Related Manuals for Thermo Electron 96-09
Summary of Contents for Thermo Electron 96-09
- Page 1 Orion 94-09, 96-09 Orion ionplus Fluoride Electrode INSTRUCTION MANUAL Analyze Detect Measure Control ™ • • •...
- Page 2 PerpHecT, PerpHecTion, pHISA, pHix, pHuture, Pure Water, Sage, Sensing the Future, SensorLink, ROSS Ultra, Sure-Flow, TEA Analyzer, Titrator PLUS, TURBO2 and Wine Master are registered trademarks of Thermo Electron Corporation. 1-888-pHAX-ION, A+, All in One, Aplus, AQUAsnap, AssuredAccuracy, AUTO-BAR, AUTO-CAL, AUTO DISPENSER, Auto-ID, AUTO-LOG, AUTO-READ,...
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Page 3: Table Of Contents
TABLE OF CONTENTS General Information Introduction Required Equipment Required Solutions Using The Electrode Electrode Preparation Filling Instructions Checking Electrode Operation (Slope) Before Analysis Units of Measurement Sample Requirements Measuring Hints Analytical Procedures Analytical Techniques Direct Calibration Low-Level Measurement Known Addition Titrations Fluoride in Acid Solutions Fluoride in Alkaline Solutions... -
Page 4: General Information
GENERAL INFORMATION Introduction The Orion 94-09 Half-Cell Fluoride and Orion 96-09 Combination Fluoride Electrodes measure free fluoride ions in aqueous solutions quickly, simply, accurately, and economically. General analytical procedures, required solutions, electrode characteristics, and electrode theory are discussed in this manual. -
Page 5: Required Equipment
Orion’s 420A, 420Aplus, 520A, 520Aplus, 525A or 525Aplus. Reference Electrode For Orion 94-09: Use with Orion 90-01 Single Junction Reference Electrode. For Orion 96-09: None required. Stirring Accessories Magnetic stirrer or stir bars are highly recommended for laboratory measurements. -
Page 6: Required Solutions
Required Solutions Distilled or Deionized Water To prepare all solutions and standards. Standard Solutions Select the appropriate Thermo Electron Corporation standard(s) from the list below. Standard Solutions Orion No. 0.1 M Sodium Fluoride Standard 940906 100 ppm Fluoride Standard 940907... -
Page 8: Using The Electrode
2. Fill outer chamber with Orion No. 900061. NOTE: The Optimum Result A filling solution (Orion No. 900061) supplied with Orion 96-09 electrode is designed to minimize junction potentials and fluoride ion contamination of the sample, and can be used for all fluoride measurements. -
Page 9: Checking Electrode Operation (Slope)
Checking Electrode Operation (Slope) These are general instructions, which can be used with most meters to check electrode operation. See individual meter instruction manuals for more specific information. This procedure measures electrode slope. Slope is defined as the change in millivolts observed with every tenfold change in concentration. -
Page 10: Before Analysis
F - Moles/Liter 1900 Sample Requirements The epoxy electrode body Orion 94-09 and Orion 96-09 are resistant to attack by inorganic solutions. The electrode may be used intermittently in solutions containing methanol benzene or acetone. Consult Thermo’s Technical Service Chemists for information on using the electrode in specific applications. -
Page 11: Measuring Hints
Measuring Hints • Pipet 50 mL of TISAB II per 50 mL standard or sample, or 10 mL of TISAB III per 90 mL standard or sample. • Stir all standards and samples at a uniform rate during measurement. Magnetic stirrers may generate sufficient heat to change solution temperature. -
Page 12: Analytical Procedures
Analytical Procedures A variety of analytical techniques are available to the analyst. The following is a description of these techniques. Direct Calibration This simple procedure is for measuring a large number of samples. Only one meter reading is required for each sample. Calibration is performed in a series of standards. - Page 13 • Analate Addition is often used to measure soluble solid samples, viscous samples, small or very concentrated samples, or to diminish the effects of varying sample temperatures. This method is not suitable for dilute or low concentration samples. Total concentration is measured even in the presence of complexing agents.
