Thermo Scientific 8102BNUWP, 8103BNUWP, 8257BNU, 8302BNUMD, 8207BNU Instruction Manual

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Orion ROSS Ultra
pH Electrode
INSTRUCTION MANUAL
pH
Orion 8102BNU, 8102SCU, 8103BNU, 8103SCU, 8104BNU, 8104SCU, 8115BNU, 8115SCU, 8135BNU, 8135SCU, 8156BNU, 8156SCU, 800500U
®
ROSS and the COIL trade dress are trademarks of Thermo Electron Corporation
Analyze • Detect • Measure • Control
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ROSS and the COIL trade dress are trademarks of Thermo Electron Corporation.
AQUAfast, Cahn, EZ Flash, Ionalyzer, ionplus, KNIpHE, No Cal, ORION, perpHect, 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, AUTO-STIR, Auto-Test, BOD AutoEZ, Cable-Free, CERTI-CAL, CISA, DataCOLLECT, DataPLUS, digital LogR, DirectCal, DuraProbe, Environmental Product Authority, Extra Easy/Extra Value, FAST QC, Flash Titration, Flash Titrator, GAP, GLPcal, GLPcheck, GLPdoc, ISEasy, KAP, LabConnect, LogR, Low Maintenance Triode, Minimum Stir Requirement, MSR, NISS, One-Touch, One-Touch Calibration, One-Touch Measurement, Optimum Results, Pentrode, pHuture MMS, pHuture Pentrode, pHuture Quatrode, pHuture Triode, Quatrode, QuiKcheK, rf link, ROSS, ROSS Resolution, SAOB, Smart CheK, Stacked, Stat Face, The Enhanced Lab, ThermaSense, Triode, TRIUMpH, Unbreakable pH, Universal Access are trademarks of Thermo.
Guaranteed Success and The Technical Edge are service marks of Thermo.
PerpHecT meters are protected by U.S. patent 6,168,707.
PerpHecT ROSS are protected by U.S. patent 6,168,707.
ORION Series A meters and 900A printer are protected by U.S. patents 5,108,578, 5,198,093 and German patents D334,208 and D346,753.
Sure-Flow electrodes are protected by European Patent 278,979 and Canadian Patent 1,286,720.
ionplus electrodes and Optimum Results solutions are protected by US Patent 5,830,338.
ROSS Ultra electrodes have patents pending.
ORION ORP Standard is protected by US Patent 6,350,367.
ORION Series A conductivity meters are protected by US Patent 5,872,454.
© Copyright 2004, Thermo Electron Corporation. All rights reserved. Question everything, and Analyze.Detect.Measure.Control are trademarks of Thermo Electron Corporation.
The specifications, descriptions, drawings, ordering information and part numbers within this document are subject to change without notice.
This publication supersedes all previous publications on this subject.
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TABLE OF CONTENTS
General Information 1
Introduction 1 Required Equipment 2 Required Solutions 2
Using the Electrode 3
Electrode Preparation 3 Sample Requirements 4 Measuring Hints 5
pH Calibration & Measurement 7
General Calibration Procedure 7 Single Buffer Calibration 7 Two-Buffer Calibration 8 pH Measurement 9 Electrode Storage 9 Electrode Maintenance 10 Cleaning Electrode 10
Troubleshooting 11
Troubleshooting Guide 11 Assistance 12
Electrode Characteristics 13
Temperature Effects 13 Interferences 13
Ordering Information 15
Electrode 15 Accessories 26
Specifications 17
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1
GENERAL INFORMATION
Introduction
This manual contains instructions for the Orion ROSS Ultra®series of pH electrodes. Operation and maintenance instructions for the following electrodes are included.
