STANDARD OPERATING PROCEDURE Dissolved Oxygen Measurement, Meter Calibration and Maintenance



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Page 1 of 9 KEY WORDS- Dissolved Oxygen, calibration, probe preparation, meter preparation APPROVALS APPROVED BY: Kean S. Go, DATE: +/?? APPROVED BY: A Pement DATE: a// A/? f Lisa Ross, EHAP Senior Scientist APPROVED BY: C DATE: icer + &5/ j j9 PREPARED BY: DeeAn Jones/Andrea Hoffman Environmental Research Scientist DATE: 02/I 6199 (EHAP) organization and personnel such as management, senior scientist, quality assurance officer, project leader, etc. are defined and discussed in SOP ADMN002.

Page 2 of 9 STANDARDOPERATINGPROCEDURE 1.O INTRODUCTION 1.I Purpose To provide standardized instruction for the operation of the Yellow Springs Instruments (YSI) model 57 and 58 dissolved oxygen meters with a model 5739 probe. 1.2 Scope This document will provide specific instructions for meter and probe preparation, probe reconditioning, calibration, dissolved oxygen measurement in the field, and instrument storage. 2.0 MATERIALS 2.1 Dissolved oxygen meter model 57 or 58 2.2 Probe model 5739 2.3 KCI solution (electrolyte) 2.4 Standard size Teflon@ membrane (0.1 mm) 2.5 O-ring 2.6 Pencil with eraser 2.7 Distilled Water 2.8 Razor blade or scissors 2.9 Sanding tool 2.10 Adhesive sanding disk 2.1 I 3% ammonia solution (standard household ammonia) 2.12 Extra batteries (size C for model 57 and size D for model 58) 2.13 Flathead screwdriver 2.14 Humidity chamber 3.0 PROCEDURES 3.1 Laboratory Probe Preparation/Routine Maintenance Always handle membrane material carefully, touching at the ends only. Replace KC! solution and membrane when the membrane appears damaged, if bubbles appear under membrane or if erratic readings occur.

Page 3 of 9 3.1.1 Detach probe cord from meter. Unscrew the sensor guard, remove the O-ring and membrane, then thoroughly rinse the sensor with distilled water. 3.1.2 Rinse the sensor with KCI solution to remove distilled water. 3.1.3 Successively fill the sensor body with KCI solution while pumping the diaphragm with the eraser end of a pencil. Be very careful to avoid damaging the diaphragm and probe. Continue filling and pumping until no air bubbles appear. 3.1.4 Secure a Teflon@ membrane between your thumb and the probe body. Add more KCI solution to the probe until a large meniscus covers the gold cathode. 3.1.5 With the other hand, grasp the end of the membrane and with a continuous motion stretch it up, over and down the other side of the sensor. 3.1.6 Secure the end of the membrane under your forefinger, and roll the O-ring over the edge of the probe, being careful not to touch the membrane surface. The membrane should not contain fingerprints or wrinkles, and there should be no air bubbles under the surface. Slight wrinkles can be removed by gently tugging on the excess membrane, thereby slipping under the O-ring. 3.1.7 Trim off excess membrane with scissors or a razor, ensuring that the stainless steel temperature rod is not covered by excess membrane. 3.1.8 Shake off excess electrolyte, rinse with distilled water and reinstall the sensor guard. 3.2 Probe Reconditioning The condition of the gold cathode and silver anode are essential to successful calibration and obtaining an accurate dissolved oxygen reading. Recondition the probe if the gold cathode looks dull and tarnished or the silver anode has been contaminated (grayish). 3.2.1 Detach probe cord from meter. Unscrew the sensor guard, remove the O-ring and membrane, then thoroughly rinse the sensor with distilled water. 3.2.2 Examine the sanding tool carefully for nicks and scratches. Replace if damaged.