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Page 14: Direct Calibration
1. Remove the rubber cap covering the electrode(s) tip. 2. If using Orion 94-09 electrode with Orion 90-01 Reference Electrode, fill the reference electrode chamber with Orion No. 900001. If using Orion 96-09, fill the chamber of the electrode with Orion No. 900061. 3. Connect electrode(s) to meter. - Page 15 electrode potential (mV) 10-fold change ~ 56 mV ppm fluoride as F 1000 molarity Figure 1 Typical Calibration Curve In the direct measurement procedure using a pH/mV meter, a calibration curve is constructed on semilogarithmic paper. Electrode potentials of standard solutions are measured and plotted on the linear axis against their concentrations on the log axis.
- Page 16 Using a meter with millivolt readout only 1. Adjust the meter to measure mV. 2. Measure 50 mL of the more dilute standard with 50 mL of TISAB II or with 5 mL of TISAB III into a 150 mL beaker. Stir thoroughly.
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Page 17: Low-Level Measurement
2. If using Orion 94-09 Fluoride Half Cell, fill the Orion 90-01 Single Junction Reference Electrode with Orion No. 900001. If using Orion 96-09 Fluoride Combination Electrode, fill the electrode chamber with Orion No. 900061. 3. Connect the electrodes to the meter. Set the meter to read mV. - Page 18 Making Measurements 1. Measure 50 mL deionized water and 50 mL low-level TISAB into a 150 mL beaker. 2. Rinse the electrode(s) with deionized water and place into beaker. Stir thoroughly. 3. Add increments of 19 ppm or 10 M, which has been diluted with low-level TISAB standard, to the beaker using steps outlined in Table 2.
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Page 19: Known Addition
Known Addition Known addition is a convenient technique for measuring samples because no calibration curve is required. It can be used to verify the results of a direct calibration or to measure the total concentration of an ion in the presence of a large excess of a complexing agent. - Page 20 2. If using Orion 94-09 Fluoride Half Cell, fill the Orion 90-01 Single Junction Reference Electrode with Orion No. 900001. If using Orion 96-09 Fluoride Combination Electrode, fill the electrode chamber with Orion No. 900061. 3. Connect the electrode(s) to the meter.
- Page 21 Using a meter with millivolt readout only Use this procedure when known addition is not available. 1. Set the meter to relative millivolt mode; if unavailable, use millivolt mode. 2. Measure 50 mL of sample and 50 mL of TISAB, or 5 ml of TISAB III into a 150 mL beaker.
- Page 22 6. From Table 4, find the value, Q, which corresponds to the change in potential, ∆E. To determine the original sample concentration, multiply Q by the concentration of the added standard: = QC where: = standard concentration = sample concentration = reading from known addition table The table of Q values is calculated for a 10% volume Change.
- Page 23 Table 4 Known Addition Values for Q vs. ∆E at 25 °C for 10% Volume Addition. Slopes are in units of mV/decade. ∆E Concentration Ratio Monovalent (57.2) (58.2) (59.2) (60.1) 0.2894 0.2933 0.2972 0.3011 0.2806 0.2844 0.2883 0.2921 0.2722 0.2760 0.2798 0.2835 0.2642...
- Page 24 ∆E Concentration Ratio Monovalent (57.2) (58.2) (59.2) (60.1) 18.0 0.0786 0.0804 0.0822 0.0839 18.5 0.0759 0.0776 0.0793 0.0810 19.0 0.0733 0.0749 0.0766 0.0783 19.5 0.0708 0.0724 0.0740 0.0757 20.0 0.0684 0.0700 0.0716 0.0732 20.5 0.0661 0.0677 0.0693 0.0708 21.0 0.0640 0.0655 0.0670 0.0686...
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Page 25: Titrations
Titrations The electrode makes a highly sensitive endpoint detector for titrations of a fluoride-containing sample using lanthanum nitrate as the titrant. Titrations are more time-consuming than direct electrode measurements, but results are more accurate and reproducible. With careful technique, titrations are accurate to ±... - Page 26 6. Calculate sample concentration, C Where: = sample concentration = fluoride standard concentration (0.1M) = volume of titrant added in unknown sample titration at endpoint = volume of titrant added in standardization titration at endpoint = volume of sample used in sample titration (25 mL) = volume of standard used in standardization titration (25 mL) -100...
