Horiba - Ozarks Environmental and Water Resources Institute
Contents
1. Turn OFF the power Wash the probe thoroughly with tap water Be sure to flush off all of sample solution from the probe When storing the U 22 for brief periods of a week or less fill the protective rubber cap with distilled water and fit the probe over it The pH sensor must always be kept moist For longer storage remove the sensor from the sensor probe and check that the internal solution replenishment port is closed Then attach a seal to the liquid junction and attach rubber caps Also remove the DO sensor and set the short socket and store in a cool dark place Recharge the reference sensor with reference solution about once every 2 months 1 Remove the liquid junction rubber cap from the reference sensor and pour out the old solution 2 Fill the reference sensor completely with new reference solution Make sure that there are no air bubbles Replace the liquid junction rubber cap 4 Carefully wash off all excess reference solution from the probe 5 Record the date of the reference sensor recharge in the instrument log book See Horiba manual for maintenance procedures for DO sensor diaphragm replacement page 89 Automatic Data Storage a b C Measured values are stored automatically at constant time intervals See the Horiba user s manual for details on how to use this function There are three options that can be set for automatic data storage e Waiting time for initial data storage e Data storage interv2. and also software for data transfer to a PC Microsoft Excel is used for recording and reviewing the final data from the Horiba This document is created using Microsoft Word The Word file name for this SOP is 1050R01 Horiba U 22 doc Method performance There are no published method performance data for this method Pollution prevention All wastes from these procedures shall be collected and disposed of according to existing waste policies within the MSU College of Natural and Applied Sciences Volumes of reagents made should mirror the number of samples being analyzed These adjustments should be made to reduce waste Data assessment and acceptable criteria for quality control measures 20 1 20 2 20 3 20 4 The analyst should review all data for correctness Precision values are calculated for pairs of duplicate analyses The desired precision is 20 The completed Excel spreadsheet is reviewed by the analyst s supervisor or the OEWRI QA coordinator Corrective actions for out of control or unacceptable data 21 1 21 2 21 3 The results for precision and blank data are compared to the acceptable values for this analysis 20 and 0 for all analytes respectively lf data are unacceptable for any reason the analyst should review their analytical technique prior to conducting this analysis again The instrument may require trouble shooting techniques if the data are unacceptable Clean the probes P
3. and place under identical circumstances and that are treated identically throughout field and laboratory procedures Analysis of field duplicates indicates the precision associated with sample collection preservation and storage as well as laboratory procedures Method detection limit MDL The lowest level at which an analyte can be detected with 99 percent confidence that the analyte concentration is greater than zero The MDL is defined by the instrument manufacturer and is the lowest value of the instrument s detection range see Table 1 in section 14 Interferences An improperly calibrated instrument can lead to erroneous results See the manufacturer s instruction manual for proper calibration procedures and in sections 14 and 15 The U 22 probes should be clean prior to use to avoid contamination for any of the analytes Health and safety 8 1 When wading in streams where water depths may be 1 meter deep or more wear a life preserver and or remove hip boots or chest waders Currents can force wading field workers into deep water and water filled boots can make swimming difficult 10 11 8 2 8 3 8 4 ID Horiba U 22 Revision 1 September 2006 Page 5 of 14 When walking through densely vegetated areas along streams be sure to look for and avoid toxic plants like poison ivy Be sure to wear appropriate insect repellent and protective clothing for protection from mosquitoes chiggers and ticks In additi
