Omega Products SMP40 Installation Manual

MPS40

Melting Point Apparatus

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User’s Guide

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MADE IN UNITED KINGDOM

Servicing North America:

U.S.A.: OMEGA Engineering, Inc.

ISO 9001 Certified One Omega Drive

P.O. Box 4047
Stamford, CT 06907-0047 USA
Toll-Free: 1-800-826-6342 TEL: [phone]
FAX: [phone] e-mail: [e-mail]

Canada: 976 Bergar

Laval (Quebec), H7L 5A1 Canada
Toll-Free: 1-800-826-6342 TEL: [phone]
FAX: [phone] e-mail: [e-mail]

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U.S.A. and Canada: Sales Service: 1-800-826-6342/1-800-TC-OMEGA

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Customer Service: 1-800-622-2378 /1-800-622-BEST

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Servicing Europe:

Benelux: Managed by the United Kingdom Office

Toll-Free: 0800 099 3344 TEL: [phone]
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Czech Republic: Frystatska 184

733 01 Karviná, Czech Republic
Toll-Free: 0800-1-66342 TEL: [phone]
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Germany/Austria: Daimlerstrasse 26

D-75392 Deckenpfronn, Germany
Toll-Free: 0800 6397678 TEL: [phone]
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United Kingdom: OMEGA Engineering Ltd.

ISO 9001 Certified

One Omega Drive, River Bend Technology Centre, Northbank
Irlam, Manchester M44 5BD United Kingdom
Toll-Free: 0800-488-488 TEL: [phone]
FAX: [phone] e-mail: [e-mail]

OMEGAnet®Online Service Internet e-mail

omega.com [e-mail]

It is the policy of OMEGA Engineering, Inc. to comply with all worldwide safety and EMC/EMI
regulations that apply. OMEGA is constantly pursuing certification of its products to the European New
Approach Directives. OMEGA will add the CE mark to every appropriate device upon certification.

The information contained in this document is believed to be correct, but OMEGA accepts no liability for any
errors it contains, and reserves the right to alter specifications without notice.
WARNING: These products are not designed for use in, and should not be used for, human applications.

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Melting Point

automatic melt ing point

SMP40

Apparatus SMP40

Instructions for use

Version 1.0

1. Introduction 1

2. Safety Advice Before Use 1

3. General Description 1

3.1 Module Separation 2

3.2 Melting Point Determination 3

3.3 Temperature Settings 3

3.4 Sample Preparation 3

4. Preparation for Use 4

4.1 Electrical Installation 4

4.2 Installation 4

5. Instrument and Software Controls 5

5.1 Instrument 5

5.2 Main Menu Screen 6

6 Setting up New Methods 10

6.1 Creating a New Method 11

6.2 Preset Methods 12

6.3 Carry out a Rapid-Melt 13

7 Performing Melt Determinations 14

8 Results 17

8.1 View Previous Results 17

8.2 Re-use Result Parameters 25

9 File Management 26

9.1 Manage Files 26

9.2 View Storage Information 28

10 Settings and Calibration 29

10.1 User Settings 29

10.2 Maintenance Settings 31

10.3 Instrument Calibration 31

11 Maintenance & Servicing 36

11.1 Repairs and Support 36

11.2 Cleaning the Sample Block 36

11.3 Accessories 36

12 Warranty 37

13 Specification 37

1. Introduction

Thank you for purchasing this piece of Stuart
equipment. To get the best performance from the
SMP40 please read these instructions carefully
before use. Before discarding the packaging
check that all parts are present and correct.

For your own safety and that of others please
read and understand the safety advice given
below before using the equipment.

2. Safety Advice Before
Use

! If the equipment is not used in the manner
described in this manual and with accessories
other than those recommended by Stuart, the
protection provided might be impaired.

