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Mercury
Work Group
Phase I Reports >> Operations Report
Executive Summary | End-of-Pipe Report |
Operations Report | Infrastructure Report
For more information,
contact David Eppstein by email at
deppstein@masco.harvard.edu,
or by calling 617-632-2860.
IV. SAMPLING AND ANALYSIS
Problem Definition:
After determining that sample analysis would be the most sure
method for ascertaining whether a suspect material might contain
low levels of mercury, the Subcommittee realized that a standardized
protocol for sample collection, field preservation, proper analytical
procedure and QA/QC measures would need to be prepared prior to
contracting the services of a DEP certified commercial testing
laboratory. Also, for cost saving purposes, the Subcommittee needed
to establish the criteria that would help ensure that competitive
pricing from commercial laboratories would be obtained in response
to a request for proposals (RFP). The Subcommittee also realized
that sampling and analytical services would potentially be required
by all three (3) of the MASCO Hospital Mercury Work Group Subcommittees,
so delineation of the types of samples involved (aqueous vs solid,
concentrated vs dilute, etc.), requirements for field sampling
support and sample identification and preservation all had to
be detailed.
Approach:
At the outset of the process, each Subcommittee was asked to identify
their respective needs for field sampling assistance, the number
of samples expected to be analyzed and the form(s) of the samples
(liquid or solid). Using these responses, the Operations Subcommittee
(taking the lead on this common effort) structured the RFP for
sample testing according to the three categories identified by
each of Subcommittees. Broadly, the categories were reagents used
in clinical and research laboratories, other chemicals used within
the institutions and biomass contained within a facility infrastructure
and wastewater.
The above efforts resulted in the preparation of a template type
Request For Proposal (RFP) as shown in Appendix H. With assistance
and technical guidance from the MWRA's, Toxic Reduction and Control
Department (TRAC), Field Sampling Unit and Central Laboratory,
standardized field and laboratory analytical protocols were developed
and incorporated in the RFP.
Hospitals wishing to have samples analyzed can take advantage
of the RFP, in whole or in part, as follows:
- Task 1 is intended for the analysis of reagents that are being
discharged from a hospital into the wastewater.
- Task 2 is intended for the analysis of biological buildup (biomass)
within the piping and is a twofold procedure (as is fully detailed
in the Pipe Cleaning Protocol presented in the Infrastructure
Subcommittee Report). A goal of the Protocol was to find a chemical
which would dislodge or dissolve the biomass buildup using only
chemical means. The theory employed was that removal of the biomass
would also remove the adsorbed mercury.
- Task 3 is intended for the analysis of samples of industrial
wastewater discharges from a facility.
The RFP outlines the parameters that should be required of a contract
laboratory when providing services relating to the collection
and proper analysis of samples for mercury. The laboratory is
asked to prepare, handle and/or analyze all samples according
to the detailed quality assurance/quality control procedures already
approved by the MWRA. Aside from the individual Task implementation
details, the following are common requirements of the RFP:
A. Certification:
- The laboratory must be fully certified by the Commonwealth
of Massachusetts and must be currently certified for mercury (code
number 212 in non-potable water).
- The laboratory must use EPA Method 245, "Cold Vapor Technique"
when analyzing samples for mercury.
B. Sample Preparation:
- Sample containers must be prepared according to QA/QC procedures.
- Sampling containers must be clean.
- Labels should be affixed to the outside of the containers with
the listed preservatives, if any, checked off.
C. Sample Collection:
- Samples must be collected according to QA/QC procedures. (Both
grab and composite sampling techniques are outlined). Field preservation
of samples must be performed according to the requirements of
40 CFR 136.3 (copy included in Appendix B). These, in part, include
preparation of duplicate and blank analyses as well as matrix
spike analyses.
- The sampler must be familiar with the inspection, calibration
and use of the sampling equipment being used.
- All sampling equipment used must be in good condition and clean.
- All samples must be recorded on "Composite and Grab Sample
Record Forms". "Chain of Custody" Forms must also
be executed. The chain-of-custody forms are to be provided by
the certified laboratory that will analyze the samples. The chain-of-custody
procedure includes recording all relevant sample collection data
on the provided form at the time that the sample label is filled
out. Data on the form must be checked to ensure that it matches
label data and data collected in the sampling log book. Relevant
information to be included on the Chain-of-Custody is:
- Laboratory name & address.
- Facility name & address.
- Sampling date.
- Date sample was received by lab.
- Date sample results due.
- Chain of custody #.
- Sample ID.
- Container (# and type).
- Preservative.
- Type of analysis required.
The chain-of-custody form is transported with the samples and
is signed, countersigned, timed and dated whenever the samples
are transferred into new custody. Copies of all forms are kept
on file.
- Arrangements between the contractor and laboratory must be
made to determine whether the samples will be delivered to the
lab or picked up by the lab.
D. Sample Analysis:
- Samples must be analyzed according to stipulated QA/QC procedures.
The director of the certified laboratory is responsible for determining
the frequency with which in-lab QA/QC procedures are conducted.
- The contract laboratory must have established experience in
the field of mercury analysis using EPA Method 245 "Cold
Vapor Technique". Appendix C contains two descriptions of
the method: Method 245.2 - Automated Cold Vapor Technique which
is used in the analysis of mercury on surface water, and Method
245.5 Manual Cold Vapor Technique which is used in the analysis
of mercury in soils and sediment. Any necessary changes in the
above techniques, (e.g. changes in dilution amounts etc.) shall
be determined by the laboratory.
- The contract laboratory must be familiar with the inspection,
calibration and use of the monitoring equipment necessary for
this type of analysis.
- All monitoring equipment must be in good working condition
and clean.
- All inspections and calibrations must be recorded.
E. Laboratory Reports:
- Laboratory Reports must include, but should not be limited
to, the following:
- Laboratory name and address.
- Date sample received and reported.
- Method used for analysis.
- Results of analysis.
Sample analysis must be completed in an efficient manner. A mercury
detection limit of not less than 1 part per billion (ppb) must
be used though 0.2 ppb is preferred. A minimum turnaround time
of 24 hours following sample receipt at the laboratory (without
premium cost escalator) is expected but negotiable. Since the
overall cost of each set of analysis would be significant, the
RFP requires the laboratory to consider the number of samples
to be taken and to offer the most economical and competitive price
rates for sample analysis.
Findings:
Following the preparation of the RFP, but before it could be issued,
the MWRA offered the services of its Central Laboratory for the
sample testing and analysis required by the MASCO Hospital Mercury
Work Group. Accordingly, the RFP was not implemented during the
course of the Work Group's tenure.
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