Instruction Manual HI 84502 TITRABLE TOTAL ACIDITY 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.
GENERAL DESCRIPTION The HI 84502 is a low-cost, easy to use, microprocessor-based automatic titrator that benefits from Hanna’s years of experience as manufacturer of analytical instruments. The instrument incorporates a simple and reliable dosing pump which ensures high dosing reproducibility. Pump calibrations, performed with the provided Hanna reagents, assure the accuracy of the instrument. The instrument comes with a preprogrammed method for Total Titratable Acidity measurements in wine.
SIGNIFICANCE OF USE Acids occur naturally during the growing of grapes and as part of the fermentation process. Wines show lower levels of acid when there are hot growing seasons or when the grapes come from hotter regions. In the proper proportion, acids are a desirable trait and give the wine character. The three predominant acids in wine are tartaric, malic and citric, all of which are intrinsic to the grape.
SPECIFICATIONS Titrator Range Low Range: 0.1 to 5.0 g/L of tartaric acid High Range: 4.0 to 25.0 g/L of tartaric acid Resolution 0.1 g/L Accuracy 3 % of reading or ± 0.1 g/L @ 25 °C whichever is greater Sample volume 10 mL (Low Range) / 2 mL (High Range) Titration method Acid-base titration Principle End point titration: 7.00 pH or 8.20 pH Pump speed 10 mL/min Stirring speed 600 rpm Log data Up to 200 samples pH meter pH meter -2.0 to 16.0 pH / -2.00 to 16.00 pH pH Resolution 0.1 pH / 0.
REQUIRED REAGENTS Code HI 84502-50 HI 84502-55 Description Titrant Calibration Standard PRINCIPLE OF OPERATION The determination of total acids in wine is made according to a neutralization reaction, that is the reaction between the acids found in wine and a base. Titratable acidity is measured on a degassed sample at the end-point of 8.20. The results are expressed as g/L tartaric acid. For precise results it is very important to know the sample volume, titrant volume and concentration.
FUNCTIONAL DESCRIPTION OVERHEAD VIEW 1) 2) 3) 4) 5) Titrant bottle Liquid Crystal Display (LCD) Keypad Electrode holder Dispensing tube FRONT VIEW REAR VIEW 6) Temperature probe 7) pH Electrode 8) Beaker 9) Dosing pump 10) Power switch 11) Power adapter 12) USB connector (PC interface) 13) USB connector (Storage interface) 14) Temperature connector 15) BNC electrode connector 16) Reference connector 17) Titrant bottle 18) Syringe 19) Aspiration tube 20) Dosing Pump Valve 8
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.
5) 6) 7) 8) Stirrer and reading status Main reading information pH temperature compensation mode (Manual or Automatic) Temperature reading 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.
SETUP MENU The titrator’s setup menu may be accessed from the main screen (meter or titrator) 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 0.1 - 5.0 g/L.
Temperature Unit °C, °F or K. Press the virtual option key to change the option. Time Press the Modify key to change the time and time format. Press Format to switch between 12 hour (am/pm) and 24 hour mode. 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. Date Press the Modify key to change the date and date format. Press Format to cycle between the available date formats.
Error Beep Select Enable to activate or Disable to deactivate the Error Beep function. If enabled, a beep will be heard when an error condition occurs. Decimal Separator This option allows the user to select the symbol used for a decimal separator. LCD Contrast This option is used to set the display’s contrast. Press Modify to change the display’s contrast. The default value is 8. Use the ARROW keys or / to increase/ decrease the value. Press Accept to confirm the value or ESC to return to the setup menu.
Language 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”. In “safe mode” all messages are displayed in English. Tutorial and help information are not available. Tutorial Enable or Disable the Tutorial. This helpful tool offers additional information during calibration and titration.
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. This screen appears when the titrator is in calibration mode. Press Pump to calibrate Pump.
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 error message appears during pump calibration when the end point can not be reached and the maximum amount of titrant is exceeded. Check standard, electrode and/or dosing system and try again. The calibration was outside the acceptable limits. Prepare a new standard and try again.
pH CALIBRATION MESSAGES pH calibration mode. When the reading has stabilized press Confirm to accept the calibration or Clear to restore the default calibration. The “Wrong Buffer” message is displayed when the pH value is outside of the acceptable range. Clean the electrode by following the Cleaning Procedure and/or check the buffer concentration before continuing the pH calibration. Press the ESC key to exit pH calibration mode.
