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OHIO DEPARTMENT OF HEALTH
BUREAU OF RADIATION PROTECTION
Date Page
02/20/2014 1 of 5
Title
Acceptable TENORM Analytical Methods for Radium-226 and Radium-228
1. Purpose
The Ohio Department of Health (ODH) has established this list of acceptable
analytical methods for assaying Radium-226 (Ra-226) and Radium-228 (Ra-228) to
assist disposal site operators in verifying that:
 All waste containing Technologically Enhanced Naturally Occurring Radioactive
Material (TENORM) has been accurately assayed for Ra-226 / Ra-228 using an
ODH acceptable analytical method; and
 The reported “combined Ra-226 / Ra-228” concentration for waste being received
for disposal, satisfies the exempt TENORM concentration criteria listed in
paragraph (A) of rule 3701:1-43-07 of the Ohio Administrative Code, making the
waste acceptable for disposal at their facility. Exempt TENORM concentrations are
<5 picocuries per gram (<5 pCi/gm) excluding natural background radiation.
Natural background is 2 pCi/gm, unless an individual location submits an
alternative background concentration request and obtains approval from ODH.
 TENORM loads accepted at solid waste landfills licensed under ORC Chapter 3734
must be accompanied by lab results referencing analytical methods recognized by
this protocol.
 A representative composite sample must be obtained from each container used to
collect waste defined as TENORM.
1
Note: Taking one sample for a production operation or geographic region is not acceptable.
2. Recognized Methods
ODH recognizes the radium analytical methods published in the U.S. Department of
Energy’s document, Compendium of EPA-Approved Analytical Methods For Measuring
Radionuclides In Drinking Water, published in June of 1998.
http://www.orau.org/ptp/PTP%20Library/library/DOE/Misc/radmeth3.pdf
Table 1 – ODH acceptable analytical methods for Ra-226. This Table includes all
recognized proposed or modified methods.
Table 2 – ODH acceptable analytical methods for Ra-228. This Table includes all
recognized proposed or modified methods.
Table 3 – ODH approved In-Situ methods for radium. This Table includes all methods
that have been approved by the Director of Health.
OHIO DEPARTMENT OF HEALTH
BUREAU OF RADIATION PROTECTION
Date Page
02/20/2014 2 of 5
Title
Acceptable TENORM Analytical Methods for Radium-226 and Radium-228
Table 1. Acceptable Methods: Ra-226
Method Reference Methodology Noteworthy Features
1. Method 901.1M EPA 2009
HPGE or equivalent gamma
spectroscopy
This method does not include
specifics on sample
preparation. Sample
preparation procedure should
include 21-day ingrowth for
measuring radon daughters.
1
EPA, 1980, Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-80-
032, U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory,
August. [Available from NTIS (U.S. Department of Commerce, National Technical Information Service,
5285 Port Royal Road, Springfield, VA 22161), document no. PB80-224744.]
Table 2. Acceptable Methods: Ra-228
Method Reference Methodology Noteworthy Features
1. Method 901.1M EPA 2009
HpGE or equivalent gamma
spectroscopy
This method does not include
specifics on sample
preparation. Sample
preparation procedure should
include reporting Ra-228 in
secular equilibrium with Ac-
228
1
EPA, 1980, Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-80-
032, U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory,
August. [Available from NTIS (U.S. Department of Commerce, National Technical Information Service,
5285 Port Royal Road, Springfield, VA 22161), document no. PB80-224744.]
Table 3. Approved Methods: In-Situ - Radium
Method Reference Methodology Noteworthy Features
1. ODH In-Situ
ODH License
#03219510
000
In-situ gamma spectroscopy
using Canberra’s ISOCS
system.
This is a direct measurement
technique for analysis of
gamma emitting
radionuclides in a specific
volume of containerized
material.
OHIO DEPARTMENT OF HEALTH
BUREAU OF RADIATION PROTECTION
Date Page
02/20/2014 3 of 5
Title
Acceptable TENORM Analytical Methods for Radium-226 and Radium-228
3. Submit for Approval of a Modified or Proposed Alternate Analytical Method
for Ra-226 and Ra-228
An individual may submit to the Director of Health for:
 Approval of a modification to Ra-226 or Ra-228 analytical methods listed in
Table 1 or in Table 2; or
 Approval of a proposed alternate to Ra-226 or Ra-228 analytical methods not
listed in Table 1 or in Table 2.
Each submission shall include:
 A description of the material containing Ra-226 or Ra-228 to be analyzed,
including any physical and chemical properties that will impact the analysis;
 An evaluation of the empirical data that demonstrates the accuracy and
reproducibility of the modified or proposed alternate method; and
 A copy of the Quality Management Plan (QMP), or Quality Assurance Project
Plan (QAPP).
