User notes for R&K Langmuir trough users

Joe Strzalka

Overview and Specifications

This page documents procedures and useful information for users interested in collecting x-ray scattering data from Langmuir monolayers at beamline X22B of the National Synchrotron Light Source or at CMC CAT, sector 9 of the Advanced Photon Source. Each location has a liquid surface spectrometer (LSS) and a Langmuir trough that can be mounted onto the sample stage of the LSS. The troughs can be shipped between locations, but since they are primarily intended for use at X22B or CMC CAT, they will be referred to here as the X22B and CMC troughs.

CMC trough X22B trough
trough dimensions (mm)
-- width 160 160
-- length 476 388
-- depth 12 6
maximum area (cm2) 762 620
minimum area (cm2) 80
constant pressure mode? yes yes
automated data collection? yes yes
automated trough control? possible possible
temperature control? yes yes
compression speeds (mm/min) 0-180 0-180
canister dimensions (mm)
-- width ? ?
-- length ? ?
-- depth ? ?
glass block dimensions (mm)
-- width 152.5 ?
-- length 152.5 ?
-- thickness 12.0 ?

Acknowledgments

These directions are based on instructions from the manufacturer (R&K GmbH) and experience gained from the work of Andrey Tronin, Songyan Zheng and myself with our collaborators at X22-B (Ben Ocko, Elaine Dimasi and Scott Coburn) and CMC CAT (Thomas Gog and Chitra Venkataraman). Special thanks to Jarek Majewski for overseeing the design and construction of the trough. Large parts of the isotherm macros were cribbed directly from macros written by John Gray of David Vaknin's group for controling their trough. Any errors or omissions are solely my responsibility. Please direct comments to strzalka@sas.upenn.edu.

Unpacking and Mounting the Trough

The CMC trough comes in two boxes, a large one containing the trough canister and a smaller one containing the trough itself, the control unit, the connecting cables and a box with various accessories. We have recently fitted the trough canister with spacer plates to position the trough higher in the canister and thereby decrease the time necessary to fill the trough with helium. (Before you put the trough into the canister, it's a good idea to clean it under the hood in the lab.) The levelling feet on the trough fit into depressions in the top spacer plate. Make the connections between the trough and the waterbath hoses and the control box cable feedthroughs. In the cardboard accessory box, find the surface pressure transducer, mount it on the post on the trough, and connect the wires. Hang the Wilhelmy plate and hook from the plastic loop on the transducer. Mount the canister and the trough on the sample stage. The foot of the canister near the window should be approximately centered on the center of the sample theta, two-theta rotation stages. The other two feet, along with a fair amount of the canister, will hang over the side of the sample stage's adapter plate. Make the connections between the canister feedthroughs and the circulating bath and the control box cables. Level the trough using the three adjustable feet on the trough. Put the (clean) glass block into the trough and fill the trough with water.

At X22-B, you may have to mount the trough after an experiment not requiring the trough. There is hardware at the beamline that holds the trough in place. (The plates are stored in the X22 cabinet, along with the anti-vibration stages. The dogs for the anti-vibration stages are in the cabinet in the hutch. The screws and bolts are in a green cardboard box in the hutch. The anti-vibration controller and cables are beneath the table holding the 4-circle. ) See the photos below.

The base plate was centered on the sample stage for the previous experiment. To mount the trough, the base plate must be offset from the center.
The anti-vibration stages hang over the edge of the base plate and are secured with dogs. Keep the dogs loose until the other components are also in place. The letters marked on the plate and anti-vibration stages ensure the correct alignment of the components.
The adapter plate is secured by only 3 screws to each anti-vibration stage. The translation state goes on next. It has spacer plates installed so that no washers are necessary. The trough base plate goes on next, and then the dogs on the anti-vibration stages can be tightened.
The outline of the trough is marked on its base plate. Use c-clamps and metal pieces to secure the trough in position.

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Cleaning the trough and glass block

At the start of the run, it's best to clean the trough thoroughly under the hood. Put in gloves and wipe all the teflon surfaces of the trough with Kim-Wipes moistened with solvents (chloroform, methanol, acetone) and then wipe it dry. Collect the used wipes and gloves for appropriate disposal. Remember: chloroform is carcinogenic, so it is best to minimize its use and adhere to the Standard Operating Procedure for handling chloroform at CMC CAT.

We clean the glass block using nitric acid. Put on appropriate gloves and a lab coat. Remember: nitric acid and its fumes are corrosive. Under the hood, put the glass block into the tray and pour enough acid into the tray to cover the block, but try to minimize the volume used. Let the block soak while you clean the trough, mount it and calibrate it. Before you leave the block unattended, be sure to leave a note warning others that you have an open tray of nitric acid in the hood. Afterwards, pour the acid into a container appropriately labeled "used nitric acid," and save it for re-use and eventual disposal. Rinse the block with pure water several times. It should appear uniformly hydrophilic. If there are any hydrophobic patches, wiping them with kim-wipes wet with solvent in the manner described above for cleaning the trough should help. Soaking the block in a solution of detergent (Hellmanex or RBS) should also help, but be careful as this will require a lot of rinsing afterwards to ensure that all the detergent is washed from the block.

