PAT940 Smart Titrator - GR Scientific · 2016-02-08 · 10.1 Performing a Single Determination----- 71 10.1.1 Performing a Run from Loading a ... 12.2.1 Titration Curves ... materials

PAT940 Smart Titrator

User Manual Edition 1.4 Oct 2015

Contents

Chapter 1 Introduction---------------------------------------------------------------------------------7

1.1 Instrument Description------------------------------------------------------------ 7 1.2 Instrument Connections---------------------------------------------------------- 8

Chapter 2 Safety Information------------------------------------------------------------------------ 9

2.1 General Safety Points-------------------------------------------------------------- 9 2.2 Electrical Safety---------------------------------------------------------------------- 9 2.3 Tubing and Connections----------------------------------------------------------- 9 2.4 Solvent and Chemical Safety----------------------------------------------------- 9

2.5 Recycling and Disposal------------------------------------------------------------- 9

Chapter 3 Instrument Overview--------------------------------------------------------------------- 10

3.1 System Schematic Overview------------------------------------------------- 10 3.2 Control POD®------------------------------------------------------------------- 11

3.2.1 Front of Control POD®-------------------------------------------- 11 3.2.2 Back of Control POD®--------------------------------------------- 11 3.3 Titrate POD®-------------------------------------------------------------------- 12 3.3.1 Front of Titrate POD®--------------------------------------------- 12 3.3.2 Back of Titrate POD®---------------------------------------------- 12 3.4 Dispense POD®----------------------------------------------------------------- 13 3.4.1 Front of Dispense POD®------------------------------------------ 13 3.4.2 Back of Dispense POD®------------------------------------------- 13

Chapter 4 Instrument Set Up------------------------------------------------------------------------- 14

4.1 Receiving PAT940------------------------------------------------------------------- 14 4.1.1 Packaging---------------------------------------------------------------- 14 4.1.2 Checks-------------------------------------------------------------------- 14 4.1.3 Location------------------------------------------------------------------ 14 4.2 Connecting the Power Supply---------------------------------------------------- 15 4.3 Connecting the Dispense POD®-------------------------------------------------- 16 4.3.1 Connecting a Primary Dispense POD®---------------------------- 16 4.3.2 Installation of Syringe------------------------------------------------- 17 4.3.3 Removal of Syringe---------------------------------------------------- 18 4.3.4 Connecting the Tubing------------------------------------------------ 18 4.4 Connecting the Titrate POD®----------------------------------------------------- 19 4.4.1 Connecting a Primary Titrate POD®------------------------------- 19 4.5 Connecting Electrodes and Temperature Probe----------------------------- 20 4.5.1 Connecting an Electrode--------------------------------------------- 20 4.5.2 Connecting an Additional Electrode------------------------------- 20 4.5.3 Connecting a Temperature Probe----------------------------------21

4.6 Connecting Additional Pods------------------------------------------------------ 22 4.6.1 Connecting an additional Titrate POD®-------------------------- 22 4.6.2 Connecting an additional Dispense POD®----------------------- 23 4.7 Connecting External Devices----------------------------------------------------- 24

4.6.1 Connecting a USB Device--------------------------------------------- 24

Chapter 5 Basics of Operation------------------------------------------------------------------------ 25

5.1 Switching ON and OFF------------------------------------------------------------ 25

5.1.1 Switching PODs ON ----------------------------------------------25 5.1.1 Switching PODs OFF ---------------------------------------------26 5.2 Capacitive Touch Screen---------------------------------------------------------- 26 5.3 Home Page Navigation------------------------------------------------------------ 27 5.4 Electrode Recognition------------------------------------------------------------- 27

Chapter 6 System Settings----------------------------------------------------------------------------- 28

6.1 Administrators---------------------------------------------------------------------- 28 6.2 Configuration------------------------------------------------------------------------ 29 6.3 Manage------------------------------------------------------------------------------- 30 6.3.1 Software Update------------------------------------------------------30 6.3.2 Screenshot--------------------------------------------------------------30 6.3.3 Sound-------------------------------------------------------------------- 30 6.4 Data Manage------------------------------------------------------------------------ 31 6.5 About---------------------------------------------------------------------------------- 32

Chapter 7 Manual Operations------------------------------------------------------------------------ 33

7.1 Titrate POD® Operations--------------------------------------------------------- 33 7.2 Dispense POD® Operations------------------------------------------------------ 34 7.2.1 Syringe Initialisation------------------------------------------------ 34 7.2.2 Syringe Flushing------------------------------------------------------ 36 7.2.3 Syringe Control------------------------------------------------------- 37 7.2.4 Dispense Control----------------------------------------------------- 38 7.2.5 Dosing Rate------------------------------------------------------------ 39 7.2.5.1 Continuous Dosing---------------------------------------39 7.3 Calibration--------------------------------------------------------------------------- 41

7.3.1 Calibration from Automatic Electrode Recognition--------- 41 7.3.2 Dual Electrode Calibration----------------------------------------- 42

7.3.3 Calibration Parameters--------------------------------------------- 43 7.3.4 Stirrer Settings-------------------------------------------------------- 44 7.3.5 Performing a Calibration------------------------------------------- 45 7.3.6 Calibration Report--------------------------------------------------- 46 7.3.7 Calibration History--------------------------------------------------- 48 7.4 mV/pH Measure------------------------------------------------------------------- 49

Chapter 8 Method Centre----------------------------------------------------------------------------- 50

8.1 The Main Screen------------------------------------------------------------------- 50 8.2 Loading a Method----------------------------------------------------------------- 52 8.2.1 Favourites-------------------------------------------------------------- 53 8.3 Creating a New Method---------------------------------------------------------- 54 8.4 Saving a Method------------------------------------------------------------------- 55 8.5 Editing a Method------------------------------------------------------------------- 55 8.5.1 Deleting a Method--------------------------------------------------- 56 8.6 Parameters-------------------------------------------------------------------------- 56

8.6.1 Method Information------------------------------------------------ 56 8.6.2 Pre-Dispense Criteria----------------------------------------------- 58

8.6.3 Stirrer Settings-------------------------------------------------------- 59 8.6.4 Titrant Addition------------------------------------------------------ 59 8.6.5 Rate Control----------------------------------------------------------- 60 8.6.6 Equivalence Point Evaluation------------------------------------- 62

8.6.7 Stop Criteria------------------------------------------------------------------------64

8.7 Calculations--------------------------------------------------------------------------- 65 8.7.1 Adding a New Formula--------------------------------------------- 65 8.7.2 Using the Formula Editor Keypad-------------------------------- 66 8.7.3 Variable Function---------------------------------------------------- 67

8.7.4 Saving a Formula----------------------------------------------------- 68

8.7.5 Deleting a Formula-------------------------------------------------- 68

Chapter 9 Titrants--------------------------------------------------------------------------------------- 69

9.1 Selecting a Titrant------------------------------------------------------------------- 69 9.2 Adding a New Titrant--------------------------------------------------------------- 69 9.3 Deleting a Titrant-------------------------------------------------------------------- 70

Chapter 10 Running a Method------------------------------------------------------------------------- 71

10.1 Performing a Single Determination------------------------------------------- 71 10.1.1 Performing a Run from Loading a Method------------------- 71 10.1.2 Performing a Run from Editing a Method-------------------- 71 10.1.3 Quick Start from Favourites------------------------------------- 72 10.2 Entering Sample Information--------------------------------------------------- 72 10.2.1 Running a Blank Determination-------------------------------- 73 10.3 Auto Prime-------------------------------------------------------------------------- 74 10.4 Cancelling a Determination----------------------------------------------------- 74 10.5 End of a Run------------------------------------------------------------------------ 74 10.6 Performing a Dual Determination--------------------------------------------- 76 10.6.1 Preparing Determination RUN 1-------------------------------- 76 10.6.2 Indicator icons during screen navigation in a single run-- 76 10.6.3 Preparing Determination RUN 2-------------------------------- 77 10.6.4 Indicator icons during screen navigation in a dual run---- 77

Chapter 11 Sample Running Screen----------------------------------------------------------------- 78

11.1 Live Display-------------------------------------------------------------------------- 78 11.1.1 Primary Curve------------------------------------------------------- 78 11.1.2 First Derivative------------------------------------------------------ 78 11.1.3 Second Derivative-------------------------------------------------- 79 11.1.4 Data Table------------------------------------------------------------ 79 11.2 Adjusting Stirrer-------------------------------------------------------------------- 79 11.3 Aborting a Run--------------------------------------------------------------------- 80 11.4 Screen Navigation During a Run----------------------------------------------- 80 11.5 Real Time Curve-------------------------------------------------------------------- 81

Chapter 12 Results Centre----------------------------------------------------------------------------- 82

12.1 Result List---------------------------------------------------------------------------- 82 12.2 Result Information---------------------------------------------------------------- 82 12.2.1 Titration Curves---------------------------------------------------- 85 12.2.2 Curve Functions---------------------------------------------------- 85 12.3 Filter---------------------------------------------------------------------------------- 86 12.4 Statistics----------------------------------------------------------------------------- 87 12.4.1 Selecting a Result-------------------------------------------------- 88 12.5 Recalculate------------------------------------------------------------------------- 90 12.6 Deleting Results-------------------------------------------------------------------- 91

Chapter 13 Technical Specifications----------------------------------------------------------------- 92

Chapter 14 Parts and Accessories-------------------------------------------------------------------- 93

14.1 Standalone System 1------------------------------------------------------------ 93 14.2 Standalone System 2------------------------------------------------------------ 94 14.3 Accessories and Spare Parts--------------------------------------------------- 95

Chapter 15 Conformity and Warranty-------------------------------------------------------------- 96

15.1 Declaration of Conformity------------------------------------------------------ 96 15.2 Quality Control-------------------------------------------------------------------- 96 15.3 Customer Support and Service------------------------------------------------ 96 15.4 Warranty--------------------------------------------------------------------------- 96 15.5 Warranty Exemptions----------------------------------------------------------- 96

Chapter 1 Introduction

1.1 Instrument Description

Standalone PAT940 titration system consists of three PODs; Control POD®, Titrate POD® and

Dispense POD® that can be fixed into an organised work tray or arranged by the user in their own

work area. The materials of each POD are manufactured from chemically resistant surface treated

materials including anodised aluminium side panels to repel aggressive solvents.

PAT940 is a modular titration system consisting of PODs for potentiometric titration. PAT940 is

designed for ease of use, increased sampling productivity and convenience through its capacitance

touch screen colour interface.

The following titration modes are available within PAT940:

(1) Dynamic Equivalence Point Titration

pH (potentiometric pH measurement)

mV (potentiometric voltage measurement)

(2) Incremental Equivalence Point Titration

pH (potentiometric pH measurement)

mV (potentiometric voltage measurement)

(3) pH Calibration

pH (automatic buffer recognition of pH electrodes)

1.2 Instrument Connections

Various ports are located on each POD, essential for instrument set-up. Below is a list of ports that

can be found on each POD.

(1) Power Supply Ports

The power supply ports are for connecting to a 24V mains power supply between the PODs,

using the supplied kycon to kycon cables.

(2) Dispense POD® Ports

These ports are for connecting up to 16 Dispense PODs®, in series, using 2-pin LEMO connectors.

(3) Titrate POD® Ports

These ports are for connecting up to two Titrate PODS®, in parallel, using 9-pin RS232 Cables.

(4) Balance Port

This port is for connecting a Balance using a 9-pin RS232 Cable.

(5) Electrode Ports

These ports are for connecting up to two electrodes, using 2-pin LEMO connectors.

