Revised by: Tim Bridges, Benjamin Brill and Tom Faber. Originally prepared by: - (Tom ~ab&) Date. Approved by: 6/2//05 (Katrina Kipp, &Lager)

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SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC SOP Title: YSI Sondes Revision #7 Page 1of 27 STANDARD OPERATING PROCEDURE FOR CALIBRATION AND FIELD MEASUREMENT PROCEDURES FOR THE YSI
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SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC SOP Title: YSI Sondes Revision #7 Page 1of 27 STANDARD OPERATING PROCEDURE FOR CALIBRATION AND FIELD MEASUREMENT PROCEDURES FOR THE YSI MODEL 6-SERIES SONDES AND DATA LOGGER (INCLUDING: TEMPERATURE, ph, SPECIFIC CONDUCTANCE, TURBIDITY, DISSOLVED OXYGEN, CHLOROPHYLL, RHODAMINE WT, ORP, AND BARAMETRIC PRESSURE). The Office of Environmental Measurement and Evaluation Ecosystem Assessment - Ecology Monitoring Team EPA New England - Region Technology Dr North Chelmsford, MA The controlled version of this document is the electronic version viewed on-line only. If this is a printed copy of the document, it is an uncontrolled version and may or may not be the version currently in use. This document contains direction developed solely to provide internal guidance to U.S. Environmental Protection Agency (EPA) personnel. EPA retains the discretion to adopt approaches that differ from these procedures on a case by case basis. The procedures set forth do not create any rights, substantive or procedural, enforceable at law by a party to litigation with EPA or the United States. Revised by: Tim Bridges, Benjamin Brill and Tom Faber Originally prepared by: - (Tom ~ab&) n Date Approved by: 6/2//05 (Katrina Kipp, &Lager) Date SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC SOP Title: YSI Sondes Revision #7 Page 2 of 27 Revision Page Date Rev# Summary of Changes Sections 4/23/02 0 Initial Approval 5/31/02 1 Changed DO requirement to 1.Omg/l /18/02 2 Added Oxygen Solubility Table - Billie Gould 11.O (added) 1/9/03 3 Conductivity from.15% to 15% (WP problem - thanks C. Porfert) 7/9/03 4 Added values to Oxygen Solubility Table and Sonde Calibration Form - Kosuke Kawai Changed zero DO criterion from 1.0 mgll to 0.5mgA - TF Table /25/03 5 Updated App. B, and parameter updates - TF App. B, , /5/04 6 Updated calibration information & cal. form - TF App. B, General update and added parameters -BB, TB, TF all SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC SOP Title: YSI Sondes Revision #7 Page 3 of 27 Table of Contents Section Subject Page Scope and Application...5 I Summary of Method...5 Health and Safety Warnings... 5 Equipment and Supplies Calibration Temperature ph Specific Conductance Turbidity Dissolved Oxygen Calibration Procedure for Discrete Sampling Applications Calibration Procedure for Continuous Monitoring Applications Chlorophyll RhodamineWT (dye tracking) Oxidation Reduction Potential Barometric Pressure Troubleshooting Measurements Discrete sample measurements Deploying Sonde for Unattended Logging Post Sampling Verification and Data Evaluation Dissolved Oxygen post sampling verification ph. conductivity. turbidity post sampling verification Adjacent Measurement Check (for deployed sondes)...22 Data and Record Management References Appendix A: Oxygen Solubility in Water...24 Appendix B: Performance check work sheet Appendix C: Sonde Calibration & Verification Form... 27 SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 4 of 27 Tables: 8.1 'Quality Control Goals for Sondes Quality Control Goals between the Adjacent Measurements and Deployed Sonde Oxygen Solublllty in Water...24 SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC Page 5 of Scope and Application The purpose of this standard operating procedure (SOP) is provide a framework for calibrating sondes used to measure water quality parameters for ground water and surface water. Water quality parameters include temperature, ph, dissolved oxygen, conductivity/specific conductance, turbidity, and chlorophyll, oxidationfreduction potential and rhodamine. This SOP is written specifically for the YSI model 6-Series Sondes (which include the 600R, 600XL, 600XLM, 6820,6920 and 6600 models), the YSI 650 MDS (Multi parameter Display System) displayaogger, and YSI EcoWatch software. The general calibration processes discussed herein are applicable to other manufactures sondes and displaysaoggers. Consult the manufacture's instruction manuals for specific procedures. 2.0 Summary of Methods This document describes a process for calibrating and performing water quality field measurements.- using YSI 6-Series Sondes. 3.0 Health and Safety Warnings 3.1 All proper personal protection clothing and equipment is to be worn. 3.2 The standard solutions for calibrating conductivity contain Iodine and Potassium Chloride. When using the standards, avoid inhalation, skin contact, eye contact or ingestion. If skin contact occurs remove contaminated clothing immediately. Wash the affected areas thoroughly with large amounts of water. If inhalation, eye contact or ingestion occurs, consult the Material Data Safety Sheets (MSDS) for prompt action, and in all casesseek medical attention immediately. 