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Page 27: Fluoride In Acid Solutions
Fluoride in Acid Solutions In solutions with a pH below 5, hydrogen ion complexes a portion of the fluoride ion, forming HF or HF which cannot be detected by the electrode. To free the complexed fluoride, the pH of the solution must be adjusted into the weakly acidic to weakly basic region before making the determination. -
Page 28: Fluoride In Alkaline Solutions
Fluoride in Alkaline Solutions In basic solutions containing low fluoride content (less than M at a pH of 9.5 or above), the electrode responds to hydroxide ion as well as to fluoride ion. The potential reading, caused by the concentration of both hydroxide and fluoride ion, is lower than it would be if fluoride alone were present. -
Page 29: Electrode Storage
When storing for long periods of time, replace the cap to protect the sensing element. Orion 96-09 The solution in the Orion 96-09 Fluoride Combination Electrode should not be allowed to evaporate, causing crystallization. For short periods of time between sample measurements, and up to one week, store the electrode in least fluoride concentration standard. - Page 30 3. If the chamber is not completely cleaned, repeat the procedure. 4. Refill with Thermo Filling Solution Orion 900001 for Orion 90-01 or with Orion 900061 for Orion 96-09. If a more thorough cleaning is required, the electrode can be disassembled using the following instructions: 1.
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Page 31: Troubleshooting
TROUBLESHOOTING Troubleshooting Checklist Possible Causes Symptom Defective meter Off-scale or Over-range reading Electrodes not plugged in properly Reference electrode junction is dry No reference electrode Reference electrode not filled Air bubble on element Electrodes not in solution Static electricity Defective meter Noisy or unstable Meter or stirrer improperly grounded... - Page 32 Use Orion 90-01 Reference Electrode with Orion 94-09 Be sure reference electrode is filled with Orion No. 900001 and Orion 96-09 filled with Orion No. 900061 Remove bubble by redipping electrode in solution Put electrodes in solution Wipe plastic parts of meter with detergent solution...
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Page 33: Troubleshooting Guide
Troubleshooting Guide The most important principle in troubleshooting is to isolate the components of the system and check each in turn. The components of the system are: 1) Meter, 2) Electrodes, 3) Standard, 4) Sample, and 5) Technique. Meter The meter is the easiest component to eliminate as a possible cause of error. - Page 34 Standard The quality of results depends greatly upon the quality of the standards- ALWAYS prepare fresh standards when problems arise - it could save hours of frustrating troubleshooting! Error may result from contamination of prepared standards, accuracy of dilution, quality of distilled water, or a mathematical error in calculating the concentrations.
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Page 35: Assistance
Assistance After troubleshooting all components of your measurement system, contact The Technical Edge for Orion products. Within the United States call 1.800.225.1480, outside the United States call 978.232.6000 or fax 978.232.6031. In Europe, the Middle East and Africa, contact your local authorized dealer. For the most current contact information, visit www.thermo.com. -
Page 36: Electrode Characteristics
ELECTRODE CHARACTERISTICS Electrode Response The electrode potential plotted against concentration on semilogarithmic paper results in a straight line with a slope of about 54-60 mV per decade. See Figure 1 The time response of the electrode, that is, the time required to reach 99% of the stable potential reading, varies from several seconds in concentrated solutions to several minutes near the limit of detection. -
Page 37: Limits Of Detection
Limits of Detection In neutral solutions, fluoride concentration can be measured down to 10 M (0.02 ppm) fluoride. However, care must be taken in making determinations below 10 M to avoid sample contamination. The upper limit of detection is a saturated fluoride solution. -
Page 38: Interferences
Interferences Most cations and anions do not interfere with the response of the fluoride electrode to fluoride. Anions commonly associated with fluoride, such as Cl , Br , S0 , HC0 , P0 , and acetate, do not interfere with electrode operation. The OH ion is an electrode interference. - Page 39 Figure 4 Fraction of Free Fluoride As a function of solution pH, hydrogen is the only complexing species. electrode potential (mV) solution pH Figure 5 Electrode Response in Alkaline Solutions...
