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3. Analytical Methods
This section describes parameters to be analyzed and appropriate analytical
methods for analyzing the samples collected. A discussion on the appropriate
detection limits and laboratory certification is provided. Applicable
Standard Reference Methods are also identified.
3.1 Parameters to be Analyzed
3.1.1 Air
Air samples should be analyzed as required by regulations or permits.
Where specific requirements are not specified in regulation or permits,
samples from air monitoring should be analyzed for (at a minimum):
- CEPA-toxics (i.e., inorganic arsenic compounds, inorganic
cadmium compounds, lead, mercury and oxidic, sulphidic and soluble
inorganic nickel compounds);
- particulate matter (PM, PM10 and PM2.5);
and
- sulphur dioxide.
It is recommended that a full metals scan should be conducted on air
samples.
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3.1.2 Water
Water samples should be analyzed as required by regulations or permits.
Relevant parameters to be measured for the Metal Mining Effluent Regulation
are arsenic, copper, lead, nickel, zinc, total suspended solids, radium
226, total cyanide, pH, aluminum, cadmium, iron, manganese, molybdenum,
mercury, selenium, uranium, fluoride, total ammonia nitrogen, nitrate+nitrite,
total phosphorus, chloride, sulphate, calcium, magnesium, potassium,
sodium, conductivity, hardness, alkalinity and acidity.
Where specific requirements are not specified in regulation or permits,
wastewater samples should be analyzed for (at a minimum):
- CEPA-toxics;
- total suspended solids; and
- pH.
It is recommended that a full metals scan should be conducted on water
samples.
The samples should also be analyzed for other parameters that can be
used to characterize the discharge (e.g., fluoride, chloride, magnesium,
calcium).
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3.1.3 Parameters Not Present
When it is believed that a particular parameter is not present in the
releases based on technical knowledge and experience of the facility,
analysis for this parameter should be periodically undertaken, but is
not necessary on every sample. Documentation should be maintained to
validate that the parameter is not present in the releases including
reasons the parameter is unlikely to be released. However, when significant
changes to process inputs or processes have occurred, analysis for all
parameters should be conducted.
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3.2 Analytical Methods
The selection of analytical methods should be appropriate to meet the
data quality objectives. Methods selected should be generally accepted
and in common use in laboratories in Canada. A list of reference documents
on analytical methods which may be applicable to the BMSS are presented
in Section 3.5.
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3.3 Laboratory Certification
In 1994, the Canadian Association for Environmental Analytical Laboratories
(CAEAL) and the Standards Council of Canada (SCC) signed a partnership
agreement, producing a formal accreditation program for environmental
laboratories across Canada. Under the jointly administered program, CAEAL
conducts site audits and evaluates each laboratory's performance at regular
intervals, and SCC grants accreditation to the laboratory on CAEAL's
recommendation. Laboratories are assessed in accordance with ISO standards.
To obtain SCC/CAEAL accreditation, each laboratory must comply with Canada's
national standard, called the Requirements for the Competence of Environmental
Laboratories, which is based on ISO Guide 25 and addresses specific quality
and technical aspects related to environmental laboratories. More information
on these standards are provided in Section 4.3 on Reference Documents
for Quality Assurance/Quality Control.
It is recommended that all environmental samples be analyzed by a SCC/CAEAL
accredited laboratory. A list of SCC/CAEAL accredited laboratories can
be found on the SCC web-site at www.scc.ca/certific/labs.html.
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3.4 Detection Limit Issues
A detection limit is "the smallest concentration or amount of parameter
or analyte that can be measured with a stated level of confidence or
quality assurance". A laboratory method detection limit (LMDL) can
be defined as the "detection limit calculated and stated by the
laboratory performing the analysis". The LMDL is determined through
standard methods such as the USEPA Definition and Method for MDL, 40
CFR (7-1-95 Edition) Part 136, Appendix B Definition And Procedure For
The Determination Of The Method Detection Limit.
Laboratory method detection limits are specified in Environment Canada's
Guidance Document for the Sampling and Analysis of Metal Mining Effluents.
Method detection limits may also be specified in other federal or provincial
guidelines.
The Mining Association of Canada (Data Integrity Group) in the its Guideline
for Reporting ARET Data recommends that the LMDL be 2 to 10 times
lower than the government-regulated discharge limits for the facility.
The MAC Guideline explains that this recommendation is based on practices
in Ontario where the Ministry of Environment has developed a list of
Regulatory Method Detection Limits (RMDL) which specify maximum allowable
value for a LMDL. The Ontario Ministry of Environment recommends that
the LMDL be about half the RMDL. For example, if the RMDL is 0.50 mg/L,
the LMDL should be about 0.25 mg/L. Also, the LMDL should not be less
than 1/10th the RMDL. The MAC concluded
that a recommendation based on the RMDL was not possible, since RMDL
only applies to Ontario operations.
