider distillation:
67
What I Don’t Know Can’t Hurt Me
At a school far, far away; at a time long, long ago; there was an organic student performing a

reaction that required heat. So the student, happily and cheerfully set about to heat the

solution. The procedure stressed the need to prevent loss of material due to boiling off of

solvent during the heating process. The student did not read over all the details carefully, but

she did think to cap the top of the apparatus to prevent the solvent from boiling off. Pleased

with herself for having remembered that little detail, she was shocked and mad when her

instructor saw what she had done and asked her, in a rather loud and obnoxious voice: “What

the heck are you doing?” Look at the picture when it pops up and see if you can identify what

it was that had the instructor so upset. When the student was told by the instructor what the

problem was, her response was (this is a true story): “Well I do not think that matters, what I

don’t know can’t hurt me.” Trust us, you do not want to be that student.

68
The “Apparatus”
If Heated,
What
Would
Happen?
HINT: PV = n RT

69
 Distillation Do’s
• Have apparatus inspected by instructor before using it
• Have apparatus elevated off bench top so heat can be
removed quickly if needed
• Have a clamp around neck of flask so if heat source is
removed, apparatus is still supported
• Make sure water flow goes uphill, and cooling water
ends up going unimpeded down a drain.
• Perform inside hood, behind safety shield, with shield
between your face and the apparatus.

70
 Distillation Don’ts
• Heat a closed system
• Plug in heating mantel directly into outlet
• Use a Bunsen burner as the heat source
• Set up apparatus at awkward angles
• Leave glassware unsupported by clamps
• Let distillate come in contact with hot surfaces
• Have gaps or leaks between joints in glassware

71
 Open System v. Closed System
Always make sure there
is pathway for gases to
go in order to get out
of a container BEFORE
starting any chemical
reaction unless using
specialized equipment
designed to withstand
large pressure
NO, A BOMB LIKE THIS
increases. YES
CAN AND WILL HURT YOU

72
 OSHA FACT SHEET
Laboratory Safety Chemical Hygiene Plan (CHP)

OSHA’s Occupational Exposure to Hazardous Chemicals in

Laboratories standard (29 CFR 1910.1450), referred to as the
Laboratory standard, specifies the mandatory requirements of a
Chemical Hygiene Plan (CHP) to protect laboratory workers
from harm due to hazardous chemicals. The CHP is a written
program stating the policies, procedures and responsibilities
that protect workers (at CofC “workers” includes faculty,
students and staff) from the health hazards associated with the
hazardous chemicals used in that particular workplace.
73
 CofC - CHP
Who wrote the CofC CHP?
• Director of Environmental Health & Safety
(with input from faculty & staff)
Where can you find the CofC CHP?
• In the lab
• On the lab web site or OAKS page
• On Departmental Web Site

74
 GHS
• Now that you’ve had an overview of the various
factors that will help you be safe in a lab, we need to
introduce the next generation proposals:
• GHS: the Global Harmonization System
• GHS is being incorporated by OSHA into the Hazards
Communication Standard (HAZCOM) that ensures
people who handle chemicals are properly trained
• New symbols for labels with universal usage are
being developed:

75
GHS Symbols
Once again, the number to call in an emergency is:

843-953-5611
Please take a moment now to program
this number into your cell phone.

77
 Report any concerns
• If you have any safety concerns about the lab you
are working in or the people working around you,
you can contact:
– Your lab instructor
– Dr. Wendy Cory – Head of the departmental safety
committee
– Dr. Pamela Riggs-Gelasco – Department Chair for
Chemistry and Biochemistry
– Dr. Jim Deavor, Associate Dean of the School of Science
and Mathematics.

78