This equipment is designed to operate under the
following conditions:

❖ For indoor use only

❖ Use in a well ventilated area

❖ Ambient temperature range +5°C to +40°C

❖ Altitude to 2000m

❖ Relative humidity not exceeding 80%

❖ Mains supply fluctuation not exceeding 10%

❖ Over-voltage category II IEC 60364-4-443

❖ Pollution degree 2

Never move or carry the unit when in use or
connected to the mains electricity supply.

The unit should be carried using both hands with
fingers under each side of the frame.

The ventilation slots at the back or side of the
device should not be sealed or obstructed.

*

The number of result files that can be stored on the SMP40 is largely dependant upon the runtime and size of

the video file for each sample.

The user is able to review the result file and video, reprocessing the automatically determined results if required.

3. General Description

The device is designed to automatically measure
and record the melting temperatures of crystalline
samples held within capillary tubes. Up to three
tubes can be accommodated in an illuminated
chamber within an aluminium block. The tubes
are monitored by a digital camera; the image of
which can be viewed on the instruments display
during the melting process. The device is
designed to be independently operated using the
colour touch screen allowing all operational and
data management functions to be performed
without the need to attach an external computer
or keyboard. The unit can be split into two
modules to allow the heating module to be
located in an environment suitable for the types
of samples being tested, while the control
module can be kept in a more convenient
location.

The temperature range of the device is ambient
to 400°C and the heating rate is variable
between 0.1°C and 20°C/minute. Temperature
data and information on the instruments status is
displayed on the screen at all times. All of the
instruments functions and menus are accessed
using the colour touch screen interface which
allows fast and intuitive navigation throughout a
substance’s melting point determination (melt
determination). The instrument has sufficient
internal storage capacity for an almost unlimited
number of preset method programs and typically
between 100 and 200 result files*. When
required, result files can be transferred from the
instrument to a PC or USB flash drive for external
storage and archiving.

When a melt cycle is started the SMP40 heats up
to the pre-programmed plateau temperature at
the maximum rate before stabilising at the
plateau temperature for 60 seconds. The SMP40
will then start to heat at the pre-programmed
rate until the melt is complete or until the device
reaches a pre-determined end temperature. Once
a melt determination has been completed,
cooling is automatically engaged until the
instrument reaches 50°C.

1

3.1 Module Separation

automatic melting point

SMP40

automatic melting point

SMP40

automatic melting point

SMP40

Control module

Figure 1: SMP40 module separation

The SMP40 can be split into two separate
modules using the split module release
mechanism located at the rear of the “Control”
module. Using the supplied accessory cables the
modules can be placed in separate locations up
to 1m apart.

Please ensure that the instruments electrical
power supply is switched off or disconnected
before commencing the following procedure.

1. Rotate the split module release mechanism
clockwise until it cannot be turned any further.

2. Gently pull the “Control” and “Melt” modules
apart taking care not to strain the connecting
USB cable.

3. Disconnect the USB cable on the control
module that connects the two modules.

4. Using the accessory cables supplied with your
SMP40 reconnect the power and USB
connections between the modules.

5. Once the devices power supply is
re-established the unit can then be used as
described in this manual.

6. Reconnecting the modules is the reverse of the
above.

Please ensure that the extension cables are
not removed from their connections when
the unit is connected to the electrical power
supply and switched on.

Melt module

The SMP40s touchscreen display is fitted with an
accelerometer device.

Flat

Upright

2

3.2 Melting Point Determination

The capillary technique is a standard method for
determining the melting point of a substance. In
this method, thin glass capillary tubes containing
prepared samples of a substance are introduced
into the heating block of a suitable device. The
block is then heated at a fixed rate over a
temperature range that brackets the expected
melting temperature of the substance, until the
substance is completely melted (i.e. clear point).

During the heating cycle the substance under test
will often undergo a number of observable
physical changes:

1. Fine droplets adhere uniformly to the inside of
the capillary tube.

2. A clearance between the sample and the
capillary wall becomes visible.

3. The substance collapses and begins to liquefy.

4. A meniscus is visible at the samples surface

but solid particles remains visible. (Meniscus
Point)

5. The sample is a clear liquid and no solid
particles remain visible. (Clear Point)

When determining the melting point of a
substance it is necessary to select one stage in
the melting process which will be used to define
the melting point. The meniscus point or clear
point is commonly used to define the melting
point of a substance.