4. error has occurred Press the CLR key to cancel the error code and re start the auto calibration by pressing the ENT key Manual or Span Calibration Pal Calibration DO OLEON ON 10 11 12 13 Wash the sensor two or three times with DI Immerse the sensor into 7 00 pH buffer in the calibration beaker Press the CAL key twice in the pH Measurement mode MAN ZERO and CAL light up Use the UP DOWN A Y keys to input the temperature adjusted value for the pH 7 00 standard When the indicated value has stabilized DATA IN lights up and the calibration finishes Wash the sensor two or three times with DI Immerse the sensor in 4 00 pH buffer in the calibration beaker Press the CAL key to make sure that the instrument is in the Manual Span Calibration mode MAN SPAN and CAL light up Use the UP DOWN A Y keys to set the value for the pH 4 00 solution at the measurement temperature Press the ENT key Manual span calibration starts When the indicated value has stabilized DATA IN lights up and the calibration has finished Record that the instrument has been calibrated for pH in the Horiba instrument log book ee Calibration 11 Prepare the calibration solution weigh 0 746 g of KCI into a 200 mL volumetric flask Dilute to 200 mL with DI Final concentration is 667 mS m 0 667 S m Wash the conductivity sensor two or three times with DI Completely remove the water on the sensor and calibrate the sensor i
5. Standard Operating Procedure for Horiba U 22XD Multi Parameter Water Quality Monitoring System 1050R01 Horiba U 22 doc Missouri State University and Ozarks Environmental and Water Resources Institute OQEWRI Prepared by Date OEWRI Quality Assurance Coordinator Approved by Date OEWRI Director ID Horiba U 22 Revision 1 September 2006 Page 2 of 14 Table of Contents 1 Identification of the test method cccccsssssseeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeneeeeneeeeeeeeesseeseeennees 3 2 Applicable matrix or MatriC S cccseeeeeeeeeeeeeeeeeeeeeeeeeeeeeeeseeeeeeeeeeeeeeeeseeseeeeeeeeeeeenaneees 3 3 Detection Limit ssccsstcsstetotssteeschoeiases dasarctslocsseddaseeatutocsuwndasaratulocsuastdasavataiscmaendascuasuiocenas 3 4 Scope of the test Method wiis iesccise dec see ectiniet ieee iar een 3 5 Summary of test method siseasi inienn innnan echen teehee ieedeedee es aKa aHan iaiia 3 6 Baiil E TA A A T TTA 4 7 ae AT A A A is 4 8 Health and Saleh y ssc iecassies coed cccinca tesa aces inaa eaea A soctcce cncececctciecucdencadztatsaxsacecaness 4 9 Personnel qualifications 22 0ccccess 10 _ EERE nee neeeeeeenensnnnnneceneeseesensnnneneees 5 10 Equipment and supplies 22 ccccccesssnene gfMMBBMMMMre nee ccneeeceneessnnnecceneeeseeenssnnaneceneeeess 5 11 Reagents and standards 22 ccces IBEMEEEEMg canes seneeeceeeessnnnecceneeseeeenssnnneeeeeeesees 5 12 Sample collect
6. al that is time between data storage measurements e Data storage measurement period The time period between the first and last data storage measurements Data retrieval is by the same process as listed below section 16 1 and 16 2 for manual data storage ID Horiba U 22 Revision 1 September 2006 Page 12 of 14 16 Data acquisition calculations and reporting Horiba U 22XD Data Download Procedure Note The download cable and interface software are installed on GGP 111990 in Temple 125 If Horiba U 20 icon does not appear on your desktop when logged onto that computer navigate to C U20 and double click on U 20System exe to start program at step d below 16 1 16 2 a b Install data link unit on back of Horiba Attach cable to port on data link unit Simultaneously press SET and POWER buttons on Horiba to put unit into PC mode PC 232C is shown on the display in this mode Open Horiba U 20 program use above procedure if necessary Choose SENSOR gt SOPEN DATA to access all data files saved on unit When data has finished loading to screen may take several minutes select desired records by holding shift key and clicking data numbers Press SELECT on download window Data will appear in Data Screen Individual records may be examined in this screen if desired Click DATA gt CLOSE to return to Main Screen On Main Screen click FILE gt SAVE AS and choose a file name and destination Filename should inc
