Guidance on Sulfuryl Fluoride Clearance Device Testing
On this page:
- How to Test Clearance Devices
- How to Submit a Protocol to EPA
- How to Submit Data to EPA
- Submission and Contact Information
- Docket Links
How to Test Clearance Devices
The Agency’s goal is to ensure the safety of people when re-entering fumigated structures. A reliable and effective clearance device is one of the tools to mitigate the risks in re-entering fumigated structures. The Analytical Chemistry Branch (ACB) within the Office of Pesticide Programs (OPP) at EPA developed guidance for assessing portable devices for their effectiveness in detecting sulfuryl fluoride (SF) at clearance level.
Data submitters must first submit a protocol based on the procedures described below. The protocol must be approved by the Agency prior to initiating a study. After the Agency approves the protocol and a study is conducted and submitted to the Agency, the Agency will determine if the study was conducted according to the protocol and if the criteria for effectiveness are met. Once the Agency determines the effectiveness of a device based on an approved study, EPA will add the portable clearance device to the SF Clearance Devices webpage.
Portable SF monitoring devices (also referred to as clearance devices, or gas analyzers) are used to measure, monitor, or detect the level of SF in air after fumigation. All tested devices must have current and valid calibration and an up-to-date user’s manual. They should operate normally and be calibrated, as scheduled, by the vendors or authorized service providers. A minimum of two devices per model are tested.
How to Submit a Protocol to EPA
The protocol objective is to evaluate the performance of portable SF monitoring devices at different SF levels, particularly the reliability of detecting SF at the safe entry level of 1 ppm. Data submitters must first submit a protocol based on the requirements and details described in the data submission section. The protocol must be approved by the Agency prior to initiating a study. EPA’s response to all submitted protocols will be posted to the sulfuryl fluoride docket.
Additional information on the clearance device testing can be found in the ACB test protocol (https://www.regulations.gov/document/EPA-HQ-OPP-2009-0136-0106).
Please submit a proposed protocol by e-mail to Moana Appleyard at appleyard.moana@epa.gov that includes:
- A cover letter that indicates the clearance device to be tested.
- A PDF file containing the protocol.
- If the file is too large to email, please send by mail to the following addresses:
Attn: Moana Appleyard
U.S. Environmental Protection Agency
Office of Chemical Safety and Pollution Prevention
Office of Pesticide Programs, Pesticide Reevaluation Division
1200 Pennsylvania Ave., NW
Mail Code 7508P
Washington D.C. 20460
Attn: Branch Chief
Analytical Chemistry Branch
Environmental Science Center
701 Mapes Road
Fort George G. Meade, Maryland 20755-5350
How to Submit Data to EPA
After the Agency approves the submitted protocol and a study is conducted and submitted to the Agency, the Agency will determine if the study was conducted according to the protocol and if the criteria for effectiveness are met. EPA’s response to all submitted protocols will be posted to the SF docket. Once the Agency determines the effectiveness of a device based on an approved study, EPA will add the portable clearance device to the Sulfuryl Fluoride Clearance Devices webpage.
General guidance for testing
- Tests over several days (minimum of five different days) at each concentration level, for each device. Tests with freshly prepared SF gas bags each day.
- Triplicate readings at each SF concentration, one device at a time.
- Tests for all SF concentration levels each day at the clearance levels of 1 ppm and at least three higher levels such as 3, 5 and 10 ppm.
- Minimum of two devices per model.
Additional information on the clearance device testing can be found in the ACB test protocol (https://www.regulations.gov/document/EPA-HQ-OPP-2009-0136-0106).
A) Description and calibration of portable clearance device tested
- Manufacturer
- Model name/designation
- Serial number
- Vendor
- Manufacturer’s recommended re-calibration interval
- Calibration date(s)
- Other relevant descriptors or technical specifications
B) Sulfuryl fluoride gas standards
- Source
- Nominal concentrations
- Certificate value (ppm)
- Lot number
C) Equipment
- Gas bags (model, manufacturer)
- Analytical instrument, such as gas chromatograph with mass spectrometer detector (GC-MSD) or flame photometric detector (GC-FPD).