(6) Temperature Probe Port

This port is for connecting a temperature probe, using a 2-pin LEMO connector.

(7) USB Ports

These are for connecting a USB flash drive or peripheral devices, up to two of these can be

connected at once, unless it is a serial device.

(8) Network Port

This is for connecting the instrument to a network. The instrument is not provided with a

network cable and will need to be sourced elsewhere.

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Chapter 2 Safety Information

2.1 General Safety Points

GR Scientific products are in conformity with the EU Directives 2004/108/EC and

2006/95/EC. This is based upon the compliance of the products with the

harmonised standards: BS EN 61000-6-1:2007; BS EN 61010-2-030:2010; and BS

EN 61326-1:2013.

GR Scientific products are manufactured in accordance to RoHS following the EU

Directive 2011/65/EU; it does not contain any of the restricted substances in

concentrations and applications banned by this directive.

2.2 Electrical Safety PAT940 complies with the international standard IEC 61010.

Only operate this instrument within the mains voltage supply that is specified on

the back of the Control POD®, an incorrect mains supply can damage the

instrument. Never open the housing of the instrument, only GR Scientific

personnel who are trained to service the instrument can open the housing.

There is risk of electrocution if live components are touched.

Always ensure the instrument is disconnected from the mains power supply

when connecting or disconnecting cables from the back of the PODs, as

electrostatic discharge can build up.

2.3 Tubing and Connections

Leaks in the tubing are a safety risk if left without attention. Ensure that all

tubing is screwed into the Dispense POD® tightly by hand, without excessive

force. Breaks in the tubing connections or on the tubing can lead to spillages;

check the connections regularly to avoid this.

2.4 Solvent and Chemical Safety

When using flammable or irritant solvents and chemicals, follow suitable safety

measures to protect yourself and others around. Always use the instrument in a

well ventilated area, clean up spilled fluids immediately, and keep flame

sources away from the work area. Always follow the safety instructions of the

chemical manufacturer and apply the correct countermeasures that are

required.

2.5 Recycling and Disposal

PAT940 is covered by the WEEE (Waste Electronic and Electrical Equipment)

Directive 2012/19/EU to prevent the negative and harmful effects on the

environment and public health. For more information on how to dispose of the

PAT940 safely, please contact your local authority, your local waste disposal

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8

9

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company or GR Scientific directly.

Chapter 3 Instrument Overview

3.1 System Schematic Overview

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3.2 Control POD®

3.2.1 Front of Control POD®

(1) Display

3.2.2 Back of Control POD®

(1) Titrate POD® 1 (9) Electrode 2 (combined pH/ref) (2) Titrate POD® 2 (10) Dispense POD® (RS485 BUS) (3) Balance (11) Temperature Probe (4) Auto POD (12) Power Output (24V DC 7A Max) (5) USB 1 (13) Power Input (6) USB 2 (14) Fuse 0.2A (7) Network (15) Mains Switch (8) Electrode 1 (combined pH/ref)

1

1 2 3 4

6 5 7

8

9

10

11

12

13

14

15

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3.3 Titrate POD®

3.3.1 Front of Titrate POD®

(1) Titration Vessel Holder (3) Magnetic Stirrer Mechanism

(2) Electrode Platform

3.3.2 Back of Titrate POD®

(1) Fuse (4) 24V DC Output

(2) I/O Switch (5) RS232 Serial Port

(3) 24v DC Input (6) RS485 Serial Bus Port

1

2

1

2

3

5 4

6

3

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3.4 Dispense POD®

3.4.1 Front of Dispense POD®

(1) Syringe Cylinder (4) Switching Valve

(2) Inlet Hole for Bottle to Syringe Tubing (5) Plunger

(3) Outlet Hole for dispensing tube and tip (6) Retaining Screw

3.4.2 Back of Dispense POD®

(1) Fuse 0.2A (5) RS485 Serial Bus Port

(2) I/O Switch (6) RS232 Serial Port

(3) Configuration Access Plate (7) 24V DC Input

(4) RS485 Serial Bus Port (8) 24V DC Output

1

1

2 3

2

3

4

5

6

4

5

6

8

7

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Chapter 4 Instrument Set Up

4.1 Receiving PAT940

4.1.1 Packaging

PAT940 is packaged in suitable protective packaging to ensure that no damage occurs during transit,

only this packaging is suitable for the safe transportation during transit. All PODs are boxed

individually within an overpack. Please keep this packaging as transit of the individual PODs may

need to occur in the future as well.

4.1.2 Checks

Once you have received the instrument, immediately check to make sure that there is no damage

and no parts are missing. A delivery note will be included within the overpack to use to compare

with the shipment.

Ensure that inside the shipment is a calibration certificate for each POD, if not please request from

the manufacturer.

4.1.3 Location

PAT940 has been developed for indoor use only. Locate the instrument within the work area where

it is free from:

vibrations

direct sunlight

contamination from chemicals

explosive environments

corrosive atmospheres

major temperature fluctuations

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4.2 Connecting the Power Supply

PAT940 is powered by an external mains source, with a power pack to ensure this connection is the

correct voltage of 24V DC for the instrument.

Damage may occur beyond repair and the user may be suspect to electric static shocks if the

incorrect power is supplied.

Note: Refer to Chapter 2 for more safety information.

(1) Connect the 24V 7A power adaptor from a mains power source to the power input port on

the back of the Control POD®.

(2) Attach one kycon to kycon cable from the power output port on the Control POD® to the

power input port on the Titrate POD®.

(3) Attach the other kycon to kycon cable from the power output port on the Titrate POD® to

the power input port on the Dispense POD®.

To avoid risk of electrocution, make

sure all I/O switches area set to OFF

before connecting the power supply

leads.

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4.3 Connecting the Dispense POD®

Ensure the Dispense POD® is sitting the correct way up before connecting any cables into the back of

the POD. See image below.

4.3.1 Connecting a Primary Dispense POD®

(1) Connect one end of the RS485 to RS485 2-pin 500 mm cable into the RS485 serial bus port

on the Control POD®.

(2) Connect the other end of the cable to one of the RS485 serial bus ports on the Dispense

POD®.

Note: Once connected, this will be automatically detected by the Control POD®. Dispense POD® 1 is

set to default and is ready to use within the software.

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4.3.2 Installation of Syringe

Installing a syringe to the Dispense POD® is necessary when first receiving PAT940. To install a

syringe, follow the procedure below:

(1) Remove the syringe from its packaging within the Dispense POD box.

(2) Pull the plunger down so that it sits halfway within the syringe cavity.

(3) Position the top of the syringe into the electrovalve and screw in firmly in an anticlockwise

direction.

(4) Loosen the retaining screw on the Dispense POD®.

(5) Pull the plunger down and seat into the syringe plunger holder

(6) Tighten the retaining screw.

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Note: Keep the syringe straight

and do NOT overtighten when

installing the syringe.

Secure the plunger in place using

the retaining screw.

4.3.3 Removal of Syringe

To remove the syringe from the Dispense POD® for replacement or cleaning, follow the procedure

below:

(1) Select [Manual Operation] and [Syringe]

(2) Empty the contents of the syringe by using the SYRINGE CONTROL icons; Empty to Vessel or

Return to Bottle.

(3) Remove the bottle tubing from the titrant bottle and press [FILL] icon to fully extend the

plunger.

(4) Loosen the retaining screw

(5) Push the plunger upwards slightly into the syringe cavity and unscrew the syringe from the

electrovalve in a clockwise direction.

4.3.4 Connecting the Tubing

(1) Attach the bottle to syringe tubing (700mm) into the inlet hole securely using the black

threaded screw fitting.

(2) Feed the other end of the tubing through the DIN45 Bottle Cap into the titrant bottle

securely using the black threaded screw fitting.

(3) Attach the tubing from syringe to dispensing Tip (600mm) to the outlet hole securely using

the black threaded screw fitting.

(4) Feed the dispensing tip into the electrode platform attached to the Titrate POD®.

Leaks in the tubing are a safety risk. Ensure that all tubing is screwed

into the Dispense POD® tightly by hand, without excessive force.

Breaks in the tubing or connections can lead to spillages. Check the

connections and tubing before using to avoid this.

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Note: Refer to Chapter 2.4

for solvent and chemical

safety information.

4.4 Connecting the Titrate POD®

Ensure the Titrate POD® is sitting the correct way up before connecting any cables into the back of

the POD. Do not rotate as this may cause unnecessary damage.

4.4.1 Connecting a Primary Titrate POD®

(1) Connect one end of the RS232 to RS232 Cable (9 pin d-sub) to Titrate POD® 1 serial port on

the Control POD®.

(2) Connect the other end of the RS232 Cable to the RS232 serial port on the Titrate POD®.

Note: Once connected, this will be automatically detected by the Control POD®.

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4.5 Connecting Electrodes and Temperature Probe

4.5.1 Connecting an Electrode

(1) Connect the electrode LEMO connector into Electrode 1 port on the Control POD®.

(2) The electrode rests in the electrode platform on the Titrate POD®.

4.5.2 Connecting an Additional Electrode

(1) Connect the electrode LEMO connector into Electrode 2 port on the Control POD®.

(2) The electrode rests in the electrode platform on the Titrate POD®.

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4.5.3 Connecting a Temperature Probe

(1) Connect the temperature sensor connector of the Pt100 type into the temperature probe port on the back of the Control POD® (2) The Pt100 rests in the electrode platform on the Titrate POD®.

(3) Once connected the temperature will be visible at the top of the screen during a run only. By

pressing the thermometer icon you can switch between Celsius and Fahrenheit. If the probe is

NOT connected then N.C will be present during a live run.

Temperature Probe connected – CELCIUS Temperature Probe connected - FARHENHEIT

Temperature Probe Not Connected

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4.6 Connecting Additional PODs®

4.6.1 Connecting an additional Titrate POD®

Place the Titrate POD® 2 next to Dispense POD® 1.

(1) Connect one end of the RS232 to RS232 Cable (9 pin d-sub) to Titrate POD® 2 serial port on the Control POD®. (2) Connect the other end of the RS232 Cable to the RS232 serial port on Titrate POD 2®

Note: refer to 7.1 Titrate POD® Operations for syringe activation.

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4.6.2 Connecting an additional Dispense POD®2

Place the Dispense POD® 2 next to Titrate POD® 2; refer to picture on page 23.

(1) Connect one end of the second RS485 to RS485 2-pin 500 mm cable into Dispense POD® 1 and

the other end into RS485 serial bus port on Dispense POD® 2. Note: the red dot marks the orientation of the pins when connecting to the ports.

(2) Attach one kycon to kycon cable into POWER OUT port of Titrate POD® 2 and connect the other end into the POWER IN port of Dispense POD® 2.

Note: refer to 7.2 Dispense POD® Operations for syringe initialisation.

Very important that Dispense POD® 2 is connected as the additional POD and not in Standalone 1

System set up.

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4.7 Connecting External Devices

4.7.1 Connecting a USB Device

A USB device is any peripheral device that will connect to the instrument using either of these ports;

USB1 or USB2.

Note: Both of these ports are USB/A type connections.

(1) Insert the USB Device into one of the USB Ports. The USB device is automatically recognised. A message will appear when navigating though System Settings; ‘USB Stick Inserted’.

Note: Refer to Chapter 6 System Settings for instructions on how to use the USB device.

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Chapter 5 Basics of Operation

This chapter describes the basic operation of PAT940 which includes:

- switching PODs ON

- switching PODs OFF

- using the capacitive touch screen

- homepage navigation

- electrode recognition system.

