READ AND REVIEW ANY APPLICABLE MANUFACTURER/VENDOR SAFETY INFORMATION BEFORE
DEVELOPING STANDARD OPERATING PROCEDURE AND PERFORMING WORK.
PI Name: Sergey Nizkorodov
Date Modified: February 12, 2016
Name of Work Unit: Aerosol Photochemistry Group
Standard Operating Procedure (SOP) for
Peroxide Tests
#1
Scope of Work/Activity: Describe the experiment purpose/scope.
- Identify all apparatus that will be used, and associated requirements.
- List special equipment (X-ray generators, lasers, furnaces, etc.) that will be used for
the project.
- Identify measurement and test equipment, apparatus operating conditions,
Include process flow diagrams, pressures, and required maintenance procedures as
appropriate.
This iodiometric peroxide test originally proposed by Banerjee and Budke in 1964 is
used to quantify an unknown peroxide concentration by comparison with a peroxide of
known concentration. This test detects visible absorption of I3- ions formed from the
reaction of a water soluble peroxide with excess I-. With a peroxide of known
concentration (usually hydrogen peroxide), a calibration curve relating peroxide
concentration with I3- absorbance is needed to determine the unknown concentration.
The following materials are required:
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Pressurized Nitrogen Cylinder
Tube with needle mounted to the end for purging solutions with nitrogen. This
needle should have an upstream needle valve to regulate the flow of nitrogen
gas to prevent splashing of the solution
Shimatzu 1800 or 2350 UV-Vis. Both UV-Vis spectrometers are sufficient to
measure the absorption of the I3- complex.
Conical glass vials with septa mounted in the caps. Reactions are completed in
these vials. The septa allow for purging of the vials.
In a typical experiment, dilute peroxide solutions are purged with nitrogen gas to
eliminate any dissolved oxygen. These peroxide solutions are then reacted with a
solution of potassium iodide, water, and acetic acid. The headspace above the solution
must be filled with nitrogen gas to eliminate the ambient oxygen that entered when the
solution was added. The solutions are then allowed to react until their absorbance
(measured at 490 nm) does not change over time.
#2
Specific Safety and Environmental Hazards: State the specific hazard and
consequences if procedure not followed to person, environment, or property.
Organic peroxides react with ketones to form explosive substances.
Concentrated peroxide solutions are explosive.
Acetic acid is corrosive.
#3
Describe in detail how the hazards will be controlled.
a. Identify the Engineering Controls (e.g. interlocks, shielding), Standard Operating
Procedures, or Personal Protective Equipment (e.g. respirators, gloves;) that will be
employed to reduce hazards to acceptable levels.
All experiments should be conducted in a fume hood. Protective gloves and goggles should be used
at all times. All chemical waste should be disposed in a “peroxide waste” container free of ketones.
No glassware should be cleaned with acetone. Organic peroxide solutions should never sit
uncapped for long periods of time as evaporation of water will concentrate the peroxide.
b. Address emergency shutdown procedures.
Cap all uncovered peroxide solutions and turn off UV-Vis spectrometer.
#4
Designated Area: Indicate the designated area for performing this process in the
laboratory.
This process is conducted in the fume hood farthest away from the adjacent offices due
to its proximity to the nitrogen cylinder(s) and the UV-Vis spectrometers.
#5
Personal Protective Equipment (PPE): State the personal protective equipment selected and
required. Examples: safety spectacles, work gloves, respiratory protection, steel toe shoes.
Protective gloves and goggles should be used at all times. Closed toe shoes are also required.
Handle all chemicals in a fume hood.
#6
Important Steps to Follow: List the specific sequence staff should follow to avoid
hazard.
Use all recommended PPE. Do not mix organic peroxides with ketones. Do not let
solutions of organic peroxides evaporate.
#7
Emergency First Aid Procedures:
a. Describe immediate medical treatment required in case of personnel exposure.
-Complete online incident report form at www.ehs.uci.edu
In case of personal exposure, follow MSDS recommendations for that specific
chemical.
#8
Training & Competency Requirements: Describe necessary training and demonstration
of competency for performing the hazardous operation.
Exhibit understanding of risks and hazards inherent with iodiometric peroxide tests.
Demonstrate thorough understanding of the procedures.
#9
Identify waste stream and disposition of unused stock of chemicals
List concentrations and amounts of hazardous wastes or emissions and control
measures.
Additional guidelines regarding hazardous waste at :
http://www.ehs.uci.edu/programs/enviro/
Acidic I3- solutions are produced as waste (~ 5mL per data point, <40 mL per
experiment). Peroxide will be completely consumed before disposal. An un-reacted
peroxide solutions will be dilute (<<1 M) and small (<1 mL)
#10
Decontamination and spill clean-up procedures
Handle small organic peroxide spills by soaking them up with an inert absorbent
material and placing in a bag for disposal with Environmental Health and Safety. Acid
spills should be handled with an acid spill kit. Spills of Potassium Iodide should be
handled as a typical dry chemical spill. All glassware can be cleaned with water and
organic solvents (not acetone).
As the Principal Investigator, it is your responsibility to ensure that all individuals listed in this protocol is
taught correct procedures for the safe handling of hazardous materials involved in this study. It is also your
responsibility to assure that your personnel attend Lab Core Safety Training and other applicable safety training
courses.
Both PI and all persons associated with the protocol must sign the following acknowledgement:
I have read, asked questions, and understand the hazards of and safe working procedures for the
activity/materials described herein.
PI Signature:
DATE
Other Personnel:
Name/ Signature
DATE
Name/Signature
DATE
Name/Signature
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