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5.2 Reagents for Alsterberg-Azide method: See method I-1575. These reagents are required
when using calibration procedure 6.3.1B.
6. Procedure
6.1 Prepare oxygen meter for calibration in accordance with the manufacturers instructions
(Notes 1. 2. 3. 4. and 5).
Note 1. A number of precautions should be observed when using the oxygen meter, particularly
when the instrument is used for field measurements. (l) Check mechanical zero before turning
meter on and adjust if necessary, (2) turn instrument on to any operational position 1 hour before
use to insure stability of operation; meter should be left on until final measurement for day is
completed. (3) Check REDLINE and ZERO and adjust as needed; If meter will not adjust to
REDLINE recharge or replace batteries, (4) Protect instrument from temperature changes that
may result from exposure to direct sunlight or contact with ice or cold wind.
Note 2. The DO probe requires periodic replacement of electrolyte and membrane. Follow
manufacturers directions but observe these points: (l) There should be no bubbles of air behind
membrane. Electrodes with pressure compensators should have the pressure compensation
membrane moved in and out with the eraser end of a pencil to insure that all bubbles are
removed from pressure compensation chamber. (2) the membrane should be smooth with no
wrinkles (3) excess membrane material should be trimmed to within 2 to 3 mm of the o-ring.
Note 3. O-rings stretch with use and must be replaced before they become loose. A common
cause of electrode malfunction is leakage of electrolyte around the O-ring seal. To check for this
problem, rinse the probe unit to remove traces of electrolyte remaining from membrane
replacement. Place the probe in a 250-mL beaker of distilled water; Measure the specific
conductance with an appropriate instrument. An increase in specific conductance indicates
leakage of the electrolyte around the o-ring. Check the probe for physical damage. Replace the
membrane and repeat the test. It may be necessary to replace the o-ring also.
Note 4. Keep DO probe in water when not in use to prevent drying out of the membrane.
Note 5. Periodically check the thermistor in the DO probe against a certified mercury
thermometer over the normal operating temperature range of the instrument. If the two readings
are not in agreement a correction curve should be constructed or an electronic adjustment should
be made to the instrument by the manufacturer or qualified service center.
6.2 Once daily, check that the instrument will read zero in a dissolved-oxygen free solution. This
may be accomplished by inserting the probe into the sodium sulfite solution and measuring
the dissolved oxygen. If instrument reading exceeds 0.2 mg/L the probe needs repair or the
membrane and electrolyte need replacement.
6.3 Calibrate the DO meter in accordance with one of the following four procedures. Procedure
A is the preferred procedure. Procedures B, C and D may be used in situations where procedure
A cannot be used. These four procedures are given in order of preference.
6.3.1A Air Calibration Chamber in water : The air calibration chamber (Yellow Springs
Instrument number 5075, or equivalent) permits calibration of the oxygen meter at the
temperature of the water in which the DO content is to be measured, thereby minimizing errors
due to temperature differences. Dip the calibration chamber into the water; pour out excess
water, and then insert DO probe into the wet chamber. This insures that the air inside the
chamber is saturated with water vapor. Caution: Be sure that no water can leak into the
calibration chamber and that the membrane has no droplets of water adhering to it since this
would reduce the rate of oxygen diffusion through the membrane and would produce erroneous
results.
6.3.2A Place calibration chamber in the water in which the DO content is to be measured. Allow
10-15 minutes for the temperature of the air inside the chamber to equilibrate with the water.
Note 6. The calibration chamber (model 5075) is designed to allow the membrane surface of the
DO probe (Model 5739) to be at ambient atmospheric pressure while in the chamber, but the
chamber is not large enough for the entire DO probe and pressure compensator to fit inside.
Since the pressure compensator must remain at atmospheric pressure care must be taken to insure
that the pressure compensator is not submerged below the water surface if method 6.3.1A is
used.
6.3.3A Read true atmospheric pressure from pocket altimeter-barometer to the nearest 5 mm of
mercury.
6.3.4A Recheck the REDLINE and ZERO reading on the oxygen meter and adjust if necessary.
6.3.5A Measure temperature in the calibration chamber to the nearest 0.5 deg. C, using the
thermistor in the DO probe.
