UNLV RM&S RSO FORM 22 University of Nevada Las Vegas Protocol for Use of Radioactive Materials 1. AUTHORIZED USER Name Thomas Hartmann 2. PROJECT NAME XRD Analysis of U-238 and Tc-99 containing materials Phone 895-1934, Cell: (208) 346-0273 3. FACILITY Building Lab MSM 234/236 SEB 1138 4. PROJECT DESCRIPTION Preparation of U-238 and Tc-99 containing materials and the subsequent analysis by X-ray powder diffraction. The maximum powder activity is 0.01 μCi for U-238 based materials (such as oxides, metals, nitrides, etc.) and 170 μCi for Tc-99-containing materials. This protocol assumes maximum activities of 0.01 μCi for U-238-based material and 170 μCi for Tc-99 based materials per experiment. The sample preparation will be performed in a HEPA filtered fume hood. The total sample amounts are 10 mg for Tc-99 and less than 30 mg for U-238 which translates to an activity of not more than 0.001 ALI by ingestion and 0.25 ALI by inhalation for U-238, as well as 0.04 ALI by ingestion and 0.24 ALI for inhalation for Tc-99. The minimum particle size achieved by grinding using agate mortars is typically 50-20 m. Under normal conditions and at typical fume hood air velocities of around 100 linear ft/minute (0.5 m/s) particles with an expected density of 6.8 g/cm3 (TcO2) and 10.97 g/cm3 (UO2) have no or very little tendency in becoming airborne. The powder is kept moist at all times by the aid of alcohol. Contamination control/monitoring protocols developed for the radiochemistry laboratories will be used for this work. Appropriate PPE will be used at all times. 1. Previously synthesized or received U-238 or Tc-99 containing samples as well as XRD line standard (Si, LaB6) will be transferred to the laboratory in MSM 234/236 using glass vials and secondary containment. 2. Samples will be placed on a tray (covered with disposable absorbent mat and moistened paper towel) in a HEPA filtered fume hood in MSM 234/236. Tc-99 based samples are prepared behind an additional β-shield. 3. Pre-Grinding: About 10 to 30 mg of the solids will be transferred to an agate mortar, suspended with few mL of alcohol (e.g. ethanol) and the mortar will be covered with Parafilm. 4. Grinding: The agate pestle will be introduced through an opening in the Parafilm to grind the samples with slow movements with the aid of ethanol to a particle size of about 50-20 m. About 5 mg of XRD line standard will be added if required and blended with the ground sample with the aid of ethanol. Hereby the solids are continuously moisturized or covered by alcohol. 5. Transfer to XRD sample holder: The ground powder will be sweep to the center of the mortar and transferred to the center of the XRD specimen holder using disposable paper-strips. 6. XRD sample preparation: The powder in the center of the holder will be suspended with few drops of alcohol and distributed as a thin layer over the Si-single crystal inlet of the airtight low-background sample holder. After the evaporation of the alcohol, the sample holder will be cleaned using ethanolwet Kimwipes and subsequently sealed by screwing on the airtight acrylic dome. 7. The outside surface of the holder will be cleaned using ethanol-moistened Kimwipes. 8. Unused sample powder will be transferred into a scintillation vial and the agate mortar/pestle will be Page 1 of 12 RAM Protocol v8 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas cleaned and stored in a desiccator. 9. XRD Measurement: The air-tight sample holder will be transferred to the XRD laboratory at SEB 1138 using secondary containment. The sample holder will be loaded into the sample stage and the XRD enclosure closed. After the analysis is completed, the sample holder will be place in the secondary containment and the sample stage surveyed for potential contamination. The sample holder will be returned to MSM 234/236 and the sample transferred into a glass vial. 10. Sample holder survey: Smears from sample holder surface will be taken and analyzed for /β contamination. 11. Survey of the work area: After the experiment is completed, the work area will be decontaminated if necessary and complete end-of-day/experiment surveys using a handheld detector (α/β probe) and swipe surveys will be performed. 