During a run operators need to find the right compromise that keeps the trough clean without taking too much time away from data collection. If consecutive monolayers are to be spread from the same or similar samples on the identical subphase, it is generally sufficient to aspirate the monolayer from the surface without exchanging the subphase completely. Since there is only a thin film of water between the glass block and the monolayer, be sure to add more subphase behind the moving barrier before you start aspirating. This will reduce the risk of the monolayer coming in contact with the block. Aspirate until the pressure is close to zero, move the barrier to the minimum position and aspirate again. Add some more subphase and aspirate again. With experience you will gain a feel for how much aspiration is sufficient to remove the monolayer completely.

Sometimes the trough needs to be cleaned more thoroughly, for example when the next sample is very different, or requires a different subphase, or if the previous monolayer's meniscus collapsed and contaminated the teflon edges of the trough. Aspirate the monolayer carefully as just described, then take out the block from the subphase and either put it aside (best to keep it covered with clean water) or clean it. Then aspirate the subphase completely and wipe down the trough and barrier as necessary, paying careful attention to any hydrophilic patches you may have noticed. Be extra careful using solvents in the hutch. Transfer a few milliliters to clean vials for use in the hood. You don't need much to clean the trough. Collect the contaminated Kim-Wipes and your gloves for disposal. Fill the trough with clean water and aspirate it out a few times before returning the block to the trough and adding the subphase for the experiment.
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Vibration Isolation


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Controling the Trough

The trough control unit consists of three modules, as seen in the above picture. From left to right we see the Pressure, Area and Barrier modules. The Pressure module has three trimpots that affect the pressure calibration and offset, and the gain of the transducer. The area module has an LED display that displays pressure or area, depending on the setting of the togggle switch to the right of the display. Additionally, depressing the pushbutton to the left of the display switches the readout from 'MEASure' mode (current pressure/area displayed) to 'COMmand' mode (the pressure/area setpoint is displayed). The display on the barrier module shows a number proportional to the velocity of the moving barrier or the temperature of the probe in the subphase of the trough, depending on the setting of the toggle switch to the right. It contains the switches for moving the barrier manually or engaging constant pressure mode. The knob below the display determines the barrier speed.

Connect the trough control unit to power and connect all the cables from the trough. Use short coax cables from the cardboard accessory box to connect the Pout terminal from the Pressure module to the Pin terminal on the Area module and the Sout terminal of the Area module to the Sin terminal of the Barrier module. Now the control unit can read out the total area of the monolayer, the surface pressure and the temperature. To record pressure-area diagrams, interface the control box with the computer running Surf. The details are different for CMC CAT and X22B. At X22B, connect the Pout terminal to the digital multimeter (labelled GPIB 03) located above the computer terminal via the patch panel in the hutch. Similarly, connect the Aout terminal to the DMM labelled GPIB 05. The macro below will tell Surf how to read in the data. (Note that without a third DMM, there is no provision for reading in the temperature from the probe in the subphase. However, the NESLAB chiller can be computer-interfaced so that the bath temperature can be recorded. See Elaine Dimasi's notes for the chiller unit on her LSS documentation page.) At CMC CAT, the Pout, Aout and T terminals should be connected to voltage to frequency converters (VFC) in the B-Hutch and the output connected to scaler channels. See the information in the macros section for more details.

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Computer-Interfaced Control of the Trough


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Trough Calibration

Pi calibration The filter paper used as the Wilhelmy plate should be 3 mm wide and should extend approx. 12 mm from the hole for the hook. For a coarse, but generally reliable, calibration:

You may need to repeat the first few steps a couple times until you can achieve a consistent difference between paper in and paper out. Make sure that the paper is fully wet before you pull it out, and try and get the reading as soon as you pull the paper out of the water -- the reading changes as the paper dries out. The offset will be sensitive to the level of water in the trough. Once you have calibrated the surface pressure transducer, you can tweak the offset everytime you refill the trough without affecting the calibration. Conversely, you can add or remove subphase until the offset is about zero and so ensure that you are consistently filling the trough to the same level. This simple calibration procedure is described in greater detail by the manufacturers in their instruction sheet for the balance head.

Generally speaking, this calibration is sufficient. You may want to test things out by taking an isotherm of a standard substance, like arachidic acid.

