Standard Operating Procedure

Cryogenic Liquid
Department:
Completion Date:
Approval (by PI / Lab Manger) Date:
Principal Investigator:

Principal Investigator Signature:

Internal Lab Safety Coordinator/Lab

Manager:
Lab Phone:
Office Phone:

Emergency Contact:
(Name and Phone Number)

Location(s) covered by this SOP:

(Building/Room Number)

Type of SOP: ☐ Process ☐Hazardous Chemical ☐ Experiment ☐Equipment Use

Contents
Purpose Scope of Work/Activity First aid Procedure
Responsibility Step-by-step Operation Procedure
Hazard Analysis Emergency Response Plan
Common Hazards Reference
Hazard Control/Engineering Controls Appendix
Administrative Controls
Personal Protective Equipment (PPE)
Anatomy of the Liquid Cryogenic Container
Special Handling Procedure
Location of Nearest Emergency Safety
Equipment
Shipping and Receiving Requirements

SOP template 1 Revised: 02/11/2020

 Read and review any applicable manufacturer/vendor safety information before developing
standard operating procedure and performing work
*** NOTE: Each section needs to be complete with clear and detailed information based on the
Red/italic font instruction. SOP must be approved and dated by the PI or lab supervisor.

1. Purpose and Scope of work/activity

This document is intended to describe the best practice for cryogenic material and explain the
hazards and risks associated with various type of cryogens and ways to have them in control.
However, it is not designed to be substituted for hands-on training and supervision by experience
laboratory personnel.

2. Responsibility

a. The Principal Investigator must provide his/her laboratory personnel with a copy of
this SOP and a copies of any SDS provided by the manufacturer for any chemicals
used.
b. The Principal Investigator must ensure that his/her laboratory personnel have
attended appropriate laboratory safety training or refresher training annually.
c. Any repair or maintenance must be done by a trained person
Identify the personnel that have a primary roles in the SOP and describe how their responsibilities
relates to this SOP. If necessary, include contact information.
3. Definition
Cryogen Liquid An extremely cold substance in liquid phase which produce large amount of
gas at atmospheric temperature and pressure
Asphyxiation Oxygen depletion can cause a condition of breathing difficulties
(suffocation), loss of consciousness and ultimately death
Dewar A vacuum-jacketed pressure vessel designed to hold liquids at below
ambient temperature which is used for storing/transportation of cryogenic
liquids
SDS Safety Data Sheet
Venting The discharge of gas vapor out of an over-pressurized container

4. Hazards Analysis

The process of completing the hazard and risk assessment is needed for locations that storing
quantities of cryogenics can present a significant risk of asphyxiation. For performing hazard & risk
assessment follow the general rules listed below:
- Identify hazards
- Determine hazard effects and who might be harmed
- Determine the severity and probability of potential incident (Risk Assessment)
- Determine the potential likelihood of the potential incident (Hazard Control)

SOP template 2 Revised: 02/11/2020

 After Hazard Analysis, research group can develop a plan to minimize the risks of operating
tube furnace in the process. This includes using engineering control, administrative control
and adequate PPE. Safety needs to be continuously evaluated to identify additional controls
and better work practices.

5. Common Hazards

Most of the cryogenic liquids are colorless, odorless liquid with a boiling point blow -150 °C (-
238°F). It means they stay in gaseous phase at normal temperature and pressures. They generate
large volumes of gas when vaporize. The expansion ratio for the most common liquids are as below:
Common Liquid Expansion Ratio
Argon 1 to 841
Helium 1 to 754
Hydrogen 1 to 848
Nitrogen 1 to 696
Oxygen 1 to 861

In general the main hazards associated with cryogenic liquids are as following:

Hazard How to control?

Cold burn/Frostbite - Use compatible transfer hoses
- Exposure to the cryogenic liquid itself or - Use appropriate PPE including full face
contacting with the substance that liquid shield, and gloves
is flowing through or stored - Place a Cold Burn Hazard label

Asphyxiation - Use and store in the well-ventilated area

- The main danger of using and storage of - Use methods in Appendix A to calculate the
cryogenic liquid is asphyxiation. potential for oxygen displacement
- Use O2 monitor system if required
- Contact EH&S for further assessment
- Don’t get in the elevator with the container
- Don’t fill more than 80% of the capacity of a
secondary container

Over-pressurization - Complete “Compressed Gas Safety” training

- Cryogens generate large volume of gas - Use appropriate PPE
which can pressure build up inside the - Review Safety Data Sheet
container - Ensure dewar is equipped with Pressure
Relief Valve
- If two or more containers connected to
create higher product withdrawal rate, then
vent valves should be connected as well. This
practice is needed to equilibrate the
containers pressure