5.1 Powering up PAT940 PODS

5.1.1 Switching PODs ON

Each individual POD has its own I/O switch and is powered by a serial BUS supply system linking one

POD to the next.

Note: Refer to Chapter 4.2 for power supply connections.

Press the I/O switch on the Control POD to the ON position. You will hear a loud beep and the

screen will power up with the GR Scientific logo for 40 seconds, then the homepage will load.

Press the I/O switch on the Dispense POD to the ON position. You will hear a beep which indicates

that the Dispense POD is connected correctly and is ready for initialisation.

IMPORTANT: Leave the Titrate POD switched OFF until the Homepage has loaded.

Once the home page has loaded (refer to Chapter 5.3 on page 26) then press the I/O switch on the

Titrate POD to the ON position. You will hear a quiet beep and the Titrate POD will home itself.

Proceed to Chapter 7.2 Dispense POD Operations for syringe initialisation.

Note: The syringe must be initialised after powering up the PAT system before any other activity can

take place.

Prior to switching the PODs ON, ensure the I/O switches

are switched to OFF and then connect the power supply.

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5.1.2 Switching PODs OFF

Each POD must be turned OFF within the PAT system when powering down. This can be performed

in any order.

Simply press the I/O switch to the OFF position on each POD. When powering PAT system back up

follow Chapter

5.2 Capacitive Touch Screen

The capacitive touch screen is very sensitive, pressing too hard will damage

the instrument.

Use the touch screen with a fingertip, even while wearing gloves or if you

prefer you can use a stylus. Avoid using sharp objects on the screen such as a

ballpoint pen even though it is robust, the screen can still be damaged from

scratches.

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5.3 HOMEPAGE Navigation

The HOMEPAGE provides access to the main operations of the titration system.

- Method centre,

- System settings,

- Manual operations,

- Result,

- Real-time curve.

Favourite methods are displayed in a scroll down table for quick start access. [FLUSH] and [EMPTY]

functions for the Dispense POD® can be activated on the HOMEPAGE. Flushing cycle should

commence prior to any new titration.

Note: Refer to Chapter 7.2.1 for syringe flushing operation.

5.4 Electrode Recognition

When a coloured electrode is plugged in, an electrode shaped icon will appear in top the right corner

of the screen to identify which electrode type is connected. The same coloured application icon will

enlarge automatically. The methods saved within that coloured icon are now ready to be loaded. If

two electrodes are connected both associated coloured icons will enlarge. Therefore methods saved

within both of the activated coloured icons can also be loaded.

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Chapter 6 System Settings

This chapter describes various configurations and system settings:

- Administration - Display - Printer

- Configuration - Data Output - Device Manager

- Electrodes - Error - About

To access system settings, press [SYSTEM SETTINGS] from the Homepage.

6.1 Adminstrators

USER SETTINGS is the default page when entering SYSTEM SETTINGS.

Adding a User

To add a new user, press the NAME field and enter the user name using the automatic pop up

keypad. The number of characters in this field is unlimited.

Press ENTER [] to store the name.

Activating a User

To activate the user select [ON] from the drop down box. Press [ADD USER] to create the listing in

the table. A blue tick will appear in the state column which shows the user is active.

Deactivating a User

To deactivate a user select one from the table, change the state to OFF and press [SAVE USER]. The

blue tick will disappear and the user is therefore deactivated.

Editing a User

To edit a user select one from the table, amend the NAME as desired using the pop up keypad, press

ENTER [] and then press [SAVE USER].

Deleting a User

To delete a user, select a user from the table, press [DELETE USER] and the name will be removed

from the table.

Note: The number of users you can add is unlimited but only one user can be deleted at a time.

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6.2 Configuration

Follow the procedure below to set the date, time and local time.

Once you have amended the configuration settings press the [SAVE] button to save the changes and

the current time will then be displayed.

1) Date Format

Select the date format from the dropdown box, choose from:

DD/MM/YYYY (default setting)

MM/DD/YYYY

YYYY/MM/DD

2) Date Setting

Tap on the date setting box and enter the current date using the pop up calendar.

Use the arrow keys to navigate through each month.

Select the date by pressing a number. The date selected will appear at the bottom of the

calendar.

Press [OK] to confirm.

3) Time setting

Tap on the time setting field. The automatic keypad will appear. Use the blue cursor to move

between the characters. Press key to delete numbers if necessary. Press [ENTER] key,

to confirm.

4) Language

Press the language field to choose from English, Spanish, Russian or Chinese (simplified).

Note: Pressing [SAVE] will save ALL the settings within configuration settings. Make sure you have

the correct information in all fields before saving.

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6.3 Manage

Press [MANAGE] to perform software updates, activate the screenshot function and control sound.

6.3.1 Software Update

To install the latest software:

1) Upload file onto USB device and insert into USB1 on the back of the Control POD®

2) Wait a few seconds until you see a message update available. Install now

3) Press the Update icon

4) Press [OK] and [INSTALL] this may take a few minutes

5) Once complete press [OPEN] and PAT will reload to the homepage

6.3.2 Screenshot

The screenshot function allows you to save any screen of your choice to a USB device which can be

downloaded to a PC.

To activate press [OPEN SCREENSHOT] and a circular icon will appear at the top of the screen. To

deactivate the screenshot function, press [CLOSE SCREENSHOT].

6.3.3 Sound

To activate a beep at the start and end of a run determination press the START RUN icon to ON and

press the END RUN icon to ON.

To switch the sound to OFF, press the ON icon again.

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6.4 Data Manage

This function allows you to manage results, methods, favourites, calibration data and calculations

within the software. Press a box to activate a file. Choose from importing, exporting or deleting the

files.

1) Export Files

Choose one or more files from file selection and press [EXPORT] to send to a USB device.

All of the following files will be exported when ALL is activated and [Export] is pressed:

- Settings - Calibration

- Result - Crash

- PAT_PDF’s - Favourite methods

- Methods - Formula

Note: Files can only be exported to via a USB device which must be inserted in either USB1 or

USB2.

2) Import File

Choose one or more files from file selection and press [Import File]. Once successfully

imported, a message will appear: File Imported successfully.

3) Export Log

This is for manufacturer access only.

4) Delete all files

Choose one or more files from file selection and press [DELETE] To clear the Control POD®

memory of all files listed in export file, activate the box ALL and press [Delete all files]

All system settings will return to default.

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6.5 About

This section contains contact information about GR Scientific, software version, serial number of the

instrument and a QR code which can be scanned via your android/iOS phone that links to the GR

Scientific website.

When a software update is performed through System Settings the latest version will appear in

[System Settings] [About].

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Chapter 7 Manual Operations

7.1 Titrate POD® Operations

The electrode platform can be activated manually along with stirrer speed adjustment through the

Control POD®.

Initialise the Titrate POD®(s) that are connected by pressing the [INITIALISE TitratePOD] button.

Activate by pressing the box, a tick will then appear. The electrode platform will home itself at the

top of the Titrate POD® tower.

ELEVATION: Select vessel size by pressing the vessel button choosing either 170ml (standard with all

standalone PAT units) or 210ml. Press [ZERO] once and the electrode platform will automatically rise

to the home position. Press [DOWN] and the electrode platform will automatically lower to the size

of the vessel selected.

The position of the electrode platform is indicated in steps in STIRRER CURRENT INFO.

STIRRER SPEED: Increase the speed of the stirrer bar clockwise by pressing [>]. Decrease the speed

by pressing [<]. Each time the arrow keys are pressed the stirring rate is increased or reduced by one

level.

The stirrer will automatically start when the stirrer speed is activated by pressing the arrow buttons

and the rate is set in steps of -10 to +10.

+ Clockwise Rotation

Anti-Clockwise Rotation

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7.2 Dispense POD® Operations

7.2.1 Syringe Initialisation

Before the syringes are operational, they must be initialised.

(1) Switch each POD, ON, refer to Chapter 5.1 for Switching ON procedure.

(2) A message will appear once the homepage has loaded, see below:

Note: Dispense POD 1 is activated as default for PAT Standalone System 1.

(3) If a dual PAT system is set up simply select Dispense POD 2 to activate both syringes.

(4) Press [OK] and the message below will appear. If [CANCEL] is pressed the Control POD

recognises if the syringe has been initialised and will prompt you to do so.

34

(5) Insert the platform hole plugs (Part no: 594061) supplied with each PAT system, into the

electrode platform.

(6) Insert the dispensing tip into the electrode platform, see image below:

(7) Insert the vessel into the Titrate POD

(8) Select the correct vessel size.

(9) Press [INITIALISE].

The Titrate POD will lower to the vessel and the syringe will empty to vessel and refill for one cycle.

The electrode platform will automatically home once the initialisation cycle is over.

In a dual PAT System if both Dispense PODs are selected then both syringes will empty to vessel

and refill for one cycle. Both electrode platforms will automatically home once the initialisation cycle

is over.

Note: It is very important to have the plugs fitted into the electrode platform to avoid splashback of

any titrant during the initialisation procedure.

35

7.2.2 Syringe Flushing

The flushing function is used to rinse and fill the syringe and tubings attached to the syringe

assembly to remove any air bubbles within the system.

There are two areas where Flushing can be performed. From the HOMEPAGE or within [MANUAL

OPERATION] – [SYRINGE]

(1) Press [FLUSH]

(2) Insert the platform hole plugs (Part no: 594061) supplied with each PAT system, into the

electrode platform.

(6) Insert the dispensing tip into the electrode platform, see image below:

(7) Insert the vessel into the Titrate POD

(8) Select the correct vessel size.

(9) Press [FLUSH].

36

Pressing [CANCEL] will return to homepage.

Note: It is recommended that you should FLUSH before the first determination, if necessary more

than once.

The Titrate POD will lower to the vessel and the syringe will empty to vessel and refill for three

cycles. The electrode platform will automatically home once the initialisation cycle is over.

In a dual PAT System if both Dispense PODs are selected then both syringes will empty to vessel

and refill for three cycles. Both electrode platforms will automatically home once the initialisation

cycle is over.

7.2.3 Syringe Control

Activate the syringe or multiple syringes by pressing the number correlating to the number of

Dispense POD®(s) connected in SYRINGES SELECTION. For PAT940 Standalone System 1, [1] will

already be activated as this is a default setting. To empty the syringe press [] Empty to Vessel,

making sure the dispensing tip is located in a vessel. The Dispense POD® will empty the contents of

the syringe at maximum rate.

Press [>] RETURN TO BOTTLE, the syringe will empty completely back into the titrant bottle.

Note: Check the tubing lines have been primed and there is no suspected contamination before

returning to bottle.

37

Press [] FILL to lower the syringe and fill to maximum capacity with titrant.

For multiple Dispense PODs connected, select the desired quantity you wish to manually operate by

pressing the numbers in [SYRINGES SELECTION].

7.2.4 Dispense Control

Syringe Volume:

To manually dispense titrant select the syringe volume which matches the size of the syringe

installed. Use the drop down box to select either 5ml or 12.5ml.

Note: Ensure the correct number of syringes has been selected in syringes selection.

Dispensed Volume (µl):

Press this field to enter the desired volume. Use the automatic keypad to enter the volume and

press [DISPENSE] to enter.

Range: 0-12500 µl

Note: Volume limit is maximum syringe volume, 12.5ml. If the next volume to be dispensed is more

than the spare volume remaining, then the syringe will not function. The FILL icon must be pressed

and then the next volume can be dispensed.

Press [DISPENSE] to activate. Spare volume is automatically calculated during dispensation and is

displayed in (µl).

Note: For installation and removal of the syringe refer to Chapters 4.3.2 and 4.3.3

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7.2.5 Dosing Rate

This function describes the rate at which the syringe doses and fills.