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. ELECTRODE PREPARATION PREPARATION PROCEDURE Remove the electrode protective cap. DO NOT BE ALARMED IF ANY SALT DEPOSITS ARE PRESENT.
ELECTRODE CALIBRATION PROCEDURE It is recommended to calibrate the instrument frequently, especially if high accuracy is required.
Point 1 calibration • The default buffer selected will be 7.01 if end point was set to 7.00 pH or else 8.20 pH will be selected. If necessary, press the ARROW keys in order to select a different buffer value. • The (unstable measurement) symbol will be shown on the display until the reading becomes stable. • When the reading is stable and close to the selected buffer, the (unstable measurement) symbol will disappear and the Confirm key will become active.
• The (unstable measurement) symbol will be shown on the display until the reading becomes stable. • When the reading is stable and close to the selected buffer, the (unstable measurement) symbol will disappear and the Confirm key will become active. • Press Confirm to confirm the calibration. • The calibrated value will be shown on the display and the third expected buffer value will be automatically selected.
• If the measured offset isn’t within the preset limits (±45 mV), the meter will display the message “Buffer Contaminated” alternatively with ”Electrode Dirty/Broken”. • If the computed slope isn’t within the preset limits, the meter will display the message “Wrong Slope”. If the slope is too high the symbol will be displayed. If the slope is too low the symbol will be displayed.
Note: • To clear a previous calibration and to return to the default value, press Clear at any time after entering calibration mode. If Clear is invoked during the first calibration point the instrument returns to the measurement mode. • The Clear key is displayed only if a previous calibration exists. pH BUFFER TEMPERATURE DEPENDENCE Temperature has an effect on pH. The calibration buffer solutions are affected by temperature changes to a lesser degree than normal solutions.
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. • To prime the burette, select Prime option from Titration mode. • Adjust the rinses number by pressing the and keys and press Start. • The number of syringe rinses can be set between 1 and 5 (at least three rinses are recommended to ensure that the air bubbles are completely removed). • To pause the prime process press the Pause key; to continue press the Continue key.
PUMP CALIBRATION PROCEDURE The calibration of the pump must be performed every time the syringe, pump tube, the titrant bottle or the pH electrode is changed. It is recommended to perform the pump calibration before each set of titration or after the titrator is left idle for several hours. • Press MENU, select Setup and select the corresponding range according to the table below: Low Range High Range 0.1 to 5.0 g/L 4.0 to 25.0 g/L • Verify the electrode has been calibrated in 8.20 pH buffer or in 7.
• Insert the dosing tip into the titrant tube sleeve. IT IS CRITICAL THAT THE TIP BE IMMERSED APPROXIMATELY 0.25 CM (0.1") INTO THE SOLUTION BEING TITRATED. • Press Continue to begin the calibration and Stop to abort it. • At the end of the calibration, ”Calibration Completed“ appears on display. To repeat the calibration press Restart or ESC to return to the main screen. Note: • If temperature probe is not connected, Manual Temperature Compensation is used and MTC appears on the right side of the screen.
TITRATION 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 26). Note: Verify that the instrument has been calibrated (pH and pump) before performing any titrations. • Refer to “Setup Menu” (see page 11) to set up the instrument for your measurement. • Select the corresponding range according to the table below: Low Range High Range 0.1 to 5.0 g/L 4.0 to 25.
• Insert the dosing tip into the titrant tube sleeve. IT IS CRITICAL THAT THE TIP BE IMMERSED APPROXIMATELY 0.25 CM (0.1") INTO THE SOLUTION BEING TITRATED. • Press Continue to begin the titration and Stop to abort it. • The instrument will continuously update the concentration on the display. The value will be displayed blinking. When the reading is under range “----” symbol appears blinking. • The titration curve can be visualized during a titration by pressing Plot ON. Press Plot OFF to exit this mode.
• Press Restart to begin a new titration or ESC to return to the titration menu. • If the concentration exceeds the range limits (> 5.0 g/L for Low Range, > 25.0 g/L for High Range) the exceeded range limit will be displayed blinking. Another titration can be started by pressing Restart. • “Wrong input” error message appears when the input reading (pH, temperature) exceeds the specified limits. The pH or temperature value and the concentration will blink indicating an error.
VIEW/DELETE TITRATOR RECORDED DATA Press MENU then Recall to access the Titrator 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. Press Meter or Titrator to view the respective logs. The instrument will display a list of all the records stored in the log. Use the ARROW keys to scroll the stored records list.
