Instruction Manual HI 84500 FREE & TOTAL SULFUR DIOXIDE MINITITRATOR for wine analysis w w w. h a n n a i n s t .
Dear Customer, Thank you for choosing a Hanna Instruments product. Please read this instruction manual carefully before using this instrument. This manual will provide you with the necessary information for correct use of this instrument, as well as a precise idea of its versatility. If you need additional technical information, do not hesitate to e-mail us at tech@hannainst.com or view our worldwide contact list at www.hannainst.com. TABLE OF CONTENTS PRELIMINARY EXAMINATION...............................
PRELIMINARY EXAMINATION Please examine this product carefully. Make sure that the instrument is not damaged. If any damage occurred during shipment, please notify your Dealer.
A dedicated HELP key aids in setup, calibration, status and troubleshooting.
SPECIFICATIONS Titrator Range Low Range: 1.0 to 40.0 ppm of SO2 High Range: 30 to 400 ppm of SO2 Resolution Low Range: 0.1 ppm High Range: 1 ppm Accuracy Low Range: 3% of reading or ±0.5 ppm @ 25 °C, whichever is greater High Range: 3% of reading or ±1 ppm @ 25 °C, whichever is greater Sample volume 50 mL Titration method Ripper method Principle Equivalence point redox titration Pump speed 10 mL/min Stirring speed 700 rpm Log data Up to 200 samples ORP meter ORP meter -2000.0 to 2000.
PRINCIPLE OF OPERATION The HI 84500 determines the free and total sulfur dioxide concentration in wine using the Ripper method. Excess iodide added to the wine sample reacts with iodate introduced by the titrant to produce iodine. + IO3- + 5I- + 6H → 3I2 + 3H2O The iodine produced in the sample then reacts with sulfur dioxide in the wine according to the redox reaction below: H2SO3 + I2 → H2SO4 + 2HI The HI 84500 utilizes an ORP electrode to monitor the redox titration.
FUNCTIONAL DESCRIPTION OVERHEAD VIEW 1) Titrant bottle 2) Liquid Crystal Display (LCD) 3) Keypad 4) Electrode holder 5) Dispensing tube FRONT VIEW REAR VIEW 6) ORP Electrode 7) Beaker 8) Dosing pump 9) Power switch 10) Power adapter 11) USB connector (PC interface) 12) USB connector (Storage interface) 13) BNC electrode connector 14) Titrant bottle 15) Syringe 16) Aspiration tube 17) Dosing Pump Valve 7
KEYPAD FUNCTION ESC - used to leave the current screen and to return either to the previous screen or to the main screen. In Setup menu, exits a parameter without changing the value.
DOSING PUMP The dosing pump is based on a valve that automatically moves the titrant between the titrant bottle and syringe when filling the syringe and between the syringe and sample when dispensing. A replaceable 5 mL plastic syringe is used to limit the amount of titrant used per test to ensure the highest possible accuracy. Before a set of titrations, it is necessary to prime the dosing system.
SETUP MENU The titrator’s setup menu may be accessed from the main screen (meter or titrator mode) by pressing the MENU key, then Setup. A list of setup parameters will be displayed with currently configured setting. While in the setup menu it is possible to modify the instrument’s operation parameters. The ARROW keys permit the user to scroll the setup parameters. Press HELP to view the contextual help. Press ESC to return to the main screen. Range Setup Use Low measurement range for 1.0 - 40.0 ppm.
Press Format to cycle between the available date formats. Press to highlight the value to be modified. Use the ARROW keys to change the value. Press Accept to confirm the new value or ESC to return to the setup. Key Beep Select Enable to activate or Disable to deactivate the Key Beep function. If enabled, a short beep will be heard every time a key is pressed. Error Beep Select Enable to activate or Disable to deactivate the Error Beep function.
LCD Backlight Press Modify to change the backlight level. The default value is 3. Use the ARROW keys or / to increase/ decrease the backlight level. Press Accept to confirm or ESC to return to the setup menu. Language Tutorial Press the corresponding virtual option key to change the language. If the selected language cannot be loaded, the previously selected language will be reloaded. If no language can be loaded at startup the instrument will work in “safe mode”.
Restore Factory Settings Press Select to restore the factory settings. Press Yes to confirm the restore process or No to return without restoring. Press ESC to return to the setup menu. GUIDE TO DISPLAY CODES This screen appears when the instrument is turned on during the initialization process. Titration screen display. Titration screen when a titration is in progress. Prime burette screen.