6.3.6A Using the oxygen solubility table from section 7.2 determine the DO saturation value at
the measured water temperature and true atmospheric pressure. Apply a salinity correction if
appropriate.
Note 7. The solubility of oxygen in water decreases as salinityincreases. Oxygen saturation
values may be corrected for salinityusing the correction factors based on either chloride
concentration or specific conductance. Correction factors based on chloride concentration are
given in the oxygen solubility tab1e in section 7.2. Correction factors based on specific
conductance are also given in a table in section 7.2. The correction based on specific
conductance may be more useful since specific conductance can be easily determined from a
field measurement. The solubility of oxygen at 25!C and 760 mm of mercury in water containing
5,000 mg/L of chloride is calculated as follows using the chloride correction factors:
8.3 mg/L
5,000 mg/L Cl x 0.008 =
7.9 mg/L
(Saturation DO at
100
(Difference per
O mg/L chloride
100 mg/L chloride
and 760 mm Hg from
from section 7.2)
oxygen solubility
table)
If, in the above example, specific conductance of the water was 15,000 micromhos per cm at 25
deg. C the calculation could be made as follows using the specific conductance correction
factors:
8.3 mg/L
x
0.951
= 7.9 mg/L
(Saturation DO at (Correction factor from O mg/L chloride and
760 mm Hg from oxygen specific conductance ofsolubility table)
a temperature of 25 deg. C)
In both of the above examples the DO meter would be adjusted to 7.9 mg/L rather than 8.3 mg/L.
The YSI model 57 DO meter has a manual salinity correction builtinto the instrument. Follow
the manufacturer's instructions in its use.
The salinity value required for use with the YSI model 57 meter may be estimated from a field
measurement of specific conductance by the following equation:
Salinity, in parts per
= 0.677
l000
6.3.7A Select the scale (0-10 mg/L or 0-20 mg/L) to be used for the DO measurement and adjust
CALIBRATION control until meter reads the DO saturation value determined in 6.3.6A. Do not
change scales without recalibrating meter or verifying that identical readings are obtained on
both scales.
6.3.8A Remove probe from calibration chamber and place in water to be measured. Move probe
through water to insure a velocity of at least 1 foot per second past the probe (alternatively, a
submersible stirrer, YSI Model 5491, or equivalent may be used) to prevent localized depletion
of DO at the membrane-water interface.
6.3.9A Switch meter to TEMPERATURE; after meter reading has stabilized record temperature
to the nearest 0.5 deg. C.
6.3.10A Switch meter to the proper DO scale; after meter reading has stabilized record DO
concentration to the nearest 0.1 mg/L.
6.3.1B Calibration by Winkler titration : The DO meter is calibrated with distilled or deionized
water in which the DO concentration has been determined by the Winkler method.
6.3.2B Place 1 to 2 liters of distilled or deionized water in a large container. The water should
preferrably be near saturation with respect to DO and the water temperature should be reasonably
close to the ambient temperature. These conditions should insure that the DO concentration in
the distilled water remains constant.
6.3.3B Place DO probe in the distilled water. Maintain a velocity
of at least 1 foot per second past the DO probe with a magnetic stirrer or other means.
reading on meter is observed for a period of 4-5 minutes the water can be assumed to be
saturated.
6.3.4C Read true atmospheric pressure from pocket altimeter-barometer to the nearest 5 mm of
mercury.
6.3.5C Recheck the REDLINE and ZERO reading on the oxygen meter and adjust if necessary.
6.3.6C Measure temperature of the calibration water to the nearest 0.5 deg. C.
6.3.7C Using oxygen the oxygen solubility table from section 7.2 determine the DO saturation
value at the measured calibration water temperature and true atmospheric pressure. Apply a
salinity correction if appropriate (Note 7).
6.3.8C Select the scale (0-10 mg/L or 0-20 mg/L) to be used for the DO measurement. Turn off
aerator and adjust CALIBRATION control until meter reads the DO saturation value determined
in
6.3.7C. Do not change scales without recalibrating meter or verifying that identical readings are
obtained on both scales.