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Page 40: Complexation
Complexation Fluoride forms complexes with aluminum, silicon, iron (+3), and other polyvalent cations as well as hydrogen. The extent of complexation depends on the concentration of complexing agent, the total fluoride concentration, and pH of the solution, and the total ionic strength of the solution. TISAB II and III contain a reagent, CDTA, that preferentially complexes aluminum or iron in the sample. -
Page 41: Theory Of Operation
Theory of Operation The fluoride electrode consists of a sensing element bonded into an epoxy body. When the sensing element is in contact with a solution containing fluoride ions, an electrode potential develops across the sensing element. This potential, which depends on the level of free fluoride ion in solution, is measured against a constant reference potential with a digital pH/mV meter or specific ion meter. - Page 42 Reference electrode conditions must also be considered. Liquid junction potentials arise any time when two solutions of different composition are brought into contact. The potential results from the interdiffusion of ions in the two solutions. Since ions diffuse at different rates, the electrode charge will be carried unequally across the solution boundary resulting in a potential difference between the two solutions.
- Page 43 Orion 96-09 Combination Fluoride Electrode epoxy-coated spring cable O-ring filling hole electrode body filling solution chamber outer inner reference element inner cone The most important variable, which analysts have under their control, is the composition of the liquid junction filling solution.
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Page 44: Warranty
Warranty For the most current warranty information, visit www.thermo.com. The Thermo Electron Corporation, Orion products warranty covers failures due to manufacturer’s workmanship or material defects from the date of purchase by the user. User should return the warranty card and retain proof of purchase. Warranty is void if product has been abused, misused, or repairs attempted by unauthorized persons. - Page 45 pH/ISE Meters (Orion 310, 320, 330, 350, 370) pH/ISE Meters (Orion 210Aplus ™ , 230Aplus ™ , 250Aplus ™ , 290Aplus ™ 410Aplus ™ , 420Aplus ™ , 520Aplus ™ , 525Aplus ™ , 710Aplus ™ 720Aplus ™ and 920Aplus ™...
- Page 46 indicated on the package. Six months from date of purchase by the user (or twelve months from date of shipment from Thermo) • Orion Flash Titration ™ Probe (Orion 092518), pHuture ™ Electrode (Orion 615700), pHuture MMS ™ Pentrode ™ (Orion 617500), Quatrode ™...
- Page 47 CONSEQUENTIAL DAMAGES WHETHER THE CLAIMS ARE BASED IN CONTRACT, IN TORT (INCLUDING NEGLIGENCE), OR OTHERWISE WITH RESPECT TO OR ARISING OUT OF THE PRODUCT FURNISHED HEREUNDER. REPRESENTATION AND WARRANTIES MADE BY ANY PERSON, INCLUDING ITS AUTHORIZED DEALERS, REPRESENTATIVES AND EMPLOYEES OF THERMO WHICH ALTER OR ARE IN ADDITION TO THE TERMS OF THIS WARRANTY SHALL NOT BE BINDING UPON THERMO UNLESS IN WRITING AND SIGNED BY ONE OF ITS OFFICERS.
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Page 48: Ordering Information
900100 Orion 90-01 Single Junction Reference Electrode 900001 Filling Solution for Orion 90-01 900061 Optimum Fluoride Filling Solution for Orion 96-09 Combination Fluoride Electrode 940906 0.1 M Sodium Fluoride Standard Solution, 475 mL 940907 100 ppm Fluoride Standard Solution, 475 mL... -
Page 49: Specifications
0 to 80 °C continuous use, 80 to 100 °C intermittent use Electrode Resistance 150 - 200 kilohms Reproducibility ± 2% Minimum Sample Size 3 mL in a 50 mL beaker Size Orion 96-09 94-09 Body Diameter 13 mm 12 mm Cap Diameter 16 mm 16 mm Cable Length... - Page 50 Environmental Instruments Water Analysis North America 166 Cummings Center Beverly, MA 01915 USA Tel: 978-232-6000 Dom. Fax: 978-232-6015 Int’l. Fax: 978-232-6031 Europe 12-16 Sedgeway Business Park Witchford, Cambridgeshire England, CB6 2HY Tel: 44-1353-666111 Fax: 44-1353-666001 Far East Room 904, Federal Building 369 Lockhart Road Wanchai, Hong Kong Tel: 852-2836-0981...
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