The study of the numerous specific hardware / tools of analysis is beyond the scope
of this course, but it is worth remembering that whatever tools / methods are employed for
analysis the procedures must be conducted by qualified personnel using approved methods.
The use of "test samples" or "spiked
samples" sent through an analytical laboratory is one way of testing
procedural accuracy.
2. Standardization / Calibration
Standardization and Calibration can sometimes imply different meanings to different
parties.
For the purposes of this course we will consider "standardization" to be the
daily test of a piece of equipment against known traceable
standards. Standardization is conducted to ensure a daily measurement /
operation is conducted within clearly-defined operating limits.
"Calibration" is a less frequent but equally important test of equipment by a
qualified third party. This type of
measurement may involve bringing in a certified professional or, (if a company is
sufficiently large) there may be an in-house calibration team.
Meticulous records are maintained for standardization and
calibration records: after all, these activities ensure that all
analytical procedures will be conducted using equipment operating within narrowly-defined
parameters. Quality and analytical functions often overlap with respect to standardization
/ calibration methods and records.
- Validating Standards, Methods and equipment
For analysis to be meaningful analytical data must be
referenced against known "standards". This is essential to
determine if specific hardware is functioning within exact parameters for any given
analysis. It is common for an analytical team to maintain a "library" of
catalogued reference samples. These samples are usually finite, meaning when they run out
a comparable appropriate reference sample must be used as a replacement.
Validation studies are used to validate a replacement reference material, to confirm
the performance of replacement / new hardware or systems. These are
highly
organized studies which test the extremes of the operation as well as the expected
standard operating conditions of the procedure.
Extremely precise records are needed to confirm the efficacy of validation studies:
along with process deviations and non-conforming products these studies are often a focus
of audits since their accuracy is essential to the quality of results affecting entire
procedures.
4. Sampling
Sampling is the
process
of acquiring part of a material, typically for later testing / analysis. Although this may
seem simple, there must be strict guidelines to ensure a sample is pepresentative of the
entire batch (material) that is supposed to represent. Let's examine the simple process of
acquiring a liquid sample of a material undergoing processing in a 2000L reactor. There
can be many considerations:
Obviously the simple act of taking a sample can obviously involve considerable
detail. Typically, if taking a sample is important, there will be a detailed sampling
protocol describing what hardware and methods are needed.
5. Training
Training of analytical staff may be quite detailed since it affects all aspects of
production. Training is often related to a specific test procedure can involve both
theoretical as well as hands-on training. Analytical staff are expected to demonstrate
proficiency before being signed-off on a particular function.
With particularly complex hardware the manufacturer may deliver training as part of a
technical seminar. Other analytical training will come from supervisors with appropriate
experience and background. Actual training may involve not only the procedure itself but
also the required standardization, cleaning maintenance and trouble-shooting activities.
Records of all training activities must be kept up-to-date and accessible since these
are also highly-auditable documents.
6. Cleaning, repair and maintenance of analytical hardware
Depending on the nature of the analytical system, analytical staff may be responsible
for cleaning, minor repair and maintenance, or these activities may be left to other
technicians. Cleaning may be a simple "rinse" cycle of buffer / solvent or may
be a complex protocol demanding considerable time and effort. The method should meet the
requirements of both the equipment manufacturer and industry itself and have
well-documented evidence demonstrating procedure effectiveness.
It is also important that there is a clear understanding of what types of routine
maintenance are within the scope of the analytical technicians. Analytical staff should
perform their duties within established limits and be well aware of which maintenance
procedures beyond their responsibility.
Complete, comprehensive records of all repair /
maintenance activities must be maintained for all equipment and this is
usually managed as part of the quality system.
7. Record keeping: documentation / forms
As in the production area, record-keeping and
documentation is of critical importance. These records ensure the
analytical information for any stage of production is readily available and accurate.
As expected, routine methods may employ simplified forms which are appropriately filled
in, dated, signed / initialed by the analyst. Sign-of by supervisory personnel is common.
Analytical records may be maintained as part of the "batch records" for a
particular "Lot" or production run. The location, length of maintenance and
traceability of analytical records is often a shared responsibility of the analytical and
quality functions.
Occasionally, a laboratory notebook will be used instead of official forms or records.
All the same rules previously described for production laboratory notebooks applies to
analytical notebooks. They are expected to be hardbound books with numbered pages, entries
are made in ink and errors being "stroked out" with a single line and an
initial / signature of the author acknowledging the error. Again, appropriate titling,
dates and signatures are expected. As well, these books also remain property of the
institution and may not be removed form the site as they contain critical information.
8. Documentation: work instructions//flow charts: SOP's, STM’s
STM’s (standard test methods) are the dedicated written testing procedure used
for analyses. As with production documents, STM’s are usually prepared through the
quality system and are critically reviewed for accuracy. These are comprehensive documents
describing each and every aspect of the test method in complete detail.
The same scope of responsibility applies to STMs and SOPs in analysis as those
described in the "Production" section (Chapter 2, Section 4-5). Please refer to
those examples for a review of SOP/STM details.
9. Process deviations (PD’s), non-conformance reports
(NCR’s)
Just as in production, unexpected deviations irregularities will occasionally occur
during analysis. As in production these variations must be accurately recorded as
"process
deviations" (PD); or as non-conforming product" (NCP), etc. The
analyst must accurately document changes / variations in the analytical procedure, and to
maintain an accurate record of the analyses which are "out of specification". As
in production, sign-off on this type of document will certainly require supervisory
sign-off and likely the involvement of the analytical and /or quality systems personnel.
In analysis there should not be a large number of deviations providing the method is
being appropriately applied by trained personnel.