Press [DOSING RATE] and the screen shown below will appear:

The syringe volume, set in dispense control, dictates the dosing range available.

Input Range

5ml syringe 0.01 – 75ml/min

12.5ml syringe 0.01 – 187.5ml/min

Enter a value using the automatic pop up keypad within the specified syringe range.

Press [OK] to accept or [CANCEL] to return to SYRINGE screen.

Once the rate has been set, enter in the desired volume to be dispensed within DISPENSE CONTROL

and press [DISPENSE].

Note: the syringe will refill at the same speed as the dosing rate.

7.2.5.1 Continuous dosing

Press the Continuous dosing box, a blue tick will appear indicating it has been activated. Press again

to deactivate.

Enter in a maximum dosing volume within the range specified using the automatic pop up keypad.

Input Range 0 - 9999.99 (ml)

Press [OK] or [CANCEL] to return to SYRINGE screen.

Enter desired dispensed volume in (µl) within DISPENSE CONTROL if the value has not been entered

already.

Press [DISPENSE] to perform continuous dosing.

Spare volume is automatically calculated during dispensation and is displayed in (µl).

39

Note: when the volume of one syringe has been dosed, the dosing cylinder will refill automatically.

40

7.3 Calibration

7.3.1 Calibration from Automatic Electrode Recognition

A calibration is required to match the instrument being used to the current characteristics of the

used pH sensor. In practice, the response of a real pH sensor does not exactly follow the Nernst

Equation. This difference between the theoretical and actual behaviour of a pH electrode must be

therefore compensated for.

The Control POD® will automatically recognise if there is an electrode connected. When the Control

POD® is switched ON, if an electrode is connected in port 1, the screen shown below will appear.

If an electrode is connected in port 2, the screen shown below will appear:

Press [YES] and the calibration screen will load. Press [NO] to return to the homepage.

When an electrode is disconnected from either port 1 or port 2 the electrode icon(s) will disappear.

41

7.3.2 Dual Electrode Calibration

If two electrodes are connected and then the Control POD® is powered up, a dual electrode message

will appear for calibration of both electrodes. Press [YES] to go to calibration screen or [NO] to

return to homepage.

In the case of a dual electrode calibration, the calibration of electrode 1 will commence first, a

prompt will then appear:

INSERT ELECTRODE 1 INTO pH BUFFER and follow calibration procedure as described in 7.3.5

Performing a Calibration

Once the calibration report is generated and [SAVE] is pressed for Electrode 1, a message will appear

to calibrate electrode 2.

Press [YES] to proceed with the calibration of electrode 2 and follow procedure as described in 7.3.5

Performing a Calibration. The electrode no will automatically change to 2 and INSERT ELECTRODE 2

INTO pH BUFFER will appear on the Calibration screen.

Press [NO] to return to calibration screen.

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7.3.3 Calibration Parameters

These are the parameters that the user can define which influence the sequence of steps during the

calibration.

Electrode No:

Use the drop down box to select numbers 1 or 2 which is an indication of how many electrodes are

required to be calibrated. This number is purely for reporting purposes and does not define which

electrode is being calibrated.

Note: The number of electrode icons in the top right hand corner of the screen is an indication of how

many electrodes are connected. The electrode number will only change automatically during a dual

electrode calibration.

Glassware Type:

Select Vessel size from the dropdown box: 170 or 210ml.

Buffers No:

Choose up to 5 buffers from the dropdown box that can be used for calibration. If more than two

buffers are used for a calibration then they can be used repeatedly. The first two buffers must

however always be different from one another.

Buffers are automatically detected.

mV Range: -29 to +29

Min time (s):

The measured value will not be accepted until the minimum waiting time has elapsed. Press this

field to enter in a new value using the keypad which automatically pops up.

Input Range: 0 - 99999s

Default Value: 30s

Max time (s):

The measured value will not be accepted until the maximum waiting time has elapsed. Press this

field to enter in a new value using the keypad which automatically pops up.

Input Range: 0 - 99999s

Default Value: 60s

Temperature:

43

The temperature is being continuously measured when a temperature sensor is connected.

Input Range: –20.0 - 150.0 °C

Default Value: 25.0 °C

Drift:

Drift is the gradual change in electrode response over a period of time. It is described as the

maximum change in mV per minute. This value is automatically calculated after the maximum

waiting time has elapsed.

The rate and extent of drift can vary depending on which particular electrodes are being used and

the age and degree of contamination of the electrodes. Once the extent of drift is known then it

should be possible to find the optimum time of use or number of samples analysed before a

calibration is necessary.

Time (s):

This is the min and max waiting times that have already been set and appear once the times have

elapsed. A timer also appears once the start button is pressed.

Signal (mV):

The measured potential value in mV will appear after the min and max waiting times have elapsed.

7.3.4 Stirrer Settings

Refer to Chapter 11.2 Adjust Stirrer for stirrer setting details

7.3.5 Performing a Calibration

44

To perform a calibration, insert the electrode into an electrode port and follow the procedure below:

(1) Set parameters.

(2) Rinse electrode with selected buffer and place in electrode platform.

(3) Press [START].

(4) A reading will appear in signal row after min time has elapsed.

(5) A second reading will appear after max time has elapsed and a drift reading.

(6) Repeat the procedure above for the next buffer.

(7) Once the calibration is finished a message CALIBRATION OVER will appear.

Note: Each time a new electrode is inserted the calibration message will appear on screen as a

prompt for you to decide if calibration is necessary.

(8) Press [CAL REPORT] to accept and view the results or [CANCEL] to begin the calibration

procedure again.

7.3.6 Calibration Report

Detailed information concerning the results from the last calibration performed will appear:

45

The Slope of the Graph:

Once zero point offset has been determined, the second and further buffer solutions are used to

determine the slope of the pH electrode. This slope is expressed as a percentage of the theoretical

value (100% = 0.059V per ΔpH = 1 at 25°C).

Offset: pH at 0mV

This parameter is only visible with pH electrodes. The pH 7 or zero point offset of an electrode is the

pH value at which the total output electrode voltage is equal to 0. The zero point of a pH electrode

happens at the pH value of 7.00 theoretically. However, in practice, there is almost always a zero

point offset.

It is very important to run a pH 7 buffer prior to starting a pH measurement to find out the zero

point offset.

A large zero point offset will introduce a large error in your pH measurement, if you calibrate and

measure at different temperatures.

Serial Number Entry:

Enter the serial number of the electrode in the highlighted fields using the pop up keypad. The serial

number is located on the electrode lead. Both fields must be completed otherwise the calibration

cannot be saved.

Slope Limits:

You can define your own limit values based on electrode type.

Enter the lower limit by using the pop up keypad and follow the same process for the upper limit.

Input Range Lower and Upper Limit: -999.9 to 999.9%

Press [SAVE] to store.

46

The default limits set below are based on a non-aqueous electrode type:

Default Lower Limit: 88% Upper limit: 120% These values are monitored during the calibration. If these limits are out of range Calibration Fail

will appear on the screen.

Press the [BACK] button to return to the calibration screen.

Saving a Calibration Report:

Press [SAVE] once the serial number has been entered. The results are then stored in Calibration

History. If you try to exit the screen without pressing the [SAVE] button a message will appear

prompting you to either save or discard the result.

View mV/pH:

Press [mV/pH] button to check the electrode response.

7.3.7 Calibration History

The electrode serial number and colour are listed in order of the most recent one last used, depicted

in number order, [ 1 ] being the most recent.

Up to 1000 electrodes can be stored in the electrode serial number list, simply scroll up and down to

view or select an electrode.

Calibration Information:

To view the calibration data select an electrode from the list. The slope limits for that calibration are

visible.

47

The slope curve shows the plot of the date of calibration against the % slope. Therefore the history

of the slope for that particular electrode can be monitored over time.

Data Table:

This table documents the No. of calibrations performed, the date, the slope %, and the OFFSET in

mV.

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7.4 mV/pH Measure

To perform manual measurements follow the procedure below:

(1) Insert solution to be measured in the Titrate POD®.

(2) If using ELECTRODE 1 make sure the blue tick is visible to activate the Titrate POD® and deselect ELECTRODE 2 by pressing the blue tick box.

(3) SET ELEVATION of the electrode platform by pressing [LOWER].

(4) Select the vessel size from the dropdown box.

(5) Press [DOWN] to lower the electrode platform.

(6) Press the [] button if necessary to raise the platform in small increments.

(7) Press the [] button if necessary to lower the platform in small increments.

(8) Press [CANCEL] to return to previous screen.

The measuring modes displayed show:

- pH: potentiometric pH measurement

- mV: potentiometric voltage measurement

Press [STIRRER ON] to begin stirring. Press [STIRRER OFF] to cease stirring.

Note: Stirrer speed cannot be adjusted in VIEW mV/pH mode, a default speed of 3 is pre-set.

49

Chapter 8 Method Centre

8.1 The Main Screen

The method centre contains 5 coloured icons each with their own application titration type.

Red Icon – Non-Aqueous Titrations

Blue Icon – Aqueous Titrations

Green Icon – Redox Titrations

Yellow Icon – Precipitation Titrations

White Icon – Chloride Content

Each electrode within the GR Scientific range is also colour coded to match the application area of

each method.

Method Activation:

If you enter the method centre and no electrode is connected then access is denied to operate the

main method functions.

When an electrode is connected, depending on the coloured cap of that electrode, that matching

icon will enlarge and activate

Example: A red electrode is connected, the red icon is activated; message below appears:

[Press RED icon to LOAD or create a NEW method]

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When two electrodes of different colour are connected both icons will enlarge and become

activated:

Example: Red and blue electrodes are connected, the red and blue icons are activated, message

appears:

[Press RED or BLUE icon to LOAD or create a NEW method]

Note: Only one icon can be selected at a time to load or create a new method.

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8.2 Loading a Method

To load a method, proceed as follows:

(1) Press the activated icon you wish to load the method from, the icon will reduce in size, then press [LOAD METHOD] button. The method table with the stored methods will load:

(2) Select the desired method.

(3) Press [LOAD]. The method is now loaded and the parameters can be viewed once more as a check prior to running.

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8.2.1 Favourites

This section describes how you can update a method as a favourite on your homepage to enable

quick start function and also edit a favourite.

(1) In METHOD CENTRE press [LOAD] and tick the boxes associated with the methods you wish to save to HOMEPAGE. Up to 50 methods can be saved as favourites.

(2) Press [Update Favourite] and the methods selected will appear in a scroll down list on the HOMEPAGE.

(3) To remove a favourite from the HOMEPAGE untick the box in the methods list in LOAD METHOD.

Editing a Favourite:

Select [METHOD CENTRE] then [EDIT METHOD] and press the [EDIT FAVOURITE] button.

The table shown above lists all of the methods saved as favourites which appear on your homepage.

(1) Press the Blue tick box once to deactivate.

(2) Press [UPDATE FAVOURITE].

The method will be removed from your favourites list.

Press [BACK] button to return to EDIT METHOD screen.

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8.3 Creating a New Method

(1) In METHOD CENTRE press the enlarged application icon you wish to create the method in.

(2) Press [NEW METHOD].

(3) The method parameters can now be edited individually by pressing each field to activate the pop up keypad or dropdown box.

Refer to Chapter 8.6 Parameters

(4) In the field ELECTRODE the drop down box only lists the colours based on which electrode is connected. This can be identified by the electrode icons in the top corner of the screen.

Note: Only values within the ranges set in white font can be entered. Any values outside that range

will automatically revert to the maximum value of that specified range.