5. AUTHORIZED RESEARCHERS Name Experience Name Experience Name Experience I Employee/ Student ID Thomas Hartmann NSHE1000028041 DOE-trained RadWorker for 15+ years continuously, 22 years on handling of powder, 15 + years handling radioactive powders and ceramics at KIT-INE (Germany), LANL, UNLV and INL Employee/ Ariana J. Alaniz Student ID E000133840/NSHE1000158964 2 years in handling radioactive powdered and in X-ray diffraction analysis. Completed graduate level course on X-ray diffraction Employee/ Izua J. Alaniz Student ID NSHE 1000133887 2 years of RMS chemical inventory experience, and an additional 1.5 years in biochemistry and biology lab work. 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. * 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) ALIInhalation (µCi) Tc-99 170 700 4000 700 Y 3 U-238 0.01 0.04 10 0.04 Y 3 ALIIngestion (µCi) ALI-Limiting (µCi) Potential Airborne* (Y/N) Risk Level** (1-4) Physical Form / Chemical Name Solid, mostly as oxide Solid, mostly as oxide 7. RADIATION SAFETY MATERIALS & EQUIPMENT: Check all items available to workers handling radioactive material. X Protective gloves X Lab coat X Safety glasses RAM Protocol v8 X X Warning signs/tags/tape Absorbent paper Trays Page 2 of 12 X X X Personal dosimeters Survey meter Swipe counter UNLV RM&S RSO FORM 22 University of Nevada Las Vegas Face shield Shoe covers Respirator X Secondary containers Handling tongs Shielding Other (list): 8. ENGINEERING CONTROLS: Check all items that are required. Fume hood - unfiltered X Fume hood – filtered exhaust Glove box – positive/negative pressur condary containment 9. 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) Use of powders and other finely divided solids X Other (list): Grinding, homogenizing and associated handling of wet/suspended dispersible X unsealed radioactive material 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 1. If nuclide not listed, refer to 10 CFR20, Appendix B, Table 1). None Routine X CAM X BZA 11. BIOASSAY: Check all items that are required. [Baseline bioassay and quarterly bioassay required >5 ALI dispersible (airborne). X Baseline X Quarterly Special Other 12. 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 # MSM MSM MSM 236 236 236 RAM Protocol v8 Use Fume hood (manipulating mg amounts of Tc- and U-based materials for subsequent XRD analysis) Desiccator central bench-top (storage of mg amounts U and Tc) Desiccator in glove box (storage of mg amounts U and Tc) Page 3 of 12 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas 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 Conditions During normal conditions, there is no realistic inhalation risk of RAM. The U-238/Tc-99 materials are not volatile at room temperature. Samples introduced into the XRD for analysis are fully contained within the air-tight sample holder and the instrument enclosure during the analysis. The maximum sample amounts are 30 mg for U-238 and 10 mg for Tc-99, and correspond to an activity of 0.001 ALI by ingestion and 0.25 ALI by inhalation for U-238 and 0.04 ALI by ingestion and 0.24 ALI for inhalation for Tc-99. An uptake of 5000 mrem annual radiation dose associated with this protocol is highly unlikely. Off-Normal Conditions / Accident Scenarios The most realistic accident scenario would be a potential powder spill e.g. during the sample transfer between mortar and sample holder. The worst case scenario would be the release of 10 mg Tc-99 (170 μCi) or 30 mg U-238 (0.01 μCi) into the HEPA filtered hood and its subsequent contamination. For Tc-99 the NRC lists for injection an ALI of 4000 μCi (236 mg Tc-99) and an ALI for inhalation of 700 μCi (41 mg Tc-99), and for U-238, an ALI for injection of 10 μCi (30 g U-238)and for inhalation an ALI of 0.04 μCi (120 mg U-238). Using the inhalation ALI’s as binding values, this accidental full inhalation would be far lower than 1 ALI. This worst case inhalation is very unlikely due to engineering controls (HEPA filtered fume hood). In terms of contamination, the most significant accident would be a powder spill of an entire sample. Sample masses are 30 mg total. Assuming that all of the material actually escaped the mortar, this would correspond to an activity of about 70 μCi for Tc-99, and 0.01 μCi for U-238. To mitigate the potential for powder spills during sample preparation a pre-moistened paper towel cloth will be used on top of the absorbed pads and the fume hood bottom and walls will be covered with sticky mats. There is no potential for airborne/inhalation exposure in the room MSM 234/236 from the samples under normal conditions due to particle sizes (50-20 m) and the high density of the ceramic powders 7 to 11 g/cm3. 