La. Admin. Code tit. 33 § I-5309

Current through Register Vol. 50, No. 9, September 20, 2024

Section I-5309 - Radiochemistry and Radionuclide Assay

A. General Requirements. Radiochemistry and radionuclide assay laboratories shall be subject to the requirements set forth throughout these regulations and to those specific requirements established in this Section. These are minimum specifications, and more stringent criteria may be utilized.

B. Quality Control Practices

1. The laboratory shall continually evaluate its performance for each method and matrix that includes the determination of accuracy and precision.

2. Supervisory personnel shall conduct a documented review of the data calculations and quality control (QC) results.

3. Deviations or deficiencies shall be reported to management and documented. QC data shall be retrievable for all analyses.

4. Method detection limits shall be determined and documented. Confirmation of detection limits shall be done yearly or as required by the method.

C. Quality Assurance Checks

1. Radiochemistry and Associated Radionuclide Assay. Ten percent of all analyses shall be QC, unless otherwise specified by the specific method. A minimum of three QC samples should be performed for each batch. The lab should repeat all samples if the QC check standard is outside the 95 percent confidence interval (+ two standard deviations). Samples should be performed as follows:

a. QC samples should include one spike in 10 or one spike per batch if less than 10;

b. QC samples should include one blank in 10 or one blank per batch if less than 10;

c. QC samples should include one duplicate or spiked duplicate in 10 or one duplicate per batch if less than 10; and

d. spike samples should be representative of specified regulatory limits and/or they should approach the method-specific minimum detectable activities or lower limit of detections.

2. Radionuclide Assay Other than Radiochemistry. Ten percent of all analyses shall be QC, unless otherwise specified by the method. A minimum of three QC samples should be performed for each batch. The lab should repeat all samples if the QC check standard is outside the 95 percent confidence interval + two standard deviations. Samples should be performed as follows:

a. QC samples should include one spike in 10 or one spike per batch if less than 10;

b. QC samples should include one blank in 10 or one blank per batch if less than 10;

c. QC samples should include one duplicate or spiked duplicate in 10 or one duplicate or spiked duplicate per batch if less than 10;

d. spike samples should be representative of specified regulatory limits and/or they should approach the method-specific minimum detectable activities or lower limit of detections; and

e. standard NIST traceable sources may be substituted for spike analysis.

D. General Equipment and Supplies

1. Supplies

a. Distilled and/or deionized water shall be demonstrated to be free of interferants at applicable detection limits. This may be accomplished through the use of blanks.

b. Analytical reagents shall be demonstrated to be free of interferants at applicable detection limits. This may be accomplished through the use of blanks.

c. Reference sources should be traceable to NIST or an equivalent and shall be replaced after an appropriate period of time, not to exceed five half-lives of a single nuclide or, in the case of mixed nuclide standards, they should be replaced after they have been determined to be unusable. Unusable is determined by the inability to meet calibration criteria as set forth by the method or technical manual.

2. Equipment-Auto Pipetors/Diluters

a. Apparatus having sufficient sensitivity for the application shall be used.

b. Records shall be kept showing delivery volumes are checked periodically.

c. Laboratory technicians shall periodically demonstrate the ability to properly use the equipment. This shall be documented.

E. Analytical Instrumentation. Maintenance logbook(s) shall be maintained on all instrumentation or measuring devices. Each log shall include:

1. information as set forth in LAC 33:I.5303.D;

2. calibration frequency;

3. standards used for calibration;

4. calibration history;

5. the authorized calibration personnel or institute; and

6. records of all maintenance performed.

F. Environmental Testing Equipment. Equipment used for environmental testing shall meet the following minimums:

1. low background alpha/beta counting systems:

a. the systems shall be calibrated at least yearly;

b. the systems shall be calibrated in accordance with the appropriate methodologies or their appropriate technical manual;

c. attenuation curves shall be developed for appropriate alpha/beta energies that best represent the energies of the radionuclide of concern;

d. voltage plateaus shall be performed yearly, whenever counting gas has been changed, or if major maintenance is performed to the system. If the voltage plateau changes by more than 50 volts, the calibration curves shall be performed;

e. daily backgrounds and reference source checks shall be performed when in use or weekly when not in use; and

f. sample logbooks shall be maintained for all samples that were counted/analyzed on the appropriate systems;

2. gamma spectroscopy systems:

a. the systems shall be calibrated at least yearly and shall include energy, peak width, and efficiency;

b. the systems shall be calibrated according to the appropriate methodologies or the manufacturer's technical manual;

c. daily reference source checks shall be performed when in use or weekly when not in use;

d. monthly background checks shall be performed; and

e. sample logbooks shall be maintained for all samples that were counted/analyzed on the appropriate systems;

3. liquid scintillation systems:

a. the systems shall be calibrated at least yearly and shall include energy, peak width, and efficiency;

b. the systems shall be calibrated according to the appropriate methodologies or the manufacturer's technical manual;

c. daily backgrounds and reference source checks shall be performed when in use or weekly when not in use; and

d. sample logbooks shall be maintained for all samples that were counted/analyzed on the appropriate systems;

4. alpha spectroscopy systems:

a. the systems shall be calibrated at least yearly;

b. the systems shall be calibrated according to the appropriate methodologies or the manufacturer's technical manual;

c. daily reference source checks shall be performed when in use or weekly when not in use;

d. monthly background checks shall be performed; and

e. sample logbooks shall be maintained for all samples that were counted/analyzed on the appropriate systems; and

5. analytical instrumentation not mentioned above, such as counter scalers or ionizing radiation detection equipment:

a. the instrumentation shall be calibrated at least yearly or as mandated by a specific regulatory agency such as EPA, Nuclear Regulatory Commission (NRC), or state governments;

b. the instrumentation shall be calibrated according to the appropriate methodologies or to the manufacturer's technical manual;

c. daily backgrounds and reference source checks shall be performed when in use or weekly when not in use, if applicable; and

d. sample logbooks shall be maintained for all samples that were counted/analyzed on the appropriate systems.

G. Laboratory Environment

1. Radiochemistry and radionuclide assay counting rooms, wet chemistry rooms, and sample preparation and sample storage rooms shall be physically separated. Access and egress shall be controlled.

2. Radiochemistry and radionuclide assay counting rooms shall be adequately monitored for room temperature, humidity, pressure, and electrical supply characteristics on a daily basis when in use. These characteristics shall be maintained to ensure proper operation of the analytical equipment. Records shall be maintained.

3. Adequate measures shall be taken to ensure good housekeeping in the laboratory.

H. Waste Disposal. Radioactive waste disposal shall be thoroughly documented. The documentation shall include the following:

1. quantity disposed of;

2. where the radioactive material was disposed;

3. when it was disposed;

4. who disposed of the material; and

5. activity of disposed material, as applicable.

I. Records (Control Charts)

1. Control charts shall be updated at least monthly.

2. Copies of the control charts shall be available for technician review.

3. Control charts shall have at a minimum the following information:

a. all axes labeled;

b. instrument I.D. and/or serial number;

c. one and two sigma values as well as the normal expected values; and

d. applicable units as necessary.

La. Admin. Code tit. 33, § I-5309

Promulgated by the Department of Environmental Quality, Office of the Secretary, LR 24:928 (May 1998).

AUTHORITY NOTE: Promulgated in accordance with R.S. 30:2011.