Sample Procedure for Method Validation

1. Introduction

This is the metrology laboratory policy and procedure for developing and validating test or
calibration methods when no international or national procedures are available, when deviating
from standardized methods, or when no standard procedures are available.

2. Purpose

The Metrology Laboratory follows this procedure to ensure that all laboratory methods selected,
modified, or developed for tests and calibrations are appropriate for the intended use, properly
documented, validated, accepted by laboratory management, and agreed upon by the client.
Customers of the Laboratory expect a given service to provide acceptable measurement results
when they request a test or calibration. The laboratory must evaluate each method to ensure that
it has qualified and competent staff, suitable facilities, equipment, and standards with acceptable
metrological traceability to perform the test or calibration.

3. Responsibility

a. The Laboratory Supervisor or Quality Manager ensures the following, in

consultation with the laboratory staff as needed:
i. Development of methods is a planned activity and assigned to qualified
staff with appropriate resources.
ii. For larger projects, plans are updated as progress is made and effectively
communicated to all personnel.
iii. Ensure the report for the test or calibration is compliant with standard
requirements and customer needs.

b. The Technical Manager reviews the documented procedure, data and analysis,
and recommends final acceptance to the Laboratory Manager or Quality Manager
based on the procedure assessment and analysis of measurement data.

c. The Laboratory Supervisor or Quality Manager is responsible for final acceptance

of new calibration methods, training staff on the new procedure, and for
consistent implementation.

4. Operations

a. If the laboratory does not have an appropriate method for a calibration or test, or
the test or calibration requires deviation to meet the needs of the customer, the
Technical Manager is notified and this procedure is implemented.

b. When determining whether to proceed in developing new test or calibration

method to meet the needs of a customer, the Laboratory Supervisor or Quality
Manager and Technical Manager consider at least the following factors:
i. Availability of alternative procedures (national or international standards);
ii. Resources of the laboratory and staffing (time, efficiency); and

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 iii. Likely future demand for the service.

c. The staff conducting the Contract Review for the calibration or test must obtain a
clear specification of the customer requirements and the purpose of the test or
calibration including any tolerances or maximum uncertainties that are required
for the artifact’s end usage (to ensure that the measurement results will be fit for
purpose).

d. New methods must be developed prior to performing the tests or calibrations and
contain the following information:
i. appropriate identification (title);
ii. scope or range of test;
iii. description of the type of item to be tested or calibrated;
iv. parameters or quantities and ranges to be determined;
v. apparatus and equipment, including technical performance requirements;
vi. reference standards and reference materials required;
vii. environmental conditions required and any stabilization period needed;
viii. description of the procedure, including any special items as noted in this
list:
- affixing of identification marks, handling, transporting, storing and
preparation of items,
- checks to be made before the work is started,
- checks that the equipment is working properly and, where required,
calibration and adjustment of the equipment before each use,
- the method of recording the observations, data to be recorded, data
reduction, method of analysis, and presentation of results, and
- any safety measures to be observed;
ix. criteria and/or requirements for approval/rejection where applicable;
x. data to be recorded and method of analysis and presentation; and
xi. the uncertainty or the procedure for estimating uncertainty.

5. Method Validation

a. Non-standardized methods, which include all laboratory developed methods,

standardized methods modified beyond their intended scope and amplifications
and modifications of standardized methods, are validated by
i. examination to ensure completeness and compliance with requirements for
essential components of metrological traceability; and
ii. analysis of objective evidence to ensure the requirements for a specific
intended purpose are fulfilled prior to use.

b. Validation methods are to be as extensive as necessary to meet the needs of their

intended application. The accuracy and uncertainty of test or calibration results
shall be assessed for the intended use, and shall be relevant to the client’s needs.

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 c. Validation procedures and results are recorded, with a statement concerning the
appropriateness of the new method as it pertains to the intended use.

d. Validation techniques include one or a combination of the following:

i. Calibration/Verification using calibrated working standards;
ii. Comparison of results achieved with other standardized methods;
iii. Inter-laboratory comparisons when practical;
iv. Systematic assessment of factors influencing the results; and
v. Assessment of the uncertainty of results based on scientific understanding
of the theoretical principles associated with the method and practical
experience.

e. When changes are made in the validated non-standardized procedures, the

influence of such changes must be documented and, if appropriate, a new
validation process carried out.

f. The following types of assessments, with data and statistical analysis are
examples that may be used to assess the measurement results:
i. Inspection and technical assessment of the essential elements of
metrological traceability to ensure presence and adequacy (technical
review may include representatives from other laboratories, working
groups, technical experts and assessors):
i. Unbroken chain of comparisons to national and/or international
standards;
ii. Documented procedure (reviewed to ensure completeness against the
list of items in Section 4.d.);
iii. Documented measurement uncertainty (as noted in Section 4.d.v.);
iv. Demonstrated technical competence;
v. Reference to the international system of units (SI);
vi. Suitable and up to date calibration intervals for standards used in the
procedure; and
vii. Adequate measurement assurance approach and supporting data.
ii. Accuracy or Limits to Bias may use data obtained from internal testing
and/or interlaboratory comparisons: t-test, normalized error (En), absolute
or relative bias versus required tolerance limits;
iii. Precision: standard deviation, normalized precision (Pn), F-test,
comparison to required uncertainties (fit for purpose and meeting needs of
the customer)
iv. Repeatability: assessment of results over time and by different operators
following the procedure as documented
v. Reproducibility: assessment of data from other laboratories following the
procedure

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6. Implementation

a. A laboratory developed test or calibration method is validated, reviewed by the

Technical Manager, reviewed by the Quality Manager, and approved by the
Laboratory Supervisor.

b. The method is typed and formatted into a written Standard Operating Procedure
(SOP) document and assigned an identification number. The new SOP will be
added to the laboratory Master List.

c. All laboratory method validation documentation is kept on file in the laboratory

and maintained according to the Quality Management System.