7. andard Buffer Fisher Scientific SB107 500 pH internal reference solution Horiba model 330 part number 9037 0052 00 250 mL bottle DO probe Internal Solution Horiba model 305 Caution contains Potassium hydroxide Sodium sulfite for DO calibration dissolve 12 5 g of Sodium sulfite with deionized water Dilute to 250mL with DI in a 250 mL volumetric flask 12 13 14 ID Horiba U 22 Revision 1 September 2006 Page 6 of 14 11 6 Potassium chloride KCI solution weigh 0 746 g of KCI into a 200 mL volumetric flask Dilute to 200 mL with DI Final concentration is 667 mS m 0 667 S m 11 7 Turbidity standard 100 NTU or other high value turbidity 40 100 NTU standard Purchased form Fisher Scientific or other vendor 11 8 Deionized water DI Sample collection preservation shipment and storage Water samples are not collected using this procedure The analyses are conducted in situ and only data are collected and stored in the instrument Quality control 13 1 Laboratory Reagent Blank LRB before leaving the laboratory the analyst should perform one measurement of deionized water This operation will show that the auto calibration has been performed and that the unit is reading blanks correctly 13 2 Field Duplicates FD Two measurement readings taken at the same sampling location The results are compared after downloading the data One FD will be collected with every ten samples collected in the f
8. erform maintenance procedures as outlined in manual Replace defective sensors Send the instrument to the manufacturer for repair aog 22 23 24 ID Horiba U 22 Revision 1 September 2006 Page 14 of 14 Waste management The wastes generated in this method are not hazardous The quantities are very small and can be discarded in the laboratory sink References 23 1 Operation Manual Horiba Multi parameter Water Quality Monitoring System U 22XD 2001 Scientific and Water Quality 17671 Armstrong Ave Irvine CA USA 92614 23 2 Standard Methods for the Examination of Water and Wastewater 2005 21 Edition APHA AWWA WEF Publishers Tables diagrams flowcharts and validation data There are no tables diagrams flowcharts or validation data for this method
9. f 0 to 14 The pH is a measure of the hydrogen ion H activity in a solution Activity of the hydrogen ion as moles L can be calculated as pH logio H Or H 1 10 The pH scale is logarithmic so that a decrease of 1 pH unit is equivalent to a ten fold increase in the hydrogen ion activity For example a solution that has a pH of 4 0 is ten times more acidic than a solution with a pH of 5 0 The neutral point for pH is temperature dependent at 25 C pH 7 0 is neutral at 0 C the neutral point is pH 7 5 and pH 6 5 is the neutral point at 60 C Standard Methods 2005 The glass electrode method is used by the U 22 The known pH of a reference solution is determined by using two electrodes a glass electrode and a reference electrode and measuring the voltage difference in potential generated between the two electrodes The difference in pH between solutions inside and outside the thin glass membrane creates electromotive force in proportion to this difference in pH The reporting unit is the standard unit of pH for example 7 00 pH units Turbidity in water is caused by suspended and colloidal matter such as clay silt finely divided organic and inorganic matter and plankton and other microscopic organisms Turbidity is measured in the U 22 using the light transmission scattering method The unit for turbidity is NTU Nephelometric Turbidity Unit Definitions 6 1 6 2 Field duplicate Two samples taken at the same time
10. he TEMP measurement mode ID Horiba U 22 Revision 1 September 2006 Page 10 of 14 2 Immerse the sensor in water at a known temperature use a NIST traceable thermometer to determine the known temperature 3 Use the UP DOWN A Y keys to set the value at this temperature 4 Press the ENT key The manual calibration starts 5 When the indicated value has stabilized DATA IN lights up and the calibration finishes 6 Record that the instrument has been calibrated for temperature in the Horiba instrument log book 15 Procedure 15 1 15 2 Measuring Water Parameters a Turn the power on and gently place the probe into the water body to be sampled Never drop or throw the probe into the water body Each of the probes is sensitive to extremes This includes impact and heat do not leave the probe inside a vehicle with the windows closed or in prolonged direct sunlight b All parameters should be taken from the flowing portion of the stream or if in a pool at least one foot from shore and at least 6 inches below the surface 9 The dissolved oxygen parameter should be taken from a flowing portion of the stream if possible but should avoid areas of turbulence where atmospheric gases may be entrained in the water column In addition a dissolved oxygen measurement should be made 6 inches below the surface and 6 inches above the bottom or at depth of 4 feet whichever is less All parameters are measured simultaneously d T