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Area calibration It is possible to adjust the offsets of the electronics so that the area signal is proportional to the total area of the trough, but the procedure is cumbersome. It is more convenient to set the calibration in the software instead. Both troughs are exactly 16 cm wide. Use a ruler and measure the distance from the barrier to the front end of the trough for two different points and record the voltage of the area signal at each position. The area signal is very linear with barrier position, so from the two points you can derive the slope and y-intercept of the line through the two area-voltage pairs.

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Temperature calibration isn't really necessary for the probe in the subphase. The analog signal from the control unit is the temperature divided by ten (20 deg=2.0 V). At CMC CAT in config mode make sure that the scale factor is set appropriately. At X22B without a third DMM there is no way to record the temperature reading.

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Constant Pressure Mode

The constant pressure mode of the trough controller allows you to compress the monolayer to a set pressure (or area) that you determine and then maintain the monolayer at that pressure (or area). (The area control is intended for different troughs with two moving barriers.) To set the target pressure (0) check that the toggle switch at the bottom of the middle module (modus) is in the P position; (1) look at the LED display on the moddle module and make sure that the toggle switch on the right side is set to pressure (P); (2) depress the pushbutton (com/measure) to the left of the display; the LED display now shows the target pressure; (3) turn the knob at the lower left of the display (P/A command) until the desired target pressure is displayed. To engage constant pressure mode (1) check that the toggle switch on the right side of the right module (mot stop) is in the up position and the LED is lit; (2) put the three-way toggle switch on the left side of that module (exp auto comp) into the auto position; (3) as soon as you toggle the (mot stop) switch to the down position, the monolayer will be compressed until the target pressure is achieved. The Gain knob on the middle module controls the characteristics of the feedback loop that moves the barrier. To disengage constant pressure mode toggle the mot stop switch to the up position and stop the barrier motion, or put the three-way switch into the exp or comp position, which will immediately start expanding or compressing the monolayer.

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Isotherm Macros

global  PRESSURE        # last pressure reading  			
global  PRESSURE_SLOPE  # linear coefficient for pressure reading	
global  PRESSURE_OFFSET # constant term for pressure reading	
global  AREA            # last area reading			
global  AREA_SLOPE      # linear coefficient for area reading	
global  AREA_OFFSET     # constant term for area reading	
global  DEGC            # temperature				
global  ISO_GROUP       # group number for isotherm data (choose 7)

PRESSURE_SLOPE = 10							
PRESSURE_OFFSET = 0							
#####March 2001 values for correctly calibrated trough (readout		
#####on control unit is accurate					
AREA_SLOPE = 109.7							
AREA_OFFSET = -1.2464							
ISO_GROUP = 7								

def getpia '								
        PRESSURE=gpib_get(3)*PRESSURE_SLOPE+PRESSURE_OFFSET		
        AREA=gpib_get(5)*AREA_SLOPE+AREA_OFFSET				
        '								

def press '								
        getpia								
        print "Pressure = ", PRESSURE, "\tArea =", AREA			
        '								

#measure1 is called from the "scan_loop" in the standard macros		
def measure1 '								
        getpia								
        '								

def iso_Fheader '_cols += 3;printf("#X %gKohm (%gC)\n", TEMP_SP,DEGC_SP)'  
def iso_Plabel  'sprintf("%7.7s %7.7s %8.8s ","Area","T-degC","Pressure")' 
def iso_Pout    'sprintf("%7.5g %7.5g %8.5g ",AREA,DEGC,PRESSURE)'	    
def iso_Flabel  '"Area  DegC  Pressure  "'				
def iso_Fout    'sprintf("%g %g %g ",AREA,DEGC,PRESSURE)'		
def iso_Ftail   ''							

        rdef Fheader "iso_Fheader"					
        rdef Plabel  "iso_Plabel"					
        rdef Pout    "iso_Pout"						
        rdef Flabel  "iso_Flabel"					
        rdef Fout    "iso_Fout"						
        rdef Ftail   "iso_Ftail"					

# this macro stuffs the scan data at each point of the scan		
# 9/26/98  Put in commands to fix plotting ranges--seems to work.	
def isoplot '								 
	_sx = _sx * 1.16 - 0.4						
        _fx = _fx * 1.16 - 0.4						
        data_put(ISO_GROUP, NPTS, 2, AREA)				
        data_put(ISO_GROUP, NPTS, 3, DEGC)				
        data_put(ISO_GROUP, NPTS, 4, PRESSURE)				
        X_L = "Area"							
        Y_L = "Pressure"						
	'								

def iso ' def _cleanup3 \' PL_G = 0 PL_X = 0 PL_Y = 1 rdef scan_plot "_plot" \' rdef scan_plot "isoplot ; _plot" data_grp(ISO_GROUP, 4096, 5) PL_G=ISO_GROUP PL_X=2 PL_Y=4 ascan sh A[sh] A[sh] 4000 1 '

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User notes for the CMC CAT Langmuir trough / Revised August 2005 / send comments to strzalka@sas.upenn.edu