Note 9. It is essential that calibration be completed with the temperature of the calibration water
at the value measured in 6.3.6C, otherwise the calibration water may be undersaturated or
oversaturated with oxygen. If the temperature changes or later recalibration of the meter is
necessary the calibration procedure must be repeated beginning with step 6.3.2 C.
6.3.9C Remove probe from calibration container and place in water to be measured. Move probe
through water at a velocity of at least 1 foot per second (alternatively, a submersible stirrer, YSI
Model 5491, or equivalent may be used) to prevent localized depletion of DO at the membranewater interface.
6.3.10C Switch meter to TEMPERATURE; after meter reading has stabilized record temperature
to the nearest 0.5 deg. C.
6.3.11C Switch meter to the proper DO scale; after meter reading has stabilized record DO
concentration to the nearest 0.1 mg/L.
6.3.1D Air Calibration Chamber in Air: This procedure is similar to the procedure described in
6.3.1A, except that calibration is performed with the air calibration chamber in air rather than in
water. This procedure can only be used with probes that have the temperature sensing thermistor
located adjacent to the membrane. The probe must be capable of automatically compensating for
temperature changes. However, it is recommnded that this procedure not be used if the air
temperature differs from the water temperature by more than 10 degrees. Also, the calibration
chamber must be shielded from direct sunlight and wind to avoid large temperature fluctuations.
6.3.2D Wet the inside of the calibration chamber with water; pour out the excess water and insert
the probe into the wet chamber.
This insures 100 percent humidity. Allow sufficient time (10-15 minutes) for the DO probe and
air inside the calibration chamber to equilibrate. Observe precautions stated in 6.3.lD.
6.3.3D Read true atmospheric pressure from pocket altimeter-barometer to the nearest 5 mm of
mercury.
6.3.4D Recheck the REDLINE and ZERO readings on the oxygen meter and adjust if necessary.
6.3.5D Measure temperature in the calibration chamber to the nearest 0.5 deg. C using the
thermistor in the DO probe.
6.3.6D Using oxygen the oxygen solubility table from section 7.2 determine the DO saturation at
the measured temperature and true atmospheric pressure. Apply a salinity correction if necessary.
(Notes 7)
6.3.7D Select the scale (0-10 mg/L or 0-20 mg/L) to be used for the DO measurement and adjust
CALIBRATION control until the meter reading is at the DO saturation value determined in
6.3.6D. Do not change scales without recalibrating meter or verifying that identical readings are
obtained on both scales.
6.3.8D Remove probe from calibration chamber and place in water to be measured. Move probe
through water at a velocity of at least 1 foot per second (alternatively, a submersible stirrer, YSI
Model 5491, or equivalent may be used) to prevent localized depletion of DO at the membranewater interface.
6.3.9D Switch meter to TEMPERATURE; after meter reading has stabilized record temperature
to the nearest 0.5!C.
6.3.10D Switch meter to the proper DO scale; after meter reading has stabilized record DO
concentration to the nearest 0.1 mg/L.
7. Calculations
7.1 Read the concentration of dissolved oxygen in milligrams per liter directly from the meter of
the instrument.
7.2 The following table of values for the solubility of oxygen in water exposed to water-saturated
air should be used to calibrate the DO meter. The table may also be used to determine dissolved
oxygen as percent saturation at the measured temperature and true atmospheric pressure as
follows.
DO (percent saturation) = Measured DO (mg/L)/saturation DO (mg/L) x 100
8. Report
8.1 Report dissolved oxygen concentrations to the nearest 0.1 mg/L.
8.2 Report dissolved oxygen as percent saturation to the nearestpercent.
9. Precision
9.1 Precision data are not available for this method.
References
American Public Health Association and others, 1976, Standard methods for the examination of
water and wastewater (14th ed.): New York, Am. Public Health Assoc., Inc., p. 446
Brown, Eugene, Skougstad, M. W. and Fishman, M. J., 1970, Methods for the Collection and
Analysis of Water Samples for Dissolved Minerals and Gases: Techniques of Water-Resources
Inv. of the U.S. Geological Survey, book 5, ch. Al, p. 129.
Green, E. J. and Carritt, D. E., 1967, New Tables for Oxygen Saturation of Seawater: Journal of
Marine Research, p 140.