Adding a Formula:

To add a formula, scroll down to the bottom of the parameters list and press [ADD].

A table containing a list of calculations will appear, select one and press [YES] to add. Press [NO] to

go back to formula list.

54

8.4 Saving a Method

To save a method, follow the procedures below:

Note: When the [NEW METHOD] button is pressed the next sequential number available is

automatically created in method no. field.

(1) Press [NEW METHOD] or [EDIT METHOD] depending on whether you are creating or editing

a method.

(2) Press [SAVE METHOD]; view the parameters as a check.

(3) Press [SAVE] to store or press [CANCEL] to return to method parameters.

(4) Press [BACK] to return to method centre.

In [EDIT METHOD], there is an option to run the method after saving. Press the blue box to activate

then press [SAVE] to start the running process.

8.5 Editing a Method

(1) In METHOD CENTRE press the enlarged application icon you wish to create the method in.

(2) Press [EDIT METHOD]

The screen is split up into 3 sections:

- Electrodes List Shows the electrode application icons associated with the colour coded electrodes.

- Methods List Shows all the methods that have been created within each electrode type, with the most

recently created method at the top of the list.

- Parameters List Once a method from the methods list has been activated the parameters saved in the

method are available to edit.

Note: You can edit any method regardless of which coloured electrode is connected.

To edit a method follow the procedure below:

(1) Press the chosen coloured icon from the electrodes list.

(2) Press the method you wish to edit from the methods list.

(3) Edit the fields required within the parameters list.

55

8.5.1 Deleting a method

Deleting a single method:

(1) Select a method from the methods list and press [DELETE METHOD].

(2) Press [YES] to delete method and the method will be removed from the list.

(3) Press [NO] to return to EDIT METHOD screen.

Deleting all methods:

(1) Press [DELETE ALL] in EDIT METHOD screen

(2) Press [YES] and all methods will be deleted from each coloured icon in the electrodes list.

(3) Press [NO] to return to EDIT METHOD screen.

8.6 Parameters

The parameters within the instrument give instructions as to how the titrant should be added.

Depending on the type of sample and chemical reaction that occurs and the type of electrode used

for indication, dynamic or incremental titration are selectable modes.

8.6.1 Method Information

The parameters defined under method information are defined in the following order:

Method No:

This is an automatically generated number when a new method is created and then populated

sequentially. This number cannot be changed.

Method Name:

Enter up to 42 characters to define your method name using the automatic pop up keypad.

Titration Type:

Choose one of the following from the drop down box:

(1) Non-aqueous associated with the RED icon;

Non- aqueous titrations are the titrations in which weakly acidic or basic substances are carried

out using non–aqueous solvents to achieve a sharp inflection point.

(2) Aqueous associated with the BLUE icon;

Aqueous titrations are an acid-base neutralization reaction in an aqueous solution to determine

the concentration of the acid or base, one of which has a known concentration.

(3) Redox associated with the GREEN icon;

Redox titrations are based on a reaction between the analyte and titrant. A common example of

a redox titration is treating a solution of iodine with a reducing agent and using starch as an

indicator.

(4) Precipitation associated with the YELLOW icon;

Precipitation titrations involve the titrant and analyte reacting to form an insoluble salt.

56

(5) Chloride content associated with the WHITE icon;

Precipitation titration for determination of Chloride in Crude Oil.

Titrant Name:

Choose one of the pre-programmed titrants from the drop down box or add a titrant to the list.

Note: Refer to Chapter 9 for details on adding a new titrant.

Titrant Conc.:

Enter the titrant concentration using the numbered automatic pop up keypad. Units are in mol/L.

Titer:

Enter the titer value manually; up to 13 characters can be entered using the pop up numbered

keypad. This value will automatically be used in any calculations involving the titer value.

Electrode:

Select the electrode colour from the drop down box which only lists the colours based on the type of

electrode is connected. This can be identified by the electrode icons in the top corner of the screen.

57

Titration Mode:

Choose either incremental or dynamic from the drop down box.

Syringe Selection:

Choose either 5 or 12.5ml from the drop down box, checking which size is installed on the Dispense

POD® beforehand.

8.6.2 Pre-Dispense Criteria

The parameters below are performed before the start of the titration.

Pre-Dispense Criteria:

Before starting the titration, titrant addition will occur at maximum rate unless specified until the

measured value set in the criteria has been reached.

If a volume has been set in pre-dispense volume (µl) and the measured value is reached within this

pre-dispense volume, then the titration will automatically begin.

Default: OFF

Measuring Mode pH:

Enter a value using the pop up numbered keypad.

Input Range: 0 – 14

Measuring Mode Potentiometric Voltage, mV:

Input Range: -2000.0 to +2000.0

Pre-Dispense Rate:

This is the rate at which dosing of the titrant occurs until the pre-dispense criteria is reached.

Input Range

5ml syringe: 0.01 – 75ml/min

12.5ml syringe: 0.01 – 187.5ml/min

Default: Maximum

Maximum dose rate depends on syringe volume: 12.5ml syringe 187.5 ml/min 5ml syringe 75 ml/min

58

8.6.3 Stirrer Settings

Set the stirrer parameters for titration as follows:

Stirrer Speed:

The stirring rate can be set in steps of –10 to +10.

+ Clockwise Rotation

- Anti-Clockwise Rotation

Initial Stir Time:

This is the wait time set, in seconds, before the start of the titration to give the electrode time to

settle down. The initial stir time will only begin after the pre-dispensing criteria has been met.

Press the blank field using the pop up numbered keypad to enter the desired value.

Input Range: 0-999 (s)

Glassware Type:

Choose your vessel size either 170ml or 210ml from the drop down box.

Note: 170ml is the standard vessel size.

8.6.4 Titrant Addition

The addition of a titrant to a sample solution can be added in two ways. One way is the volume of

titrant dispensed is determined by an algorithm built in within the titrator which is free to determine

(within certain limits) how much to add – dynamic addition. The other way is where fixed volumes

of titrant are added for every new measuring point – incremental addition.

Incremental Equivalence Point Titrations

Increment Volume:

The titrant is dispensed at fixed volume (ml) increments for each new measuring point.

Default: OFF

Remove the default by pressing the blue tick box. Press the blank field to enter in a value using the

pop up keypad.

Input Range: 0.00001 – 20,000ml

59

Wait Between Doses:

This is the delay time between doses, in seconds (s) before the next measured value is accepted.

Press the blank field to enter a value using the pop up keypad.

Input Range: 1 – 999 (s)

Default: NONE

Dose Rate:

This is the rate at which the volume increments are dispensed. Enter in a value in ml/min using the

pop up numbered keypad once the tick box maximum has been deactivated.

Input Range

5ml syringe: 0.01 – 75ml/min

12.5ml syringe: 0.01 – 187.5ml/min

Default: Maximum

Maximum dose rate depends on syringe volume: 12.5ml syringe 187.5 ml/min 5ml syringe 75 ml/min

8.6.5 Rate Control

Dynamic Equivalence Point Titrations

Signal Drift (∆E):

This is a measure of how stable the signal is and the potential difference that should be reached with

each increment. The instrument looks for the maximum change of the measured value per minute.

A constant measured value can only be reached after a certain amount of time has elapsed.

In case the titration does not reach equilibrium, a maximum waiting time is defined by t (max) and in

order to avoid too quick addition a minimum waiting time is defined as t (min).

Enter a drift value by deactivating the blue tick box and using the pop numbered keypad.

Input Range: 0.1 – 999.0 mV/min

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Drift OFF:

Turn the drift function OFF by pressing in the box - OFF, a blue tick will appear in the field.

A measured value will only be recorded when the maximum waiting time has elapsed. This is

relevant for very slow reacting titrations or less responsive electrodes.

Note: A consistent and constant measured value is often only reached after the increment of titrant

dispensed has reacted with the sample solution. The electrode may also take time to reach a good

response which means reaching an accepted measured value can take longer. It is recommended

that the drift function is set in this case.

Fixed Time Interval (∆t):

A fixed time interval tells the titrator at which point the measured value needs to be recorded and

the next increment to be dispensed in seconds (s).

When a fixed time interval is set, the titrator will wait a set time interval before adding the next

increment. This parameter is very common for unstable titrations such as non-aqueous.

Enter a fixed time interval by pressing the blank field and entering a number using the numbered

keypad.

Input Range: 1-60 (s)

Default: NONE

t (min):

An accepted measured value will not be recorded until the minimum waiting time has elapsed

regardless if the signal is stable and drift has been reached.

The minimum waiting time is important for drift controlled measurements to avoid fluctuations in

signal changes when an increment is dispensed.

Press the blank field using the pop up numbered keypad to enter the desired value.

Input Range: 0-99,999 (s)

t (max):

An accepted measured value will not be recorded until the maximum waiting time has elapsed. This

depends on two factors only:

(1) If a stable drift reading has NOT been reached (2) If the signal drift has been set to OFF.


61

∆ V (min):

This is the smallest volume in (µl) that is dispensed at the beginning of the titration and again at the

steepest parts of the titration curve in order to accurately evaluate the exact position of the

inflection point. This avoids long titration times but bear in mind the accuracy of the evaluation

might not necessarily be increased by using smaller increments. Very small increments can give a

measured value in the same region as signal noise.

Press the blank field using the pop up keypad to enter the desired value.

Input Range: 0.1 – 12,500 (µl)

∆ V (max):

This is the largest volume of titrant in (µl) that is dispensed to prevent the titrator from adding too

large increments which could cause the end point to be overshot.

Larger increments are dispensed in the flatter parts of the titration curve so fewer measured data

points are recorded.

A maximum volume should be set if there is an excessive jump in signal or its very abrupt otherwise

a large volume will be dispensed in the region of the inflection point.

Press the blank field using the pop up numbered keypad to enter the desired value after deactivating

blue tick box.

Input Range: 0.1 – 12,500 (µl)

8.6.6 Equivalence Point Evaluation

The parameters for identification of the curve are shown below:

EQP Selection:

This function allows you to filter out which equivalence point you are looking for:

1st - The first defined equivalence point will be identified

Last - The last defined equivalence point will be identified

Largest - The equivalence point with the greatest Equivalence Point Recognition

criteria and the steepest region of the curve will be identified

All - All equivalence points will be identified

Press the drop down box to select 1st, last, largest or all from the list.

62

Threshold Value:

The threshold value is a minimum number that is set in order to recognise any peak in the 1st

derivative.

To set the threshold press the blank field and enter a value using the pop up numbered keypad

Input Range: 0-32,000

Note: In order for any peak to be recognised, the threshold set is the minimum size that any peak in

the 1st derivative should be.

A good check is to look at the 1st derivative column in the data table of measured values, then the

actual size of the peak can be determined and a suitable threshold can be applied. Bear in mind that

the purpose of the threshold is to prevent identification of minor peaks, therefore the level set need

only be bigger than the next largest peak.

Slope Tendency:

This identifies the trend of the curve. If the mV signal rises with every increment dispensed the trend

is positive. If the mV signal drops with every increment dispensed ie more negative with dosing or

positive to negative, then the trend is negative.

Press the drop down box to choose from positive or negative to identify the slope tendency.

Set Window:

Setting a window allows recognition of the correct equivalence point within a correct range on the

curve. This range is given in the unit of measure of the electrode used for the titration. If the

equivalence points fall outside of these windows then they will not be identified.

Multiple inflection points can be identified within a window.

Select the measuring mode in Window 1 Start, press either, mV, pH or OFF.

Default: OFF

When using set windows the START 1 Value must be less than the END 1 Value this applies to both

mV and pH.

