Hanna Instruments HI 84533 Manuel utilisateur

Instruction Manual

HI 84533

FORMOL NUMBER

MINITITRATOR

for Fruit Juices and Wines analysis

www.hannainst.com

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 [email protected]

or view our worldwide contact list at www.hannainst.com.

All rights are reserved. Reproduction in whole or in part is prohibited without the written consent

of the copyright owner, Hanna Instruments Inc., Woonsocket, Rhode Island, 02895, USA.

TABLE OF CONTENTS

PRELIMINARY EXAMINATION................................................................................................. 3

GENERAL DESCRIPTION ........................................................................................................ 3

SPECIFICATIONS ................................................................................................................... 5

PRINCIPLE OF OPERATION .................................................................................................... 6

FUNCTIONAL DESCRIPTION................................................................................................... 7

TITRATOR STARTUP ............................................................................................................. 9

SETUP MENU .................................................................................................................... 10

GUIDE TO DISPLAY CODES ................................................................................................... 14

ELECTRODE PREPARATION .................................................................................................. 18

ELECTRODE CALIBRATION PROCEDURE ................................................................................. 19

pH BUFFER TEMPERATURE DEPENDENCE............................................................................ 23

DOSING PUMP INSTALLATION ............................................................................................. 24

DOSING PUMP PRIME PROCEDURE ..................................................................................... 24

PUMP CALIBRATION PROCEDURE ........................................................................................ 26

TITRATION PROCEDURE ..................................................................................................... 28

pH MEASUREMENT ............................................................................................................ 34

PC INTERFACE AND DATA TRANSFER ................................................................................... 38

TROUBLESHOOTING GUIDE ................................................................................................ 39

ELECTRODE CONDITIONING AND MAINTENANCE .................................................................. 41

ACCESSORIES ..................................................................................................................... 42

WARRANTY........................................................................................................................ 43

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.

Each HI 84533 minititrator is supplied complete with:

•HI 84533-70 Reagent kit for formol number in wine and fruit juices

•HI 1131B pH electrode

•HI 7662-T Temperature probe

•HI 7082 Electrode Fill Solution (30 mL)

•Two 100 mL beakers

•Tube set (aspiration tube with titrant bottle cap and dispensing tube with tip)

•Dosing Pump Valve

•5 mL Syringe (2 pcs.)

•2000 µL automatic pipette with two plastic tips

•1 mL Plastic Pipette

•Stir bar

•Power Adapter

•Two sachets of cleaning solution for wine deposits

•Two sachets of cleaning solution for wine stains

•Instruction manual

Note:Save all packing material until you are sure that the instrument works correctly.

Any defective item must be returned in its original packing.

GENERAL DESCRIPTION

The HI 84533 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 Formol measurements in fruit juices and

wines.

The HI 84533 performs the analysis and all the necessary calculations, with a simple and effective

user interface.

SIGNIFICANCE OF USE

The amino-acid content in fruit juices and wines is expressed as nitrogen total assimilable determined

by formol method using an acid-base titration.

The formol number (known also as formol index) is a parameter used for evaluation of the quality

of fruit juices or wines (eg: 150-200 mg/L of assimilable N is the minimum required to avoid any

problem of stuck fermentation due to lack of nitrogen). The concentration of alpha amino nitrogen

in grapes changes as a function of maturity and crop load. The concentration increases with fruit

maturation and decreases with crop load.

Because of the importance of N on fermentation and fermentation volatiles, it is desirable to

determine the N status before fermentation.

The employment of the acid-base titration for determining the total amino-acid concentration is

possible only after neutralization of the titratable acidity of the samples (wines or fruit juices) and

blockage of the amino groups by reaction with formol base reagent. To decrease the pretitration

duration, neutralization of the titrable acidity is performed using two titrants and the pre-titration

stops at 8.2 pH endpoint value. After the reaction with formol base reagent (with pH adjusted

between 8.1 and 8.2 pH), in order to ensure it stops at set point pH value, the titration is performed

using a low concentrated titrant.