Orion Description
800500U ROSS Ultra Reference Electrode, glass body, pin tip
8102BNU ROSS Ultra Combination pH Electrode, 0-14 pH,
glass body, BNC
8103BNU ROSS Ultra Combination Semi-micro pH Electrode,
0-14 pH, glass body, BNC
8104BNU ROSS Ultra Combination pH Electrode, 0-14 pH,
glass body with rugged bulb, BNC
8115BNU ROSS Ultra Combination Semi-micro pH Electrode,
0-14 pH, epoxy body, BNC
8135BNU ROSS Ultra Combination Flat Surface Electrode,
0-14 pH, epoxy body, BNC
8156BNU ROSS Ultra Combination pH Electrode, 0-14 pH,
epoxy body, BNC
8102SCU ROSS Ultra Combination pH Electrode, 0-14 pH,
glass body, SC*
8103SCU ROSS Ultra Combination Semi-micro pH Electrode,
0-14 pH, glass body, SC*
8104SCU ROSS Ultra Combination pH Electrode, 0-14 pH,
glass body with rugged bulb, SC*
8115SCU ROSS Ultra Combination Semi-micro pH Electrode,
0-14 pH, epoxy body, SC
8135SCU ROSS Ultra Combination Flat Surface Electrode,
0-14 pH, epoxy body, SC
8156SCU ROSS Ultra Combination pH Electrode, 0-14 pH,
epoxy body, SC
* Screw cap requires cable, Orion 91CBNC to connect to
BNC meters.
The ROSS Ultra series of electrodes provides readings stable to
0.01 pH in less than 30 seconds, even in the extreme case of samples varying from one another by 50 °C or more. Results are three to five times more precise than those obtained with conventional electrodes.
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2
Required Equipment
Meter — Any Orion pH or ion selective meter, or other pH/ISE meter
with appropriate connectors.
Electrode — ROSS Ultra
®
Combination electrodes or ROSS Ultra
reference electrode with ROSS 8101 ROSS pH Half-cell electrode.
ATC Probe — for temperature measurement. Select ATC probe compatible with meter.
Beakers — Plastic or glass.
Magnetic Stirrer — Suggested for precision measurements.
Required Solutions
pH Buffers — Two are recommended for precise measurement. The
first, near the electrode isopotential point (pH 7) and the second near the expected sample pH (e.g., pH 4 or 10).
ROSS
Internal Filling Solution - 3M KCl, Orion 810007. Do not use
any filling solution which contains silver. (Electrode damage may result.)
Figure 1: Orion 8102BNU ROSS Ultra Combination Electrode
Fill Hole
ROSS Ultra
Internal Reference
pH Sensing Bulb
Filling Solution Chamber
Ceramic Reference Junction
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USING THE ELECTRODE
Electrode Preparation
1. Remove the protective shipping cap from sensing element and save for storage.
2. Clean any salt deposits from exterior by rinsing with distilled water.
3. Uncover fill hole and add ROSS
Filling Solution, Orion 810007, to electrode. See Figure 2. To maintain an adequate flow rate, the level of filling solution must cover the end of the coil and be at least one inch above the sample level on immersion. The fill hole should be open whenever the electrode is in use.
4. Place the electrode in the electrode holder and suspend in air for 15 minutes to thoroughly wet the reference junction. Once the junction is wet, do not allow the electrode to dry out.
5. Carefully shake down the electrode (as a clinical thermometer) to remove air bubbles.
6. Soak electrode in pH Electrode Storage Solution, Orion 910001, for one hour.
7. Connect electrode to meter.
Figure 2: Filling an Electrode
3
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Sample Requirements
One of the benefits of the ROSS Ultra®pH Electrode is that the reference electrode filling solution composition may be changed depending on sample requirements.
The ROSS
pH Electrode Filling Solution, Orion 810007 is 3M KCl. For solutions with components that precipitate in the presence of chloride ion, the ROSS Ultra pH Electrode could be filled with 10% KNO
3
, Orion 900003.
Samples should be aqueous if using epoxy body electrodes (e.g., Orion 8115, 8135, 8156 ROSS Ultra electrodes).
In organic solutions, use an all glass ROSS Ultra Electrode (e.g., Orion 8102, 8103 and 8104 ROSS Ultra electrodes). For good results a minimum of 20% water must be present in the sample. If there is a great deal of drift when using the ROSS Ultra Electrode filled with ROSS Filling Solution, Orion 810007, try filling the electrode with a mixture of methanol and water saturated with KCl.
Figure 3: Measuring Hints
4
Fill hole should
be uncovered
Filling solution level must be higher than sample level
Fresh pH buffer
Stir all samples
and buffers
Reference junction must be immersed in sample or buffer
Place insulation between stirrer and beaker
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Measuring Hints
See Figure 3
Always use fresh buffers for calibration. Choose buffers that are no more than 3 pH units apart.
Check electrode slope daily by performing two buffer calibration. Slope should be 92 to 102%.
