Section 13: Dissolved Oxygen—Polarographicdepleted solution such as sodium sulfite or nitrogen-saturatedwater. A 2-point calibration is recommended• when you expect to measure very low D.O. values (< 5 mg/L),• when required by Standard Operating Procedures.Nominal vs. StableTo shorten the calibration time, you have the option to accept thecalibration when “Nominal” stability is achieved. If the early value isaccepted, the calibration point will be designated “USER SET” in thecalibration report. If the calibration report indicates that calibrationwas performed through to stability then the instrument will operate asintended by In-Situ’s quality standards.Calibration Solutions & <strong>Equipment</strong>100% D.O. calibrations may be performed in water saturated with air,or in air saturated with water. Deionized water is available from In-SituInc., but any clean water may be used. In-Situ’s bubbler calibration kitis designed for an efficient water calibration.An oxygen-depleted solution is used to calibrate the 0% D.O. Sodiumsulfite is available from In-Situ Inc. For a cleaner calibration, nitrogensaturatedwater may be used.Recommended Calibration FrequencyYour own experience is the best guide to how often the polarographicD.O. sensor will benefit from recalibration under conditions of normalusage. Refer to the general guidelines under “How Often to Calibrate”in Section 10, and the tech note on “Instrument Calibration.”Until a new polarographic sensor has been thoroughly conditioned, itmay require more frequent calibration. In the absence of other indications,a calibration should be performed every 2-4 weeks.In addition, the polarographic D.O. sensor should be conditioned for2-4 hours and recalibrated in the following circumstances:• after cleaning the sensor,• after replacing the membrane module,Q:A:I did a Quick Cal. Why should I recalibrate D.O.?The D.O. Quick Cal, especially if done through to stability,can provide accurate measurement results. However, someprocedures require a look-up table for the stimulus at a giventemperature and pressure. This can be done in the traditionalD.O. calibration. Also, better measurement results will beobtained when the 100% calibration is done in water saturatedwith air. This procedure is not provided for in Quick Cal. In addition,the traditional calibration provides for a 0% (0 ppm, 0 mg/L)calibration, which is recommended when measuring very lowD.O. values.• when taking measurements at an elevation different from that atwhich the sensor was last calibrated.Dissolved Oxygen Calibration TipsThe following discussion may help you to obtain the best results fromthe polarographic D.O. calibration.• Air or Water? The software provides two options for conducting a100% D.O. calibration:∗ in air (saturated with water). This is the condition during a QuickCal in the inverted Cal Cup with the sensor membrane exposedto air, temperature sensor submerged, and Cal Cup vented tothe atmosphere.∗ in water (saturated with air). In-Situ’s bubbler calibration kitprovides everything needed to create a vigorous bubbling actionto insure air-saturated water. The Cal Cup is not used.Since dissolved oxygen measurements are typically made in water,calibrating in water will often yield better results. When calibrated inair, the membrane’s behavior in water must be estimated.• The D.O. calibration procedure is very sensitive to changes intemperature. Ideally, it should be done in an area protected fromdirect sunlight and away from ventilation ducts.• The nature of the sensor membrane influences the response. Besure to note the membrane thickness before starting the calibration.(If no thickness is indicated, the membrane is 1-mil Teflon.)Membrane thickness is more important with a 100% calibration inair.Dissolved Oxygen Quick CalThe procedure to Quick Cal the polarographic D.O. sensor, along withother Basic sensors, is in Section 3, Getting Started. This is a singlepoint100% calibration in air (saturated with water).The following traditional calibration is recommended for use when• the user is required to enter a specific stimulus at the calibrationtemperature and pressure,• calibration in water is preferred,• a 0% calibration point is needed.Traditional Dissolved Oxygen Calibration ProcedureYou may select a 1-point or a 2-point calibration. The first point (100%saturation) may be taken in air or in water.Prepare the MP <strong>TROLL</strong> <strong>9500</strong> for water or air calibration as describedin Steps 1-6 on the following page.<strong>TROLL</strong> <strong>9500</strong> Operator’s <strong>Manual</strong> 810095110 rev. 007 01/09
Section 13: Dissolved Oxygen—PolarographicPreparation for 100% D.O. Calibration in WaterThe bubbler cal kit for the Polarographic D.O. sensor comes with(1) Battery-powered air pump and 2 alkaline D-cells, (2) Bubblercup with aquarium stone, tubing, check valve and pinch valve, (3)Grey PVC adapter to support the <strong>TROLL</strong> <strong>9500</strong> in the top of thebubbler cup.1. Install the batteries in the portable air pump as shown in thediagram on the inside of the lid.2. Fill the bubbler container almost to the top with clean water. Theoptimum amount depends on the volume of the sensors installedin the MP <strong>TROLL</strong> <strong>9500</strong>.TIP: Tap water is fine, unless it is high in salinity. It is easierto achieve 100% oxygen saturation in low-salinity water.Distilled water is readily available and works well.3. About 10 minutes before calibration, turn on the bubbler. Regulatebubbling with the pinch valve. For best results, run at the fullflow rate to achieve saturation; after 10 minutes you can use thecontrol valve to match the water turbulence conditions expectedin the field.4. Before beginning the calibration procedure, note the membranethickness stamped on the membrane module.5. With the D.O. sensor installed and plugs or sensors in theother sensor ports, rinse the front end of the MP <strong>TROLL</strong> <strong>9500</strong>thoroughly in clean water to remove contaminants and traces offluids used for earlier calibrations.6. When ready to calibrate, place the adaptersecurely in the top of the bubbler housingand insert the front (sensor) end of the MP<strong>TROLL</strong> <strong>9500</strong> into the adapter.• Insure the D.O. sensor is not in theaeration path. Rotate as necessary toprevent air bubbles from collecting onthe membrane surface.• Insure the temperature sensor is submerged at least 0.5” (12mm) in the aerated water.Allow a few minutes for the temperature to stabilize,especially if you plan to enter a temperature dependentvalue from a look-up table.6Preparation for 100% D.O. Calibration in AirTIP: Before beginning the calibration procedure, checkthe side of the membrane module for the membranethickness.1. With the D.O. sensor installed and plugs or sensors in theother sensor ports, rinse the front end of the MP <strong>TROLL</strong> <strong>9500</strong>thoroughly in clean water to remove contaminants and traces offluids used for earlier calibrations.2. Dry the D.O. sensor membrane by shaking the probe and/orgently wiping with a soft swab or the corner of a tissue.3. Rinse the empty Cal Cup and attach it to the MP <strong>TROLL</strong> <strong>9500</strong>.Thread the Cal Cup onto the body until it is seated against theo-ring, then back off slightly to avoid overtightening.4. Invert the <strong>TROLL</strong> with Cal Cup attached and remove the blackend cap from the Cal Cup.5. Gently fill the Cal Cup with clean water until the temperaturesensor is completely covered and the membrane at the tip of theD.O. sensor is in air. If any water splashes onto the membrane,gently blot the center of the membranewith a clean cotton swab or the corner ofa soft lint-free tissue.6. Loosely attach the end cap to the CalCup. For proper venting, a small hole inthe threads of the cap should be at leastpartly visible to achieve ambient pressureconditions.You may wish to use a clamp or othersupport to maintain the <strong>TROLL</strong> <strong>9500</strong> inthis inverted position.Allow a few minutes for the temperature to stabilize,especially if you plan to enter a temperature dependentvalue from a look-up table.6<strong>TROLL</strong> <strong>9500</strong> Operator’s <strong>Manual</strong> 820095110 rev. 007 01/09