a short user manual for the liquid surface
Contents
1. 2 5 21 1 scan of the monochromator height 3 gt ptzm midp 4 gt remo tz2 t2he 5 gt remo tz3 70 70 is the parkPSD position 6 gt prsc 0 7 gt ssli 1 5 1 5 21 1 slit scan 8 gt ssls MIDP SH2 move sH1 to midp and leave sH2 where it is 9 gt smon tzi tzi 1 tz1 1 21 1 10 gt tzl midp 11 gt remo tzi tihe remo rol tiro Maybe 12 gt prsc 1 13 gt saux tzs tzs 0 25 tzs 0 25 26 5000 tzs midp or press F2 14 gt remo tzs sahe Maybe 15 gt saux tz2 tz2 1 tz2 1 21 5000 tz2 midp or press F3 16 gt tz2r midp 17 gt ptz2d 18 gt ro2 ro2 19 gt saux tz2 tz2 1 tz2 1 21 5000 Or press F3 20 gt tz2d midp 21 gt tzs tzs 2 tz2 tz2r ro2 ro2 cout INote that here the scan limits are exceptionally given relative to the present positions instead of as absolute positions June 14 2006 17 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 22 gt QTRU 1 23 gt qpri QTRUE O qpri 0 85 0 24 gt qcap qtrue 0 The QTRUE value should be equal to 0 85 0 03 If not do gt qi 0 85 qtoa and go back to saux tzs and repeat the procedure from there June 14 2006 calculate QTRUE REMOing according to QTRUE 18 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 9 description of some motors Motor movements can be directly carried out using the following syntax gt mot2. krkj BW1 BW1 liquid surface manual pdf 4 starting a new sample The tascom data files begin with two lines of text One of the text lines is meant to be a descriptive comment that can be set with gt dfit comment gt log dfit to log the text Further gt spread will ask for spread volume concentration in mg mL or Molar and molar mass or just the number of molecules spread gt lspr to log the spread values gt comm to type in a further description comment gt tls 15 to translate the sample across the beam fi gt new monolaver to achieve all of the above 5 measuring an isotherm To measure an isotherm use gt isot 0 5 You can also use isox to additionally record the oxygen concentration in the trough compartment at the same time or isotxi to further also repeat counting To plot the data use the programs gnuplot or idl 4 In gnuplot gt pl lenbi234 dat u 6 2 w 1 or gt pl lt tda lenb2345 dat AMOL PI_SURF w 1 In idl idl gt tapl ctasrd lenb1234 dat Amol Pi psym 0 or better idl gt pliso ctasrd lenb1234 dat or 4Note that these and most other linux commands must be typed in lower case By contrast tascom idl and gnuplot will accept either case except when referring to names of file to be supplied by the linux file system Shttp www fys ku dk krkj IDL_stuff June 14 2006 6 http www fys ku dk krkj BW1
3. Alu atten not used in the present set up M monochromator S sample Aux PSD are detectors Not a motor Movement implemented by means of motors RO1 TZ1 resp RO2 TZ2 resp RO3 TZ3 June 14 2006 21 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 10 Appendix Perl scripts bv Markus Wevgand The perlscript ct2gpl helps to deal with reflectivitv data inside or ouside gnuplot In a shell it prints the result to standart output that is your terminal and you may pipe to other tools or directly into a file you want to generate It wants the prefix of your current data names e g lenb otherwise it takes a default one which is likely not the one you are currently using Additionaly you have to supply at least one number of a data file that contains reflectivity data e g 3456 You may provide two in this case ct2gpl regards the second number as the last file in a sequence of reflectivity mesasurents the containing reflectivity data not the background data which is usually the file following If you must subtract backround from your data file you have to use the option b and ct2gp1 calculates background corrected data In the case there are fewer background data points than data point it does linerly interpolate background data points Use the option p to cut out data points that are measured too fast by the detector Sometimes you may not have reflectivity and background data as two files in a sequence
4. BW1 liquid surface manual pdf idl gt iterate pliso ctasrd lenbi234 dat or idl gt pliso ctasrd lenbi1234 dat hc to get a hard copy June 14 2006 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 6 reflectivitv scan To move all the motors and the detector to their home position i e the same as q1 0 85 q2 0 qtoa go vert in reflection mode use gt go home To save the sample from beam damage vou mav decide to move the trough across the beam motor TLS between parts of the reflectivitv scan pref attempts to do this automaticallv For a new monolaver set tls back to 15 In this way you will have the maximum space for movement of the trough To do this use gt tls 15 that is part of the command gt new_monolayer After changing the gas in the trough cannister you need to remeasure the normalization constant with gt mkiOO One way to start a reflectivity scan is by gt piba The macro piba calls the macros pexs x ray scan with indirect detector and pref x ray scan with direct detector The macro pref requires the parameters qstart qend qzstep spres maxdosis and qzstepm see file command main piba tas where qzstep is the initial step width spres the initial detector counts maxdosis the maximum dose before moving the trough and qzstepm the maximum step width in qz Note q values are expressed as multiples of Qc You can change the parameters in the file piba