11. ield 13 3 After calibration pH is checked against a NIST traceable standard pH 7 00 units 13 4 Annually the Horiba thermistor is compared to a NIST certified thermometer The results are recorded in the Horiba instrument log book A correction factor is noted and applied to all data 13 5 The DO calibration can be compared to a manual oxygen analysis such as the Winkler See Standard Methods 4500 0 13 6 All calibration and quality control information is recorded in the instrument log book Calibration and standardization 14 1 Specifications for the U 22 are listed in Table 1 Table 1 Specifications for Horiba U 22 Conductivity 0 99Sim 1 F S Dissolved Oxygen Diaphragm 0 19 9 mg L 0 1 mg L ID Horiba U 22 Revision 1 September 2006 Page 7 of 14 pH Ciass electrode 0 14 pH units 0 05 units Turbidity Penetration and Scattering 0 800 NTU 5 Depth Pressure method 0 100m 3 Total Dissolved Solids 2 g L Seawater specific gravity 20 14 2 To increase accuracy for conductivity the U 22 uses the 4 electrode method that reduces the amount of polarization that occurs on the electrode plates The U 22 uses an automatic temperature conversion function to calculate conductivity at 25 C at a temperature coefficient of 2 C based on the measured value of the temperature See equation 1 Equation1 Los Li 1 0 02 t 25 Where Ls Conductivity of solution converted to 25 C value disp
12. ion preservation shipment and storage cccccesseeeseeeeeeteeeeeeeees 6 13 Quality Control P ETE T 6 14 Calibration and standardization ccccccceeseeeeeeeeneeeeeeeeeneneeneeeeeeeeeeeseeeeeeeeeeeeeeeesnneees 6 15 PROC e UNa TETE T icc Ses seca dvs vedauaG wieesaes 10 16 Data acquisition calculations and reporting ssseeceeeeeeeseeeeneeeeeeeeeeeeeeeeeeneeeeeeees 12 17 Computer hardware and software 0cccccccsseesesneeeeeeeeeeeeeeeeeeeeeeeeeeeeaseeeeneeeeeeeeeeenneees 13 18 Method performance g ceccccce nn0 See See eee nsnnneeeeeeee ceeee ss Eenennaam 13 19 Pollution prevention Seba 22 0 SRRIMMEMED eee ceeeessnnnecceeeeeseeeessnnn RGD mnnn nrnna 13 20 Data assessment and acceptable criteria for quality control measures 13 21 Corrective actions for out of control or unacceptable data ssssssseeeeeeeeeeeeeees 13 22 Waste management 2 C Semis n aeee ARMS ce eeeeeenessnnnencneneeseeeessnnneceeeeeseeeeseaee 14 23 References sssssssusunnnnnnnnnnn annn a Resse o O ae a a aaa aa aa AQ Dpsssssssssssssssssssssssssssssssssssssssssssess 14 24 Tables diagrams flowcharts and validation Gata cccccccccssceeeseceseeeseeeeeeeeeeeees 14 ID Horiba U 22 Revision 1 September 2006 Page 3 of 14 Identification of the test method Horiba U 22XD Multi Parameter Water Quality Monitoring System Applicable matrix or matrices This ins
13. layed on U 22 t Temperature of solution at time of measurement C and L Conductivity of solution at t C 14 3 Calibrating the U 22 There are two types of calibration for the U 22 an AUTO calibration and a Manual or Span calibration For routine operation the AUTO calibration will result in sufficient accuracy The Manual calibration should be performed after any maintenance to the instrument a AUTO calibration 1 In this mode the pH COND and TURB sensors are calibrated in the pH 4 standard solution and the DO and DEP sensors are calibrated in the atmosphere simultaneously 2 Fill the calibration beaker to the marked line with the pH 4 standard solution Horiba 100 4 3 Immerse the sensor into the beaker and press the CAL key 4 AUTO and CAL appear on the instrument screen The lower cursor should be on the AUTO sub mode if it is not then use the MODE key to move the lower cursor to AUTO 5 Press the ENT key to start AUTO calibration The readout will show CAL Wait about a minute and the upper cursor will gradually move across the auto calibration parameters one by one pH COND TURB and DO The upper cursor will blink while the auto calibration is taking place 6 When the calibration is complete the readout will briefly show END and then press the MEAS key to switch to the MEAS mode ID Horiba U 22 Revision 1 September 2006 Page 8 of 14 If the unit shows an error message an auto calibration
14. lude project name and date Destination could be Desktop floppy disk zip disk or flash drive If you save on the desktop and you will have many Horiba files please make a folder for your files After saving data close HoribaU 20 program turn off Horiba U 22XD unit and disengage data cable f necessary follow Horiba cleanup procedures Horiba Data Handling Note The Horiba data files are saved as csv Be sure to set Excel to look for All Files to find it a Open data file in Excel Note that Horiba numbers are not included as a field and the only identifiers other than record order are DATE and TIME Some fields are blank and filled with delete these Other fields are not pertinent DEP SAL ot and others may not be important for your uses delete these also Add fields for SITE and any other information you need to associate with the water quality data Save As an Excel xls file Make sure that the filename includes project and date or some other unique identifier a desktop cluttered with Horiba1 xls 17 18 19 20 21 ID Horiba U 22 Revision 1 September 2006 Page 13 of 14 files will become confusing very quickly This will leave you with two files the original csv file and the new and updated xls file e If necessary e mail the file to yourself if it s saved on the desktop Computer hardware and software 17 1 17 2 17 3 The Horiba U 22 has internal software
