KSV 5000 User manual

Operation Manual
LB device
KSV 5000
Revision 1.1

Table Of Contents
1. INTRODUCTION------------------------------------------------------------------------- 1
2. PHYSICAL DESCRIPTION ----------------------------------------------------------- 2
2.1. Overview ------------------------------------------------------------------------------2
2.2. System 1 -------------------------------------------------------------------------------3
2.3. System 2 -------------------------------------------------------------------------------4
2.4. System 3 -------------------------------------------------------------------------------5
2.5. Mechanics -----------------------------------------------------------------------------6
2.6. Additional Devices ---------------------------------------------------------------- 10
2.7. Special Troughs-------------------------------------------------------------------- 11
3. PRELIMINARIES -----------------------------------------------------------------------15
3.1. Connections------------------------------------------------------------------------- 15
3.2. Cleaning ----------------------------------------------------------------------------- 16
3.3. Dipper Substrate Attachment -------------------------------------------------- 19
3.4. Monolayer Material Spreading ------------------------------------------------ 19
3.5. Experimental Setup --------------------------------------------------------------- 20
4. TECHNICAL SPECIFICATIONS ---------------------------------------------------21
4.1. Deposition System ----------------------------------------------------------------- 21
4.2. Film Pressure Measuring System---------------------------------------------- 21
4.3. Film Area Control System------------------------------------------------------- 21
4.4. Trough ------------------------------------------------------------------------------- 22
4.5. General ------------------------------------------------------------------------------ 22
5. CONTACT INFORMATION----------------------------------------------------------23

1
1. Introduction
The Langmuir and Langmuir-Blodgett (LB) devices available from KSV
Instruments are efficient and effective in investigating the properties of floating
monolayers, precise deposition of multilayers onto solid substrates or simply
as platforms for use in observing surface chemistry effects such as the
breakdown of an enzyme or the crystalline structure of a surfactant. The wide
range of available systems and the many modules available make
customisation a charm, and if the troughs available do not suit your needs
then contact us about designing a particular trough to your specifications.
There are four series of LB systems available today, the KSV 5000, 2000,
Minitrough and the Minimicro in descending order of size. The differences
between the systems are mechanical, the same software and interface unit
operates all of the LB devices. KSV 2000 is the basic multipurpose LB device.
KSV 5000 adds a sturdy frame with automatic elevator arms for attaching
additional measurement devices, becoming the most versatile LB device
available today. The KSV Minitrough is a more compact and economical LB
device. The KSV Minimicro is a small and elegant LB device brilliant for
depositions on small substrates or to minimise sample volumes.
This is the device-specific manual for the KSV 5000 LB device, featuring
details such as physical descriptions and cleaning instructions. Please see the
LB installation manual or the LB software manual for details on installation,
calibration, measurement taking or data analysis.

2
2. Physical Description
2.1. Overview
The general physical layout of the KSV 5000 Langmuir-Blodgett (LB) system
consists of the trough with the subphase and the surfactant, barriers which
can adjust the surface pressure by reducing the area available to the
surfactant, a balance with a Wilhelmy plate which monitors the surface
pressure and an interface unit to control the devices and communicate with
the computer running the experiment.
The available systems are:
System Trough Devices Available
experiments
1 Flat Balance Langmuir
film balance
2 Flat with well Balance and
dipper
Multilayer
LB-films on
solid
substrate
and
Langmuir
film balance
3 Compartmentalised
with half-circle well
Balance
and
two-
armed
dipper
Alternating
LB-films, one
component
LB-films and
Langmuir
film balance

3
2.2. System 1
The appearance of the instrument depends on the system in use. System 1 is
the most basic setup, consisting of a balance and a trough with a barrier drive
system.
Image 2.1: KSV 5000 System 1.
1) Balance
2) Trough
3) Barriers
4) LayerBuilder
System 1 is designed for the study of floating monolayers.
PTFE trough with a surface area of 870 cm2, (L580 x W150 x D9 mm3) and a
subphase volume of 780 ml.
1
2
3
4

4
2.3. System 2
The System 2 additions over System 1 are the dipper, a second stand for the
dipper and a trough with a well.
Image 2.2: KSV 5000 System 2.
1) Balance
2) Trough
3) Barriers
4) LayerBuilder
5) Dipper
6) Well
System 2 is designed for the study of floating monolayers and for the
deposition of multilayer films of one substance on a solid substrate.
PTFE trough with a surface area of 870 cm2, (L580 x W150 x D9 mm3), a
dipping well (L37 x W117 x D90 mm3) and a subphase volume of 1172 ml.
1
2
3
4
5
6