5. and thus want specifically to specify data and background file numbers This is easily done by using the option m and providing the data file and background number Furthermore option a preserves units of critical angle and f normalizes output to fresnel reflectivity For an overwiev of more options you may type ct2gpl h In a more general context another perlhack tasrd provides you save acces ct2gpl is also save i e it does not rely on a specific column number where to fetch its input to tascom data file columns Lets say if you want to look just in a reflectivty data file you may type tasrd s Q1 REFL SREF wolb0764 dat or looking at a isotherm you are recording by TASCOM you may use tasrd s AMOL PI_SURF wolb0440 dat You can access header parameter instead of data columns by choosing the option p fx tasrd s TEMP p wolb0764 dat gives you the temperature TASCOM recorded during the scan June 14 2006 22
6. prints the current state of the oxygen content on the screen every 10 sec The macro will stop when the oxygen content is less than 0 3 Alternatively the commands gt isox or gt isotxi record the surface pressure and area and the oxygen concentration in the trough container For the diffraction scan of 2TL there are two macros you may want to use gt ttlm From To NoOfPoints Monitor_preset gt ttlt From To NoOfPoints Monitor_preset mm_per_100kMonitor The commands execute a scan with the position sensitive detector ttlt additionally translates the sample under the beam so that fresh spots of the sample are exposed to radiation The parameters necessary to calculate the Qz value from the channel number in the PSD file are given in the data file headers x THTO critical angle in DEG i e the position of the Vineyard peak VCHA the number of the corresponding channel SLOP PSD channels per DEG These macros remove any absorber thicker than AL1 0 2 mm from in front of the sample To exceptionally scan with thicker absorbers use ttln Here is an example of a ttit scan gt ttlt 18 16 81 1e5 0 1 If you want to extend a GIXD scan or any other scan use the command TNote that all 2TL are negative numbers 8given for ExAn3 4 5 DEG for historical reasons Hence for ExAn3 6 you should observe the Vineyard peak in channel VCHA SLOP 1 5 June 14 2006 11 http www fys ku dk krkj BW1
7. tas To get an overview of the parameters used type pref_para The command gt ql 0 85 q2 0 qtoa calculates inan and exan according to q1 q2 calculates corresponding target values for all the motors concerned and moves the the motors accordingly To plot the reflectivity scan consisting of two data files in the above example you can use gnuplot or idl In gnuplot type Vv pl lenb3456 dat u 6 2 3 we Vv repl lenb3457 dat u 12 4 5 we or Vv pl lt tda lenb3456 dat q iof siof we gt repl lt tda lenb3457 dat q iof siof we June 14 2006 8 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf In idl tvpe idl gt pwd idl gt cd lenb if required idl gt 1enb3456 3457 makerefl lenb 3456 3457 maxrate 12000 purge write and idl gt plotrefl lenb3456 3457 or idl gt plotrefl ctasrd lenb3456 ctasrd lenb3457 Other macros which you can use are gt go vert mi m2 m3 m4 m50 gt go dir m6 m7 m8 m8 m9 m100 these record the reflectivity measurement for the following ranges scan ml m2 m3 m4 m50 m6 m7 m8 m9 m100 m110 m120 q range 0 5 1 2 Qe 1 1 1 8 Qc 1 4 2 2 Qe 1 93 5 Qe 3 6 5 8 Qe 05 09 Qc 08 15 Qc 12 22 Qe 17 26 Qe 27 35 Qc 36 42 Qe 43 47 Qe Ib m110 angles 0 06 0 16 DEG 0 14 0 23 DEG 0 18 0 28 DEG 0 25 0 45 DEG 0 47 0 75 DEG 0 65 1 16 D
8. the trough one can easily happen to offset the rotation of AL1 since the holding torque of the motor is weak Only visual inspection of the orientation of the aluminium absorber wheel will reveal such an offset June 14 2006 20 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 9 1 movements of the horizontal scattering diffractometer 3 hum SIN g are C Vertical Incidence Angle to Sample M S PI arm Rotation M S N 2TM INAN RO1 Z1 PI arm Vertical Translation M S Vertical positions of slit 1 Vertical positions of slit 2 S S N 2 S OMS H m Horizontal Translation Floor Sample Rotation H N Vertical Translation H a H H TF TZ TU TL T T Q mn a lux e rf mh H 3 F gt amp U L 4 b S GUS GLS Q 1 S S 2TL 2TU EXAN EXAN3 D mm mm Deg Deg Deg eg eg eg eg mm mm mm m eg mm mm m m mm eg eg eg eg mm eg eg mm D D fee om ized S mm Lower Translation fs Upper Goniometer arc not present eed mm e s Horizontal Lower arm Rotation S PSD Horizontal Upper arm Rotation D D D Vertical angle from Sample to middle of PSD S PSD E ET M S Anx iu eee Q J w a 8 i S i S jati g ati S S Vertical Exit Angle from Sample PI arm Rotation S Aux PI arm Vertical Translation 1 a MOL ener ALI mm Alu Alu atten before beam monitor L AL2 mm Alu Additional