3.3 The standard solutions for calibrating turbidity contain Styrene divinylbenzene copolymer spheres. While the material is not volatile and has no known physical effects on skin, eyes, or on ingestion, general health and safety precautions should be adopted to minimize unnecessary contact. If skin contact occurs remove contaminated clothing immediately. Wash the affected areas thoroughly with large amounts of water. If inhalation, eye contact or ingestion occurs, consult the MSDS for prompt action, and in all cases seek medical attention immediately 3.4 The standard solutions for calibrating ph contain deionized water, potassium acid phthalate, inert dye, potassium phosphate, sodium phosphate, potassium chloride, and preservatives (no mercury or formaldehyde). Avoid inhalation, skin contact, eye contact or ingestion. If skin contact occurs remove contaminated clothing immediately. Wash the affected areas thoroughly with large amounts of water. If inhalation, eye contact or ingestion occurs, consult the MSDS for prompt action, and in all cases seek medical attention immediately. 3.5 The Zero DO solution contains sodium sulfite and in some cases a trace amount of cobalt chloride. SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 6 of 27 This solution should be handled with care; the cobalt chloride is a suspected carcinogen. If skin' contact occurs remove contaminated clothing immediately. Wash the affected areas thoroughly with large amounts of water. If inhalation, eye contact or ingestion occurs, consult the MSDS for prompt action, and in all cases seek medical attention immediately. I Rhodamine WT dye should be handled with care. The active indgredient in this dye is trimettlic acid. Very little is known about its long term effects on humans so it should be handled with care. If contact occurs, wash the affected areas thoroughly with large amounts of water. If inhalation, eye contact or ingestion occurs, consult the MSDS for prompt action, and in all cases seek medical attention immediately. The Zobell solution used for calibrating ORP contains potassium chloride, potassium ferrocyanide (trihydrate), and Potassium ferricyande. If contact occurs, wash the affected areas thoroughly with large amounts of water. Cyanides in general are often considered toxic to humans. For more info, see the MSDS. Follow the most updated Boat Safety SOP when conducting sampling from a boat. Equipment and Supplies NIST traceable thermometer (only needed once per year) ph Standards of 4,7, and 10 Conductivity standards (concentration dependent upon expected field conditions) Turbiditiy standards (concentration dependent upon expected field conditions) Deionized and tap water Calibration cups YSI Sonde with attached pworp, Conductivity, Dissolved Oxygen, Turbidity, Chlorophyll, and Rhodamine probes YSI 650 MDS Multiparameter Display System (display logger) Sonde communications cable Notebook Pen Disposable gloves, goggles and safety glasses Zobell Solution Rhodamine WT dye (Access to) Princo Mercury Barometer N.I.S.T. traceable thermometer Batteries Calibration Check the displayllogger to determine the battery level in the displayllogger to see if recharging or new batteries are necessary. Prior to calibration, all instrument probes on the sonde must be SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 7 of 27 cleaned according to the manufacture's instructions. Failure to perform this step can lead to erratic measurements. The probes must also be cleaned by rinsing with deionized water before and after immersing the probe in a calibration solution. For each of the calibration solutions provide just enough volume so that the probe and the temperature sensor are sufficiently covered. When done with the calibration solutions do not return it to the original bottle, save solution in separate container or dispose of it properly. When using the Sonde for long-term deployment and using the Autosleep RS232, and Autosleep SDI12 functions, the instrument must be calibrated in these modes. For manual measurements this function should be turned off (see section ) prior to calibration. 5.1 Temperature For instrument probes that rely on the temperature sensor (ph, dissolved oxygenlspecific conductance, and oxidation-reduction potential), the sonde temperature sensor needs to be checked for accuracy against a thermometer that is traceable to the National Institute of Standards and Technology (NIST). This accuracy check should be performed at least once a year, and the date and results of the check kept on file. Below is the verification procedure Once a year, the accuracy of the instrument must be verified by checking the endpoints of the desired temperature range. For example, if the desired temperature range is O C to 40.0 C, the instrument must be with in the C of both end points Place a thermometer that is traceable to the NIST into the water and wait for both temperature readings to