5
2.4. System 3
In addition to system 1 the trough is fitted with a bigger, half circle well and a
two-armed dipper is positioned above the well. Two pairs of barriers and two
balances operate different sides of the trough.
Image 2.3: KSV 5000 System 3.
1) Balances 4)
LayerBuilder
2) Trough 5)
Dipper
3) Barriers 6)
Well
System 3 is in effect two different LB troughs where the subphases are
connected through the dipping well. Two barrier drives operate independent
pairs of barriers so the surface pressures of both sample compartments can
be adjusted separately. A two-armed dipper with one arm operating above the
surface and the other operating below the surface means that only the
substrate breaks the surface. A central compartment with a clean water
surface gives unlimited choice in which layer is next deposited onto the
substrate and from which direction (immersing into or withdrawing from the
subphase).
PTFE trough with a surface area of 2 x 930 cm2, (L775 x W120 x D10 mm3), a
half-circle (radius 133mm) dipping well in the centre divided into 3
compartments and a subphase volume of 6000 ml.
1
2
3
4
5
6

6
2.5. Mechanics
A) Computer
The computer controls all functions of the instrument. Because each device
includes its own microprocessor, the computer sends only high level
commands to them (for instance "Move with certain speed" or "Go to certain
position" and so on). All devices are listening to every message, but they
become active only when they recognise their own address.
The computer should be a PC running Windows 2000/XP/Vista. A 1GHz
processor and 512MB RAM memory are recommended.
B) Barrier Driving System
The barrier position is controlled by a micro step driven stepping motor. The
motor moves the barrier holder using a tooth belt. The holder itself is attached
to a linear motion system, which is equipped with ball bearings.
The barrier driving system is equipped with adjustable safety switches which
stop the barrier immediately when the barrier holder hits the switches. The
position of the barrier is measured using an optical encoder. The position is
relative and so a zero point at a known position must be set manually.
The control electronics are located inside of the barrier driving unit. There is a
15-pin connector on the rear of the unit. The barrier driving unit should be
connected to the Interface unit through this connector.

7
Image 2.4: Block diagram of the barrier driving system
C) Surface Balance
The surface pressure is measured by using the Wilhelmy plate method (round
rod optional). The Wilhelmy plate is a carefully sandblasted platinum plate or a
clean paper plate, which is put partly under the surface of the subphase.
Normal practice is to position the plate so that one third of it is under the
subphase. The force acting on the plate depends on surface pressure. This
force is measured using the electro-balance. The total measurement range of
the balance is +/- 2000 mg. The width of the platinum Wilhelmy plate has
been chosen so that 1 mN/m corresponds to 4 mg. For paper Wilhelmy plates
this value is commonly about half as great as with the platinum plates.

8
Image 2.5: Block diagram of the surface balance.
D) Deposition system
The deposition system is DC motor controlled to ensure vibration-free
operation. The speed range of the dipping arm is 0.1...85 mm/min and
maximum stroke is about 145 mm. The DC motor is servo controlled to keep
the speed constant. The position is determined with an optical encoder. The
deposition system is equipped with safety switches which stop the motor
automatically in both ends.

9
Image 2.6: Block diagram of the deposition system.
E) Trough and Barriers
The troughs are made of a solid piece of PTFE. The trough is glued onto an
aluminium base plate, in which there are water channels for the thermostation
of the subphase. The temperature is adjusted with a water bath circulator,
which is connected to the trough with special connectors. These connectors
include valves in both parts, so the connection can be opened without any
leakage.
The maximum temperature allowed is 60C!
The barriers are made out of hydrophilic material, which ensures that the film
does not escape the barrier. The barrier material is polyacetal (Delrin) and it
should be noted that Delrin is not resistant to acids or chloroform, so do
not use these as cleaning agents. Chlorinated solvents such as these can
still be used as spreading solvents. The barrier is equipped with a round rod,
which fits into the barrier holder.

10
2.6. Additional Devices
Various additional devices can be used to improve measurement conditions,
enable additional measurement methods or to provide additional data.
A) Thermostation
The temperature of the subphase can be monitored with a temperature probe
that connects directly to the Interface Unit. A temperature probe is shown in
image 5.7.
The temperature sensor is covered with a thin PTFE tube and it can be
attached to the trough with a special holder. The display units are in degrees
Celcius, though Fahrenheit is available on request.
This keeps a full record of the temperature conditions of the experiment, but to
adjust that temperature a water bath is required. KSV troughs have built-in
piping in the aluminum block which holds the teflon trough. Connect the water
bath to the ports along one end of the trough. KSV Instruments recommends
the Julabo water bath also available from KSV, though others can be used as
well.
Connect the water bath to an available COM port on the computer. Use the
software's Manual Control Unit to adjust the temperature settings for the water
bath, see section 4.5 Control Panel for details.
B) pH Probe
The acidity of the subphase can be monitored with a pH probe that connects
directly to the LayerBuilder interface unit.
C) Stirrer
A magnetic stirrer consists of a rotating magnetic field source and a small
magnetic bar. The rate of rotations can be adjusted with the control knob on
the power supply. A magnetic stirrer is used particularly with enzyme reaction
studies.
D) Cabinet
A cabinet that can be placed around the LB device to isolate it more from the
environment. Includes appropriate holes for water bath circulator tubes and
cables.