14. CONTROL MEASURES: Describe the procedures and equipment used to limit external dose and/or contamination. All of the unsealed source work will be performed in a HEPA filtered fume hood of the radioactive materials laboratories. 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. Handheld survey equipment (A/B probes, GM pancake). Smear Surveys (A/B Scintillator or gas proportional counter). RAM Protocol v8 Page 4 of 12 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas 16. RADIOACTIVE WASTE DISPOSAL: Describe the radioactive waste that will be produced and how it will be managed. 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 discharged from the box and disposed with other wastes from the radiochemistry laboratory. 17. EMERGENCY PROCEDURES: Describe or reference. For a powder spill during the sample preparation, the spilled powder will be scooped up if easily achievable using paper strips and transferred to the secondary containment. Remaining loose powder will be fixed and removed using sticky tape. Absorbent material will be used to absorb any residual radioactive material. A pre-moistened cloth will be used as a protection layer on top of the absorption pads and also to decontaminate the area. The bottom and the walls of the fume hood are covered with sticky mats. Smear surveys will be taken to check for residual contamination. The user will be notified of the incident. For any spills involving more than 10 mg Tc-99 and 30 mg U-239, the RSO will also be notified. 18. RSO Conditions/Comments: Describe or reference. Conditions: Comments: RAM Protocol v8 Page 5 of 12 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas DECLARATION by RESEARCHER(S) I have read and understood the UNLV Radiation Safety Manual. I agree to read any additional rules or guidelines issued by UNLV or external regulatory agencies. I agree to abide by these rules or to discontinue working with radioactive material. Date Insert additional boxes as needed. Date PROTOCOL REVIEW AND WALKTHROUGH Authorized User Print Name Thomas Hartmann Date Sign Exp. Date PROTOCOL APPROVAL Radiation Safety Officer (if required) Print Name Date Sign Exp. Date RAM Protocol v8 Page 6 of 12 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas ATTACHMENT 1 ACTIVITY LIMITS FOR UNLV RADIATION SAFETY LEVELS FOR RADIOACITVE MATERIALS Limiting Values - Radiological Health* Nuclide Am-241 Am-242m Am-243 Ba-133 C-14 Cd-109 Cl-36 Cm-244 Cm-248 Co-57 Co-60 Cs-137 Eu-152 Eu-154 Eu-155 Gd-148 H-3 Hf-175 I-125 I-131 Mn-54 Na-22 Np-237 P-32 P-33 Pb-210 Po-210 Pu-236 Pu-238 Pu-239 Pu-240 Pu-241 Pu-242 Ra-226 Sb-125 Sm-147 Sr-85 Sr-90 Tc-99 Tc-99m Th-229 Th-230 Th-232 Tl-204 U-232 U-233 U-235 U-238 Zn-65 Zr-95 ALI Ingestion (µCi) 0.8 0.8 ALI Inhalation (µCi) 0.006 0.006 0.8 2,000 2,000 300 2,000 1.0 0.2 4,000 200 100 800 500 4,000 10 80,000 3,000 40 30 2,000 400 0.5 600 6,000 1.0 3.0 2.0 0.9 0.8 0.8 40 0.8 2.0 2,000 20 3,000 30 4,000 80,000 0.6 4.0 0.7 2,000 2.0 10 10 10 400 1,000 0.006 700 2,000 40 2,000 0.010 0.002 700 30 200 20 20 90 0.008 80,000 900 60 50 800 600 0.004 400 3,000 20 0.60 0.020 0.007 0.006 0.006 0.30 0.007 0.60 500 0.070 2,000 4.00 700 200,000 0.001 0.006 0.001 2,000 0.008 0.040 0.040 0.040 300 100 RAM Protocol v8 Rad Level 1** Rad Level 2 Less Than (µCi) 0.000060 0.000060 If NOT Airborne Less Than (µCi) 40 40 If Airborne Less Than (µCi) 133 133 Limiting ALI (µCi) 0.01 0.01 Not Airborne & Less Than (µCi) 0.80 0.80 133 2.86 1.00 7.50 1.00 100 100 5.71 6.67 0.50 40 25 44 1,250 1.00 3.33 0.67 0.60 2.50 0.67 125 1.50 2 0.05 5.00 100 129 