stabilize Compare the two measurements. The instrument's temperature sensor must agree with the reference thermometer within the accuracy of the sensor (+I- 0.15OC). If the measurements do not agree, the instrument may not be working correctly and the manufacturer should be contacted. The ph of a sample is determined electrometrically using a glass electrode. Choose the appropriate standards that will bracket the expected values at the sampling locations. For this procedure three standards will be used (ph 4, ph7, & ph10). If the probe is slow to response refer to the section 6.0 Troubleshooting Rinse probe with deionized water and shake off excess water. Allow the buffered samples to equilibrate to the ambient temperature Place the probes (at least ph and temperature probes) on the sonde into the ph 7 buffer On the displayllogger use the upldown arrow keys to highlight the Calibrate option and SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC SOP Title:YSI Sondes Page 8 of 27 press the enter key Highlight the ph option and press enter Highlight the 3-point option and press enter Input the value of the buffer, which is 7.00 and press enter Wait for the value of ph to stabilize and then press enter. Wait for Calibrated message. If an Out of Range message appears, do not accept, check the probe and refer to operator's manual or section 6.0 Troubleshooting Place the ph probe into a ph 4.00 buffer Press enter key to continue calibration When prompted, enter the ph of the second buffer, 4.00. Wait for Calibrated message, and press any key to continue Rinse probe with deionized water and shake off excess water Place the ph probe into a ph buffer Press enter key to continue calibration When prompted, enter the ph of the third buffer, 10.00 . Wait for Calibrated message, and press any key to continue Rinse probe with deionized water and shake off excess water Exit the calibration menu and go to the Sonde Run mode. Insert probe into ph 7 buffer and make sure it is reading correctly 0.05). If buffer reading is not correct, repeat the calibration procedure. 5.3 Specific Conductance Conductivity is used to measure the ability of an aqueous solution to carry and electrical current. Specific conductance is the conductivity value corrected at 25OC Place the cleaned probes into the specific conductivity standard solution, making sure that the specific conductivity probe is fully submerged. For studies where conductivity is a critical parameter (non-critical parameters will be identified in the QAPP), the accuracy of the instrument must be verified by checking the endpoints of the desired conductivity range SOP file:f:\user\tfaber\qa\sops\ysisondes REV 7 (JUNE ).DOC Page 9 of 27 to insure linearity. Calibrate with one of the standards (the high standard) and check the instrument with a low standard. At the end of the monitoring period check the instruments with both standards. If you are using a small amount of calibration solution or standards that are easily contaminated first rinse the probe(s) with the conductivity standard. Where conductivity is a non-critical measurement you can check and calibrate the instrument with one calibration solution Return to the displayflogger main menu and select Calibrate and press enter Select Conductivityyy and press enter Select SpCond and press enter Enter the standard concentration in ms/cm and press enter. The standard concentration should be just above the highest concentrations you expect to measure After the specific conductivity reading has stabilized press enter to calibrate. Wait for the calibrated message to appear. If the Sonde should report Out of Range do not override the error message, instead recheck the standard and go to the section 6.0 Troubleshooting for more help Exit the calibration menu and go to the Sonde Run mode and record the concentration (make sure it is reading with in 5% of standard value) To check the calibration with a second standard (low), rinse probe with deionized water and insert probe in second standard and make sure it is reading with in 10%. A second standard is used to check the calibration at the low range and to bracket the expected concentrations. This must be performed when conductivity is a critical measurement. 5.4 Turbidity The turbidity method is based upon a comparison of intensity of light scattered by a sample under defined conditions with the intensity of light scattered by a standard reference solutions. Critical to the instrument's operation is that the lens covering the detection unit is kept clean both during calibration and field use. The turbidity probes used on the YSI 6-Series sondes include an automated optics wiper. This wiper can be activated using the displayflogger. The calibration and post calibration check should be performed in the laboratory before and after sampling The following procedure is specified for the YSI Probe. (Note there is a different procedure for the older YSI 6026 Probe). With the use of the 6136 probe you must use the extended probe guard and the black bottom calibration cup. Use only