READ AND REVIEW ANY APPLICABLE MANUFACTURER/VENDOR SAFETY INFORMATION BEFORE
DEVELOPING STANDARD OPERATING PROCEDURE AND PERFORMING WORK.
PI Name: Sergey Nizkorodov
Date Modified: February 8, 2016
Name of Work Unit: Aerosol Photochemistry Group
#1
Standard Operating Procedure (SOP) for
Operating Flow Tube Reactor
Scope of Work/Activity: Describe the experiment purpose/scope.
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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,
The system consists of:
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Pressurized oxygen gas cylinder
Commercial ozone generator
Purge gas generator
Ozone meter
Voltmeter
Mass flow control box
Flow tube (glass of Plexiglas depending on the version)
Syringe pump
Denuder
Vacuum pump
Test equipment needed:
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Flow meter to occasionally check calibration of mass flow control box.
Valve 2
Notice
valve
locations
Valve 1
This is what the system set up looks like. It does not display the mass flow control box.
It is important to monitor the pressure in the system, which is displayed above the mass
flow control box, to maintain 760 Torr (depending on the operation mode, it may
deviate from this value but should not deviate by more than 200 Torr). Also be sure to
check the moisture indicator attached to the purge gas generator to make sure only dry
air is flowing. The VOC injection point should routinely be cleaned by sonication in an
organic solvent. Do not vacuum pump VOCs or ozone. The denuder must be connected
to the flow tube.
#2
Specific Safety and Environmental Hazards: State the specific hazard and
consequences if procedure not followed to person, environment, or property.
Exposure to ozone can cause inflammation of the airways, leading to increased
susceptibility to infections, difficulty breathing, and aggravated asthma, coughing or
wheezing. Long term side effects of excessive ozone exposure can lead to diminished
lung capacity, accelerated aging of the lungs, decreased lung function and other
serious lung infections.
#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.
Active engineering controls include:
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Power switch on ozone generator to turn off the discharge and to stop producing ozone.
Charcoal filter can be connected to airflow to prevent ozone from entering room air and
preventing ozone exposure.
 Regulator valves located on the pressurized oxygen gas cylinder in “closed” position will
not provide oxygen gas flow to the ozone generator and ozone will not be produced.
 Valves 1 and 2 labeled on the flow tube diagram will inhibit ozone containing air from
flowing throughout the system.
 Switch on mass flow control box in the “off” position will stop all airflow throughout the
system.
Passive engineering controls include:
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The room has an air filtration system and if ozone is leaked it will be slowly removed.
b. Address emergency shutdown procedures.
Possible emergencies: exposure to high levels of ozone and increased system pressure.
High levels of ozone exposure can occur IF
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Ozone generator is on and ozone is discharged in the room without protection
by a charcoal filter.
Strong “electrical” or “metallic” odor is present in the room that can cause
lightheadedness or dizziness.
Do the following:
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Turn off the ozone generator.
Close all valves in the O2 supply line, and leave the room.
Overpressure in the system can occur IF
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The tube exist is constrained with filter, plug, or other follow element with a
high resistance. If this happens, one of the inlet tubes will “pop off”
Do the following:
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#4
Close the bleeder valve on the regulator connected to the oxygen gas tank.
Close all inlet valves on the flow tube diagram.
Designated Area: Indicate the designated area for performing this process in the
laboratory.
Large table in Room 350 is the only area where the system can be operated.
#5
Personal Protective Equipment (PPE): State the personal protective equipment selected and required.
Examples: safety spectacles, work gloves, respiratory protection, steel toe shoes.
Personal protective equipment includes:
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#6
Safety goggles must be worn by all people in the vicinity of the operating flow tube.
Closed toe shoes must be worn by all people in the vicinity of the operating flow tube.
Long sleeves must be worn by all people in the vicinity of the operating flow tube.
Long hair should be tied back by the person operating the flow tube when using the vacuum
pump or MOUDI.
Important Steps to Follow: List the specific sequence staff should follow to avoid
hazard.
Refer to the instrument manual for the start up and power down procedures. A short
version of these procedures is provided at the end of this document.
#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
If someone is exposed to excessive levels of ozone:
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Make an appointment with a physician if the individual is experiencing
symptoms of coughing, pain with breathing, and/or airway inflammation.
Take the person to the emergency room if they are experiencing deep wheezing,
difficulty breathing, and aggravated asthma or lung infections.
If someone has been cut by glass shards then take the person to the emergency room for
necessary treatment.
