Current through Register Vol. 54, No. 44, November 2, 2024
(a) In addition to the requirements of §
252.401 (relating to basic
requirements), laboratories performing testing or analysis of environmental
samples in the area of radiochemistry shall comply with this section.
(b) When the method selected by an
environmental laboratory in accordance with §
252.307 (relating to methodology)
contains more stringent requirements than the requirements of this section, the
environmental laboratory shall follow the more stringent requirements contained
in the method.
(c) The requirements
for initial calibration are as follows:
(1) An
environmental laboratory shall follow the initial calibration requirements of
the method or regulation.
(2)
Initial calibrations shall be performed using calibration standards that have
the same general characteristics as the associated environmental samples, for
example geometry, homogeneity and density.
(3) The initial calibration must include,
when applicable, determination of instrument background, efficiency, mass
attenuation and energy calibration.
(4) The results of testing or analysis of
environmental samples shall be determined from an initial calibration that is
not more than 12 months old and may not be determined from any continuing
calibration verification, unless otherwise required by regulation, method or
program.
(5) The details of the
initial calibration procedures including calculations, integrations, acceptance
criteria and associated statistics shall be included or referenced in the
laboratory's standard operating procedures.
(6) Raw data records shall be retained to
permit reconstruction of the initial calibration.
(d) The requirements for an instrument
suitability verification are as follows:
(1)
An instrument suitability verification standard shall be analyzed at the
beginning of each analysis day, unless a higher frequency is required in the
method or regulation.
(2) The
instrument suitability verification standard shall be a check source that
provides adequate counting statistics for a relatively short count time and is
sealed or encapsulated to prevent loss of activity and contamination of the
instrument and laboratory personnel.
(3) For alpha and gamma spectroscopy systems,
the instrument suitability verification standard must include determination of
instrument counting efficiency, energy calibration and peak
resolution.
(4) For
gas-proportional and liquid scintillation counters, the instrument suitability
verification standard must include determination of instrument counting
efficiency.
(5) For scintillation
counters, the instrument suitability verification standard must include
determination of instrument counting efficiency.
(6) Details of the instrument suitability
verification procedure including calculations, integrations, acceptance
criteria and associated statistics shall be included or referenced in the
laboratory's standard operating procedures.
(7) Raw data records shall be retained to
permit reconstruction of the instrument suitability verification.
(8) Acceptance criteria for instrument
suitability verification standards in the method or regulation shall be
followed. When there are no established criteria in the method or regulation,
an environmental laboratory shall determine internal criteria and document the
procedure used to establish the criteria.
(9) If an instrument suitability verification
standard fails the acceptance criteria, an environmental laboratory shall
initiate corrective actions.
(10)
Environmental samples not bracketed by acceptable instrument suitability
verification standards shall be reanalyzed.
(e) The requirements for an instrument
background measurement are as follows:
(1) An
instrument background check shall be analyzed every analysis day.
(2) Instrument background values shall be
subtracted from the total measured activity in the determination of the sample
activity.
(3) Each individual
background check shall be compared to the acceptance criteria in the method or
regulation. When there are no established criteria in the method or regulation,
an environmental laboratory shall determine internal criteria and document the
procedure used to establish the limits.
(4) Environmental samples associated with an
out of control instrument background check shall be reprocessed and reanalyzed
from the beginning of the method or the results reported with the appropriate
data qualifiers.
(f) The
requirements for a method blank are as follows:
(1) A method blank shall be processed along
with and under the same conditions as the associated samples including all
steps of the preparation and analytical procedure.
(2) A method blank shall be analyzed at a
minimum of one per preparation batch. When no separate preparation method is
used, such as gamma analysis in water, the batch shall be defined as no more
than 20 environmental samples that are analyzed together using the same method,
personnel and lots of reagents.
(3)
A method blank must consist of a matrix that is similar to the associated
environmental samples and is free of the isotopes of interest. When a matrix
that is similar to the associated environmental samples that is free of the
analytes of interest does not exist and cannot be prepared, reagent water or an
artificial or simulated matrix may be used.
(4) When an environmental sample is analyzed
by gamma spectrometry by placing the sample matrix into a calibrated counting
geometry, the method blank must consist of a similar counting geometry that is
filled to a similar volume with reagent water to partially simulate gamma
attenuation due to a sample matrix.
(5) The method blank result may not be
subtracted from the sample results in the associated preparation or analytical
batch unless permitted by the method or regulation.
(6) The method blank shall be prepared with
similar aliquot size to that of the routine samples for analysis. The method
blank result and acceptance criteria shall be calculated in a manner that
compensates for sample results based upon differing aliquot size.
(7) If a contaminant is detected in the
method blank, the source of contamination shall be investigated and measures
shall be taken to minimize or eliminate the contamination. A method blank is
considered contaminated if one of the following applies:
(i) The activity of a target isotope in the
method blank is at or above the reporting limit established by the method or by
regulation.
(ii) The contamination
in the method blank otherwise affects the environmental sample results as
described in the method, regulation or in individual project data quality
objectives.
(8)
Environmental samples associated with a contaminated method blank shall be
reprocessed for analysis or the results reported with the appropriate data
qualifiers.
(g) The
requirements for a laboratory control sample are as follows:
(1) A laboratory control sample must be
processed along with and under the same conditions as the associated
environmental samples, including all steps of the preparation and analytical
procedure.