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 Appendix A
Evaluation Form for Method Validation Review

Procedure Evaluated: ____________________________________

Evaluation Conducted by: ____________________________________

Method Evaluation Observations

Procedure is complete and contains:
appropriate identification (title);
scope or range of test;
description of the type of item to be tested or calibrated;
parameters or quantities and ranges to be determined;
apparatus and equipment, including technical performance
requirements;
reference standards and reference materials required;
environmental conditions required and any stabilization period
needed;
description of the procedure, including any special items as
noted in this list:
affixing of identification marks, handling, transporting,
storing and preparation of items,
checks to be made before the work is started,
checks that the equipment is working properly and, where
required, calibration and adjustment of the equipment
before each use,
the method of recording the observations, data to be
recorded, data reduction, method of analysis, and
presentation of results, and
any safety measures to be observed;
criteria and/or requirements for approval/rejection where
applicable;
data to be recorded and method of analysis and presentation;
and
the uncertainty or the procedure for estimating uncertainty.
Essential Elements of Traceability are Defined (5.f,i) See GMP 13.
Unbroken chain of comparisons. A documented system of
comparisons with each step having the essential elements of
metrological traceability going back to a standard acceptable to the
parties, usually a national or international standard; Are suitable
standards identified in the procedure?
Documented Measurement Uncertainty. The measurement
uncertainty for each step in the traceability chain must be
calculated according to defined methods and must be stated so that
an overall uncertainty for the whole chain may be calculated (see
SOP 29); Is the uncertainty budget completely defined based on a
comparison of similar procedures or technical reference
documents (describe the procedures and/or references)

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 Method Evaluation Observations
Documented Measurement Procedure. Each step in the chain must
be performed according to documented and generally
acknowledged procedures (see GMP 12) and the results must be
documented (i.e., in a calibration certificate, see SOP 1); Is the
procedure complete according to all required elements?
(4.d)
Accredited Technical Competence. The laboratories or bodies
performing one or more steps in the chain must supply evidence of
technical competence (e.g., by maintaining appropriate training
records, participating in interlaboratory comparisons, and by
demonstrating that they are accredited by a recognized
accreditation body); Have all staff been trained and have they
demonstrated competency with the procedure? Have any other
laboratories provided input or tried to duplicate the procedure?
Was an interlaboratory comparison or proficiency test conducted?
Describe the results.
Realization of SI Units. The primary national, international or
intrinsic standards must be primary standards for the realization of
the International System of Units (SI);
Documented Calibration Intervals. Calibrations of standards (and
equipment where appropriate) must be repeated at established
(may be defined through measurement assurance) and appropriate
intervals to preserve metrological traceability of the standard over
time and use (see GLP 4, GMP 11); Are suitable calibration
intervals defined for the standards used in this procedure?
Measurement assurance. A proper measurement assurance
program must be established to ensure the validity of the
measurement process and the accuracy of standard used at the time
of the measurement (see SOPs 9, 17, 20, 30). What type of
measurement assurance is integrated into the procedure? Describe
what the measurement assurance monitors (standards, process,
both? How?)
Additional Assessments
Comparison of Results with Other Procedures. Describe what
other procedures or standards were considered and why/why not
chosen? Describe the results obtained and analysis conducted with
multiple procedures.
Evaluation of Accuracy. (5.f.ii)
What are the limits to bias or error? How do you know the results
are right? Describe the recently calibrated standard/set of
standards that were used. Describe any standard reference
materials that were used. How were the results assessed for
Accuracy?

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 Method Evaluation Observations
Evaluation of Precision. How was data for repeatability obtained?
Describe whether the precision assessment is short-term or long-
term and if short-term, how do you know how the procedure will
repeat over time? How do you know whether the precision is
sufficiently small when incorporated into uncertainties? Describe
the statistical assessments that were completed and document the
analysis results.
Evaluation of Repeatability. E.g., two different units were
evaluated after a recent (enter dates) calibration by multiple
metrologists; what kind of statistics were used and what were the
results? (Consider repeatability with different staff, equipment,
standards/nominal values and not just short-term precision.)
Evaluation of Reproducibility. Have any other laboratories
provided input or tried to duplicate the procedure? Was an
interlaboratory comparison or proficiency test conducted?
Describe the results.
3rd Party Assessment or Technical Reviews. Have any other
technical experts reviewed the procedure and provided input?
Describe their assessment and any recommended improvements or
changes that were implemented as a result of the review.

This procedure has found to be complete, fit for its intended use, technically validated, meets customer needs,
and is approved for use.

Quality Manager Signature Technical Manager Signature

Quality Manager Name (Printed) Technical Manager Name (Printed)

Date Date

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