11
E) Horizontal Dipping Clamp
The standard dipper clamp can be replaced by a horizontal dipping clamp for
the purpose of conducting Langmuir-Schaefer experiments. The two dipping
clamps can be interchanged quickly and easily, and no software upgrade is
necessary. Set the zero position of the dipper as the level at which the plate is
wetted first. With longer experiments the dipping depth might need to be
increased over time to reach the surface due to evaporation.
F) Surface Potential Probe SPOT
A surface potential probe (KSV SPOT) is a tool for measuring the surface
potential of an interface or a solid. KSV SPOT uses the vibrating plate
capacitor method.
G) Brewster Angle Microscopy BAM
Brewster angle microscopy (BAM) provides visual information of two
dimensional structures in monolayer films. It utilises a laser and a CCD
camera to obtain images at 25 fps.
H) Interfacial Shear Rheometer ISR
The ISR 400 provides information on the shear stress of interfaces,
particularly useful for low viscosity applications. A teflon-coated magnetic
needle rests at the interface, and as a magnetic field is induced the movement
of the needle is observed with a microscope.
2.7. Special Troughs
The choice of trough is one of the most important ones to make when
acquiring and using a LB device. Several troughs are available designed, and
many more can be manufactured according to specifications. The specialized
trough types available at the moment are alternate dipping, conductivity,
compartmentalised, enzyme reaction, oil/water interface and surface potential
troughs. Additionally several features can be incorporated into most of the
troughs, these are an injection port, a quartz window and low subphase
volume.
A) Alternate Dipping Trough
The alternate dipping trough allows precisely constructed layers of two
different surfactant substances for KSV 2000 System 3. Subphase volume
reduced from 6000 ml to 1500 ml. Maximum size of substrate 20mm x 45mm.

12
B) Conductivity Trough
The conductivity trough is used to measure the conductivity of the monolayer.
Four electrodes are placed near the center of the trough, two on each side of
a central rise. The central rise divides the trough into two compartments with a
narrow band of glass connecting the subphases of the different
compartments.
Image 2.7: The conductivity trough
The exterior electrodes introduce a current and the interior electrodes
measure the potential between them. The subphase volume through which
the current can flow is minimized with the use of the glass band.
C) Enzyme Reaction Trough
The enzyme zero order breakdown reaction can be observed with this special
trough. The center compartment is connected to the outer compartments with
glass bridges allowing the pressures to be adjusted without disturbing the
center compartment.
Image 2.8: The enzyme reaction observation trough.
The enzyme is placed in the centre trough and the initial surface pressure is
measured. A protein is placed through an injection port and as the protein

13
interacts with the monolayer the amount of monolayer material decreases and
surface pressure decreases. The barriers approach the centre to keep the
surface pressure (and thus mean molecular area) constant, and the area
removed by them can be used to calculate the activity of the enzyme.
A stirrer might be necessary to properly observe the activity of the enzyme.
D) Oil/Water Interface
The oil/water interface trough places the monolayer material between two
liquids as opposed to between a liquid and a gas. The denser liquid, usually
water or another polar liquid, is poured into the trough up to the first notch.
The monolayer is placed onto the surface of the polar liquid. The organic
liquid is then poured gently on top of the water so that the holes in the barriers
are distinctly above the interface but covered by the oil. When the barriers are
brought closer together the monolayer material is compressed.
Image 2.9: The oil/water interface trough
Alternatively the monolayer material can be mixed into the oil and as the oil is
poured the monolayer material forms a monolayer at the interface due to the
strong polar attractions between the polar subphase and the hydrophilic end
of the monolayer material.
E) Surface Potential Trough
The trough especially designed for surface potential measurements is long
and narrow to maximise compression area. Surface potential is much more
sensitive than surface pressure, and changes in surface potential occur at
higher mean molecular areas than changes in surface pressure. Additionally a
long trough could be useful in investigating a material with curious properties
at high mean molecular areas but with a collapse point at low mean molecular
areas.