The laboratory method detection limit (LMDL) should be limits specified
in Environment Canada's Guidance Document for the Sampling and Analysis
of Metal Mining Effluents or 2 to 10 times lower than the government-regulated
discharge limits for the facility, where requirements are not specified.
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3.5 Standard Reference Methods
The following methods may be applicable to the analysis of samples from
the Base Metals Smelting Sector.
3.5.1 Air
The list of methods presented in the section on sampling air releases
(Section 2.3.1) contain guidance on analysis of the samples and may be
applicable to the analysis of samples obtained from stack testing of
air releases from the Base Metals Smelting Sector.
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3.5.2 Water
The following methods may be applicable to the analysis of water samples
from the Base Metals Smelting Sector:
- Environment Canada's Guidance Document for the Sampling
and Analysis of Metal Mining Effluents
- This document discusses sampling and chemical analysis considerations
and procedures for use with metal mining effluents. The document stresses
performance- based methods and how such methods should be applied to
the mining industry. Data quality measures and objectives and overall
quality control procedures are outlined for effluent sampling and analysis.
References to suitable analytical methods are also provided.
- Standard Methods for the Examination of Water and Wastewater31
- This comprehensive reference covers all aspects of water
analysis techniques. It includes more than 400 methods. Published jointly
by the American Water Works Association, the American Public Health
Association, and the Water Environment Federation.
- Ontario Ministry of Environment's Protocol for the Sampling
and Analysis of Industrial/Municipal Wastewater32
- This guidance document is described in the previous section
on sampling.
- British Columbia Environmental Lab Manual -For the Analysis
of Water, Wastewater, Sediment and Biological Materials.
- This electronic Manual is produced by the Ministry of Environment
Land and Parks, in cooperation with the BC Laboratory Quality Assurance
Advisory Committee. The manual is used for the analysis of water, wastewater,
sediment and biological materials.
- Biological Test Method: Acute Lethality Test Using Rainbow
Trout33
- Methods recommended by Environment Canada for performing
acute lethality tests with rainbow trout (Oncorhynchus mykiss) are
described in this report. Universal conditions and procedures are outlined
for undertaking an acute lethality test using a variety of materials.
Additional conditions and procedures stipulated are specific for assessing
samples of chemicals, effluents, elutriates, leachates, or receiving
waters. Included are instructions on care and acclimatization of test
organisms, sample handling and storage, test facility requirements,
procedures for preparing test solutions and test initiation, specified
test conditions, appropriate observations and measurements, endpoints,
methods of calculation, and the use of reference toxicants.
- Biological Test Method: Reference Method for Determining
Acute Lethality of Effluents to Rainbow Trout 34
- This document describes procedures for measuring the acute
lethality of effluents to rainbow trout and completes the guidance
provided in the generic methodology report
"Acute Lethality Test Using Rainbow Trout" (EPS 1/RM/9).
Methods are given for a single-concentration test, a multi-concentration
test, and a test with a reference toxicant. Instructions are included
on care of trout in the laboratory, facilities and water supply,
handling and storage of samples, preparation of test solutions,
test conditions, observations, endpoints, methods of calculation,
and reporting requirements.
- Biological Test Method: Acute Lethality Test Using Daphnia
spp.35
- This is the method recommended by Environment Canada for
performing acute lethality toxicity tests using daphnids (Daphnia magna
and/or D. pulex). Procedures and standard test conditions are outlined
for undertaking an acute lethality test using various samples of chemicals,
effluents, elutriates, leachates, or receiving waters. Included are
instructions on culturing conditions and requirements, sample handling
and storage, test facility requirements, procedures for preparing test
solutions and test initiation, specified test conditions, appropriate
observations and measurements, endpoints, methods of calculation, and
the use of reference toxicants.
- Biological Test Method: Reference Method for Determining
Acute Lethality of Effluents to Daphnia magna36
- This report describes procedures for measuring the acute lethality
of effluents to Daphnia magna and completes the guidance provided
in the generic methodology report
"Acute Lethality Test Using Daphnia spp." (EPS 1/RM/11).
Methods are given for a single-concentration test, a multi-concentration
test, and a test with a reference toxicant. Instructions are included
on care and culture of the daphnid crustaceans, facilities and
water supply, handling and storage of samples, preparation of solutions,
test conditions, observations, endpoints with methods of calculation,
and reporting requirements.
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