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Appendix D
5/20/2009
10
problem and reanalyzing the samples. If not enough
sample exists, the data must be qualified if reported.
9.4
Data Assessment and Acceptance Criteria for Quality Control Measures
9.4.1 The Acceptance Criteria for chlα is 0.9990. If the r
2
is less
than acceptable, the standards must be made again.
9.5 Corrective Actions for Out of Control Data
9.5.1
If the samples do not fall within the range of the standards,
they must be diluted.
10
CALIBRATION AND STANDARDIZATION
10.1
Calibration – Quarterly calibrations with standards of known
concentration are performed. Checks with a solid secondary standard are
made daily. If the solid standard has drifted more than 2.5 % from the
original calibration, the instrument is reset to that setting.
10.2
If using Anacystis nidulans algae, the concentration must be
determined by spectrophotometer.
10.3
The fluorometric standards received from Turner Designs are
certified for concentration, and are ready for use on the fluorometer.
10.4
To calibrate either the TD700 or the Trilogy, refer to the operating
manuals.
11
PROCEDURE
11.1
Sample Preparation – water column
11.1.1 Filter a known volume of water through a Whatman GF/F filter
pad (nominal pore size 0.7 µm). Only a faint color is needed on
the pad. Do not rinse the pad.
11.1.2 Fold pad in half, sample inside, wrap in aluminum foil, label and
freeze for analysis within 4 weeks.
11.1.3 Before analysis, briefly thaw pads, and then place in a 15 ml
centrifuge tube. Add 10 ml of 90% acetone.
11.1.4 Write all information in the lab notebook.
11.1.5 Using a Teflon pestle, grind the filter against the side of the tube
until the filter is well ground. If hand grinding, 10-15 seconds is
all that is necessary. Power grinding requires vigilance, because
excess heat will degrade the chlorophyll. Allow the sample to
extract for 2 - 24 hours in the dark under refrigeration. Overnight
is recommended.
11.1.6 Remove tubes from refrigerator and allow them to warm to room
temperature.