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Ref. No. [UMCES] CBL 2015-008

ACT VS15-01

9

reduced to a minimum by using a covering on the surface of the water. The test tank was

instrumented with the test instruments, as well as three factory calibrated RBR temperature

recorders (accurate to 0.02

o

C) placed near the instruments to continuously measure actual

temperature conditions experienced by the test instruments. These data were used to help

evaluate fine scale variability within the test tank and to correct for temperature offsets that

might exist during pH measurement of discrete reference samples.

The test tank pH was also monitored continuously with two glass pH electrodes

(Metrohm ECOTRODE PLUS 6.0262.100) measured to 0.1 mv, and spaced across the span of

the test instruments. These data were used to create a continuous data record of pH within the

tank, and to confirm test conditions during acid/base additions. These pH data will not be used

as reference pH data to calculate instrument offsets. The pH probes were calibrated against the

dye estimated values obtained on test tank samples during acid-base additions (at the fixed

experimental T-S conditions) to get slope responses over a pH range of approximately 7.1 to 8.3.

In this way the electrodes did not experience any change in liquid junction potential from either

freshwater or saltwater buffers (Easley and Byrne 2012).

Each week testing was conducted at a set combination of temperature and salinity (T-S).

Nominal temperature conditions were set for 10, 20 and 30

o

C, and salinity conditions were set

for nominally 0, 20 and 35 S. A week-long test was performed at each T-S combination. After

4 to 6 days of testing at a stable T-S condition and ambient pH, pH was cycled over a reasonable

range using acid-base additions to the water of the test tank (7.5 to 8.5 for seawater and 6.5 to 8.8

for freshwater). Two, raised - lowered pH cycles were conducted at each T-S condition over the

course of one day. Acid/base additions were done by first mixing known quantities of acid/base

into several liters of the current test solution and then adding this solution into the test tank to

facilitate mixing and rapid equilibration.

The sequencing of tests was to start with a fixed salinity and the tests were performed for

that salinity at the three different temperatures, starting at 10

o

C and increasing sequentially up to

30

o

C. In this way we were able to use the same source water for all three temperature

conditions. Each test was scheduled to last 1 week, except when delays were needed to

accommodate work schedules. For each new T-S test condition, the test tank was flushed and

filled with new source water while keeping all test instruments submerged and recording

continuously. Each new batch of source water was filtered through a 1 µm cartridge prior to use

in the tests.

Laboratory Test Reference Sampling -

During the stable temperature and salinity period,

reference samples were collected and analyzed at 4 timepoints each day. In addition, on one day

during the stable cycle, a burst sampling of five independent measurements was collected 5

minutes apart at one of the timepoints to evaluate the repeatability and uncertainty of the

reference measurement with respect to the variability observed within the test tank. Reference

samples were drawn directly into the spectrophotometer cell from a supply tube within the test

tank. After the cell was blanked and prior to the dye addition and spectrophotometric readings,

the temperature of the cell was measured and adjusted to within 0.1 degree or less of the tank

temperature. 10 readings of the reacted dye were recorded over 1-2 minutes for each sampling

timepoint, and a mean and standard deviation of each reference measurement was calculated.

The final temperature of the sample in the cell was recorded immediately after reading to define

any deviation from the specified reading temperature. The temperature of the sample stream was