The SMP40 automatically reports the Clear
Point (5); the point at which the sample is a
clear liquid and no solid particles remain, as
the melting point of a substance.

Other changes in the physical appearance of the
substance are sometimes observed, such as
sublimation (transition from the solid to gas
phase with no intermediate liquid stage) or
decomposition (the separation of a substance
into its elements or smaller compounds). These
changes (if observed) should be recorded
manually.

Where a single melting point is difficult to define
for a substance it is often useful to report a
substances melting range. The melting range of a
substance is defined as the interval between the
start of a melt and the clear point.

3.3 Temperature Settings

The temperature settings used to determine a
substances melting point are critical to the
accuracy of the determination.

Start or
Plateau
Temperature:

End
Temperature:

Ramp
Rate:

Ramp rate is the most important instrument
parameter with regards to the accuracy of a
substances melt determination. The use of
fast ramp rates is the most common cause of
inaccurate melt determinations.

3.4 Sample Preparation

For accurate melting point determinations the
substance being tested should be in a dry and
uniformly powdered form. Coarse crystalline and
non-homogeneous samples should be crushed
into a fine powder using a pestle and mortar
before the substance is introduced into a capillary
tube.

Each capillary tube in a substances melt
determination should be prepared in the same
way. The open end of a capillary tube is pressed
gently into a small amount of powdered
substance until the capillary contains sufficient
material to form a compact layer of 2.5-4.5mm in
height. The powder is then forced to the bottom
of the tube by repeatedly tapping the bottom of
the capillary against a hard surface.

Excessive amounts of sample in the capillary
tubes will result in inaccurate melt
determinations.

The start temperature is usually
set 5 or 10˚C below the
expected melting point of the
substance.

The end temperature is set at a
temperature where all physical
changes in the substance are
expected to be complete.

The ramp rate is the rate at
which the sample block is
heated during the melt
determination. For accurate
determinations a rate of
between 0.5˚C/min and 2.0˚C/
min is recommended.

3

The SMP40 can accommodate up to three sample
capillaries. For accurate melting point
determinations it is recommended that three
samples of the same material are prepared in the
same way and analysed at the same time. The
average of the three capillaries results can then
be reported as the substances melting point.

The appropriate mains lead should be connected
to the instrument BEFORE connection to the
mains supply. Should the mains lead require
replacement, a cable of 1mm
code H05VV-F connected to an IEC320 plug
should be used. The UK mains lead is protected
by a 10A fuse mounted in the plug top.

2

of harmonised

4. Preparation for Use

4.1 Electrical Installation

THIS EQUIPMENT MUST BE EARTHED

Before connecting the instrument, please read
and understand these instructions and ensure
that the electrical supply corresponds to that
shown on the rating plate. This unit is designed
for use with a supply rated at 115/230V,
50-60Hz. The power consumption of the unit is
60W. The unit is fitted with an IEC socket at the
side of the instrument for connection of the
mains lead.

Caution: Fuses are fitted in both live and
neutral lines.

The unit is supplied with two mains leads fitted
with IEC plugs. One lead has a UK 3 pin plug and
the other has a 2 pin “Shuko” plug for
connection to the mains supply. Choose the lead
appropriate for your electrical installation and
discard the other. Should neither lead be suitable
take the lead with the UK plug and replace the
plug with a suitable alternative. This involves
cutting off the moulded plug, preparing the cable
and connecting to the rewireable plug in
accordance with its instructions.

IT IS IMPORTANT THAT THIS OPERATION
SHOULD ONLY BE UNDERTAKEN BY A
QUALIFIED ELECTRICIAN.