Only use ROSS
Internal Filling Solution, Orion 810007, for
ROSS Ultra
®
Combination pH Electrodes. Do not use any
filling solution which may contain silver.
Remove fill hole cover during measurement to ensure uniform flow of filling solution.
Between measurements, rinse electrodes with distilled water and then with the next solution to be measured.
Stir all buffers and samples.
Place a piece of insulating material (e.g., Styrofoam or cardboard) between magnetic stirrer and beaker to prevent error from transfer of heat to sample. Since ROSS Ultra Electrodes respond faster than conventional electrodes, changes in pH which result from temperature changes will be noticed. See Electrode Characteristics.
Avoid rubbing or wiping electrode bulb, to reduce chance of error due to polarization.
Orion 8135BNU may be used on any moist surface or in liquids. See Figure 4.
Figure 4: Use of Orion 8135BNU
567
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pH CALIBRATION & MEASUREMENT
General Calibration Procedure
For detailed calibration and temperature compensation procedures, consult your meter instruction manual.
Single Buffer Calibration
1. Choose a buffer near expected sample pH.
2. Buffer should be at same temperature as sample. If buffer and samples are at varying temperatures, temperature compensation is recommended.
3. Set up meter according to meter instruction manual.
4. Rinse electrode first with distilled water and then with the buffer being used for calibration.
5. Place the electrode in the buffer. Wait for a stable display. Set the meter to the pH value of the buffer at its measured temperature. See Table 1. (A table of pH values at various temperatures is supplied on the buffer bottle.) Proceed to pH
Measurement section.
Table 1 pH Values of Buffers at Various Temperatures
Nominal value at 25 ˚C Temperature
Buffer 0 ˚C 5 ˚C 10 ˚C 20 ˚C 30 ˚C
1.68 1.67 1.67 1.67 1.67 1.68
3.78 3.86 3.84 3.82 3.79 3.77
4.01 4.00 4.00 4.00 4.00 4.02
5.00 5.12 5.04 4.97
6.86 6.98 6.95 6.92 6.87 6.85
7.00 7.11 7.08 7.06 7.01 6.98
7.41 7.53 7.50 7.47 7.43 7.40
9.18 9.46 9.40 9.33 9.23 9.14
10.01 10.32 10.25 10.18 10.06 9.97
40 ˚C 50 ˚C 60 ˚C 70 ˚C 80 ˚C 90 ˚C
1.69 1.71 1.72 1.74 1.77 1.79
3.75 3.75
4.04 4.06 4.09 4.13 4.16 4.21
4.93 4.92 4.88
6.84 6.83 6.84 6.85 6.86 6.88
6.97 6.97 6.97 6.99 7.03 7.08
7.38 7.37
9.07 9.01 8.96 8.92 8.89 8.85
9.89 9.83
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8
Two Buffer Calibration
This procedure is recommended for precise measurement.
1. Ensure that all buffers are at the same temperature. If samples are at varying temperatures, temperature compensation is recommended. (See Meter Instruction manual).
2. Select two buffers which bracket the expected sample pH. The first should be near the electrode isopotential point (pH 7) and the second near the expected sample pH (e.g., pH 4 or pH 10).
3. Rinse electrode first with distilled water and then with first (pH 7) buffer.
4. Place the electrode in first (pH 7) buffer. Wait for a stable display. Set the meter to the pH value of the buffer at its measured temperature. (A table of pH values at various temperatures is supplied on the buffer bottle). See Table 1.
5. Rinse electrode first with distilled water and then with the second buffer.
6. Place the electrode in the second buffer. When display is stable, set meter to the pH value of the buffer at its measured temperature as described in the meter instruction manual.
7. If all steps are performed correctly, proceed to the pH Measurement section. If any of the above procedures does not work, refer to Troubleshooting.
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pH Measurement
1. Calibrate the electrode as described in previous section.
2. Rinse the electrode with distilled water and then with sample.
3. Place the electrode in the sample.
4. When the display is stable, record sample pH.
Electrode Storage
To ensure a quick response and free-flowing liquid junction, the sensing bulb and reference junction must not be allowed to dry out.
NOTE: The reference chamber should remain filled at all times.
Short-term Storage (up to one week): Soak electrode in pH Electrode Storage Solution, Orion 910001.