Prime burette screen when the dosing system is running. This error message appears when the pump is not working properly. Check the tubing, valve and syringe. Press Restart to try again. PUMP CALIBRATION MESSAGES Pump calibration is initiated by pressing the Start key. This screen appears while pump calibration is in progress. Press ESC or Stop key to return to the Pump Calibration screen. This screen appears when pump calibration is complete.
The calibration was outside the acceptable limits. Prepare a new standard and try again. This error message appears when the input reading (mV) exceeds the input limits (± 2000.0 mV). This screen appears when the stirrer is not working properly. Check the stir bar and beaker content. Press Restart to try again. This error message appears when the pump is not working properly. Check the tubing, valve and syringe. Press Restart to try again.
This error message appears when the input reading (± 2000 mV) exceeds the input limits during a titration. This screen appears when the sample concentration is out of range. This screen appears when the stirrer is not working properly. Check the stir bar and beaker content. Press Restart to try again. This error message appears when the pump is not working properly. Check the tubing, valve and syringe. Press Restart to try again.
DOSING PUMP INSTALLATION To install the dosing pump follow the procedure below: • Extend the plunger on the 5 mL syringe to its maximum volume. • Place the syringe in the dedicated spot on the top of the meter (1). • Arrange the bottom of the syringe into the holder on the pump (2). Once the syringe is in place lower the barrel until it sits flush on the holder. • Put the o-ring and syringe-fixing nut over the syringe (3) and turn clockwise to secure it in place (4).
Note: • The aspiration tube must be inserted in the titrant bottle. The dosing tip must be placed over a rinse beaker. • Before starting the prime procedure, make sure you are using the appropriate titrant solution for the selected range. • To prime the burette, select Prime option from Titration mode. • Adjust the rinses number by pressing the and keys and press Start.
ELECTRODE CHECK PROCEDURE Before taking any measurements with the HI 84500 minititrator, it is recommended to check the HI 3148B ORP electrode using the following steps: • Press Meter to enter mV mode. • Pour roughly 15 mL of HI 7021 into a 20 mL beaker. This does not need to be exact, as long as the PTFE junction is covered by the solution. • Place the electrode in the solution, stir gently for a few seconds and verify the mV reading.
• Press Start, wait for the syringe to refill. • Place the stir bar in the beaker and put the beaker in the minititrator top. • Place the probe holder on the top of the beaker and secure it by turning clockwise. • Rinse the ORP electrode with deionized water and immerse into the sample until the PTFE reference junction is completely submerged. Be sure that the tip of the electrode is not hitting the stir bar. If necessary additional distilled or deionized water can be added.
• This screen appears when the stirrer is not working properly. Check the stir bar and beaker content. Press Restart to try again. • This error message appears when the pump is not working properly. Check the tubing, valve and syringe. Press Restart to try again. FREE SO2 MEASUREMENT PROCEDURE • Refer to “Setup Menu” (see page 10) to set up the instrument for your measurement.
Note: DO NOT PLACE THE TIP INTO THE SAMPLE BEAKER. PLACE THE TIP OVER A WASTE BEAKER. A SMALL AMOUNT OF TITRANT IS DISPENSED WHEN THE PUMP RESETS. • Press Start to begin a titration. • Wait for the syringe to refill. • Place the stir bar in the beaker and put the beaker into the beaker holder. • Place the probe holder on the top of the beaker and secure it by turning clockwise.
• At the end of the titration the instrument displays the concentration in ppm of SO2. The titration curve can be viewed by pressing Plot ON. Press Plot OFF to exit this mode. • Press LOG to record the concentration value and the titration curve into the instrument’s memory. A message will be displayed for a few seconds indicating the amount of free log space. Up to 200 log samples can be recorded in the instrument’s memory. • Press Restart to begin a new titration or ESC to return to the titration menu.
• This error message appears when the pump is not working properly. Check the tubing, valve and syringe. Press Restart to try again. TOTAL SO2 MEASUREMENT PROCEDURE • For best accuracy, before taking any measurement, ensure that the pump is calibrated on the selected range following the “Pump Calibration Procedure” (see page 19). • Select the corresponding range according to the table below: Low Range (50 mL sample) High Range (50 mL sample) 1.0 to 40.
Note: DO NOT PLACE THE TIP INTO THE SAMPLE BEAKER. PLACE THE TIP OVER A WASTE BEAKER. A SMALL AMOUNT OF TITRANT IS DISPENSED WHEN THE PUMP RESETS. • Press Start to begin a titration. • Wait for the syringe to refill. • Place the stir bar in the beaker and put the beaker into the beaker holder. • Place the probe holder on the top of the beaker and secure it by turning clockwise.