The HI 84533 is a potentiometric titrator that use a pH electrode for endpoint. The volume of the

titrant dispensing, necessary to reach the endpoint, is used to calculate the formol number. The

result is expressed in: meq/100 mL, meq/L or mg/L nitrogen total assimilable.

By simply pressing the Start key in Titrator mode, the instrument will automatically titrate the

sample to the endpoint. The current pH and temperature are continuously displayed during titration

process. The result is immediately displayed in g/L, then the instrument is ready for another

titration by pressing the Restart key.

A dedicated HELP key aids in setup, calibration, status and troubleshooting.

Other features:

•pH meter / mV meter

•Stir speed control

•Graphic mode to display the titration data

•Data can be stored using the log feature and then exported to a USB stick or

transferred to a PC using the USB connection

•Log on demand for up to 400 samples (200 for mV/pH measurements; 200 for

titration results)

•GLP feature, to view calibration data for pH electrode and pump

SPECIFICATIONS

Titrator Range Low Range: meq/L 2.14 to 28.57 as N

meq% 0.21 to 2.85 as N

mg/L 30.0 to 400.0 as N

High Range: meq/L 21.7 to 71.4 as N

meq% 2.14 to 7.14 as N

mg/L 300 to 1000 as N

Resolution Low Range: 0.01 meq/L; 0.01 meq%; 0.1 mg/L

High Range: 0.1 meq/L; 0.01 meq%; 1 mg/L

Accuracy 3 % of reading or ± 0.1 mg/L @ 25 °C whichever is greater

Sample volume 10 mL (Low Range) / 5 mL (High Range)

Titration method Acid-base titration

Principle Endpoint titration: 8.20 pH

Pump 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 / 0.01 pH

pH Accuracy ± 0.01 pH

pH Calibration 1, 2 or 3 calibration points;

4 available buffers (4.01, 7.01, 8.20, 10.01)

Temperature Manual or automatic

Compensation

mV meter mV meter -2000.0 to 2000.0 mV

mV Resolution 0.1 mV

mV Accuracy ± 1.0 mV

Log data Up to 200 samples (pH or mV)

Temperature Range -20.0 to 120.0 °C (-4.0 to 248.0 °F)

Resolution 0.1 °C

Accuracy ±0.4 °C without probe error

Electrode HI 1131B

Temperature Probe HI 7662-T

Environment 0 to 50 °C (32 to 122 °F); max 95% RH non-condensing

Power supply 12 Vdc power adapter

Dimensions 235 x 200 x 150 mm (9.2 x 7.9 x 5.9”)

Weight 1.9 kg (67.0 oz.)

PRINCIPLE OF OPERATION

The amino-acidic nitrogen is determined by acidimetric titration after the blockage of the amino

groups using an excess of the formol (methanal) solution:

R – CH – COOH + CH2O R – CH – COO¯+ H3O+

Chemical method steps:

1. Sample (fruit juices or wines) total acidity neutralization, by titration against base strong

solution, at pH=8.2

2. Blockage of the amino-groups with formol solution (37%) adjusted to 8.2 pH.

3. Determination of the amino-acids content by second titration with base low concentration

solution until pH=8.2 (8.1-8.5).

Can see that the formol number titration is consecutive of the fruit juices and wine acidity titration.

A potentiometric acid-base titration employs a pH electrode to establish the endpoint of the titration.

The HI 84533 minititrator is designed to determine the formol number of the wines and fruit juices.

This instrument uses two titrant solutions in acidity neutralization steps (for shorting of the titration

time) and one low concentration titrant solution in the step of the formol number determination.

The pH of the formol reagent can be adjusted daily at 8.2 pH.

For precise results is important to know the sample volume and the titrant volume and concentration.

Preparation of the wine samples must follow the procedure (see section: Titration)

It is important to titrate the fresh samples of the fruit juices and wines. In order to increase the

precision of the measurement keep the fruit juices in caped vessels (avoid the prolonged air

exposure).