Refer to the equipment’s rating plate to ensure
that the plug and fusing are suitable for the
voltage and wattage stated. The wires in the
mains cable are coloured as follows:

LIVE BROWN

NEUTRAL BLUE

EARTH GREEN/YELLOW

4.2 Installation

Connect the unit to the electricity supply but DO
NOT SWITCH ON. Place the unit on a firm, level,
non-slip surface ensuring that there is sufficient
free space on all sides without coming into
contact with anything else during use. Switch the
unit ON at the mains On/Off switch on the side
of the instrument. When switched ON, the touch
screen display will illuminate and the interface
software will load within 30 seconds.

IF IN DOUBT CONSULT A QUALIFIED
ELECTRICIAN

The sample block will become hot during

operation.

4

5. Instrument and Software

automatic melt ing point

SMP40

Controls

5.1 Instrument

Touch Screen
Interface and
Display

A/C power
input

Split Module Release
Mechanism

Sample Compartment

Capillary Storage
and Cutter

ON/OFF Switch

Mains On/Off: This is a rocker type switch found on the left hand side of the
unit. Pressing the “I” switches the unit ON. Pressing the “O”
switches the unit OFF.

Sample Compartment: This lifts to provide access to the sample block which is capable of
holding three capillary sample tubes.

Capillary tubes must be a minimum of 5.0cm in length to
ensure that they can be retrieved from the sample block.

Capillary Storage and Cutter: A compartment is provided for the storage of the glass capillaries

used in the melt determinations and incorporates a device to cut
capillary tubes.

Touch Screen Interface The touch screen interface is used to perform all control
and Display: functions on the SMP40. Live images of the sample compartment,

real-time data on the instrument’s status and the sample block’s
temperature can also be viewed on this display.

USB and Ethernet A USB flash drive can be inserted into the one of the USB ports,
Connections: allowing result files to be copied or moved from the device. If the

unit is to be connected directly to a PC please contact the technical
support department for advice. See page 35 for contact details.

The ethernet port is for service and support use only.

USB and Ethernet
Connections

Figure 2: SMP40 front view

5

5.2 Main Menu Screen

Figure 3:
Main Menu

When the instrument is first switched on the display will show “LOADING PLEASE WAIT” message.
After 30 seconds the display will show the main menu screen and the four main menu options:

Measurement: This menu gives access to options that allow a new melt determination to be
performed using new, previously stored or preset method parameters.

Results: This menu gives access to the result files stored on the device. The result files report and
video file can be accessed from this menu.

File Management: This menu allows result files on the device to be copied or moved to an inserted
USB flash drive. The devices storage information is also displayed in this menu.

Settings and Calibration: This menu gives access to the devices user adjustable settings and also
allows the device to be recalibrated if required.

The Stuart SMP40 is controlled solely through the touch screen interface of the instrument. The
header bar is located at the top of the screen in most menus within the software interface.

Back button

Figure 4: The
Touchscreen
Header Bar

Back Button: Used to return to the previous screen at anytime

Block Temperature: Displays the actual temperature reading from the sample block

Time and Date: Displays the current time and date in the format specified in the user settings

Menu Title/Name: Displays the current menus title or name

Instrument Status: Displays the current instrument status

Home Button: Used to return to the main menu at anytime

Menu title/name Instrument status

Home button

6

The command toolbar is located at the bottom of the screen in most menus within the software
interface. The command toolbar will give the user either one or two options based upon the menu
shown.

Figure 5: The Command Toolbar

If the number of options available in a menu exceeds the number that can be displayed on the screen,
a scrollbar will be displayed on the right hand side. Pressing the arrows at the top and bottom of the
scrollbar enables the list of options available in the menu to be seen.

The following controls are used to input data and adjust settings on the instrument:

Alphanumeric: Alphanumeric data can be
entered.

Numerical: Numerical data can be entered.

Date: Calender date information can be entered.

Time: 12/24hr time information can be entered.

Listed Options: Setting specific options can be

selected.

Drop Down List: Field specific options can be
selected.

Toggle Selection Field: Option is not selected or
selected respectively.

Other keys used:

BCK Removes the character directly behind the cursor or the highlighted characters.

