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Technical Operations
This section provides the reader with a view of the internal
working and protocols of Val Associates.
Sampling Procedures:
Poor sampling protocols can not be overcome at
the laboratory. Therefore, Val Associates field technicians work
closely with the sample custodian to ensure that all projects
are coordinated correctly. Val Associates uses the following publications
to ensure that sampling methods and equipment are within current
regulatory guidelines: NJDEPE's Field Sampling Procedures Manual,
May 1992; EPA/SW - 846, "Test Methods for Evaluation Solid
Waste Physical/Chemical Methods", Third Edition, USEPA, 1986;
EPA 600-4-82-029, "Handbook for Sampling and Sample Preservation
of Water and Wastewater", September 1982. Specific Guidelines
for a project for a sample site selection, selection of sampling
equipment, types of samples to be collected, standard sample collection
procedures, specific maintenance and calibration procedures for
sampling equipment and other and other considerations are based
upon site specific requirements.
Sample Receipt:
The laboratory sample custodian is responsible
for accepting custody of samples from the client. Samples to be
submitted must be accompanied by a chain of custody or company
letterhead with specific instructions on analysis, QA/QC formats,
sample preservation and any other information pertinent to the
project. The sample custodian will then check the chain of custody
against samples being submitted. At this time any discrepancies
will be resolved before samples are accepted. Information such
as date and time of acceptance, sample condition, sample temperature,
etc. will be noted on the chain of custody.
Samples accepted by the sample custodian are then
logged in on the computer, assigned an individual sample number
and placed in the appropriate storage area. All refrigerators
are kept at 4 Celsius and are monitored daily for temperature.
Sample Analysis:
Each analyst is responsible for obtaining samples
and returning them to the proper storage areas. The analyst is
required to document all analysis in the various laboratory notebooks,
which are dated. Analysis may also be traced through data reporting
sheets, extraction logbooks, etc
Analytical Procedures:
Val Associates employs only state and/or EPA approved
methods, unless a special request from the client requests otherwise.
Analytical methods and Quality Assurance protocols are based on
the following technical publications:
EA/SW-846, "Test Methods for Evaluation solid
Waste Physical/Chemical Methods", Third Edition, USEPA, 1986;
"Guidelines Establishing test Procedures
for the Analysis of Pollutants", Code of Federal Regulations
Vol. 40, No. 136;
:"Standard Methods for the Examination of
Water and Wastewater", 14th., 15th and 16th. Editions;
"Methods for Chemical Analysis of Water and
Wastes", EPA 600/4-79-020, March 1983, EMSL;
Data Collection, Validation and Reporting:
The list under Responsibility for Actions taken through the Verification
and Validation process are discussed.
- Analyst - responsible for the actual analyses
performed. If several types of analyses are performed there
will usually be more than one analyst. The data is documented
in a log book and results are entered into the LIMS.
- Analyst - responsible for verifying that the
results on the report are accurate and precise to the raw data
and log books that are also checked for accuracy.
- Word Processor - responsible for printing the
report from the LIMS including the results going to the client.
- QA/QC Manager - responsible for reviewing at
least 10% of all project files. He/she is to assure that all
steps documented are accomplished as stated. He/she will take
corrective action and proceed further with an investigation
if protocol is not adhered to.
- Laboratory Manager - ultimately responsible
for assuring that the report going to the client is accurate
according to the data provided. Final approval for release of
the report from the laboratory is given. The Lab Manager has
the authority to designated specified personnel to manage this
responsibility.
Analytical data is generated by the GC/MS computer
software; the GC software; the ICAP/AA computer; ion chromatograph;
and associated laboratory instrumentation. Outputs include identifications
of compounds, concentrations, retention times, and comparison
to standards. Outputs are in graphic form (chromatograms), bar
graph (spectra), and printed tabular form, and are in standard
formats specified for each analysis. If incomplete or incorrect
outputs are received, corrective actions are taken according to
the procedures established for each type of analysis, consistent
with manufacturer recommendations.
In the data review process, the data is compared
to information such as the sample history, sample preparation,
and QC sample data to evaluate the validity of the results. Corrective
action is minimized through the development and implementation
of routine internal system controls. Analysts are provided with
specific criteria that must be met for each procedure, operation
or measurement system.
Data Validation includes dated and signed entries
by Analysts on worksheets and logbooks used for all samples; the
use of sample tracking and numbering systems to tract the progress
of samples through the laboratory; and use of quality control
criteria to reject or accept specific data. Data validation is
documented by having each person who checks output, calculations,
units, QC data acceptability, etc., date and sign each document
as it is checked.
Steps and checks used to validate precision and accuracy
of the measured parameters, and to support the representatives,
comparability and completeness include:
- Description of the calibration performed
- Description of routine instrument checks (noise
level, drift, linearity, etc.)
- Documentation of the tract ability of instrument
standards, samples and data
- Documentation of analytical methodology and
QC methodology
- Description of the controls taken to determine
and minimize interference contaminants in analytical methods
(use of reference blanks and check standards for method accuracy
and precision)
- Description of routine maintenance performed;
and
- Documentation of sample preservation and transport
when shipped elsewhere
Data Reporting Format:
All laboratory test reports must contain the following information:
- Complete laboratory identification and certification
number
- Date and time of analysis, sample preparation
and sampling
- Project number or unique identification number
- Sufficient description of test items(s) or
parameter being tested
- Relevant analytical reference(s) including
method numbers
- Signature of responsible part (Lab Manager
or designee)
- Dilution factors
- Sample mdl's and
- Units of quantitative measurement i.e., mg/l.
Reporting Archiving Inorganics - All bench worksheets
containing data, calculations and observations shall be bound.
Organics - All data, calculations and observations recorded on
worksheets shall be inserted into the specific project files of
the GC/MS and GC laboratories. Instrument printouts, including
qualification reports, integrator peak areas, gravimetric analysis
reports and all other computer generated reports shall be filed
in the specific project folder.
Calibration and maintenance records for laboratory
instruments shall be maintained for the lifetime of the instrument.
Records for equipment no longer in use shall be removed form the
lab to prevent confusion with active records.
Notebooks shall be labeled with the proper subject
and sequence number and shall be kept in the central records area
of the lab. When retire, notebooks shall be placed into the inactive
storage area. All test reports shall be filed alphabetically according
to client name in the test file. LIMS data is backed up on a daily
basis and a copy is kept off site. All records are kept for a
minimum of 5 years.
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