(2) The laboratory
control sample must consist of a defined matrix containing known and verified
activities of isotopes. When a matrix that is similar to the associated
environmental samples that is free of the analytes of interest is not
available, reagent water or an artificial or simulated matrix may be
used.
(3) A laboratory control
sample must be analyzed at a minimum of one per preparation batch. When no
separate preparation method is used, such as gamma analysis in water, the batch
shall be defined as no more than 20 environmental samples that are analyzed
together with the same method, personnel and lots of reagents.
(4) The activity of the laboratory control
sample must be within the calibration range of the method and one of the
following:
(i) Two to ten times the detection
limit.
(ii) At an activity level
comparable to that of the environmental samples being tested or analyzed, if
the sample activities are expected to exceed ten times the detection
limit.
(5) The standard
used to prepare the laboratory control sample must be from a source independent
of the standards used for initial calibration.
(6) When a radiochemical method, other than
gamma spectroscopy, has more than one reportable isotope, for example,
plutonium, Pu 238 and Pu 239, using alpha spectrometry, only one of the
isotopes shall be included in the laboratory control sample. When more than one
isotope is present above the specified detection limit, each isotope shall be
assessed against the acceptance criteria.
(7) When gamma spectrometry is used to
identify and quantitate more than one isotope, the laboratory control sample
must contain isotopes that represent the low, for example americium-241,
medium, for example cesium-137, and high, for example cobalt-60, energy range
of the analyzed gamma spectra. The isotopes need not exactly bracket the
calibrated energy range or the range over which isotopes are identified and
quantitated.
(8) Each individual
laboratory control sample must be compared to the acceptance criteria in the
method or regulation. When there are no established criteria in the method or
regulation, an environmental laboratory shall determine internal criteria and
document the procedure used to establish the limits.
(9) Environmental samples associated with an
out of control laboratory control sample shall be reprocessed and reanalyzed
from the beginning of the method or the results reported with the appropriate
data qualifiers.
(h) The
requirements for sample duplicates are as follows:
(1) A sample duplicate shall be analyzed at a
minimum of one per preparation batch. When no separate preparation method is
used, for example gamma analysis in water, the batch shall be defined as no
more than 20 environmental samples that are analyzed together using the same
method, personnel and lots of reagents.
(2) An environmental laboratory shall
document the calculations used for determining the relative percent difference
or other statistical method for evaluation of the sample duplicate
pairs.
(3) Each sample duplicate
relative percent difference shall be compared to the acceptance criteria in the
method or regulation. When there are no established criteria in the method or
regulation, an environmental laboratory shall determine internal criteria and
document the procedure used to establish the acceptance limits.
(4) For sample duplicate results outside
established criteria, corrective action shall be documented and the affected
data reported with appropriate data qualifiers.
(i) Tracer requirements are as follows:
(1) For those methods that utilize a tracer
or internal standard, each sample result must have an associated tracer or
internal standard recovery calculated and reported.
(2) The tracer or internal standard recovery
shall be assessed against the acceptance criteria specified in the method or
regulation. When there are no established criteria in the method or regulation,
an environmental laboratory shall determine internal criteria and document the
procedure used to establish the acceptance limits.
(3) For tracer or internal standard recovery
outside established criteria, corrective action shall be documented and the
data reported with appropriate data qualifiers.
(j) Carrier requirements are as follows:
(1) For those methods that utilize a carrier,
each sample must have an associated carrier recovery calculated and
reported.
(2) The carrier recovery
for each sample shall be assessed against the acceptance criteria specified in
the method or regulation. When there are no established criteria in the method
or regulation, an environmental laboratory shall determine internal criteria
and document the procedure used to establish the acceptance limits.
(3) For carrier recovery outside established
criteria, corrective action shall be documented and the data reported with
appropriate data qualifiers.
(k) The requirements for detection limits are
as follows:
(1) A detection limit shall be
determined by the protocol in the method or regulation. If the protocol for
determining detection limits is not specified in the method or regulation, the
environmental laboratory shall select a procedure that reflects instrument
limitations and the intended application of the method.
(2) A detection limit shall be initially
determined for the isotopes of interest in each method in a matrix in which
neither the target isotope nor interferences are at a concentration that would
impact the results. The detection limit shall be determined in the matrix of
interest.
(3) A detection limit
shall be determined each time there is a change in the method that affects how
the test is performed or that affects the sensitivity of the
analysis.
(4) The sample processing
steps of the method shall be included in the determination of the detection
limit.
(5) Supporting data shall be
retained to permit reconstruction of the detection limit
determination.
(6) An environmental
laboratory shall have a written procedure to relate detection limits with
quantitation limits.
(7) The
method's lower limit of quantitation shall be established and must be above the
detection limit.
(l) Each
result shall be reported with the associated measurement uncertainty. The
procedures for determining the measurement uncertainty shall be documented and
be consistent with the method and regulation.
(m) Records of all equipment, reference
materials, reagents, and supplies shall be maintained in accordance with §
252.306 (relating to equipment,
supplies and reference materials).
The provisions of this §252.405 amended under
27 Pa.C.S. §§
4103(a),
4104 and
4105; and section 1920-A
of The Administrative Code of 1929 (71 P. S. §
510-20).