14
Image 2.10: The surface potential observation trough with a quartz window.
F) Additional Trough Features
 A quartz window can be added to most troughs to enable live
observation with a microscope or similar optical instrument.
 An injection port can be used to add a substance into the trough after
the beginning of an experiment. As it is important not to disrupt the
surface the injection port leads a needle tip from the side of the trough
to the subphase. It is a standard feature with enzyme reaction troughs.
 A low subphase volume trough reduces the area that is available for
the subphase, thus reducing the amounts of materials required.
G) Custom Troughs
Many situations arise where a custom designed trough is necessary to
accomplish a particular task. KSV Instruments supplies many custom
designed troughs, be they extensions of current designs or completely new
concepts. Ask us for more information about a trough that suits your needs!
Image 2.11: Some past custom-made troughs.

15
3. Preliminaries
3.1. Connections
Check that all devices are attached to the LayerBuilder interface unit. Check
that the power cable is connected to the interface unit and that it is turned on.
Turn on the computer and start the sgserver for LB systems. It can be located
from the Start menu under Programs >LB. Open the Manual Control Unit
by clicking on the menu Control Panel. Open the Barrier1 tab.
Image 3.1: The Manual Control Unit used to control attached devices.
Check that the safety limit switches are properly set by first closing and then
opening the barriers. Adjust the positions of the switches if necessary.

16
3.2. Cleaning
Before an experiment the trough and barriers must be cleaned. Use rubber
gloves to minimise oils from the skin contaminating the apparatus. The
importance of cleanliness cannot be overstated!
The troughs used by KSV can be removed from the frame and carried to a
sink for ease of cleaning. A recommended cleaning procedure is to first brush
with a soft brush covered in ethanol or another organic solvent (mechanical
and chemical cleaning) and then rinse with ion exchanged water. Take care
not to scratch the surface!
Images 3.2 and 3.3: Brushing the trough with ethanol (left) and rinsing the
barrier with pure water.
If the trough has not been used for a longer period of time then first washing
with hot water and a commercial detergent might be appropriate before
performing the standard cleaning described above. Replace the trough in the
frame, checking that the screws fit into the available notches.

17
Image 3.4: Replacing the trough so that the screws slot into the respective
notches.
Clean the barriers. The appropriate cleaning method is the same as with the
trough. When one barrier is cleaned place it on top of the trough before
cleaning the other barrier. Take special care in choosing the appropriate
handhold on the barrier so that replacing it will be simple, avoid touching the
delrin itself!
With an Alternate Trough Experiment the second barrier drive must be
attached on the opposite side from the first barrier drive. Fit the screw
along the side of the trough to the respective notch on the barrier drive,
just like with the first barrier drive.
Rinse the aspirator tip with ethanol and ion exchanged water.
On the Manual Control Unit click Open and wait until the barriers are in the
desired position, most often fully open. Press Zero. Fill the trough with the
subphase. In most cases pure water will be a good choice. Pour the water
gently on to the trough so that the level of the water rises distinctly (at least
3mm) above the level of the trough.
Turn on the aspirator and click on Close to start bringing the barriers together.
Contaminants on the surface of the water will be picked up by the barrier. Run
the tip of the aspirator along both barriers several times. The purpose of this is
to remove contaminants and not to suck too much of the water so run the tip
over the surface rather than plunging it into the water. When the barriers are
fully closed run the aspirator tip over the surface between the barriers several
times to pick up remaining contaminants. A systematic pattern such as three
vertical and horizontal lines (#) is recommended.
Remove enough water to lower the water surface until it is level with the
trough.

18
Image 3.5: Sucking contaminants from the barriers.
Clean the Wilhelmy plate. A thorough cleaning entails heating the platinum
Wilhelmy plate over a flame (such as a Bunsen burner). Heat the plate over a
blue flame hot enough to make the plate glow red in just a few seconds, a
flame that is too cool will leave residues on the plate surface. Alternatively
rinsing with ethanol and ion exchanged water should be enough for most
cases of frequent use. Once the experiment is finished the Wilhelmy plate
should be stored in a water-soluble organic solvent such as ethanol.
Attention! The platinum Wilhelmy plate is an excellent catalyst for the
combustion of methanol! Beware of operating the Wilhelmy plate around
methanol, especially when hot.
After the plate is completely glowing remove it from the flame and hold it for
several seconds to allow it to cool. Dip the plate into the water in the trough
and hang it from the balance hook. Set the plate so that about two thirds of it
is covered and it is perpendicular to the barriers.
For information on using a paper Wilhelmy plate, please see the LB software
manual.
Open the barriers. In the Manual Control Unit open the Balance tab and
press Zero Balance1. The reading is now zeroed with pure water, and the
measured difference in surface tension will be the surface pressure. Close the
barriers. Pure water does not cause the surface pressure to change, so any
change in surface pressure is caused by contaminants. If the surface pressure
does not exceed 0.2mN/m the water can be considered sufficiently clean.