Formol number determination, as performed on the HI 84533 minititrator, utilizes a simple sample

preparation, a high quality dosing pump for titrant, potentiometric endpoint detector and instantaneaous

computations. To maintain the high precision of the titrator, a simple pump calibration procedure is

required. The pump calibration involves the analysis of a known volume of a known solution

(standard provided) and compensates for changes in pump dosing that may occur. This procedure

should be performed regularly.

N=CH2

reaction product with acidic

character (can be titrated with NaOH)

l l

NH2

REQUIRED REAGENTS

Code Description

HI 84533-50 Titrant for Low and High Range

HI 84533-55 Calibration Standard

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

FUNCTIONAL DESCRIPTION

OVERHEAD VIEW

1) Titrant bottle

2) Liquid Crystal Display (LCD)

3) Keypad

4) Electrode holder

5) Dispensing tube

ESC -used to leave the current screen and to return either to the previous screen or to the

main screen. In Setup, exits a parameter without changing the value.

/-used to modify the parameters’ values, to scroll the information displayed while

viewing a help screen or to move between the options from the instrument’s Setup

CAL -used to access the Electrode and Pump calibration options

HELP -used to access/exit the instrument’s contextual help

LOG -used to save the current mV/pH reading in pH meter mode and the titration result

MENU -used to enter Setup, Recall or GLP selection menu, while instrument is in pH or

Titration mode

STIR -used to start/stop the stirrer

Note: The stirrer starts automatically during pump calibration and titration, it cannot

be stopped by pressing STIR key.

GUIDE TO INDICATORS

During the instrument’s operation information is displayed on the LCD.

Displayed icons:

KEYPAD FUNCTION

1) Current time and instrument mode information (pH meter or Titrator)

2) pH electrode condition

3) Instrument status

4) Virtual option keys

Unstable reading.Stirrer on. Pump running.

Parameter can be modified.Stirrer is not working properly.

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.

Note:Once titrations have been completed, the dosing system should be cleaned with deionized

water using the prime feature.

TITRATOR STARTUP

This is a general outline of the steps required to perform a titration. The following topics are

expanded upon in each section that follows.

•Place the instrument on a flat table. Do not place the instrument in direct sun light.

•Connect the power adapter to the instrument.

•Turn the instrument ON using the power switch from the rear panel of the instrument.

•Set up the instrument. See the “Setup Menu” section for details.

•Connect the pH electrode to the instrument.

•Connect the temperature sensor to the instrument.

•Calibrate the pH electrode.

•Connect the tubes and the valve. See the “Dosing Pump Installation” section for the

procedure.

•Remove the titrant bottle cap and replace it with the bottle cap with tubes. Place the titrant

bottle in the appropriate place on the titrator top.

•Prime the syringe. To assure high accuracy, verify there are no air bubbles in the syringe or

tubing.

•Calibrate the pump.

•Prepare the sample.

Note:Different volumes of wine are required based on the concentration. See “Titration

Procedure” for details.

•Run a titration and log sample results.

5) Stirrer and reading status

6) Main reading information

7) pH temperature compensation mode (Manual or Automatic)

8) Temperature reading

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.

Concentration Unit

meq/L, meq% or mg/L.

Press the corresponding function key to change the

option.

Use Low measurement range for 30.0 - 400.0 mg/L.

Use High measurement range for 300 - 1000 mg/L.

To ensure a high accuracy, it is recommended to

recalibrate the pump after the valve, titrant or

electrode has been changed.

Use the ARROW keys to select the value.

Press Select to confirm or ESC to return to the setup

menu without saving the changes.

Calibration Timeout

Disabled or 1 to 7 days.

This option is used to set the number of days before

the pH calibration expired warning message is

displayed.

Press Modify to access the calibration timeout screen.

pH Resolution

0.1 or 0.01.

Press the displayed virtual option key to change the

option.

Range Setup

Table des matières

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