SOP template 3 Revised: 02/11/2020

 Noise - Use whisper valve if the vent noise is
disturbing
- Contact EH&S for noise evaluation
Physical Injury - Always push the container with wheels
instead of pulling
- Use appropriate PPE
Thermal stress at material - Fill slowly the secondary container to
minimize thermal shock
- Place materials slowly into cryogens

Note:
- Never remove or exchange the recommended Compressed Gas Association (CGA) connection,
or use adapting fittings.
- To avoid excessive splashing of liquid at pressures more than 22 psig into open vessel, extra
precaution is needed. Please read product labels before using
- To avoid any physical injuries, it’s recommended to push the container instead of pulling it as
it shown below

- Be aware of the formation of liquid oxygen in cold-traps. Mixture of liquid oxygen and
organic solvent can cause explosion

6. Hazard Control
a. Engineering Control

In addition to the information below, follow procedures as specified in the lab-specific section of
this SOP.
Room Ventilation, - Liquid containers must be stored in well-ventilated areas or
areas with forced ventilation
- Containers should be stored from the air intakes, high traffic
areas, floor drains and other underground openings

Oxygen Deficiency - Oxygen monitor is required in rooms with poor ventilation

Monitor system to monitor the oxygen level or concentration
Pressure relief - Containers must be equipped with pressure relief valve which
Valve protects the container from over-pressurization
SOP template 4 Revised: 02/11/2020
 List any gas monitoring system available for the process with the calibration/service dates in this
section.

b. Administrative Control
In addition to the practices described below follow procedures as specified in the lab-specific and
special handling/use sections of this SOP.

Documentation - Safety Data Sheet (SDS) for each material should be reviewed.
- Standard Operating Procedure (SOP) must be completed to verify
your experimental set-up and procedures prior to use.
- Manufacturer Operating Manual should be reviewed prior to use
the equipment.
Storage & Location - Designated areas must be identified for.
- Gas cylinders/dewars and associated piping must be well
secured.
- Incompatible chemical/gases must be segregated. Examples
include flammable and oxidizers that must be segregated by
minimum of 20 ft distance
- Cryogenic liquids must be stored in well ventilated locations
Training - Training must be provided prior to conducting any work with the
equipment
- Basic trainings are: lab safety fundamental, compressed gas
safety, waste management
Note: Training should be renewed under the following conditions:
o Changes in the workplace render previous training obsolete
o Changes in the type of cylinders systems or equipment used
render previous training obsolete
o Inadequacies in an employee’s knowledge of compressed gas
cylinders or equipment or observed behavior indicate that the
employee has not grasped the required training
o Any deviation from this SOP requires approval from PI.

c. Personal Protective Equipment (PPE):

i. Full face shield
ii. Apron
iii. Thermal resistant gloves
iv. Lab coat
v. Long pants
vi. Closed toed shoes

Note: Additional PPE could be required if the process present additional risk. It would be PI
responsibly to identify and communicate any additional PPE requirements.
List all additional PPE required for the specific process
SOP template 5 Revised: 02/11/2020
 7. Anatomy of the Liquid Cryogenic Container
It is important to be familiar with the container design for handling gas or cryogenic liquid in a safe
manner. Two different containers are compared in the following table:

Low-Pressure Liquid Container High-Pressure Liquid Container

Liquid Valve: Add or withdraw the liquid product through the connection controlled by the valve.
Specific CGA connection is required for the appropriate cryogenic liquid
Relief Valve: To protect the container from over-pressurization. It consists of two relief devices; first is a reseating
spring-loaded relief valve which depending on the setting will relieve pressure at 22 psig, 230 psig or 350 psig. The
second is a burst disk rated to protect the inert vessel
Vent Valve: To release un-wanted pressure during storage and use.
Contents Gauge/Liquid Level Gauge: A float type level gauge to indicate the approximate amount of container
contents
Pressure Building Valve: to create enough operating pressure. For more information visit
https://www.airproducts.com/~/media/Files/PDF/company/safetygram-27.pdf
Gas Use Valve: To withdraw gaseous product through the vaporizer and/or the economizer

8. Special Handling Procedures and Storage Requirements

Describe special handling and storage requirements for hazardous chemicals/gases in the laboratory,
especially for highly reactive, unstable and highly flammable materials and corrosives. Describe
transport and secondary containment requirement, between the laboratories or between facilities.
9. Location of Nearest Emergency Safety Equipment

ITEMS LOCATION
EYEWASH/SAFETY
SHOWER
CHEMICAL SPILL KIT
FIRST AID KIT
FIRE EXTINGUISHER
TELEPHONE
FIRE ALARM MANUAL
PULL STATION
OTHERS/DETAILS:

SOP template 6 Revised: 02/11/2020

 10. Shipping and Receiving Requirements

Describe shipping or receiving requirement for cryogenic liquids.

