University of Nevada Las Vegas
Protocol 9: Preparation and analysis of radioactive solutions by spectroscopic or chromatographic methods
Protocol for Use of Radioactive Materials
1. AUTHORIZED USER Protocol #KRC-9
Expiration date: 13-Dec-17 Specific Protocol # KRC-9-001
Name / Ken Czerwinski / Phone / 1-702-281-04652. PROJECT NAME 3. FACILITY
Preparation and analysis of radioactive solutions by spectroscopic or chromatographic methods / Building / LabHRC / 164, 165, 172, 172A, 173, 242
4. PROJECT DESCRIPTION
Training for this protocol can be performed by Ken Czerwinski or Frederic PoineauThis protocol is for measurement of radioactive samples by a range of methods including spectroscopy (i.e., UV-Visible, IR, laser, atomic emission, mass, and NMR spectroscopy) and chromatography.
Contamination control/monitoring protocols developed for the radiochemistry laboratories will be used for this work. Appropriate PPE will be used at all times.
For spectroscopy measurement of radioactive sample the appropriate cuvette holder should be used. The cuvette or samples holder in the spectrometer will be clearly labeled “For use with radioactive samples’. For other analysis appropriate rack, syringes, vials, tubing and cells will be used.
The radioactive material analyzed is in solution. Work will be performed in the hood or on a bench top.
1. Sign up for equipment usage on the equipment calendar.
2. Determine the Risk level of the radioactive material to be used in the procedure. This can be done with the risk assessment and control guidelines. The radiation safety level is rated 1 (lowest) to 4 (highest). The appropriate control measures are based on the radiation safety level and are listed in the UNLV Risk Assessment and Control Guideline for Radioactive Materials at the end of this document and https://rms.unlv.edu/radiological/Risk%20Assessment%20&%20Control%20Guideline%20for%20RAM.doc.
A list of isotopes commonly used in the radiochemistry program is provided.
Risk Level: 2 or 3
Air Monitoring
Continuous air monitoring required if >0.1 ALI (inhalation) of dry, dispersible material.
Breathing Zone Airsampling (BZA) is required when working with ≥ 1 ALI (inhalation) dry, dispersible materials (airborne).
If no dry dispersible radioactive material is used or generated BZA is not required. If continuous air monitoring is required verify that an air sampler is running within the laboratory. If a sample is not being collected contact the RSO for assistance. Note: If required, a continuous air sampler must be running in the laboratory before you can proceed with your research.
3. Prepare breathing zone sampler if needed
3.1. Verify filter paper is properly placed in unit.
3.2. Place the sampling head of mobile or mounted unit in breathing zone
3.3. Turn on pump, verify appropriate air flow.
Risk Level 2 Data
Isotope / 99Tc / 232Th / 233U / 235U / 238U / 237Np / 239Pu / 243Am
Maximum mass (mg) / 2.36E2 / 6.36E3 / 1.04 / 4.63E3 / 3E4 / 7.10E-1 / 1.28E-2 / 4.01E-3
Risk Level 3 Data
Isotope / 99Tc / 232Th / 233U / 235U / 238U / 237Np / 239Pu / 243Am
Maximum mass (mg) / 2.95E3 / 3.18E5 / 5.18E1 / 2.31E5 / 1.5E6 / 3.55E1 / 6.42E-1 / 1.97E-1
Radionuclide: Maximum mass of radionulide (mg):
Control: (i.e., benchtop, hood, glovebox)
4. Policies and procedures within the UNLV Radiation Safety manual will be followed. Appropriate personal protection equipment will be used at all times.
5. Monitor the work area prior to experiment initiation.
6. Secure an “Experiment in Progress” sign in the area of the set-up with date and time information as well as activity, nuclides, and related information to notify others in the lab of the ongoing experiment.
7. Prepare work area with tray, absorbent padding, radioactive waste collection, vials, and other solution handling equipment as required.
8. Place solution sample with radionuclide in cuvette or sample holder via a pipette or other liquid transfer tool as appropriate.
9. Seal the cuvette or sample holder as necessary. All cuvettes and vials should be sealed and checked for removable contamination prior to leaving the sample preparation area. Cuvettes may be sealed with a lid, stopper or, parafilm. Chemical compatibility should be considered.
10. Monitor cuvette or sample holder for external contamination.
11. Place cuvette or vial in labeled secondary container. Monitor for external contamination.
12. Transport cuvettes or sample to spectrometer or chromatography equipment. Put the secondary container on the rad pad next to the equipment as needed.
13. Monitor sample holder labeled “For use with radioactive samples’ for removable activity if used for the experimental method. The equipment may have cell or cuvette holders designated for use with radioactive solution.