15. n air Press the CAL key twice in the COND measurement mode MAN ZERO and CAL light up Use the UP DOWN A Y keys to set the value at 0 0 Immerse the sensor into the calibration solution in the calibration beaker Press the CAL key twice MAN SPAN and CAL light up Use the UP DOWN A Y keys to set the standard solution value i e 0 667 S m The sensor will automatically identify the calibration solution and the relevant calibration range is displayed i e r1 r2 or r3 see manual Press the ENT key the manual calibration starts When the indicated value has stabilized DATA IN lights up and the calibration finishes Record that the instrument has been calibrated for conductivity in the Horiba instrument log book ID Horiba U 22 Revision 1 September 2006 Page 9 of 14 Turbidity Calibration 1 2 DnR 11 Make sure that the TURB sensor is clean Immerse the sensor in DI 0 NTU standard in the calibration beaker Press the CAL key twice in the TURB measurement mode MAN ZERO and CAL light up Use the UP DOWN A Y keys to set the value at 0 0 Press the ENT key the manual calibration starts Immerse the TURB sensor into the calibration beaker containing the 100 NTU standard Press the CAL key twice MAN SPAN and CAL light up Use the UP DOWN A Y keys to set the standard solution value at 100 Press the ENT key the manual calibration starts When the indicated value has stabilized DATA IN light
16. o get a uniform reading slowly move the probe up and down to circulate the water through it Wait for the readout to stabilize while doing this e Make sure that MAN is displayed in the Measurement mode screen Press the ENT key Data storage starts DATA IN and the data number are displayed on the screen The measured values are displayed in order at about 0 5 second intervals f Press the MEAS key to move to the various parameters If desired manually record pH pH conductivity COND turbidity TURB dissolved oxygen DO temperature TEMP site ID and date for each site in the field notebook Data Storage a The U 22 can store up to 2880 sets of data of the values measured for each of the parameters pH COND TURB DO and TEMP b When the readout stabilizes on a value press the ENT key This will automatically input the parameters for the measurement into memory 15 3 15 5 ID Horiba U 22 Revision 1 September 2006 Page 11 of 14 The readout will show the Data Set number first for about 2 seconds Then each parameter is automatically read into memory one by one The upper cursor skips along to show this The upper cursor then returns to pH with the U 22 in measure mode The unit can be turned off between sites to preserve battery strength Fill the storage cup with stream water if necessary to keep the probes wet between sites DI can be used to clean the probes between sites Maintenance a b C
17. on probe areas in your path with a walking stick to warn and disperse poisonous snakes like the cottonmouth and copperhead which may inhabit riparian areas Be sure to clean up with bacteria disinfectant soap and water after wading in streams This is particularly important for streams that drain livestock areas sewage treatment plant effluents and other obvious pollution sources Under no circumstances should you drink the water from any stream Protect from water borne illness by wearing protective gloves avoid touching eyes nose and mouth and washing hands frequently with soap and water Personnel qualifications Water parameters will be collected by Missouri State University MSU field personnel who have received appropriate training from experienced personnel prior coursework and field experience regarding the collection of water parameter data and who are familiar with all of MSU s sample handling and labeling procedures and appropriate SOPs Equipment and supplies 10 1 10 2 Model U 22 Water Quality Monitoring System Horiba Instruments Inc 17671 Armstrong Irvine Industrial Center Irvine California 92614 Telephone 949 250 4811 Fax 949 250 0924 http www horiba com a Main unit b Probe and cord c Carrying case d Spare parts kit Water Quality Field Book Pen Reagents and standards 11 1 pH 4 Standard solution Horiba model 100 4 part number 9003 0016 00 500 mL bottle pH 7 00 St