11. Step-by-step Operation Procedure

Describe the step-by-step procedure for using the cryogenic liquid containers properly. Include details
for potential tank failure if something is done improperly in the procedure and the procedure of
liquid/gas withdrawal.
12. Emergency Response Plan

A laboratory emergency response plan should be developed that address accidental releases and
emergency response to this process. This plan should be part of the training procedure and be
documented.
Only trained emergency response personnel with proper personal protective equipment
(i.e., SCBAs, Level A suits for gases with a Cal/OSHA Skin notation) and appropriate gas
monitoring instruments should be allowed to enter the toxic gas release area.
The following steps should be taken following below incidents:

SOP template 7 Revised: 02/11/2020

 Switch of the furnace (If Possible)
Shut off the gas suply (If Possible)
Activate the Fire Alarm
Evaccuate the building
Fire Call 911
Notify the lab PI and EH&S immediately
Note: If the fire is occured within the furnace tube;
Follow Emergency Shut Down Procedure
Leave the inert gas (nitrogen, argon) flowing to extinguish the fire

Always be aware of the hazard class of gas supplies and the reaction
products/byprodiucts
Evacuate the laboratory and close the door
Release of Gas Activate the fire alaram
Call 911
NOTE: If it is a non-hazardous gas, shut off the gas supply and terminate
the heating process according to Emergency Shut Down Procedure

On Body or Clothes:
Remove clothing
Wash body thoroughly in emergency shower for at least 15 minutes.
Seek medical attention.
Chemica Spill Notify supervisor and EH&S at x46200 immediately.

Into Eyes: Immediately rinse eyeball and inner surface of eyelid with
water from the emergency eyewash station for 15 minutes by forcibly
holding the eye open. Seek medical attention. Notify supervisor and EH&S
at x46200 immediately

In this section describe additional procedure for any other emergency events that may happen.
Indicate how accidental events should be handled and by whom. List emergency contact number.
13. Reference

The following links are referenced to support safe operation of cryogenic liquid containers:
1. Cryogenic liquid containers from Air Products manufacturer:
https://www.airproducts.com/~/media/Files/PDF/company/safetygram-27.pdf
2. General use SOP for cryogenic liquid
https://ehs.stanford.edu/wp-content/uploads/sops/Cryogenic-Liquids.pdf
3. Cryogenic substances SOP from Marywood University
http://www.marywood.edu/science/pdf-files/Cryogenics%20SOP.pdf
4. Oxygen depletion calculations
https://intranet.birmingham.ac.uk/hr/documents/public/hsu/information/
hazardoussubstances/Appendix3Oxygendepletioncalculations.pdf

SOP template 8 Revised: 02/11/2020

 Appendix A: Assessment of Ventilation Requirements
The assessment of ventilation requirements is important to mitigate the consequences of a gas
leakage that can cause asphyxiation. Gas leakage could change the concentration of the air
components. Air contains 78% Nitrogen, 21% Oxygen and 1% Argon. An atmospheres containing
less than 18% oxygen is dangerous and entry into atmosphere containing less than 20% of oxygen
must be avoided.
How to calculate the air concentration?
Case 1:
This case is about a situation that gas releases by certain evaporation rate from vessels or
pipework.
Determination of the gas concentration depends on the amount of gas release, room volume and air
change per hour which shown in the following equation:

L
C=
Vn
Where
L = gas release (ft3/hr) = Cryogen volume X Expansion factor / 1000
V = room volume (ft3)
n = air change per hour
Case 2:
Oxygen depletion resulting from a large spillage of a cryogenic liquid or sudden release from a
pressurized vessel. Always “worst Case Scenario” must be considered
Determination of the oxygen concentration (%) is as following:

100∗V o
% O 2=
Vr
Where: for nitrogen:
Vo = 0.2095 (Vr – Vg)
Vr = Room Volume (ft3)
Vg = maximum gas release = liquid volume capacity of the vessel V * gas expansion factor

SOP template 9 Revised: 02/11/2020

 I have read and understand the content of this SOP:

Name Signature Identification Date

SOP template 10 Revised: 02/11/2020