133 133 133 114 3.33 4.00 286 1.50 7.50 5.71 0.40 667 667 700 1.00 250 250 250 250 1.33 10 0.01 700 2,000 40 2,000 0.01 0.002 700 30 100 20 20 90 0.01 80,000 900 40 30 800 400 0.004 400 3,000 1.00 0.60 0.02 0.01 0.01 0.01 0.30 0.01 0.60 500 0.07 2,000 4.00 700 80,000 0.001 0.01 0.001 2,000 0.01 0.04 0.04 0.04 300 100 0.000060 7.00 20 0.400 20 0.00010 0.000020 7.00 0.300 1.00 0.200 0.200 0.900 0.000080 50 9.00 0.400 0.300 8.00 4.00 0.000040 4.00 50 0.010 0.0060 0.00020 0.000070 0.000060 0.000060 0.0030 0.000070 0.0060 5.00 0.00070 20 0.040 7.00 50 0.000009 0.000060 0.000010 20 0.000080 0.00040 0.00040 0.00040 3.00 1.00 0.80 2,000 2,000 300 2,000 1.00 0.20 4,000 200 100 800 500 4,000 10 5,000 3,000 40 30 2,000 400 0.50 600 5,000 1.00 3.00 2.00 0.90 0.80 0.80 40 0.80 2.00 2,000 20 3,000 30 4,000 5,000 0.60 4.00 0.70 2,000 2.00 10 10 10 400 1,000 40 50,000 50,000 50,000 50,000 50 10 50,000 50,000 50,000 50,000 50,000 50,000 500 50,000 50,000 2,000 1,500 50,000 50,000 25 50,000 50,000 50 150 100 45 40 40 2,000 40 100 50,000 1,000 50,000 1,500 50,000 50,000 30 200 35 50,000 100 500 500 500 50,000 50,000 Ratio Ingestion /Inhalation Page 7 of 12 Rad Level 3 Rad Level 4 If Airborne Less Than (µCi) 0.30 0.30 If NOT Airborne Less Than (µCi) 800 800 0.30 35,000 50,000 2,000 50,000 0.50 0.10 35,000 1,500 5,000 1,000 1,000 4,500 0.40 50,000 45,000 2,000 1,500 40,000 20,000 0.20 20,000 50,000 50 30 1.00 0.35 0.30 0.30 15 0.35 30 25,000 3.50 50,000 200 35,000 50,000 0.05 0.30 0.05 50,000 0.40 2.00 2.00 2.00 15,000 5,000 800 1,000,000 1,000,000 300,000 1,000,000 1,000 200 1,000,000 200,000 100,000 800,000 500,000 1,000,000 10,000 1,000,000 1,000,000 40,000 30,000 1,000,000 400,000 500 600,000 1,000,000 1,000 3,000 2,000 900 800 800 40,000 800 2,000 1,000,000 20,000 1,000,000 30,000 1,000,000 1,000,000 600 4,000 700 1,000,000 2,000 10,000 10,000 10,000 400,000 1,000,000 6.00 700,000 1,000,000 40,000 1,000,000 10 2.00 700,000 30,000 100,000 20,000 20,000 90,000 8.00 1,000,000 900,000 40,000 30,000 800,000 400,000 4.00 400,000 1,000,000 1,000 600 20 7.00 6.00 6.00 300 7.00 600 500,000 70 1,000,000 4,000 700,000 1,000,000 0.90 6.00 1.00 1,000,000 8.00 40 40 40 300,000 100,000 6.00 6.00 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas * USNRC 10 CFR20 Appendix B Table 1. Revised Aug 11 2010. ** See "UNLV Guideline for Risk Assessment and Control of Radioactive Materials" for details on derivation of risk level limits. Note: If nuclide is not listed, refer to 10 CFR 20, Appendix B, Table 1 Note: Green indicates limit is set to control the potential for FACILITY contamination. RAM Protocol v8 Page 8 of 12 UNLV RM&S RSO FORM 22 University of Nevada Las Vegas Rad Safety Level Risk Level MINIMAL RISK: Unlikely to produce a dose to a Worker greater than 100 mrem. ATTACHMENT 2 UNLV RISK ASSESSMENT and CONTROL GUIDELINE for UNSEALED-RADIOACTIVE MATERIALS Activity per Experiment * Control Measures (all apply) Bioassay Requirement and Periodicity ≤ .01 ALI-Ingestion None General supervision by the Authorized User Max. = 50 µCi None Instruction to Workers on rad risks and proper handling procedures (1 ALI intake = 5000 mrem, 0.01 ALI intake = 50 mrem) 1 Air Monitoring In procedures and post use survey by Worker Monthly inspection and quarterly survey by Radiation Safety Office LOW RISK: Possible to receive an annual dose in excess of 5 rem. Mitigated by the Worker: 2 understanding, and applying good health physics work practices and procedures use of engineering and contamination control measures Non Airborne >.01 to ≤ 1.0 ALI-Ingestion Airborne ≤ .01 ALI-Limiting All Max. = 5 mCi (1 ALI intake = 5000 merm) RAM Protocol v8 Instruction to Worker on rad risks and proper handling procedures None . Review, understand and apply research protocol Lab specific training by Authorized User followed by routine supervision In-procedure monitoring and post use surveys by Worker Monthly inspection and quarterly survey by Radiation Safety Office Page 9 of 12 None None None . UNLV RM&S RSO FORM 22 University of Nevada Las Vegas ATTACHMENT 2 UNLV RISK ASSESSMENT and CONTROL GUIDELINE for UNSEALED-RADIOACTIVE MATERIALS (cont.) Rad Safety Level