For example SET pH:

Input Range: -20 to +20

START 1 Value: pH 12 END 1 Value: pH 10 For example SET mV:

Input Range: -3200 to +3200

START 1 Value: +600 END 1 Value: +800

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8.6.7 Stop Criteria

Method Centre – New Method / Method Parameters

Method Centre – Edit Method / Parameters List

The conditions defined in this chapter are for ending the titration.

Stop V (ml):

The titration will end when the STOP volume (ml) specified has been dispensed since the start of the

titration.

Note: In order to prevent the contents in the vessel from overflowing, the STOP V should be adjusted.

Input Range: 0.000-9,999.99 ml

STOP V will not be activated unless a value is entered.

Stop E (mV):

The titration will end when the specified measured value has been reached since the beginning of

the titration.

Input Range: -3200 – 3200 mV

Default: OFF

To enter a value deactivate the blue tick box and enter a value using the automatic keypad.

Stop pH:

The titration will end when the specified measured value has been reached since the beginning of

the titration.

Input Range: 0-14

Default: OFF

To enter a value deactivate the blue tick box and enter a value using the automatic numbered

keypad.

Stop Time:

The titration will end when the time specified in seconds (s) has been reached since the beginning of

the titration.


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To enter a value deactivate the blue tick box and enter a value using the automatic numbered

keypad.

Stop EQP:

The titration will end when the specified number of equivalence points has been identified.

Input Range: 1-9

Default: 1

Select a number between the ranges from the drop down box.

Volume after End Point:

This is a volume that is dispensed when the number of equivalence points defined under Stop EQP

has been found. The shape of the curve after the EQP is also much more visible if this parameter is

set.

Input Range: 0.01 – 9,999.99 (ml)

Default: OFF

To enter a value deactivate the blue tick box and enter a value using the automatic keypad.

8.7 Calculations

Method Centre / Calculations

There are calculations pre-programmed in the table relating to ASTM methods, D664 and D2896.

You have the option of using these or creating your own and adding them to a method of your

choice.

8.7.1 Adding a New Formula

(1) Choose the result name from the dropdown list.

(2) Press the FORMULA field and the formula editor keypad will appear.

(3) Delete or amend the existing formula and press [ENTER] to disable the keypad.

(4) Select the desired units.

(5) Press [ADD FORMULA]. A message will appear asking you if you wish to add this formula.

(6) Press [YES] and the formula will be added sequentially.

(7) Press [NO] the message is removed and you return to the calculations screen. The formula you originally created will remain in the fields until you amend them.

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There are 3 fields within calculations that are required to be populated to create and save a

calculation which are:

Result Name:

This contains a drop down list of common methods within the petroleum industry.

Formulae:

The formulae for the calculations are entered using the formula editor keypad which opens when

the FORMULA field is pressed. The maximum formula length has unlimited characters.

Units:

Select the appropriate

units from the pre-

programmed drop down list.

A new formula is added to the calculations table in ascending order.

8.7.2 Using the Formula Editor Keypad

The formula editor keypad contains buttons for entering numbers, mathematical functions and

variables. Common variables can be added to the formula by pressing [VFUNC] on the keypad and

selected from a list to avoid any spelling mistakes.

Note: Refer to Chapter 8.7.3 for details on variable function.

The functions of the keys in formula editor are shown in the table below:

KEY DESCRIPTION

/ Divide by DEL Delete individual characters

CONC Value is automatically added from the parameter: Titrant Conc, within the method the formula is linked to

TITER Value is automatically added from the parameter: Titer, within the method the formula is linked to

Left scroll though the character

Right scroll through the characters

W Weight of sample in (g), value automatically added from sample

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run screen

˽ Addition of a space between characters

VFUNC Variable functions VEQ Volume of titrant required to reach equivalence point

8.7.3 Variable Function

These are variables that are stored and can be used as part of future calculations. Some common

variables include:

(1) Determination of a blank value used in the sample calculation.

(2) Standardisation of a titrant to give a titer value which is used in the sample calculation.

Adding a Variable:

(1) Press [VARIABLE FUNCTION].

(2) Press the NAME field and enter a name using the automatic pop up keypad.

(3) Enter a value using the automatic pop up keypad.

(4) Choose the units from the drop down box.

(5) Press [ADD VARIABLE] and a message will appear asking you if you wish to add.

(6) Press [YES] to add or [NO] to cancel and return to previous screen.

Saving a Variable:

Saving a variable overwrites an existing variable that is already in the table. For example, if you have

a blank value previously added to the table, you run a new one and wish to update the existing value

then follow the procedure below:

(1) Press the variable line in the table you wish to overwrite.

(2) Amend the existing value in the field using the keypad and/or name if necessary.

(3) Press [SAVE VARIABLE] and a message will appear asking if you wish to save it.

(4) Press [YES] to accept and the previous variable will be overwritten or press [NO] to cancel.

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Deleting a Variable:

(1) Press the white box in the table, a blue tick will appear highlighting which variable you wish to delete.

(2) Press more boxes for multiple variables to be deleted.

(3) Press [YES] to delete or [NO] to cancel.

8.7.4 Saving a Formula

Saving a formula overwrites an existing formula that has been selected from the formula list.

(1) Press a formula line in the table, this will activate.

(2) Amend the formula as desired and press [SAVE FORMULA].

(3) A message will appear asking if you are sure you wish to save.

(4) Press [YES] to save or [NO] to cancel and return to calculations screen.

8.7.5 Deleting a Formula

(1) Press the formula line in the table you wish to delete.

(2) Press [DELETE FORMULA]. A message will appear asking if you wish to delete.

(3) Press [YES] and the formula will be permanently removed from the table. Press [NO] to return to the calculations screen.

Note: Only one formula can be deleted from the table at a time.

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Chapter 9 Titrants

Method Centre / New Method / Titrant Name

This chapter explains how you can create a list of titrants used in the system to add to existing

titrants already pre-programmed within the software. This list includes:

KOH in 2-propanol

HCL in 2-propanol

HClO4 in Acetic Acid

Sodium Acetate in Acetic Acid

Bromide Bromate solution

AgNO3 in 2-propanol

Sodium Thiosulphate solution

9.1 Selecting a Titrant

In METHOD CENTRE select [NEW METHOD]. Press the field TITRANT NAME and select the titrant

from the drop down list by pressing down the name until it becomes highlighted.

9.2 Adding a New Titrant

If you wish to use a titrant that is not part of the pre-programmed list you will need to add in a new

one.

Press the field NEW TITRANT under TITRANT NAME, enter in your titrant by using the automatic pop

up keypad and press ENTER [].

The number of characters is unlimited.

Press [ADD] and the titrant will be added to the titrant name list.

Note: New titrants will automatically be listed under titrant name in EDIT METHOD.

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9.3 Deleting a Titrant

Only a NEW titrant that has been added to the titrant list can be deleted. You cannot delete any of

the pre-programmed titrants from the list.

Select a titrant that has been added by pressing the titrant name.

Press [DELETE] and the titrant will be removed.

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Chapter 10 Running a Method

This chapter explains how to perform a single run determination. Entering sample data is also

explained and how it is used in calculations.

Prior to any determination both the Titrate POD and Dispense POD must be initialised. Refer to

Chapter 7.1 Titrate POD Operations and Chapter 7.2 Dispense POD Operations.

10.1 Performing a Single Determination

When performing a determination there are three routes that can be taken to get to the sample run

screen and then proceed to START RUN.

Performing a run from loading a method

Performing a run from editing a method

Quick start from favourites

10.1.1 Performing a Run from Loading a Method

Once you have selected the method you wish to run, view the parameters as a final check.

Press [RUN] to enter sample data.

Note: Refer to Chapter 10.2 for entering sample information.

Press the [RUN] button to start the determination.

10.1.2 Performing a Run from Editing a Method

Note: Refer to Chapter 8.5 for details on editing a method.

In edit method choose a method you wish to save by pressing [SAVE] and the method parameters

will appear to view. An option to run this method after saving will also appear.

Press the box and a tick will appear then press [SAVE]. View the parameters as a final check.

Press [RUN] to enter sample data.

Note: Refer to Chapter 10.2 for entering sample information.

Then press the [RUN] button to start the determination.

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10.1.3 Quick Start from Favourites

On HOMEPAGE select the method you wish to RUN from your favourites list by pressing the red

arrow icon.

This feature takes you straight to Sample Information.

Note: Refer to Chapter 10.2 for details on sample information.

Press [RUN] to begin the determination.

10.2 Entering Sample Information

(1) Begin by preparing the sample for analysis.

(2) Weigh the sample in the titration vessel.

(3) Add suitable titration solvent as instructed by the method.

(4) Place the sample vessel in the Titrate POD®.

(5) Position the electrode and dispensing tip in the electrode platform.

Set Information:

Sample ID:

Press the blank field and enter in your sample ID using the automatic pop up keypad.

User Name:

Select an activated user from the dropdown box.

Note: Refer to Chapter 6.1 for user settings.

Syringe Volume:

Check the syringe volume matches the syringe that is installed. If the wrong syringe size is shown in

SET INORMATION then this will need to be amended in the parameters in EDIT METHOD.

Dispense POD Selection:

The choice of which Dispense POD is to be used during the run determination is dependent on which

electrode(s) are connected.

- Electrode connected in Port 1 – Dispense-POD 1 box is automatically activated only and a message [ELECTRODE 1 ACTIVATED] will appear.

- Electrode connected in Port 2 – Dispense-POD 2 box is automatically activated only and a

message [ELECTRODE 2 ACTIVATED] will appear.

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- If both electrode ports are occupied Dispense POD 1 and 2 will be active. Dispense POD 1 is activated as default. Select the correct Dispense POD by pressing the empty box and a green tick will appear once activated

Note: when both electrodes are connected Dispense POD 1 can only used with electrode connected in Port 1 and Dispense POD 2 can only be used with an electrode connected in Port 2. For a single determination you cannot activate more than one Dispense POD®.

Sample Size:

Entering a value manually:

Press the SAMPLE box, a green tick will appear once activated.

Enter in your sample weight by using the automatic pop up numeric keypad.

Default Value: 0.000

Select the appropriate units.

Choose from: g, mg, µg, ml, µl

Default Unit: grams (g)

Press [CANCEL] to return to the previous screen.

Adding a blank value to a sample determination:

Entering a value manually:

Enter a value using the pop up numbered keypad and then select the units from the drop down list.

Adding a saved blank value:

Press [ADD] and select a blank value from the variable function table. Press [YES] to confirm or [NO]

to select another value.

Press [CLEAR] to remove the selected blank value.

Note: for storing a blank result refer to 10.2.1 Running a Blank Determination

The blank result will automatically be added to the sample calculation associated with the method

used for running the sample.

10.2.1 Running a Blank Determination

In SAMPLE INFORMATON under SAMPLE SIZE, select BLANK by pressing the box. A green tick will

appear which activates the blank function.

Press [RUN] and the titration will start.

Note: The blank result will be saved automatically in the Result Centre after a blank determination. Storing a Blank Result

Select [CALCULATIONS] from METHOD CENTRE. Press [VARIABLE FUNCTION]. Enter the name using the pop keypad, then the result the numbered pop up keypad and select the units from the drop down list. The blank result can now be used in sample calculations.

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10.3 Auto Prime

This priming function is programmed to flush the titrant tubing and dispensing tip through in full

syringe cycles which can be set by the user. Any air bubbles that may be present just before the start

of a determination will be removed.

Auto-prime can be activated from loading a method or running after saving an edited method.

(1) Press [AUTO-PRIME].

(2) Enter your dosing rate, default is set to maximum.