Long-term Storage: The reference chamber should be filled and the filling hole securely covered. Cover the sensing element and reference junction with its protective cap containing a few drops of storage solution. Before returning the electrode to use, prepare it as a new electrode.
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Electrode Maintenance
1. Inspect the electrode for scratches, cracks, salt crystal build-up, or membrane/junction deposits.
2. Rinse off any salt build-up with distilled water, and remove any membrane/junction deposits as directed in the cleaning procedures below.
3. Drain the reference chamber, flush it with fresh ROSS
Filling
Solution, Orion 810007, and refill the chamber.
Cleaning Electrode
Thermo Electron offers Orion pH electrode cleaning kits in the following configurations:
pH Cleaning Solution Sample Kit (Orion 900020) — Includes one
bottle each of cleaning solution A, B, C and D, 15 mL Beaker and Pipette.
pH Cleaning Solution A (Orion 900021) — Protein removal.
pH Cleaning Solution B (Orion 900022) — Removal of bacterial
contaminant's.
pH Cleaning Solution C (Orion 900023) — General cleaning.
pH Cleaning Solution D (Orion 900024) — Removal of oil and grease
contaminant's.
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TROUBLESHOOTING
Troubleshooting Guide
Follow a systematic procedure to isolate the problem. The pH measuring system can be divided into four components for ease in troubleshooting: pH meter, electrodes, sample/application, and technique.
pH meter
The meter is the component which is easiest to eliminate as a possible cause of error. Thermo Electron pH meters are provided with an instrument checkout procedure and shorting cap for convenience in troubleshooting. Consult your pH meter instruction manual for directions.
Electrodes
To test electrode operation:
1. Connect electrode to a working meter.
2. Set function switch to absolute mV mode.
3. Immerse electrode in fresh pH 7 buffer.
4. Displayed value should be 0 ± 30 mV.
5. Rinse electrode and immerse in fresh pH 4 buffer.
6. Displayed value should be approximately 160 mV to 180 mV greater than in step 4. (Actual mV values may change as electrode ages, but mV differences will remain 160 to 180 mV).
If electrode fails this procedure, clean thoroughly as directed in Maintenance.
If electrode response is slow or drifting, drain and refill with fresh ROSS
Filling Solution, Thermo Electron Orion 810007. See Measuring Hints. If cleaning and maintenance fail to rejuvenate the electrode, replace the entire electrode.
Sample/Application
The electrode and meter may operate with buffers but not with your sample. In this case, check sample composition for interferences, incompatibilities, or temperature effects. Some samples, by their nature, drift or change in pH.
Technique
If trouble persists, review operating procedures. Reread calibration and measurement sections, to be sure proper technique has been followed.
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Assistance
For the most current warranty information, visit www.thermo.com.
After troubleshooting all components of your measurement system, contact The Technical Edge
SM
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.
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ELECTRODE CHARACTERISTICS
Temperature Effects
The most common cause of error in pH measurement is temperature. Ordinary electrodes drift with temperature changes. The ROSS Ultra™pH Electrode eliminates the stability problems associated with the use of conventional electrodes in samples of varying temperature.
There are, however, two effects of temperature change that should be kept in mind.
1. Electrode slope will change with varying temperature. This
slope change may be compensated for either manually, or automatically with an automatic temperature compensator (ATC) probe and properly designed pH meter. Consult your pH meter instruction manual for details.
2. Buffer and sample pH values vary with temperature because
of the temperature dependent chemical equilibrium. The problem of varying pH values is easily solved by calibrating the electrode with characterized standard buffers whose true pH values at different temperatures are known. Buffer values at different temperatures are given in Table 1. The problem of the sample equilibrium varying with temperature in an uncharacterizable manner will always remain. Therefore, pH values should be reported along with the temperature at which the measurement was made.
Interferences
Sodium ion is the principle interference of the pH electrode, causing increasing error at higher pH (lower hydrogen ion activities) and at higher temperatures. Because the ROSS Ultra® pH membrane is composed of special low sodium error glass, error due to sodium is negligible when measuring at pH values less than 12. When measuring at pH values greater than 12, add the correction value from the nomography in Figure 6 to the observed pH reading.