Page 4 of 9 3.2.3 Remove the backing from a new sanding disk and affix the adhesive side to the concave tool surface. Make sure that the disk is centered and contains no wrinkles. 3.2.4 Wet the disk with deionized water and place the abrasive face uniformly against the probe face. Slowly rotate the tool back and forth until all tarnish is removed and the gold appears bright. Excessive abrasion with shorten the life of the cathode. 3.2.5 Peel off the used disk and remove any adhesive residue from the sanding tool. Never reuse any sanding disk. 3.2.6 Rinse the probe surface with deionized water and soak the probe overnight in a 3% ammonia solution to decontaminate the anode. 3.2.7 Prepare the probe for use as described above in section 3.1. 3.3 On-site meter preparation for model 57 3.3.1 With the central meter dial set to OFF, adjust the meter pointer to zero with the screw in the center of the meter s display panel. 3.3.2 Attach the prepared probe to the PROBE connector on the meter and adjust the retaining ring so that it is finger tight. 3.3.3 Turn the meter on 15 minutes before calibrating for optimum probe stabilization. The meter is on when the central dial is set to RED LINE. The meter must remain ON until the final dissolved oxygen measurement is made for the day. 3.3.4 After reaching optimum probe stabilization, place the meter in the intended operating position. Readjustments may be necessary if the position of the meter changes. 3.3.5 Adjust RED LINE. While the central dial is on RED LINE adjust the RED LINE control knob until the meter needle aligns with the red mark at the 31 C position. Use the needles reflection in the mirror on the display panel to ensure that you are looking at the display panel straight on. When the batteries need to be replaced, the red lines will not align. 3.3.6 Switch the central dial to ZERO and adjust to zero with the ZERO control knob.

Page 5 of 9 3.4 On-site meter preparation for model 58 Model 58 has a digital display panel and does not use a RED LINE adjustment. 3.4.1 Attach the prepared probe to the PROBE connector on the meter and adjust the retaining ring so that it is finger tight. 3.4.2 Turn the meter on 15 minutes before calibrating for optimum probe stabilization. A wait is necessary whenever the meter has been OFF or the probe has been disconnected. The meter must remain ON until the final dissolved oxygen measurement is made for the day. 3.4.3 ZERO the instrument. Set the central dial switch to ZERO and with the 0, ZERO control knob adjust the display to read 00.0. 3.4.4 Set SALINITY knob to FRESH. This is the general rule when sampling fresh surface waters. If sampling different types of water, refer to operating manual. 4.0 Calibration Calibration should take place at each site where a dissolved oxygen measurement is necessary. Take temperature with alternate source, when available, (ex. EC meter) due to inaccuracy of DO temperature rod. This will give you the temperature reading you are trying to achieve on the DO meter and what temperature to calibrate for. 4.1 Calibration and DO measurements with model 57 4.1.1 Secure probe in a modified humidity chamber with a damp cloth or sponge. 4.1.2 Switch the central dial from ZERO to TEMP. 4.1.3 Set SALINITY control to FRESH. 4.1.4 Place probe (still in humidity chamber) in well mixed area of sampling site and wait for temperature to stabilize as close as possible to alternate temperature taken.

Page 6 of 9 Take the temperature reading on C scale. 4.1.5 Using the solubility of oxygen in water chart (Table I), record the maximum solubility for the measured water temperature in mg/l. Account for altitude or barometric pressure, if necessary, using section 4.3. 4.1.6 Switch central dial to CALIBRATE in the O-20 mg/l range. Adjust the CALIBRATE control knob to the value determined in 4.1.5. Use O-20 mg/l range as a general rule. If the protocol states a different range, follow the protocol. 4.1.7 Take probe out of water. Remove probe from humidity chamber. If the chamber is filled with water (or if the membrane is in contact with water), repeat calibration. 4.1.8 Place probe back into well mixed water and wait for probe equilibration by observing a stable dissolved oxygen reading for a full minute. 4.1.9 Take dissolved oxygen reading in the O-20 mg/l scale and record in mg/l. 4.2 Calibration and DO measurements with model 58 4.2.1 Secure probe in a modified humidity chamber with a damp cloth or sponge. 4.2.2 Switch central dial to TEMP. 4.2.3 Place probe (still in the humidity chamber) in well mixed area of sampling site and wait for temperature to stabilize as close as possible to alternate temperature taken. Take temperature reading on OC scale. 4.2.4 Using the solubility of oxygen in water chart (Table I), record the maximum solubility for the measured water temperature in mg/l. Account for altitude or barometric pressure, if necessary, using section 4.3. 4.2.5 Switch the central dial to 0.01 mg/l. Use 0.01 mg/l as a general rule. If this differs from the protocol, follow the protocol. 4.2.6 If locked, unlock locking ring and adjust the 0, CALIB knob to the value determined in section 4.2.4. Wait two minutes to verify stability; use locking ring to prevent inadvertent changes.