D) Documentation
- Temperature and relative humidity of the test conditions.
- Records of preparations, individual readings, and status of each device during the tests in a logbook for each device.
- Time required to reach stable maximum reading when exposed to SF and time required to return zero after removing the SF. The stable reading is defined as the reading remaining unchanged for a minimum of 15 second period.
- Test dates, starting time. Unexpected observations during the tests will be noted as well.
- Reasons for possible repair services and calibrations (internal or by manufacturers or by the authorized vendors) of the devices. Any deviations from the written procedure, any errors or abnormal performance and corrective actions taken.
- The actual readings on the devices (without regard to the significant numbers of the display) recorded for the measurements of SF levels for each device. If needed, the reading can be estimated to the nearest reading of half point, e.g., 1.5, 2.0, or 11.5, for analog display or oscillating values.
- Specific Operation Procedures as adapted from instructions of each device’s user manual.
- Averages and standard deviations of all the readings at each SF level
- Agreement among replicate devices
- Analytical instrument calibration data used in verifying concentration of gas standards
Measurement of SF Concentration
The devices must be operated and tested as close as possible to how they are operated by a typical field user. Instruction from the user’s manual must be followed with the following exceptions:
- Testing is conducted in a laboratory setting, under ambient conditions. Temperature and humidity are monitored with a portable temperature/humidity meter and recorded in a lab notebook on the days of testing.
- Gas bags (or gas chambers) are used to sample gas or “clean air” for testing.
- Suggestion for gas bags: Kynar Dual Valve gas bags (20L capacity; Cole-Parmer, Cat 01410-54)
Sampling Procedures
- For SF gas samples:
- At a minimum, test at 4 different levels, including the current clearance level of 1 ppm, for example 1, 3, 5, and 10 ppm
- Purchase SF gas standards from commercial sources with certified concentrations
- Use of in-house made SF standards is discouraged, especially when they are made from highly concentrated standards, which required serial dilutions and high dilution factors (50 and above). If a laboratory chooses to make working standards from a concentrated stock standard by dilution, the prepared working standards must be verified with independently sourced SF standards (source different than the one used to prepare the standards) and with an analytical instrument such as a gas chromatograph (GC) with a mass spectrometer (MS) detector (GC/MSD) or a flame photometric detector (GC/FPD).
- For “clean air” sample to zero the devices (i.e., to set device to register “0”)
- Use laboratory air
- If dry air is preferred, collect air from a compressed air tank through a drierite tube in a gas bag
- Collect fresh SF and “clean air” samples for each day of testing.
- Use different bags for different samples
Tips for using gas bags: Evacuate each bag with a gas-tight syringe to remove any air in the bag before filling it with gas standards. Fill the bags partially with gas (i.e., the gas pressure inside the bags would be at ambient atmospheric pressure). Connect the testing device to the on/off port of the gas bag with a quick-connect ¼ inch compression connector via a 2-inch-long Teflon tubing.
Testing Procedures
- Verify the concentration of the SF collected in the Kynar bag periodically using analytical instrument such as a GC/MSD or a GC/FPD. The analytical instrument calibration standards must be independently sourced standards from those used for the gas samples and must bracket the concentrations of the tested standards. For example, if the tested standards are 1, 3, 5, and 10 ppm, the instrument calibration curve must include a 1 and a 10-pm standard.
- Follow the user’s manual to conduct and test each SF level for each device in triplicate. This will constitute a set of measurements and should be completed in one day.
- Test each device over multiple nonconsecutive days. More than one set should not be collected in one day.
- Use freshly prepared SF gas bags for each day of testing
Note: The time required to reach stable maximum reading when exposed to SF and the time required to return zero after removing the sulfuryl fluoride vary with each device model. In general, a reading is considered stable if it remains unchanged during a 10-15 second period.
Documentation
At a minimum, the following items must be documented:
- Temperature and relative humidity of the room.
- Procedure for preparation of the SF gas bags, the individual readings and status of each device during the tests for each device.