(3) Choose the number of flush cycles from the drop down box.

Input Range: 0-20 cycles

(4) Press [START] to begin or [CANCEL] to return to previous screen.

10.4 Cancelling a Determination

A run can be cancelled at any point by pressing [ABORT RUN]. Once this is activated, the run will

stop, the electrode platform will rise to the home position and the stirrer will cease.

Note: If you are navigating through other screens during a live run press the R1 icon next to the

homepage icon in the top right corner of any screen and then press [ABORT RUN].

10.5 End of a Run

Sample information:

Date and Time: Exact date and time the run was performed

User Identification: The name of the operator assigned to the determination

Sample ID: Batch number or Lot number of the sample being analysed

Method No.: Current method number automatically assigned once saved

Syringe Vol (ml): Volume size of the syringe

Vol Dispensed (µl): The total volume of titrant dispensed from the start of the titration

Starting mV: Initial reading taken in mV before the first increment is dispensed

Run State: The status of the run before during and after analysis

Run Time: The time taken in seconds to reach equivalence point

Result:

EP1 (ml) is displayed as the volume of titrant dispensed to reach equivalence point.

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Result List:

This displays all formulae and associated results that have been determined based on the method

parameters set.

FORMULA 1:

Displays the formula used to calculate the result.

RESULT 1, 2, etc:

Displays the calculated result for the determination.

Note: If more than one formula and result has been determined this will be displayed within the

result list.

Repeat Run:

Once the run has finished and the results obtained press [REPEAT RUN].

The repeat run screen will display:

Blank

Sample

If a blank is run is to be repeated the tick box will automatically be activated shown in the screenshot

above. The same applies to a sample run.

When repeating a blank run press [RUN] to begin the determination.

When repeating a sample enter in new sample information including the weight and press [RUN] to

begin the determination.

Press [CANCEL] to return to RUNNING METHOD SCREEN.

Note: The user cannot be changed during a repeat run. Refer to Chapter 6.1 for details on how to

change a user.

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R1 F1

10.6 Performing a Dual Determination

Prior to any determinations check that the Dispense POD® and Titrate PODs® have been initialised.

Refer to Chapter 7.1 Titrate POD® operations and 7.2 Dispense POD® Operations.

Note: each determination can only be started one at a time. It is important to select which Dispense

POD® you wish to start your RUN from first when in the sample information screen. Once this

determination has begun, sample information for the second Dispense POD® can be entered and the

determination started.

10.6.1 Preparing Determination RUN 1

(1) Load the method you wish to run first, following Chapter 10.1 Performing a Single Determination.

(2) Enter sample ID and user name as required in sample information screen

(3) Activate the desired Dispense POD® for determination 1 by pressing the box. A green tick will

appear.

Note: Dispense POD 1ufrt is activated as default

Refer to Chapter 10.2 for full details on Dispense POD® selection.

(4) When running a sample enter the weight and blank value as required and press [RUN].

10.6.2 Indicator icons during screen navigation during a single run

A running icon R1 will appear next to the homepage icon whilst navigating through other screens

within the software.

Run 1 in progress indicator icon Run 1 finished indicator icon

When the run has reached completion or has been aborted, a finished icon F1 will appear whilst

navigating through other screens within the software.

- Press R1 icon to return to live running screen of RUN 1.

- Press F1 icon to return to finished RUN 1 screen.

Note: during a live a determination run, method parameters cannot be changed for that live run.

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R1 R2

F2

10.6.3 Preparing Determination RUN 2

(1) Whilst determination RUN 1 is in progress, press the Homepage icon and then load the next method following Chapter 10.1 Performing a Single determination. (2) Enter sample ID and User name as required in Sample Information screen.

(3) Dispense POD® 2 will automatically be selected prior to commencement of the determination.

(4) When running a sample, enter the weight and blank value as required and press [RUN].

10.6.4 Indicator icons during screen navigation in a dual run

When dual determination runs are in progress, screen navigation is still possible.

Both running icons R1 and R2 will appear at the top of the screen next to the homepage icon.

Homepage icon Run 1 in progress Run 2 in progress Indicator icon indicator icon

- Press R1 icon to return to live running screen of RUN 1.

- Press R2 icon to return live running screen of RUN 2.

As mentioned in Chapter 10.6.1 Indicator icons during screen navigation in a single run, when

RUN 1 has reached completion or has been aborted an F1 icon will appear during screen

navigation.

When RUN 2 has reached completion or has been aborted an F2 icon will appear during

screen navigation.

Run 2 finished indicator icon

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Chapter 11 Live Running Screen

11.1 Live Display

The display is split into two sections, the graphical display and sample information.

The following functions are available whilst a determination is running:

ABORT RUN: Terminate the run at any point during the titration.

Note: Refer to Chapter 10.5 for details on cancelling a determination.

RESULT CENTRE: View result history and titration curves.

Note: Refer to Chapter 13 for details on result history.

ADJUST STIRRER: Adjust the stirrer speed at any point during the titration.

REPEAT RUN: This function is activated once a run has finished and NOT been aborted.

Note: Refer to Chapter 10.5 for details on repeating a run.

Sample Information

This contains the system status, method that is running and information about the sample being

analysed.

Once the run has completed, the result will be displayed with EP1 (ml).

Note: Refer to Chapter 8.6 for explanation of parameters.

If more than one endpoint has been identified then each EP (ml) with the calculated result will be

displayed.

11.1.1 Primary Curve

The settings for the primary curve cannot be changed these are set:

X Axis – Volume (µl)

Y Axis – Measured Value (mV)

When an increment is dispensed, a measuring point is automatically displayed in red, on the curve.

11.1.2 First Derivative

The primary curve is evaluated by plotting the first derivative dE/dV versus titrant consumption V.

The maximum of the derivative is at the inflection point and indicates the equivalence point.

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11.1.3 Second Derivative

The equivalence point is found at the volume corresponding to the x-intercept of the second

derivative curve. This point should be coincident with the inflection point (the point at which the

curve changes direction) of the original data plot and the peak of the first derivative plot.

11.1.4 Data Table

Press the [Data Table] button and you can view the individual measured values as they are recorded

during a live titration and they can also be viewed at the end. These results are also saved in the

RESULTS CENTRE.

11.2 Adjusting Stirrer

The stirrer speed can be adjusted at any point during a titration.

Press [ADJUST STIRRER].

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Use the arrow keys to increase or decrease the speed clockwise or anticlockwise.

The stirring rate can be set in steps of –10 to +10.

+ Clockwise Rotation [>]

- Anti-Clockwise Rotation [<]

Press the ON icon to begin stirring and press the OFF icon to cease stirring.

Press [CANCEL] to return to previous screen.

11.3 Aborting a Run

A run can be cancelled at any point by pressing [ABORT RUN]. Once this is activated, the run will

stop, the electrode platform will rise to the home position and the stirrer will cease.

11.4 Screen Navigation During a Run

During a live RUN, navigation through all sections of the software is possible. You have the capability

to create and edit methods, manual operations and calibrate other electrodes when running a

titration.

A blue R1 icon will appear during a live run when you have exited the running screen.

End of a Run

When a run has finished a blue F1 icon will appear informing you that the run has finished. Press this

icon to return to the running screen.

Note: The sample parameters cannot be changed during a live determination, this can only be done

when recalculating a result after a run. Refer to Chapter 12.5.

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11.5 Real Time Curve

The real time curve is a measurement application which records and plots measured values from a run over time and is an indication of the response time of an electrode.

X-axis: time (s)

Y-axis: potential (mV)

The response of the electrode can be monitored and if necessary dosing parameters can be adjusted or the electrode reconditioned in order to improve the titration curve.

View the primary curve in full screen mode for dual titrations by pressing [REAL-TIME CURVE] on the homepage.

There are three curves available to view when running a sample:

Electrode 1

Electrode 2

Temperature

Note: If a dual titration is running then both electrode 1 and 2 curves will be active to view in real

time

Swipe the screens left or right to view. Use the magnifying glass icons to zoom in and out of the

curve at any point. Return to the homepage at any point by pressing the HOME icon or press R1 to

return to the running screen.

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Chapter 12 Results Centre

HOMEPAGE / RESULT

The result centre displays a history of all results stored in numerical order with the most recent

result at the top in RESULT LIST.

12.1 Result List

You can save up to 1000 determinations within the RESULTS LIST located on the left side of the

screen.

Six results can be displayed on the screen within the results list at a time, use your finger to scroll up

and down the results at the speed you desire.

Each result within the result list displays the following information:

Result number: This is automatically assigned to a result determination that has been

generated and proceeds in sequential order. The highest number being the

most recent result

Method: The method with which the determination was performed

Date: The date at which the determination was performed

Result: The first calculated result is displayed here. If more results have been

calculated these are listed in Sample Information.

To view a results press in the result field and once activated the result will highlight orange.

12.2 Result Information

Detailed specifications concerning the current determination, including sample information, results,

calculations, method parameters and titration curves are displayed within result information. These

are displayed in red.

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Sample Information

Sample ID: The name of the determination this could be the batch or lot no. of the sample.

Date: The date at which the determination was performed.

Syringe Vol. (ml): The volume size of the syringe used during the determination.

Run time: The time taken from the start of the analysis to reach the end point determined by STOP conditions.

Method No: The method number with which the determination was performed.

User: The name of the operator selected from the sample information screen prior to a determination.

Time: The time the determination was performed.

Starting mV: The initial mV reading taken when the electrode is immersed in the vessel solution.

Run State: The status of the run situation, either: running, run aborted or run finished.

Weight (g): The sample size, entered in (g), (mg), (µg), (ml), (µl) Default is (g)

View Method

Press the view method button to scroll through the method parameters for that determination.

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Calculate Result

Result: The numbering of results, (up to 9) are displayed based on the parameters set within

the method and correspond to the order in which they were calculated in the

determination run.

EP1 (ml): The volume of titrant dispensed to reach reaction completion known as the end

point or equivalence point.

Formula: The formula added to a method used to calculate the result.

Note: Refer to Chapter 8.7 for calculations.

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12.2.1 Titration Curves

The titration curves of the current determination are displayed in three forms; the primary curve,

first derivative and second derivative. They are made up of individual data points which correspond

to each increment of titrant dispensed.

Primary Curve

This is a symmetric titration curve where the equivalence point is defined as the inflection point of

the curve.

The equivalence point occurs when the slope of the titration curve is at a maximum. The point of

inflection can be found from the primary curve but it is much easier to read the point of maximum

slope from a plot of the first derivative of the data.

1st Derivative Curve

The curve is evaluated by plotting 1st derivative dmV/titrant consumption V (ml). Therefore the

maximum of that derivative is the point of inflection and therefore the equivalence point.

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2nd Derivative Curve

The equivalence point is found at the volume corresponding to the x-intercept of the second

derivative curve. This point should coincide with the inflection point (the point at which the curve

changes direction) of the original data plot and the peak of the first derivative plot.

12.2.2 Curve Functions

Enlarge

Press [ENLARGE] to activate.

This function allows you to zoom in and out of the graph.

To do this simply use two fingers on the screen to enlarge or reduce areas of the curve.

Press [RESET] to restore the curve to its original size.

Press [CLOSE] to return to RESULT CENTRE screen.

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12.3 Filter

The filter function allows you to select the results you want to evaluate within a specific range of

parameters which you can set.

Press [FILTER] and you can search results through setting the following parameters:

COLOUR

Choose to filter results within one colour or a choice of colours depending on the electrode and

application.

Colours:

RED

BLUE

YELLOW

GREEN

WHITE

DATE

You may wish to evaluate a set of results within a certain time period.