#8
Training & Competency Requirements: Describe necessary training and demonstration
of competency for performing the hazardous operation.
Everyone operating the flow tube must:
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Pass basic laboratory safety training
Pass the compressed gas cylinders safety course
Read this SOP
#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/
Ozone emissions >100 ppb are considered hazardous in working environments and
EH&S should be contacted. Human symptoms begin to show when ozone levels reach
≥300 ppb.
#10
Decontamination and spill clean-up procedures
VOCs injected into the flow tube reactor are on the scale of µL. Chemical spills of
VOC should be cleaned using Kim wipes and methanol.
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
DATE
Summary of Operating Procedures for Flow Tube Reactor
Last updated on February 8, 2016
Turning on the flow tube
1) Make sure the outlet from the flow cell is connected to a charcoal filter. This step is important to make
sure ozone from the system doesn’t get into the air of the room.
2) Turn on UV lamp connected to voltmeter. Allow the lamp to warm up for 1 hour. The box works
properly even though the display flashes that the wheel inside is broken.
3) Make sure the mass flow control and pressure meter boxes are on. They are usually left on all the time.
a. Changing the air flow. Switch the box to channel 4 and use knob to change the air flow. It is
usually set to about 48.4.
b. Changing the oxygen flow. Switch to channel 3 and use knob on the box. It is usual set to 95.
4) Make sure the syringe pump is on. Allow to warm up for 10 minutes if not already on.
a. The Table menu can be used to set the volume and flow rate that you are using.
b. A typical flow rate is 25 L/hr.
5) Open valves to the oxygen supply.
a. Open the main valve at the top of the gas cylinder
b. Open the left-most valve on the regulator (after opening the valve, the regulator should read
~170 Pa)
c. Following the tubing, open the next valve. It opens in a 90° motion. When the valve is up the
valve is closed.
6) Air flow is never changed. It should already be flowing correctly.
7) Turn on the voltmeter. Record the reading in millivolts.
8) Turn on the ozone generator. The knob on the box controls the amount of ozone that is made. Typical
setting is “2”. Let it run for about 10 minutes before beginning to collect sample. Record the new
reading on the voltmeter. Calculate V/V0 and use the chart by the voltmeter to determine the amount of
ozone generated.
Making samples
1) Use 50 μL syringe for sample injection. Usually about 20 μL is sufficient for sample preparation.
2) Secure syringe on syringe pump. Insert syringe through the septum in front of the syringe pump and
secure. Select desired settings on syringe pump for sample collection.
a. Set up syringe pump. Press the “Select/Menu” button and use arrows to navigate to Table
option. Press “Select/Menu” again to choose settings for volume and rate. Check to make sure
the syringe pump is set up for the type and size syringe you are using. Press select until you get
to “Volume”. Use the arrow buttons to select your volume. Press select again. Now you can
adjust the rate of injection. Use the arrow buttons to select the rate that you want. Press select
again.
b. Inject sample. Once all the desired settings have been selected, press the “Run/Stop” button to
begin injection. The syringe pump will display the volume that has been injected so far. The
syringe pump will stop once it has injected the volume you selected.
3) Connect your sample collector (MOUDI/Impactor/Filter holder) to the pump.
a. MOUDI instructions: Place MOUDI on the Deposit Impactor and flip rotating switch up. Once
secure, connect the vacuum tubing and pump to the MOUDI.
b. Impactor instructions: If using foil, prepare impactor beforehand. Then connect the top of the
impactor to the top of the T connected to the HEPA filter with conductive tubing. Connect the
bottom of the impactor to the flow meter with conductive tubing.
4) Connect the side of the T connected to the HEPA filter to the denuder.
5) Turn on the pump by flipping the switch on the power strip.
6) Test the flow rate through your sample collector using an electronic flow meter.
Turning off the flow tube:
1) Turn off the ozone generator.
2) Turn off the pump. Unplug the pump and disconnect the sample.
3) MOUDI: Disconnect from sample from air supply. Disconnect MOUDI from the air filter.
a. MOUDI Instructions: To disconnect MOUDI from the Deposit Impactor when sample collection
is complete, flip the rotating switch down until MOUDI is released.
4) Connect denuder to the dump.
5) Close the 90° valve for the oxygen flow
6) Close the left-most valve on the oxygen regulator
7) Close the valve at the top of the oxygen tank
8) Air flow is kept open
9) Turn off the UV lamp.
10) Turn off the syringe pump.
11) Turn off the voltmeter.
12) Check pressure of the system. Make sure the pressure reading is around atmospheric pressure in the
system.