14. Use gloves for handling cuvette or sample. Do not touch instrument with gloved hand.
15. Insert sample in the holder as appropriated for equipment.
16. Perform measurement.
17. Remove cuvette or sample when measurement complete. Monitor cuvette or sample holders for external contamination.
18. Place cuvette or sample in secondary containment
19. Return radioactive samples to appropriate location.
20. Clean cuvettes or holder and properly dispose of any radioactive waste.
21. The entire work area will be cleared from all unnecessary content.
22. Survey work area and document results for the sample preparation area and the analysis equipment
23. Collect breathing zone monitor sample if used
23.1. Stop pump
23.2. Remove filter and place in sealable bag
23.3. Install new filter in unit head
23.4. Label bag with date, laboratory, start time, end time, and initials
23.5. Place in breathing zone sample collection area
23.6. Contact laboratory managers for sample evaluation by RSO
5. AUTHORIZED RESEARCHERS
Name / Katherine Thornock / Employee/Student IDExperience / UNLV Radiochemistry Graduate Student
Name / Cassara Higgins / Employee/Student ID
Experience / UNLV Radiochemistry Graduate Student
Name / Grace Marnecheck / Employee/Student ID
Experience / UNLV Radiochemistry Graduate Student
Name / Andrew Swift / Employee/Student ID
Experience / UNLV Radiochemistry Graduate Student
Name / Daniel Koury / Employee/Student ID
Experience / UNLV Radiochemistry Research Professor
Name / Samundeeswari Balasekaran / Employee/Student ID
Experience / Radiochemistry Post-doctoral researcher
Name / Frederic Poineau / Employee/Student ID
Experience / UNLV Radiochemistry Professor
Name / Ken Czerwinski / Employee/Student ID
Experience / UNLV Radiochemistry Professor
Name / Bradley Childs / Employee/Student ID
Experience / UNLV Radiochemistry Graduate Student
Name / Employee/Student ID
Experience
Name / Employee/Student ID
Experience
insert rows as needed.
6. RADIOACTIVE MATERIALS USED: List each radionuclide used and the maximum amount used in any single procedure. Indicate if there is a potential for airborne contamination. *If YES, complete Attachment 1. ** Attachment 2, UNLV Risk Assessment and Control Guideline for Unsealed-Radioactive Materials. Note: If nuclide not listed, refer to 10 CFR20, Appendix B, Table 1.
Nuclide / Maximum Activity per Use(µCi) / Mass (mg) / ALI-Inhalation(µCi) / ALI-Ingestion (µCi) / ALI-Limiting (µCi) / Potential Airborne* (Y/N) / Risk Level** (1-4) / Physical Form / Chemical Name
99Tc / 50000 / 2.95E3 / 700 / 4000 / 700 / N / 3 / Solution phase
232Th / 35 / 3.18E+5 / 0.001 / 0.7 / 0.001 / N / 3 / Solution phase
233U / 500 / 5.18E1 / 0.04 / 10 / 0.04 / N / 3 / Solution phase
235U / 500 / 2.31E5 / 0.04 / 10 / 0.04 / N / 3 / Solution phase
238U / 500 / 1.5E6 / 0.04 / 10 / 0.04 / N / 3 / Solution phase
229Np / 25 / 3.55E1 / 0.004 / 0.5 / 0.004 / N / 3 / Solution phase
239Pu / 40 / 6.42E-1 / 0.006 / 0.8 / 0.006 / N / 3 / Solution phase
243Am / 40 / 1.97E-1 / 0.006 / 0.8 / 0.006 / N / 3 / Solution phase
7. RADIATION SAFETY MATERIALS & EQUIPMENT: Check all items available to workers handling radioactive material.
X / Protective gloves / X / Warning signs/tags/tape / X / Personal dosimetersX / Lab coat / X / Absorbent paper / X / Survey meter
X / Safety glasses / Trays / X / Swipe counter
Face shield / X / Secondary containers / Other (list):
X / Shoe covers / Handling tongs
Respirator / Shielding
8. ENGINEERING CONTROLS: Check all items that are required.
Fume hood - unfiltered / Fume hood–filtered exhaust / Glove box / Secondary containment9. EVALUATION OF AIRBORNE RADIOACTIVE MATERIALS: Indicate how radioactive materials could become airborne. Check all that apply.
Production or use of radioactive gas (e.g. methane, 14CO2)Grinding, pulverizing and associated handling of dry dispersible unsealed radioactive material
Volatile compound (e.g. Na125I, 3H2O, labeled solvents, Na-Borohydride)
Aerosols (e.g. evaporation of liquids) / x
Use of powders and other finely divided solids
Other (list):
Other (list):
10. AIR MONITORING: Check all items that are required. [Routine air monitoring required if > 0.01 ALI of dry, dispersible material. Continuous air monitoring required if >0.1 ALI of dry, dispersible material. Breathing Zone Air sampling (BZA) is required when working with ≥ 1 ALI dry, dispersible materials (airborne)]. (Note: For limits, see Attachment 2. If nuclide not listed, refer to 10 CFR20, Appendix B, Table 1).