18. s in water can have extreme biological effects In general as the temperature of water increases the amount of oxygen dissolved in the water decreases and there is a tendency for the amount of pollutants to increase The unit of measurement for temperature is C Celsius Conductivity is a measure of the ability of an aqueous solution to carry an electric current The conductivity of water depends upon the presence of ions their total concentration mobility valence and relative concentrations and on the temperature of the solution Adding electrolytes such as salts acids or bases to pure water increases conductance The U 22 uses the 4 electrode method to determine conductivity The conductivity of water is determined by measuring the resistance of ion flow in between charged plates because conductivity is inversely proportional to resistance The Horiba reports conductivity as mS cm milli Siemen centimeter Multiply this value by 1000 to report the conductivity value as uS cm 5 3 5 4 5 5 ID Horiba U 22 Revision 1 September 2006 Page 4 of 14 The U 22 uses the membrane electrode method for Dissolved Oxygen DO A reduction reaction in the cathode is caused by oxygen diffusing through the membrane of the sensor to create a current This current is proportional to the concentration of oxygen dissolved in water DO is reported as mgDO L Potential of hydrogen pH is a unit used to show the degree of acidity on a scale o
19. s up and the calibration finishes Record that the instrument has been calibrated for turbidity in the Horiba instrument log book DO Calibration 1 2 10 11 12 Prepare the zero calibration solution Add 50 g of sodium sulfite to 1 L of DI and mix to dissolve the sodium sulfite Immerse the sensor into the 0 DO solution in a flask large enough to accept the sensor not the calibration beaker Press the CAL key twice in the DO measurement mode MAN ZERO and CAL light up Use the UP DOWN A Y keys to set the value at 0 0 Press the ENT key When the indicated value has stabilized DATA IN lights up and the calibration is finished Prepare the air saturated water solution feed air into a large beaker or bucket of DI using a pneumatic pump Continue supplying air for several minutes to ensure saturation Press the CAL key twice MAN SPAN and CAL light up Using the temperature displayed and the table 1SO5814 table on page 56 of the manual determine the amount of DO in the water Use the UP DOWN A Y keys to set the standard solution value at from the table for example at 25 C 8 42 mgDO L will be in a saturated water sample Press the ENT key The manual span calibration starts When the indicated value has stabilized DATA IN lights up and the calibration finishes Record that the instrument has been calibrated for DO in the Horiba instrument log book Temperature Calibration 1 Press the CAL key in t
20. trument can be used for natural water samples Detection Limit The operating ranges for this instrument are temperature 0 to 55 C conductivity 0 to 9 99 S m Dissolved Oxygen DO 0 to 19 9 mg L pH 0 to 14 units turbidity 0 to 800 NTU and total dissolved solids TDS 0 to 65 0 g L Scope of the test method 4 1 4 2 This procedure will be used as a field reference guide for the collection of water quality analytes Water temperature conductivity pH dissolved oxygen and turbidity can be recorded using the Horiba U 22 Water Quality Monitoring System The Horiba U 22 meter can also measure depth oxidation reduction potential ORP total dissolved solids TDS salinity and seawater specific gravity For information on how to obtain these values refer to the Horiba user s manual which can be found on line at http www wg hii horiba com uw22xd htm and also in the OEWRI office Summary of test method 5 1 5 2 The Horiba U 22 Water Quality Monitoring System uses a thermistor to measure temperature The thermistor also measures the change in electrical resistance accompanying changes in temperature The U 22 uses the temperature data in conductivity temperature conversions dissolved oxygen temperature compensation and pH temperature compensation Temperature influences the conductivity of water As the temperature increases conductivity increases due to the increased movement of ions in the solution Temperature change
Download Pdf Manuals
Related Search