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Standard Operating Procedure for the

Set-up and Use of Cold Traps


Created by: Mitch Rock, Sept. 2015

OVERVIEW
The purpose of a cold trap is to condense vapors created during solvent evaporation. If not properly captured
these vapors are released into the lab air, exposing workers to possible health risks. Solvents can also be very
damaging to vacuum pumps if not captured using a cold trap. This standard operating procedure describes how
to set up a cold trap, and possible safety risks involved.
SAFETY
Personal protective equipment (PPE) required

Symbols from International Organization of Standards (ISO 3864-2) (http://www.safetysign.com/iso-mandatory-symbol-labels)


Eye and face protection – Face shield AND safety goggles
 Setting up a cold trap usually involves using a moderate amount (~500mL) solvent (e.g. isopropanol) and
cooling agents (dry ice). A face shield is needed because there is a possibility that the solvent may splash
up while setting up the condenser.
 Safety goggles are needed to protect the eyes from vapors released from solvents. Safety glasses are
not recommended because they still allow vapors to contact the eye.
Hand protection
 Gloves must be worn when handling chemicals. Please consult the glove chemical compatibility guide on
the group website and make sure to select the appropriate gloves for the chemicals you will be using.
 Do not handle try ice with bare hands. Use tongs, insulating gloves, or a folded piece of cloth.
Body Protection
 A lab coat must always be worn when handling chemicals.
 Close-toed shoes that cover the top of the foot are required when in the lab.
 Long pants are required when in the lab.
Emergency Protocols
Immediate danger
 If something happens and you think you, others, or the building is in immediate danger do not hesitate
to call 911 and activate the building alarm while evacuating the building.
Chemical spills
 Minor spills
o Must meet the following requirements to be cleaned up by lab worker (from EH&S):
 Chemical is known; can be cleaned in ≤10 to15 minutes
 Employees are trained to clean up spills
 Same PPE can be worn as in normal work activity
 Clean-up supplies available (Spill Kit)
 Major spills
o Evacuate the area and call 911 for further instruction
Emergency Contact Information
Dr. Michael Kessler – Principal Investigator Mitch Rock – Lab Manager
Office: 509-335-8654 Cell: 509-332-9963 Cell: 515-520-1660
michaelr.kessler@wsu.edu darman.rock@wsu.edu

PROCEDURE
Equipment commonly used

A B

C D

A) Vacuum pump – The MaximaDry pump in our lab is a diaphragm pump, making it ideal for most
situations. If you need a vacuum <70mbar use the belt-driven Edwards pump, but make sure the
solvents are being properly captured to prevent damage to the pump and oil.
B) Collection Flask –This is recommended for applications where you are collecting a large amount of
liquid, such as filtration.
C) Cold trap – Where the vapors are condensed.
D) Dewar – Holds the cooling agent and solvent
1) Make sure you are wearing the proper personal protective equipment (gloves, goggles, lab coat, face
shield).

2) Gather the necessary glassware and chemicals to set up the cold trap as shown below. This picture is a
common set up used to filter a solution using a Buchner funnel. The top of the cold trap is connected to
the vapor source (reaction vessel, filter flask, vacuum oven, rotovap, etc.) and the side is connected to
the vacuum trap. Make sure to use proper vacuum tubing.

3) Check glassware to make sure there are no cracks or chips present. Applying a vacuum and/or low
temperature to cracked glass could result in implosion.

4) It is best to first pour the solvent from the large container into a smaller beaker before adding to the
dewar. Dry ice and isopropanol baths are recommended for collecting most solvents.

5) Lower trap into dewar (or raise dewar if on labjack) Add coolant (dry ice) to about 2 inches below the
top of the dewar. Slowly add solvent to the dewar. The solution will rapidly bubble at first so take your
time as it stabilizes.

6) Turn on the vacuum pump and make sure there are no leaks in the vacuum line. Your solution should
start being filtered or evaporating, depending on your application.

7) Make sure the collected liquid doesn’t freeze and cause a blockage in the trap. If it does you may need
to switch to a higher temperature bath (ice water+salt) or add an ice water trap between the vapor
source and dry ice trap to capture the freezing liquid before it enters the dry ice trap.

8) If you are running the pump longer than 30 minutes you should add insulation over the top to maintain
temperature and reduce solvent evaporation. You may also have to continually add more dry ice.

9) When completed, remove trap from dewar, shut off vacuum pump and slowly vent.

10) Allow system to heat up to room temperature and follow proper disposal procedures. Dispose of waste
promptly to ensure it is not evaporated into the atmosphere.
Clean up and waste disposal
The waste collected in the trap should be disposed of in the appropriate waste container. Follow the Standard
Operating Procedure for waste disposal. The isopropanol can either be disposed of or saved in a properly
labeled container for use in future cold trap set ups.

APPENDIX
Common cold trap cooling bath temperatures
Ice + Water = 0 oC
1 part sodium chloride to 3 parts ice water = ~-10 to -20 oC
Dry Ice + isopropanol = -77 oC
Notes: Acetone is generally not recommended because of its volatility
If colder temperatures are needed liquid nitrogen is necessary. Liquid nitrogen vacuum traps require
special training to use because there is a chance to condense pure oxygen, which is highly reactive.

FURTHER READING
Prudent Practices in the Laboratory (p. 173-175), National Council of the National Academies on the Handling
and Management of Chemical Hazards, 2011.
Safety in Academic Chemistry Laboratories (p. 30-31) – American Chemical Society Publication