- Time required to reach stable maximum reading when exposed to SF and the amount of time required to return to zero after removing the SF will also be recorded. A reading is defined as stable when it remains unchanged during a 10-15 second period.
- Date, starting time, and end time for the tests for each device.
- Unexpected observations during the tests.
- Causes for repair services and calibrations (internal or by manufacturers or by the authorized vendors) of the devices as well as any deviations from the written procedure, or abnormal performance.
- Actual readings on the devices (without regard to the significant numbers of the display) for the measurements of SF concentrations for each device.
- Detailed procedures used to prepare SF working standards if standards are prepared by the testing laboratory. The source and certification data of the analytical instrument calibration standards, and the verifications of the prepared SF working standards.
- Analytical instrument calibration data, including calibration levels and calibration curve linearity data
Submission and Contact Information
Please submit a proposed protocol by e-mail to Moana Appleyard (appleyard.moana@epa.gov) that includes:
- A cover letter that indicates the clearance device to be tested.
- A PDF file containing the protocol.
- If the file is too large to email, please send by mail to the following addresses:
Attn: Moana Appleyard
U.S. Environmental Protection Agency
Office of Chemical Safety and Pollution Prevention
Office of Pesticide Programs, Pesticide Reevaluation Division
1200 Pennsylvania Ave., NW
Mail Code 7508P
Washington D.C. 20460
Attn: Branch Chief
Analytical Chemistry Branch
Environmental Science Center
701 Mapes Road
Fort George G. Meade, Maryland 20755-5350
Docket Links
Sulfuryl fluoride clearance device documents in the sulfuryl fluoride docket
|
Docket ID and Link |
Title |
Date Posted |
|---|---|---|
|
Attachment 1 - Protocol for Conducting Laboratory Testing of Portable Clearance Devices with Sulfuryl Fluoride Standards |
May 25, 2021 |
|
|
Attachment 2 - Laboratory Testing of Portable Clearance Devices with Sulfuryl Fluoride Standard – All Devices Final Report |
May 25, 2021 |
|
|
Protocol for Conducting Laboratory Testing of Portable Clearance Devices with Sulfuryl Fluoride Standards |
May 25, 2021 |
|
|
Assessment of Portable Devices for Their Effectiveness in Detecting Sulfuryl Fluoride (SF) at Clearance Level |
May 25, 2021 |
|
|
Protocol for Conducting Laboratory Test of the Portable Clearance Devices with Sulfuryl Fluoride Standard Revised September 3, 2019 |
May 25, 2021 |
|
|
SF Standard in Nitrogen COAs Certificate of Analysis |
Jul 29, 2021 |
|
|
FumiSpec 1 - Data Workup |
Jul 29, 2021 |
|
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CLIR Check 2 - Data Workup |
Jul 29, 2021 |
|
|
FumiSpec 2 - Data Workup |
Jul 29, 2021 |
|
|
Interscan GF1900 1 - Data Workup |
Jul 29, 2021 |
|
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Interscan GF1900 2 - Data Workup |
Jul 29, 2021 |
|
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Spectros 1 - Data Workup |
Jul 29, 2021 |
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Spectros 2 - Data Workup |
Jul 29, 2021 |
|
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CLIR Check Device1 Data Sheets |
Jul 29, 2021 |
|
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CLIR Check Device2 Datasheets |
Jul 29, 2021 |
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FumiSpec-Lo, Instrument |
Jul 29, 2021 |
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FumiSpec Device2 Datasheets |
Jul 29, 2021 |
|
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Interscan GF1900 Device1 Datasheets |
Jul 29, 2021 |
|
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lnterscan GF1900 Device2 Datasheets |
Jul 29, 2021 |
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SF Clearance Device Testing Lab Notebook |
Jul 29, 2021 |
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|
Spectros SF-ExplorIR Device1 Datasheets |
Jul 29, 2021 |
|
|
Spectros SF-ExplorIR Device2 Datasheets |
Jul 29, 2021 |
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|
Response to Comments on Clearance Device Testing Not Previously Addressed by EPA October 24, 2019 |
Sep 15, 2021 |