None / x / Routine / x / CAM / BZA11 BIOASSAY: Check all items that are required. [Baseline bioassay and quarterly bioassay required >5 ALI dispersible (airborne).
Baseline / x / Quarterly / Other12. FACILITIES: List ALL rooms where ANY radioactive material will be used or stored. Briefly describe the use of each location. Insert rows as needed.
Building / Room # / UseMSM / 173 / UV Visible spectroscopy preparation
MSM / 172 / UV Visible spectroscopy analysis
MSM / 162, 164, 165, 167, 168 172, 173 / Solution Preparation and chromatography analysis
MSM / 242 / ICP-MS, ICP-AES analysis
13. RISK ASSESSMENT: Describe the expected radiation dose associated with this protocol. Describe the likelihood and seriousness of unexpected, but realistic, problems or accidents. (Consultation is available from Radiation Safety.)
Normal ConditionsThere is no expected inhalation risk during normal conditions. The radionuclides in the samples are in solution and are not volatile at room temperature.
Off-Normal Conditions / Accident Scenarios
In terms of contamination, the most significant accident would be a spill of an entire sample container or the cuvette. Samples are put on a radioactive padding into an HEPA filter hood. To mitigate the potential for spills, sample containers will be capped while not used. The spill will be stopped, monitored and immediately cleaned.
Also another scenario with a leak while transferring using a pipette. If this happens, the spill should have been occurred on a disposable padding which will be disposed and the work area will be monitored and cleaned accordingly. If the spill did not occur on the padding, spill measurement will be use accordingly to the situation and the work area will be monitored and cleaned.
A worse accident scenario would be a leak or a spill of the radioactive solution in the instrument. The instrument will be shut down, the sample removed, and the area monitored, cleaned as necessary and surveyed.
In procedures with a volatile solution phase, the cuvettes or samples will be sealed to prevent sample evaporation. Any long term storage will require cuvettes or other sample holders with volatile solution phases to be stored sealed in secondary containers.
14. CONTROL MEASURES: Describe the procedures and equipment used to limit external dose and/or contamination.
All of the work will be performed in radioactive materials laboratories. The loading protocol will be performed in the radiochemistry laboratory at the HRC. In additional to standard PPE, the transfer will be performed in a fume hood lined with a disposable pad to control contamination. Standard contamination controls will be used, which include smear surveys at the end of the experiment (transfer), personnel monitoring (frisker, portal monitor), and hand-held detectors. The laboratory is also surveyed weekly, in addition to the end of experiment testing.15. MONITORING: Describe the procedures and equipment used to assess external dose and/or contamination.
Contamination control/monitoring protocols developed for the radiochemistry laboratories will be used for this work.Loading Protocol: Handheld survey equipment (A/B probes, GM pancake). Smear Surveys (gas proportional counter). Portal Monitor.
16. RADIOACTIVE WASTE DISPOSAL: Describe the radioactive waste that will be produced and how it will be managed.
The primary waste stream expected will be the unused samples (if not recovered for experimental use) and the instrument waste, which will contain the activity used in the analysis diluted in a solvent matrix. This solution will be collected either for recovery of the radionuclides for future experiments or for disposal with the wastes from the radiochemistry laboratories. In addition, potentially contaminated PPE (gloves, etc.) and associated materials (disposable pads, paper towels, kimwipes) will be generated from the transfer, loading, and handling of materials in this experiment. This waste material will also be disposed with other wastes from the radiochemistry laboratory. Waste materials generated during the protocol will be treated as potentially contaminated by radioactive material, and disposed of in the radioactive waste (regular, glass and liquid) for the radiochemistry labs.17. EMERGENCY PROCEDURES: Describe or reference.
For a spill during the loading of the sample, or during the analysis, the spilled sample will be capped and transferred to the secondary containment on radioactive padding inside the hood. Absorbent material will be used to sorb any residual liquid.For a spill, the following actions will be performed, depending on severity. The authorized user will be notified for any spill. The RSO will be notified in the case of personal contamination (i.e., facial), cuts, abrasions, or 10 times in access of administration limits listed in the radiation safety manual. The relevant control administrative limits for the radiation laboratories are restricted area. The contamination control limits are:
Area / Alpha (DPM/100 cm2) / Beta/Gamma (DPM/100 cm2)
Uncontrolled / 11 / 110
Controlled / 22 / 550
Restricted / 110 / 1100
The RSO should be contacted is a spill exceeds 1100 DPM/100 cm2 for alpha or 11000 DPM/100 cm2 for beta/gamma
The general treatment of a spill is below.
· The spill is to be stopped.
· Others are to be warned of the spill.
· The area should be isolated.
· The spread of activity and cross contamination is to be minimized.
· The area is to be secured to prevent further contamination.
18. RSO Conditions/Comments: Describe or reference.