Press ‘from’ and use the automatic pop up calendar to select the date you wish to filter from.

Press ‘to’ and use the automatic pop up calendar to select the date you wish to filter to.

If you select dates that are out of range, and no results are present within that date range then the

RESULT LIST will be blank.

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METHOD NAME

You may wish to evaluate set of results from a specific method. Select a method from the drop down

list to filter.

Choose ALL to select all methods.

Note: Other methods will automatically update into this list when a determination has finished and

the subsequent result is stored in the RESULT CENTRE.

Method Name / Starts with

Select ALL from the dropdown list and enter in characters that the particular method you wish to

filter begins with, using the automatic pop up keypad.

Press [OK] to filter or [CANCEL] to return to RESULT CENTRE.

12.4 Statistics

RESULT CENTRE / STATISTICS

You can statistically evaluate an unlimited number of result determinations from the result list or

filter out specific results. The most recent 10 results will be displayed, when scrolling down to the

bottom another 10 results will appear and so on.

The screen is divided into three sections:

(1) RESULT LIST

(2) FILTER LIST

(3) RESULT STATISTICS

Up to 1000 determinations can be stored within the RESULTS LIST. These are located on the left side

of the screen.

Ten results can be displayed on the screen within the results list at a time. A ‘wait’ icon will appear

for a few seconds then you can scroll through the next set of ten results.

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FILTER

The filter function allows you to select a specific range of results.

Note: Refer to Chapter 13.3 for more details on Filtering.

12.4.1 Selecting a Result

Activate the results you wish to perform statistics on by pressing the white box within each result in

the RESULT LIST. A blue tick will appear once activated.

Press [LOAD ITEMS] and the results will appear in the RESULT STATISTICS.

The following details are displayed:

Result Number

The result and units

N=x total number of single results from which the mean was calculated

Mean value

Absolute standard deviation SD

Relative standard deviation RSD %

To unload result items press the blue tick again.

Press [CLEAR ALL] to deactivate all of the selected results.

Press [BACK] to return to Result Centre.

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12.5 Recalculate

The recalculation function can be used to re-evaluate a particular result for the following reasons:

- If the parameters have been altered in a way that changes the recognized equivalence points

- If the variable functions have been altered e.g. weight, blank or titer

The following parameters can be modified during recalculation of a determination, using the

automatic pop up keypad:

- Titrant conc. (mol/L)

- Threshold Value

- Weight of sample (g)

- Blank (ml)

- Titer

To view the changes after modifying a parameter press [APPLY].

Press [SAVE] to store the changes generated in the RESULT CENTRE.

Press [CLOSE] to return to RESULT CENTRE.

All saved recalculated results will be stored in the result list unless they are deleted.

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12.6 Deleting Results

Select the result you wish to delete and press [DELETE RESULT].

Press [YES] to delete or [NO] to return to RESULT CENTRE.

To clear the result memory press [DELETE ALL].

Press [YES] to delete all results or [NO] to return to RESULT CENTRE.

Note: You cannot select more than one result to delete at a time.

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Chapter 13 Technical Specifications

Display

Resolution: Capacitance Touch Screen Width 152mm Height 89mm

Dispense POD

Multiple linking PODs: Up to 16 Dispense PODs can be linked simultaneously

Syringe volumes: 12.5 ml and 5 ml

Drive Design: Maintenance-free, direct drive stepper motor

Stroke Speed: 4.2 secs to 800 mins per stroke (3200 minutes in micro step mode)

Step Resolution: 24,000 steps

Imprecision (full stroke): ≤0.1% CV @ 50µl to 100 µl

≤0.05% CV @ 250µl to 5ml

Inaccuracy (full stroke): ≤1% syringe volume

Measurement Modes: Equilibrium Equivalence-point Titration

Incremental Equivalence-point Titration

Manual Titration

Calibration with automatic buffer recognition

Potentiometry

mV Range: -3200 - +3200 mV

Accuracy: 0.1 mV ( 0.0016 pH).

Resolution: 0.1mV

Amplifier Input Impendence: > 10 12Ω

Temperature

Measuring Range Pt100: 0.0 - 100°C

Resolution Pt100: 0.1°C

Measuring accuracy Pt100: ± 0.3°C (with linear calibration)

Interfaces

USB ports: 2 USB (Type A sockets) for connection of USB devices

Titrate POD: 2X Titrate POD 9 PIN D-type (female) RS232

Balance: 1x 9 PIN D-type (female) RS232

Auto POD: 1x 9 PIN D-type (female) RS232

Network Connection: LAN RJ-45 connector, Ethernet

Electrodes: 2x 6 pin LEMO (male)

Dispense POD: BUS RS485

Kycon 4 pin for series connections

Ambient Temperature

Operating Temp Range: -10 to +45°C

Operating humidity: 8-90% RH non-condensing

Storage Temp Range: -20 to +70°C

Storage Humidity: 5-95% RH no-condensing

External Power Supply

Supply Voltage 110V/220V

Frequency 50-60Hz

Power Consumption 160W

Electrode Recognition: Colour coded E-Chem® electrodes with auto recognition technology

Dialog Languages: English, Chinese, Russian, Spanish

92

Chapter 14 Parts and Accessories

14.1 PAT940 Smart Titrator Standalone System 1

Part no: 594000

594005 – Control POD® with 24VDC 7A PSU Power Pack

Comprises of:

594047 – Control POD®

594052 – 24VDC 7A PSU Power Pack

594006 – Titrate POD® with RS232 Cable 500mm and Cable Kycon 500mm

Comprises of:

594048 – Titrate POD®

594040 – RS232 to RS232 Cable (9Pin d-sub) 500mm

594038 – Cable Kycon to Kycon 500mm

594007 – Dispense POD® with one cable Kycon 500mm, RS485 Cable (2pin) 500mm and syringe

assembly kit

Comprises of:

594049 – Dispense POD®


594041 – RS485 to RS485 Cable (2pin) 500mm

594013 – 12.5ml Syringe Assembly Kit

594013 – 12.5ml Syringe Assembly Kit

Comprises of:

594014 – Dispensing Tip (1pk)

594015 – Bottle/Syringe Tubing (700mm)

594016 – Tubing from syringe to Dispensing tip (600mm)

594017 – Syringe 12.5ml

594010 – Bottle Cap with Drying Tube, desiccant filled

Comprises of:

594058 – Titrant Bottle Cap and Insert

594020 – Drying Tube with Desiccant

301802 – 170ml Standard Titration Vessel

503028 – PTFE Stirrer 6x20mm (Pack of 5)

594033 – E-Chem® PATrode Red (for non aqueous titrations)

93

14.2 PAT940 Smart Titrator Standalone System 2

Part no: 594001

594005 – Control POD® with 24VDC 7A PSU Power Pack

Comprises of:

594047 – Control POD®

594052 – 24VDC 7A PSU Power Pack

594006 – 2x Titrate POD® with RS232 Cable 500mm and Cable Kycon 500mm

Comprises of:

594048 – 2x Titrate POD®

594040 – 2x RS232 to RS232 Cable (9Pin d-sub) 500mm

594038 – 2x Cable Kycon to Kycon 500mm

594007 – 2x Dispense POD® with one cable Kycon 500mm, RS485 Cable (2pin) 500mm and Syringe

Assembly Kit

Comprises of:

594049 – 2x Dispense POD®

594038 – 2x Cable Kycon to Kycon 500mm

594041 – 2x RS485 to RS485 Cable (2pin) 500mm

594013 – 2x 12.5ml Syringe Assembly Kit

594013 – 2x 12.5ml Syringe Assembly Kit

Comprises of:

594014 – 2x Dispensing Tip (1pk)

594015 – 2x Bottle/Syringe Tubing (700mm)

594016 – 2x Tubing from syringe to Dispensing tip (600mm)

594017 – 2x Syringe 12.5ml

594010 – 2x Bottle Cap with Drying Tube, desiccant filled

Comprises of:

594058 – 2x Titrant Bottle Cap and Insert

594020 – 2x Drying Tube with Desiccant

301802 – 170ml Standard Titration Vessel

503028 – PTFE Stirrer 6x20mm (Pack of 5)


94

14.3 Accessories and Spare Parts

594015 – Bottle/Syringe Tubing (700mm)

594017 – 12.5ml Syringe

594022 – 1m to IEC UK Cable

594023 – 1m to IEC Euro Cable

594024 – 1m to IEC US Cable

594026 – 1m to IEC to China Cable


594034 – E-Chem® PATrode Blue (for aqueous titrations)

594056 – E-Chem® PATrode Green (for redox titrations for a change in pH value)

594063 – E-Chem® PATrode Yellow (for precipitation titrations)

594064 – E-Chem® PATrode White (chloride coated)


594043 – 210ml Titration Vessel

594047 – Control POD® (No Cables)

594048 – Titrate POD® (No Cables)

594049 – Dispense POD® (No Cables or Syringe Tubing)

594058 – Titrant Bottle Cap and Insert (DIN45)

594018 – DIN45 Red Bottle Cap

594019 – PTFE insert for DIN45 Bottle Cap +2x 1/4-UNF Helicoils+Filter Hole

594060 – ¼-UNC Bottle Cap Insert Hole Plug (2pcs)

594061 – Electrode Platform Hole Plugs (3 pcs)

594055 – Electrode Sleeve

594059 – Pt100 Temperature probe

95

Chapter 15 Conformity and Warranty

15.1 Declaration of Conformity

GR Scientific products are in conformity with the EU Directives:

2004/108/EC Electromagnetic Compatibility Directive

2006/95/EC Low Voltage Directive

This is based upon the compliance of the products with the harmonised standards:

BS EN 61000-6-1:2007 Electromagnetic Compatibility. Generic immunity standard.

Residential, commercial and light industry;

BS EN 61010-2-030:2010 Safety requirements for electrical equipment for measurement,

control and laboratory use. Particular requirements for testing and measuring circuits;

BS EN 61326-1:2013 Electrical equipment for measurement, control and laboratory use. EMC

requirements. General requirements.

15.2 Quality Control

PAT940 Smart Titrator®; is adequately and professionally Quality Controlled to ensure that it is fully

functional and to ensure that it meets all of the requirements that the instrument supports.

15.3 Customer Support and Service

We want you to maximise the return on your equipment through a service program tailored to your requirements from when you purchase our equipment which includes:

Support and Repair

Maintenance and Calibration

Training and Installation

Quality Assurance and Certification

Our dedicated service staff are on hand to help in the unlikely event that your equipment develops a fault. Please contact us using the details provided to discuss the next step.

15.4 Warranty

Under the conditions of our warranty, all faults which are proved to be due to material, construction or manufacturing defects, which occur within 24 months of the delivery date, will be repaired or replaced, (at our discretion), free of charge at our premises. Freight costs will be chargeable along with any inspection work which was not necessitated by manufacturing or material defects. Breakages of glassware or electrodes are not covered by this guarantee. In the event of instrument failure during the warranty period, written authorisation must be obtained from the manufacturer prior to shipping.

15.5 Warranty Exemptions

Some parts of the instrument and the accessories cannot be replaced under warranty. These

include:

- Glass Vessels - Syringes - Switching Valves

- Electrodes - Plungers

96

GR Scientific

Building 69

Wrest Park

Silsoe

Bedfordshire

MK45 4HS

United Kingdom

+441525 404747

[email protected]

www.grscientific.com

Documents

PAT940 Smart Titrator - GR Scientific · 2016-02-08 · 10.1 Performing a Single Determination----- 71 10.1.1 Performing a Run from Loading a ... 12.2.1 Titration Curves ... materials