4. Submit for Approval of a “Modified 901.1M Ra-226 Analytical Method Based
on Direct Scan of 186.1 keV Peak”
ODH will consider approving a method for determining Ra-226 concentrations in solid
materials only based on gamma spectroscopy of the Ra-226 186.1 keV energy peak.
This modified Ra-226 186.1 keV energy peak method would not apply to the analysis
of Ra-228 so each sample would still need to be analyzed using an approved Ra-228
analytical method, such as gamma spectroscopy to assay for Ac-228.
For this modified method, Ra-226 would be measured directly by gamma
spectroscopy of its 186.1 keV gamma energy peak. However, Uranium-235 (U-235),
which would likely be present in the sample at some lesser concentration, has a
185.7 keV energy peak that interferes with a clean Ra-226 count. Therefore, a
direct count of the 186.1 energy peak, along with interference from the U-235 185.7
keV energy peak, will create a “summed” Ra-226 / U-235 peak that will over-report
the actual Ra-226 activity.
Approval of this modified method would only apply to solid waste samples containing
relatively low concentrations (< 10 pCi/g) of combined Ra-226 / Ra-228. Approved
applicants will be included in Table 1 above.
OHIO DEPARTMENT OF HEALTH
BUREAU OF RADIATION PROTECTION
Date Page
02/20/2014 4 of 5
Title
Acceptable TENORM Analytical Methods for Radium-226 and Radium-228
Pilot Study
Individuals submitting for approval of a proposed “alternate 186.1 keV energy peak
Ra-226 analysis method” shall be required to conduct a pilot study demonstrating
that their proposed method produces a conservative initial combined radium result
when compared to the combined radium result for the same sample after a 21-day
radon daughter in-growth waiting period.
The pilot study shall include:
 Analysis of a minimum of 30 solid waste samples that contain TENORM shall
be required;
 Sample preparation - each solid waste sample must be dried for minimum 12
hours at ~105° C; ground up to a fine consistency; and canned to ensure a
reproducible geometry and a radon gas leak-proof container to maximize the
in-growth of radon daughters;
 The gamma spectroscopy system to be used must have a minimum
detectable concentration (MDC) ≤ 1 picocurie per gram (pCi/g) with an
appropriate efficiency and count time to minimize the counting error;
 Each canned waste sample shall be analyzed for Ra-226 using gamma
spectroscopy. The canned waste sample shall be analyzed initially after
canning by looking at the 186.1 keV energy peak. The same canned sample
shall be analyzed a second time for Ra-226 after a 21-day radon daughter in-
growth period, this time looking at the energy peaks of the radon daughters
Lead-214 (Pb-214) and Bismuth-214 (Bi-214);
 Each canned waste sample being analyzed for Ra-228 by gamma
spectroscopy, will be looking at the Ac-228 energy peak. A second
measurement after the 21-day radon daughter in-growth period is not
necessary;
 A comparison of the gamma spectroscopy results for the post 21-day radon
daughter in-growth combined Ra-226 / Ra-228 results to the gamma
spectroscopy results for the initial combined “summed Ra-226” / Ra-228
results for all 30 canned solid waste samples.
OHIO DEPARTMENT OF HEALTH
BUREAU OF RADIATION PROTECTION
Date Page
02/20/2014 5 of 5
Title
Acceptable TENORM Analytical Methods for Radium-226 and Radium-228
Submit for Approval
Submit to the Director of Health for a 901.1M, Ra-226 analytical method based on
the direct scan of the 186.1 keV energy peak, shall include:
 Results of the pilot study that demonstrate the post 21-day radon daughter
in-growth combined Ra-226 / Ra-228 results are less than the initial
combined “summed Ra-226” / Ra-228 results. The study should also
demonstrate the accuracy and reproducibility of the method;
 A description of the material to be analyzed, including any physical and
chemical properties that will impact the analysis;
 A copy of the individual’s Quality Management Plan (QMP) and Laboratory
Quality Control Plan (LQCP). The LQCP should include requirements of:
o 10 percent of the waste samples will be analyzed in duplicate to
establish levels of precision;
o 10 percent of the waste samples will continue to be counted a second
time after a 21-day radon daughter in-growth period to verify
laboratory performance;
o Control limits based on precision and accuracy will determine the
acceptance or rejection of laboratory data on a daily basis.