Press Plot to visualize the titration curve or ESC to return to the previous screen. On the titration curve, the end point volume and pH are displayed. The titration data (Total Titrant Volume on the x-axis and pH on the y-axis) can be scanned through with the dotted line by using the ARROW keys. To zoom on the titration curve press Zoom. 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.
Press Pump to view the pump’s last calibration time, date and slope. If a calibration hasn’t been performed, the message “Not Calibrated” will be displayed. pH MEASUREMENT The HI 84502 can be used as a pH meter for direct measurements. Verify that the instrument has been calibrated before taking pH measurements. Set the instrument to pH meter. From titrator mode press Meter until pH units are displayed.
In order to take pH measurements, follow the next steps: • Submerge the pH electrode 2 cm (0.8’’) and the temperature probe into the sample to be tested and stir gently. Make sure the PTFE junction is completely submersed. Allow time for the electrode to stabilize. When the reading becomes stable the (unstable measurement) symbol will disappear. • If the pH reading is less than -2.00 pH or greater than 16.00 pH, the closest full-scale value will be displayed blinking.
VIEW/DELETE RECORDED pH DATA To view or delete previously logged pH records, press MENU then Recall to access the pH 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. Press Meter or Titrator to view the respective logs. The instrument will display a list of all the records stored in the log.
Deleting a single record will renumber the list of records. If the pH log is empty, the message “No records available!” will be displayed. pH METER GLP INFORMATION The pH meter GLP screens displays the last pH calibration data. To view this information, press MENU key then GLP. Press Electrode to view information regarding electrode calibration. GLP contains a set of information regarding electrode calibration.
PC INTERFACE AND DATA TRANSFER Data stored on the meter with the LOG function during pH/mV measurement and titrations can be transferred from the meter to a USB stick using the Export function from the log recall menu. Two text files are transferred on the USB stick. These files can be used for further analysis on a PC. The logged data can also be transferred from the instrument to the PC using a USB cable. Connect the USB cable and the following screen will be displayed.
TROUBLESHOOTING GUIDE SYMPTOMS Slow response/excessive drift. Reading fluctuates up and down (noise). PROBLEM D irty pH electrode. Clogged/dirty junction. Low electrolyte level (refillable pH electrodes only). Cable connection. SOLUTION Soak the electrode tip in HI 7061 cleaning solution for 30 minutes. Refill with fresh fill solution. 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.
SYMPTOMS PROBLEM SOLUTION After a titration in Low Range, the instrument displays 0.1 or 5.0 g/L blinking. Wrong range selected. Concentration out of range. Change range to High Range. Recalibrate the pump. After a titration in High Range, the instrument displays 4.0 or 25.0 g/L blinking. Wrong range selected. Concentration out of range. Change range to Low Range. Recalibrate the pump. At startup the meter displays the HANNA logo One of the keys is stuck. permanently.
ELECTRODE CONDITIONING AND MAINTENANCE PREPARATION PROCEDURE Remove the protective cap of the pH electrode (HI 1048B). DO NOT BE ALARMED IF SALT DEPOSITS ARE PRESENT. This is normal with electrodes. They will disappear when rinsed with distilled/deionized water. During transport, tiny bubbles of air may form inside the glass bulb, affecting proper functioning of the electrode. These bubbles can be removed by “shaking down” the electrode as you would do with a glass thermometer.
STORAGE PROCEDURE To minimize clogging and assure a quick response time, the glass bulb and the junction of the electrode should be kept moist and not allowed to dry out. Replace the solution in the protective cap with a few drops of HI 70300 Storage Solution or, in its absence, with HI 7082 Fill Solution. Follow the Preparation Procedure before taking measurements. Note: NEVER STORE THE ELECTRODE IN DISTILLED OR DEIONIZED WATER. PERIODIC MAINTENANCE Inspect the electrode and the cable.
ACCESSORIES REAGENTS HI 84502-50 HI 84502-55 pH CALIBRATION HI 7004M HI 7007M HI 70082M HI 7010M ELECTRODES HI 1048B HI 7662-T Titrant Solution (230 mL) Calibration Standard (120 mL) SOLUTIONS Buffer solution pH 4.01 (230 mL) Buffer solution pH 7.01 (230 mL) Buffer solution pH 8.20 (230 mL) Buffer solution pH 10.
WARRANTY HI 84502 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 dealerfrom 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.