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Figure 6: Typical Sodium Error Observed at pH > 12
Example:
pH reading 12.10 Sodium concentration 0.5 N Temperature 50 ˚C Correction 0.01 Corrected pH reading 12.11
14
Sample pH reading
13
12
11
10
°C 20 0.1 M
25
0.5 M
30
40
50
60
70
80
0.1 M
0.5 M
1 M
1 M
2 M
2 M
sample sodium
concentration
5 M
20°C 25
30
40
50
60
70
80
5 M
pH correction to be added
0.005
0.01
0.02
0.03
0.04
0.05
0.06
0.08
0.10
0.15
0.20
0.25
0.30
0.40
0.50
0.60
0.70
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15
ORDERING INFORMATION
Electrodes
Type of
Orion Description Connector
800500U ROSS Ultra
®
Combination pH Electrode, Pin Tip
glass body
8102BNU ROSS Ultra
®
Combination pH Electrode, BNC
glass body
8103BNU ROSS Ultra
®
Combination Semi-micro BNC
pH Electrode, glass body
8104BNU ROSS Ultra Combination pH Electrode, BNC
glass body with rugged bulb
8115BNU ROSS Ultra Combination Semi-micro BNC
pH Electrode, epoxy body
8135BNU ROSS Ultra Combination Flat Surface BNC
pH Electrode, epoxy body
8156BNU ROSS Ultra Combination pH Electrode, BNC
epoxy body
8102SCU ROSS Ultra Combination pH Electrode, Screw Cap
glass body Connector
8103SCU ROSS Ultra Combination Semi-micro Screw Cap
pH Electrode, glass body Connector
8104SCU ROSS Ultra Combination pH Electrode, Screw Cap
glass body with rugged bulb Connector
8115SCU ROSS Ultra Combination Semi-micro Screw Cap
pH Electrode, epoxy body Connector
8135SCU ROSS Ultra Combination Flat Surface Screw Cap
pH Electrode, epoxy body Connector
8156SCU ROSS Ultra Combination pH Electrode, Screw Cap
epoxy body Connector
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Accessories
Orion Description
810007 ROSS
®
Internal Filling Solution, 3 M KCl,
five 50 mL bottles
910001 pH Electrode Storage Solution, 475 mL
910104 pH 4.01 Buffer, 475 mL
910107 pH 7.00 Buffer, 475 mL
910110 pH 10.01 Buffer, 475 mL
910410 perpHect
®
Buffer pH 4, 10 pk
910425 perpHect Buffer pH 4, 25 pk
910710 perpHect Buffer pH 7, 10 pk
910725 perpHect Buffer pH 7, 25 pk
910110 perpHect Buffer pH 10, 10 pk
910125 perpHect Buffer pH 10, 25 pk
911110 perpHect Electrode Rinse, 10 pk
911125 perpHect Electrode Rinse, 25 pk
900020 pH Cleaning Solution Sample Kit
900021 pH Cleaning Solution A – Protein Removal
900022 pH Cleaning Solution B – Bacterial Removal
900023 pH Cleaning Solution C – General Cleaning
900024 pH Cleaning Solution D – Removal of Oil and Grease
91CBNC Detachable Cable for Screw Cap Electrode,
with BNC Connector
91USCB Detachable Cable for Screw Cap Electrode,
with US Standard Connector
91CDIC Detachable Cable for Screw Cap Electrode,
with E DIN Connector
91CBRA Detachable Cable for Screw Cap Electrode,
with Radiometer No.7 Connector
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SPECIFICATIONS
Length Electrodes
Electrodes* (excluding cap) Diameter
800500U 120 mm 12 mm
8102BNU 120 mm 12 mm 8102SCU 120 mm 12 mm
8103BNU 165 mm 6 mm** 8103SCU 165 mm 6 mm**
8104BNU 120 mm 12 mm 8104SCU 120 mm 12 mm
8115BNU 185 mm 8 mm*** 8115SCU 185 mm 8 mm***
8135BNU 120 mm 12 mm 8135SCU 120 mm 12 mm
8156BNU 120 mm 12 mm 8156SCU 120 mm 12 mm
* ROSS Ultra
®
Electrodes operate in a 0-100 °C temperature range, 0-14 pH range
** 6 mm section is 100 mm long
*** 8 mm section is 100 mm long
Isopotential points are at pH 7
Standard cap diameters are 16 mm and cap lengths are 30 mm
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NOTES
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Analyze • Detect • Measure • Control
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