TIPS FOR AN ACCURATE MEASUREMENT The instructions listed below should be followed carefully to ensure measurements are conducted with the highest possible accuracy and precision. • IT IS CRITICAL THAT THE TIP BE IMMERSED IN THE SOLUTION BEING TITRATED (APPROXIMATELY 0.25 CM). • Use a clean, volumetric pipette to measure and transfer the wine sample into the titration beaker. • Calibrate the pump prior to each series of titrations. • Calibrate the pump if the meter is left idle for several hours.
The selected record data and the titration curve data file name are displayed. When a USB storage device is connected, the Export key is displayed. It saves the titration curve data as a text file on the storage device using the displayed file name. Use the ARROW keys when is displayed to scroll between the log records. Press ESC to return to the previous screen. Press Plot to visualize the titration curve or ESC to return to the previous screen.
TITRATOR GLP INFORMATION Press MENU then GLP. The pump’s last calibration time, date and slope is displayed. If a calibration hasn’t been performed, the message “Not Calibrated” will be displayed. ORP MEASUREMENT The HI 84500 can be used as an ORP meter for direct measurements. Set the instrument to ORP meter. From titrator mode press Meter until mV units are displayed. Rinse the ORP tip with distilled or deionized water. Place ORP electrode into electrode holder.
Press LOG to save the current reading. During ORP measurements with stirrer on, the stirrer icon will be displayed. In case of a stirrer malfunction, the stirrer will stop and the stirrer icon will start blinking. VIEW/DELETE RECORDED ORP DATA To view or delete previously logged ORP records, press MENU then Recall to access meter logs. When an external USB storage device is connected, the Export key is displayed. It saves the meter and titrator logs in two text format files on the storage device.
If Delete or Del.All is pressed the instrument will ask for confirmation. Press Yes to delete the record or No to return to the previous screen without deleting. Deleting a single record will renumber the list of records. If the ORP log is empty, the message “No records available!” will be displayed.
TROUBLESHOOTING GUIDE SYMPTOMS PROBLEM SOLUTI ON D irty ORP electrode. Soak the electrode tip in HI 7061 cleaning solution for 30 minutes. Refill with fresh fill solution. Cable connection. Soak the electrode tip in HI 7061 cleaning solution for 30 minutes. Refill with fresh fill solution. Check cable connection to meter and verify protective cap is off. Reading out of range. Check cable connection to meter and verify protective cap is off. Check the quality of the sample. Clean the electrodes.
SYMPTOMS PROBLEM SOLUTI ON "Stirrer error" message is displayed at the end of Check the stir bar and pump calibration or beaker content. titration. If the error persists, contact the vendor. Non-spinning stirrer icon blinking in ORP meter mode. If the error persists, contact the vendor. Check the stir bar and beaker content. "Pump error" message is Check the tubing, valve displayed. and syringe. If the error persists, contact the vendor. At startup the meter displays "Methods corrupted".
If the bulb and/or junction is dry, soak the electrode in HI 70300L Storage Solution for at least one hour. If the fill solution (electrolyte) is more than 2½ cm (1”) below the fill hole, add HI 7082 3.5M KCl Electrolyte Solution. For faster response, unscrew the fill hole screw during measurements. STORAGE PROCEDURE To minimize clogging and assure a quick response time, the glass bulb and junction of the electrode should be kept moist and not allowed to dry out.
ACCESSORIES REAGENTS HI HI HI HI HI HI 84500-50 84500-51 84500-55 84500-60 84500-61 84500-62 Low Range Titrant (230 mL) High Range Titrant (230 mL) Calibration Standard (120 mL) Acid Reagent (230 mL) Alkaline Reagent (120 mL) Stabilizer Packet (100 pcs.
WARRANTY HI 84500 is guaranteed for two years against defects in workmanship and materials when used for it’s intended purpose and maintained according to instructions. Electrodes and probes are guaranteed for six months. This warranty is limited to repair or replacement free of charge. Damage due to accidents, misuse, tampering or lack of prescribed maintenance is not covered. If service is required, contact your dealer from whom you purchased the instrument.
Hanna Instruments Inc. Highland Industrial Park 584 Park East Drive Woonsocket, RI 02895 USA Technical Support for Customers Tel. (800) 426 6287 Fax (401) 765 7575 E-mail tech@hannainst.com www.hannainst.