DEL Removes the character directly in front of the cursor or the highlighted characters.

SHIFT Toggles the keypad between higher and lower case letters for one character entry.

CAPS Toggles the keypad between higher and lower case letters for all characters entered.

CLR Clears the characters in the current entry.

To change the data in each of these fields the screen should be pressed within the border of the control.
The interface used to add or change the setting depends on the type of control.

7

5.2.1 Alphanumeric Entry Field

1 Selecting an Alphanumeric Entry Field opens

the text keypad interface.

2 The alphanumeric entry field can be

populated with letters (Abc), numbers (123)
or symbols (SYM). Text, numbers and symbols
are accessed using the Abc, 123 and SYM
keys on each of the respective keypads.

3 Entries are confirmed by pressing the “Accept

this text” button on the command toolbar.

5.2.2 Numerical Entry Field

8

1 Selecting a Numerical Entry Field opens the

numeric keypad interface.

2 The numeric entry field can only be populated

with numbers.

3 Entries are confirmed by pressing the “Accept

this number” button on the command
toolbar.

5.2.3 Date Entry Field

5.2.4 Time Entry Field

1 Selecting a Date Entry Field opens the date

keypad interface.

2 The date entry field is displayed in the

format specified in the User Settings menu.

3 Press the arrows above and below each

number to increase or decrease the value
displayed.

4 Entries are confirmed by pressing the

“Accept this date” button on the
command toolbar.

1 Selecting a Time Entry Field opens the time

keypad interface.

2 The Time Entry Field is displayed in the 24

hour format.

3 Press the arrows above and below each

number to increase or decrease the value
displayed.

4 Entries are confirmed by pressing the “Accept

this time” button on the command toolbar.

5.2.5 Listed Options Field

1 Selecting a Listed Options Field opens the

listed options keypad interface.

2 The options available in the Listed Options

entry field is specific to each individual
setting. e.g. The Temperature Units setting
gives the options Celsius (˚C), Fahrenheit (˚F)
and Kelvin (K).

3 Use the scrollbar to view the full list of

available options for each setting.

4 The option that is required is selected by

pressing on the required option button.

9

5.2.6 Drop Down List Field

5.2.7 Toggle Selection Field

6. Setting up New Methods

1 Selecting a Drop Down List Field displays the

options available for that field.

2 Arrows keys may be displayed to indicate that

further options are available. Use the arrow
buttons to view the additional options.

3 Press the required option from the list to

select it.

1 Pressing a Toggle Selection Field will add or

remove the check mark in that field.

2 A check mark indicates that the option is

active.

Touching the measurement section on the main menu screen will open the measurement menu where
three options are available:

Create a new measurement: This option
allows a new melt determination to be started.
Measurement parameters such as the Sample
Name, Start Temperature and Ramp Rate need to
be entered when using this option.

Use a preset from the library: This option
allows a new melt determination to be started
using measurement parameters stored previously
on the device.

Carry out a rapid-melt: The device will roughly
determine the melting point of the sample using
preset measurement parameters.

10

6.1 Creating a New Method

In the Measurement menu screen touch the “Create a new measurement” section of the screen.

1 Enter a sample name for the samples by

selecting the Sample Name field

2 Enter an appropriate start or plateau

temperature for the sample by selecting the
Start Temperature field.

3 Enter the required temperature ramp rate for

the samples by selecting the Ramp Rate field.

4 Optional sample and method information is

accessed by pressing the “Touch here to enter
additional information” button. If this is not
required press “Continue” and go to step 8.

5 The SMP40 will automatically detect the end

of the melt when the toggle selection field
has an X in the Automatically detect the melt
end field. Removing this check mark allows a
value to be entered into the End Temperature
field.

6 Enter any batch or reference details in the

Batch/Reference alphanumeric entry field.

7 To proceed to the melt determination select

“Go back to main information” and then
select “Continue”.

8 The option of saving this new method as a

preset method will be given. Select “Yes” to
save the method for future use or select
“No” to proceed without saving the method.

11