YSI (or a certified equivalent) calibration standard, for more information refer to the owners manual. SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 10 of Check to make sure the turbidity probe and wiper are clean and free from any material Activate the wiper to make sure it is wiping and parking correctly Allow the standard samples to equilibrate to the ambient temperature Clean all of the probes on the sonde with deionized water. Shake off excess water Place the sonde in the black bottom calibration cup containing the 0.0 NTU standard (which can be deionized water) Using a stand to hold the sonde separate the calibration cup from the bottom of the Sonde by a distance equal to the width of 3 fingers (two inches). (The distance from the threads on the sonde to the bottom of the calibration cup should be equal to the length of the extended probe guard.) From the Calibrate Menu, on the display/logger, select the Turbidity option and press enter Select the 2-point option and press enter Enter 0.0as the first calibration standard and press enter Select the clean optics option to activate the automated wipers. Once the cleaning process is completed, wait for the turbidity measurement to equilibrate, and then press the enter key Place the probe in the second standard (10 NTU or 11.3 NTU is the common standard solution). This second standard should be slightly above the highest concentration that is expected to be measured in the field. It is not necessary to clean the probe before placing into the second standard. Shake off excess DI water Press enter to continue calibration Enter the concentration of the second calibration standard (10 NTU or 11.3 NTU is the common solution of use) and press enter Again, select the clean optics option to activate the automated wipers. Once the cleaning process is completed, wait for the turbidity measurement to equilibrate, and then press the enter key Exit the calibration mode and enter the Sonde Run mode. Make sure it is reading with in +I- 10 % of the original concentration. If the buffer reading is not correct, repeat the 5.5 Dissolved Oxygen calibration procedure. SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 11 of 27 Dissolved oxygen (DO) content in water is measured using a membrane electrode. The DO probe's membrane and electrolyte solution should be inspected for any damage or air bubbles prior to calibration. If air bubbles or damage are present, replace the membrane according to manufacturer suggestions. (After changing the membrane, for,accurate measurements, you must wait 6-12 hours before use to allow the membrane to equilibrate) YSI 6-Series DO probe must be calibrated using the calibration cup provided with the sonde or by wrapping the sonde probe guard with a wet towel. The DO is calibrated in the field prior to taking measurements and the final post calibration (verification) check should also be performed in the field before the instrument is turn off and after all measurements are taken. When calibrating DO and not using the auto sleep function the instrument must be turned on (warmed up) for 15 minutes prior to calibration. When calibrating the DO for unattended sampling and using the auto sleep function, the instrument should not be warmed up before calibrating (it should be calibrated when the instrument is cool, since it is cool when the instrument is taking readings). Calibration of the DO probe requires inputting the current barometric pressure. The YSI 650 displayllogger has a barometer within the unit and automatically provides this during the calibration procedure. Other displayfloggers may not supply the barometric pressure, in this case you will need a separate barometer. Two calibration procedures are listed below for dissolved oxygen, one for sampling applications and.one for long-term monitoring applications Calibration Procedure for Discrete Sampling (non deployment) Applications The dissolved oxygen probe is calibrated each day prior to use. An initial inspection and calibration should be performed the day before to assure the membrane is in good shape the instrument is working properly. Follow the procedure below to calibrate Clean all of the probes on the sonde with tap (or clean ambient water) water. Shake off excess water Place approximately 118 inch of water in the bottom of the calibration cup. Place the probe end of the sonde into the cup. Engage only 1 or 2 threads of the calibration cup to insure the DO probe is vented to the atmosphere. [An equivalent alternative method is to wrap the probe guard (which is attached to the sonde) with r SOP file:f:\user\tfaber\qa\sops\ysi SONDES REV 7 (JUNE ).DOC Page 12 of 27 a wet towel and place the sonde in a 5 gallon bucket with 1 inch of water in it.] Make sure that the DO and temperature probes are NOT immersed in water and that the Sonde cup is not in direct sunlight. Wait approximately 10 minutes for the air in the calibration cup to become water saturated and for the temperature to equilibrate For manual sampling
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