Page 7 of 9 STANDARDOPERATINGPROCEDURE 4.2.7 Take probe out of water. Remove probe from humidity chamber. If the chamber is filled with water (or if the membrane is in contact with water), repeat calibration. 4.2.8 Place probe back into well mixed water and wait for probe equilibration by observing a stable dissolved oxygen reading for a full minute. 4.2.9 Record the dissolved oxygen reading from the display panel in mg/l. 4.3 Accounting for altitude or barometric pressure 4.3.1 Use pressure/altitude chart (Table II) to determine the atmospheric correction factor. 4.3.2 Multiply the maximum solubility value (mg/l) from Table I by the Calibration Value (%) from Table II. Record. 4.3.3 Adjust the calibration knob to the corrected value. 4.3.4 Proceed with step 4.1.6 for model 57 and step 4.2.6 for model 58. 6.0 Meter/Probe storage 6.1 Between measurements and when en route to or from the field, keep the probe in the modified humidity chamber. 6.2 Upon return to the lab, disconnect the probe from the meter, remove humidity chamber, rinse with deionized water, and place probe in a flask containing water. Make sure the membrane does not come in contact with the water and that there is a good seal between the flask and probe body. Use a parafilm sheet around flask and probe to ensure a good seal, which will help maintain the relative humidity in the flask near 100%.

TABLE I. SOLUBILITY OF OXYGEN IN WATER EXPOSED TO WATER SATURATED AIR AT 760 mm Hg PRESSURE TEMP C SOLUBILITY mg/l TEMP C SOLUBILITY mg/l TEMP C SOLUBILITY mg/l 0 14.62 16 9.87 32 7.31 1 14.22 17 9.67 33 7.18 2 13.83 18 9.47 34 7.07 3 13.46 19 9.28 35 6.95 4,13.11 20 9.09 36 6.84 5 12.77 21 8.92 37 6.73 6 12.45 22 8.74 38 6.62 7 12.14 23 8.58 39 6.52 8 11.84 24 8.42 40 6.41 9 11.56 25 8.26 41 6.31 10 11.29 26 8.11 42 6.21 11 11.03 27 7.97 43 6.12 12 10.78 28 7.83 44 6.02 13 10.54 29 7.69 45 5.93 14 10.31 '30 7.56 46 5.84 15 10.08 31 7.43 47 5.74 TABLE II. CALIBRATION VALUES FOR VARIOUS ATMOSPHERIC PRESSURES AND ALTITUDES RESSURE ALTITUDE CALIBRATION NCHES Hg mm Hg kpa Ft. VALUE (%) 30.23 768 102.3-276 -ifi 101 29.92 760 101.3 0 0 100 29.61 752 100.3 278 85 99 29.33 745 99.3 558 170 98 29.02 737 98.3 841 256 97 28.74 730 97.3 1126 343 96 28.43 722 96.3 1413 431 95 28.11 714 95.2 1703 519 94 27.83 707 94.2 1995 608 93 27.52 699 93.2 2290 698 92 27.24 692 92.2 2587 789 91 26.93 684 91.2 2887 880 90 26.61 678 90.2 3190 972 89 26.34 669 89.2 3496 1066 88 26.02 661 88.2 3804 1160 87 25.75 654 87.1 4115 1254 86 25.43 646 86.1 4430 1350 85 25.12 638 85.1 4747 1447 84 24.84 631 84.1 5067 1544 83 24.53 623 83.1 5391 1643 82 24.25 616 82.1 5717 1743 81 23.94 608 81.1 6047 1843 80 23.62 600 80.0 6381 1945 79 23.35 593 79.0 6717 2047 78 23.03 585 78.0 7058 2151 77 22.76 578 77.0 7401 2256 76 22.44 570 76.0 7749 2362 75 22.13 562 75.0 8100 2469 74 21.85 555 74.0 8455 2577 73 21.54 547 73.0 8815 2687 72 21.26 540 71.9 9178 2797 71 20.94 532 70.9 9545 2909 70 20.63 524 69.9 9917 3023 69 20.35 517 68.9 10293 3137 68 20.04 509 67.9 10673 3253 67 19.76 502 66.9 11058 3371 66 Page 8 of 9

I - Model 58 has a digital display, making this model easier to calibrate and record data. This model only needs to be zeroed once and does not have a red line function. There are,three calibration choices, including a % reading. Generally use O.Olmg/L to get a reading two places after the decimal point. Set salinity dial to fresh. I YSI model 58 Dissolved Oxygen Meter I Model 57 differs from model 58 in two ways. First, there is a screw on the display panel that must be zeroed before the meter is turned on. Also, the meter must be red lined to ensure calibration accuracy. This meter has three calibration ranges to choose from. Generally use O-20 mg/l. Set salinity dial to fresh. YSI Model 5739 Probe I I Page 9 of 9