Risk Level MODERATE RISK: Likely to receive an annual dose in excess of 5 rem. Mitigated by: 3 the Worker has thorough knowledge of radiation safety principles and practices, plus task specific training use of engineering and contamination control measures consistent use of task specific control measures demonstrating ability to effectively control radiation hazards Activity per Experiment * (all apply) Control Measures Non-Airborne Air Monitoring Protocol approval by Authorized User and RSO > 1.0 to ≤50 ALI-Ingestion Lab specific training of Worker by Authorized User followed by routine supervision Airborne > .01 to ≤50 ALI-Limiting All In-procedure monitoring and post use surveys by Worker Max. = 50 mCi Monthly inspection and survey by Radiation Safety Office Non-airborne > 10 ALI (ingestion) requires fume hood Airborne RAM Protocol v8 Bioassay Requirement and Periodicity Page 10 of 12 ≥ 0.01 ALI (limiting), requires fume hood ≥ 10 ALI (limiting), requires negative pressure glove box Baseline bioassay and quarterly bioassay required >5 ALI (limiting) dispersible-airborne Routine air monitoring required if > 0.01 ALI (inhalation) of dry, dispersible material. Continuous air monitoring required if >0.1 ALI (inhalation) of dry, dispersible material. Breathing Zone Air-sampling (BZA) is required when working with ≥ 1 ALI (inhalation) dry, dispersible materials (airborne). UNLV RM&S RSO FORM 22 University of Nevada Las Vegas ATTACHMENT 2 UNLV RISK ASSESSMENT and CONTROL GUIDELINE for UNSEALED-RADIOACTIVE MATERIALS (cont.) Rad Safety Level Risk Level HIGH RISK: Very likely to receive an annual dose in excess of 5 rem. Mitigated by: 4 the Worker has advanced knowledge in radiation safety principles and practices, plus task specific training and procedures consistently using task specific control measures Activity per Experiment * (all apply) Non-Airborne >50 to ≤ 1,000 ALI-Ingestion Airborne > 50 to ≤1,000 ALI-Limiting All Max. = 1000 mCi demonstrating the ability to effectively control radiation hazards Control Measures Air Monitoring Protocol approval by Authorized User and RSO Authorized User MUST be present in lab Initial applied training of Worker by Authorized User followed by routine supervision In-procedure monitoring and post use surveys by Worker Weekly survey by Authorized User/Staff Monthly inspection and survey by Radiation Safety Non-Airborne ≥100 ALI-(limiting), requires negative pressure glove box Airborne ≥ 10 ALI (limiting), requires negative pressure glove box - 1,000 ALI (limiting) maximum RAM Protocol v8 Bioassay Requirement and Periodicity Page 11 of 12 Baseline bioassay and quarterly bioassay required. Work activity review by the Radiation Safety Office may increase bioassay frequency. Continuous air monitoring required Breathing Zone Air-sampling (BZA) required . UNLV RM&S RSO FORM 22 University of Nevada Las Vegas ATTACHMENT 2 UNLV RISK ASSESSMENT and CONTROL GUIDELINE for UNSEALED-RADIOACTIVE MATERIALS (cont.) NOTE: * See Attachment 1, Activity Limits for UNLV Radiation Safety Levels for Radioactive Materials, for listing of activity levels by individual nuclide. Abbreviations: ALI Annual limit on intake. ALI-Limiting Lowest ALI for either ingestion or inhalation for a given nuclide. Assumed Protection Factors: - Airborne: Open Bench 1X Fume Hood 1,000X Negative Pressure Glove Box 100,000X - Non-Airborne: Open Bench 1X Fume Hood 10X Negative Pressure Glove Box 1,000X Definitions – Annual limit on intake (ALI): As defined in Title 10, Section 20.1003, of the Code of Federal Regulations (10 CFR 20.1003), ALI is “the derived limit for the amount of radioactive material taken into the body of an adult worker by inhalation or ingestion in a year. ALI is the smaller value of intake of a given radionuclide in a year by the reference man that would result in a committed effective dose equivalent of 5 rems (0.05 Sv) or a committed dose equivalent of 50 rems (0.5 Sv) to any individual organ or tissue. (ALI values for intake by ingestion and by inhalation of selected radionuclides are given in Table 1, Columns 1 and 2, of appendix B to §§ 20.1001`20.2401)." RAM Protocol v8 Page 12 of 12