 Waste sample acceptance, handling, analysis, and disposal procedures;
 A copy of the Waste Sample Analysis Report format that includes:
o Description of the waste material;
o Waste sample point of origin;
o The name of the analysis laboratory;
o The approved analytical method used; and
o Analytical results for combined Ra-226 / Ra-228 in pCi/g

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Ohio Dept. of Health Guidelines for Analyzing Samples of Oil & Gas Wastes for TENORM

  • 1. OHIO DEPARTMENT OF HEALTH BUREAU OF RADIATION PROTECTION Date Page 02/20/2014 1 of 5 Title Acceptable TENORM Analytical Methods for Radium-226 and Radium-228 1. Purpose The Ohio Department of Health (ODH) has established this list of acceptable analytical methods for assaying Radium-226 (Ra-226) and Radium-228 (Ra-228) to assist disposal site operators in verifying that:  All waste containing Technologically Enhanced Naturally Occurring Radioactive Material (TENORM) has been accurately assayed for Ra-226 / Ra-228 using an ODH acceptable analytical method; and  The reported “combined Ra-226 / Ra-228” concentration for waste being received for disposal, satisfies the exempt TENORM concentration criteria listed in paragraph (A) of rule 3701:1-43-07 of the Ohio Administrative Code, making the waste acceptable for disposal at their facility. Exempt TENORM concentrations are <5 picocuries per gram (<5 pCi/gm) excluding natural background radiation. Natural background is 2 pCi/gm, unless an individual location submits an alternative background concentration request and obtains approval from ODH.  TENORM loads accepted at solid waste landfills licensed under ORC Chapter 3734 must be accompanied by lab results referencing analytical methods recognized by this protocol.  A representative composite sample must be obtained from each container used to collect waste defined as TENORM. 1 Note: Taking one sample for a production operation or geographic region is not acceptable. 2. Recognized Methods ODH recognizes the radium analytical methods published in the U.S. Department of Energy’s document, Compendium of EPA-Approved Analytical Methods For Measuring Radionuclides In Drinking Water, published in June of 1998. http://www.orau.org/ptp/PTP%20Library/library/DOE/Misc/radmeth3.pdf Table 1 – ODH acceptable analytical methods for Ra-226. This Table includes all recognized proposed or modified methods. Table 2 – ODH acceptable analytical methods for Ra-228. This Table includes all recognized proposed or modified methods. Table 3 – ODH approved In-Situ methods for radium. This Table includes all methods that have been approved by the Director of Health.
  • 2. OHIO DEPARTMENT OF HEALTH BUREAU OF RADIATION PROTECTION Date Page 02/20/2014 2 of 5 Title Acceptable TENORM Analytical Methods for Radium-226 and Radium-228 Table 1. Acceptable Methods: Ra-226 Method Reference Methodology Noteworthy Features 1. Method 901.1M EPA 2009 HPGE or equivalent gamma spectroscopy This method does not include specifics on sample preparation. Sample preparation procedure should include 21-day ingrowth for measuring radon daughters. 1 EPA, 1980, Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-80- 032, U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, August. [Available from NTIS (U.S. Department of Commerce, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161), document no. PB80-224744.] Table 2. Acceptable Methods: Ra-228 Method Reference Methodology Noteworthy Features 1. Method 901.1M EPA 2009 HpGE or equivalent gamma spectroscopy This method does not include specifics on sample preparation. Sample preparation procedure should include reporting Ra-228 in secular equilibrium with Ac- 228 1 EPA, 1980, Prescribed Procedures for Measurement of Radioactivity in Drinking Water, EPA 600/4-80- 032, U.S. Environmental Protection Agency, Environmental Monitoring and Support Laboratory, August. [Available from NTIS (U.S. Department of Commerce, National Technical Information Service, 5285 Port Royal Road, Springfield, VA 22161), document no. PB80-224744.] Table 3. Approved Methods: In-Situ - Radium Method Reference Methodology Noteworthy Features 1. ODH In-Situ ODH License #03219510 000 In-situ gamma spectroscopy using Canberra’s ISOCS system. This is a direct measurement technique for analysis of gamma emitting radionuclides in a specific volume of containerized material.
  • 3. OHIO DEPARTMENT OF HEALTH BUREAU OF RADIATION PROTECTION Date Page 02/20/2014 3 of 5 Title Acceptable TENORM Analytical Methods for Radium-226 and Radium-228 3. Submit for Approval of a Modified or Proposed Alternate Analytical Method for Ra-226 and Ra-228 An individual may submit to the Director of Health for:  Approval of a modification to Ra-226 or Ra-228 analytical methods listed in Table 1 or in Table 2; or  Approval of a proposed alternate to Ra-226 or Ra-228 analytical methods not listed in Table 1 or in Table 2. Each submission shall include:  A description of the material containing Ra-226 or Ra-228 to be analyzed, including any physical and chemical properties that will impact the analysis;  An evaluation of the empirical data that demonstrates the accuracy and reproducibility of the modified or proposed alternate method; and  A copy of the Quality Management Plan (QMP), or Quality Assurance Project Plan (QAPP). 4. Submit for Approval of a “Modified 901.1M Ra-226 Analytical Method Based on Direct Scan of 186.1 keV Peak” ODH will consider approving a method for determining Ra-226 concentrations in solid materials only based on gamma spectroscopy of the Ra-226 186.1 keV energy peak. This modified Ra-226 186.1 keV energy peak method would not apply to the analysis of Ra-228 so each sample would still need to be analyzed using an approved Ra-228 analytical method, such as gamma spectroscopy to assay for Ac-228. For this modified method, Ra-226 would be measured directly by gamma spectroscopy of its 186.1 keV gamma energy peak. However, Uranium-235 (U-235), which would likely be present in the sample at some lesser concentration, has a 185.7 keV energy peak that interferes with a clean Ra-226 count. Therefore, a direct count of the 186.1 energy peak, along with interference from the U-235 185.7 keV energy peak, will create a “summed” Ra-226 / U-235 peak that will over-report the actual Ra-226 activity. Approval of this modified method would only apply to solid waste samples containing relatively low concentrations (< 10 pCi/g) of combined Ra-226 / Ra-228. Approved applicants will be included in Table 1 above.
  • 4. OHIO DEPARTMENT OF HEALTH BUREAU OF RADIATION PROTECTION Date Page 02/20/2014 4 of 5 Title Acceptable TENORM Analytical Methods for Radium-226 and Radium-228 Pilot Study Individuals submitting for approval of a proposed “alternate 186.1 keV energy peak Ra-226 analysis method” shall be required to conduct a pilot study demonstrating that their proposed method produces a conservative initial combined radium result when compared to the combined radium result for the same sample after a 21-day radon daughter in-growth waiting period. The pilot study shall include:  Analysis of a minimum of 30 solid waste samples that contain TENORM shall be required;  Sample preparation - each solid waste sample must be dried for minimum 12 hours at ~105° C; ground up to a fine consistency; and canned to ensure a reproducible geometry and a radon gas leak-proof container to maximize the in-growth of radon daughters;  The gamma spectroscopy system to be used must have a minimum detectable concentration (MDC) ≤ 1 picocurie per gram (pCi/g) with an appropriate efficiency and count time to minimize the counting error;  Each canned waste sample shall be analyzed for Ra-226 using gamma spectroscopy. The canned waste sample shall be analyzed initially after canning by looking at the 186.1 keV energy peak. The same canned sample shall be analyzed a second time for Ra-226 after a 21-day radon daughter in- growth period, this time looking at the energy peaks of the radon daughters Lead-214 (Pb-214) and Bismuth-214 (Bi-214);  Each canned waste sample being analyzed for Ra-228 by gamma spectroscopy, will be looking at the Ac-228 energy peak. A second measurement after the 21-day radon daughter in-growth period is not necessary;  A comparison of the gamma spectroscopy results for the post 21-day radon daughter in-growth combined Ra-226 / Ra-228 results to the gamma spectroscopy results for the initial combined “summed Ra-226” / Ra-228 results for all 30 canned solid waste samples.
  • 5. OHIO DEPARTMENT OF HEALTH BUREAU OF RADIATION PROTECTION Date Page 02/20/2014 5 of 5 Title Acceptable TENORM Analytical Methods for Radium-226 and Radium-228 Submit for Approval Submit to the Director of Health for a 901.1M, Ra-226 analytical method based on the direct scan of the 186.1 keV energy peak, shall include:  Results of the pilot study that demonstrate the post 21-day radon daughter in-growth combined Ra-226 / Ra-228 results are less than the initial combined “summed Ra-226” / Ra-228 results. The study should also demonstrate the accuracy and reproducibility of the method;  A description of the material to be analyzed, including any physical and chemical properties that will impact the analysis;  A copy of the individual’s Quality Management Plan (QMP) and Laboratory Quality Control Plan (LQCP). The LQCP should include requirements of: o 10 percent of the waste samples will be analyzed in duplicate to establish levels of precision; o 10 percent of the waste samples will continue to be counted a second time after a 21-day radon daughter in-growth period to verify laboratory performance; o Control limits based on precision and accuracy will determine the acceptance or rejection of laboratory data on a daily basis.  Waste sample acceptance, handling, analysis, and disposal procedures;  A copy of the Waste Sample Analysis Report format that includes: o Description of the waste material; o Waste sample point of origin; o The name of the analysis laboratory; o The approved analytical method used; and o Analytical results for combined Ra-226 / Ra-228 in pCi/g