9. BW1 liquid surface manual pdf gt reopen f 1 to cause the next scan to be appended to the current data file At low angles vou should change the horizontal width S3Ho of the slit behind the Soller collimator to reduce background scattering The upper software limit u2t1 which prevents the PSD from being exposed to the direct beam should also be increased from 2 6 at S3Ho 10 to 0 5 at S3Ho 1 This is all taken care of by the command set_S3Ho that will ask for S3Ho In fact merely assigning S3Ho lt VALUE gt is a mistake cf page 19 So doing will have no effect other than confusing the user S3HO angle range upper limit u2tl gt set_S3Ho 10 wide 2 6 gt set S3Ho 3 small 1 3 gt set S3Ho 2 small 0 9 gt set_S3Ho 1 small 0 5 June 14 2006 12 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf To plot the GIXD results use idl idl gt cd lenb idl gt lenb5678 cppsd 1lenb5678 update 5 idl gt ppsdget lenb5678 upd 5 To print the scan results use idl gt domp lenb5678 idl gt domp correct lenb5678 idl gt domp realq correct lenb5678 If you want to return to reflectivity mode type gt go refl Alternativelv gt tzss can be used in between diffraction scans It does essentiallv gt go refl gt saux tzs gt tzs midp gt go_difr June 14 2006 if required or 13 http www fys ku dk krkj BW1 BW1 liquid surface m
10. EG 1 03 1 94 DEG 1 55 2 85 DEG 2 20 3 37 DEG 3 50 4 55 DEG 4 68 5 48 DEG 5 61 6 14 DEG m120 for the vertical detector for the direct detector attenuator AL1 0 8 0 6 0 4 0 2 0 0 0 8 0 6 0 4 0 2 0 0 0 0 0 0 From m7 onwards a background is also measured and stored in a separate data file After m100 you can continue with m110 m120 18 data files in the above example you can use gnuplot or idl In gnuplot type gt pl lt ct2gpl r lenb a f p 3456 u 1 2 3 we if you still have signal To plot the reflectivity scan consisting of 14 to gt repl lt ct2gpl r lenb a f p 3457 u 1 2 3 we gt repl lt ct2gpl r lenb a f p b 3458 u 1 2 3 we 6cf Appendix 10 June 14 2006 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf gt pl lt tasrd s Q1 IOF SIOF lenb3456 dat u 1 2 3 we In idl type idl gt cd lenb idl gt lenb3456_3469 makerefl lenb 3450 6 7 8 9 10 11 3450 12 13 14 15 16 17 18 19 maxrate 12000 purge write idl gt plotrefl lenb3456 3469 June 14 2006 if required and 10 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 7 diffraction scan To move the setup to diffraction mode gt go difr For diffraction measurements you may want to flush the trough with helium Check the oxygen content in the trough with gt poxy The command gt wait_oxy
11. a is fa 60 Oy SAN alee A B B qa PA A eee 8 3 alignment of the slits on the incident beam V L 8 4 alignment of the detector 1 0 0 a 8 5 a complete vertical alignment 0 0 00 00 0000 000000020008 9 description of some motors 9 1 movements of the horizontal scattering diffractometer 2 000 10 Appendix Perl scripts by Markus Weygand June 14 2006 11 14 14 14 14 15 17 19 21 22 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 1 preamble This document supplements and to some extent duplicates the general manual for the tascom language and associated hardware The emphasis of the present document is on how one mav go about performing a subset of the experiments that are possible bv means of the BWI liquid surface diffractome ter Readers should first read the general tascom manual 2 login and startup The BWI horizontal surface diffractometer is controlled bv the program TASCOM Triple Axis Spec trometer COMmands which runs on a Linux system hastasbwl desy de Tascom is an interpreter of commands that are given by the user or read from tas files in the tascom command main directory and specified subdirectories Commands can be either native tascom commands e g an order for a motor move or an assignment to a variable or command files To login on hastasbwi use Username tascom Password To start the program tascom use
12. anual pdf 8 alignment 8 1 alignment procedures The alignment procedures consist of two parts A scan of a motor and its subsequent repositioning Scans are of the general type gt smon Motor From To NoOfPoints PRES to scan a motor and plot MON or gt saux Motor From To NoOfPoints PRES to scan a motor and plot AUX or gt si Motor From To NoOfPoints PRES to scan a motor and plot I Whether or not a good peak is found during the scan a peak analysis is automatically attempted and the variables midp and fwhm contain the resulting midpoint and full width at half maximum It is up to you to decide in each case whether the resulting values are meaningful or misleading The command gt motor midp moves the motor to the so computed midpoint 8 2 sample alignment Do not forget to check the sample height To scan the sample height use gt prsc 1 saux tzs tzs 0 25 tzs 0 25 26 5000 tzs midp This command is stored in function key F2 As you can see the range of this scan is calculated relative to the present motor position It may be that a coarse alignment with the joystick is necessary first Move to the new sample height with gt tzs midp Depending on circumstance you may decide to gt remo tzs sahe 8 3 alignment of the slits on the incident beam The command gt slpo June 14 2006 14 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf writes the sli
13. ctor arm gt saux tz2 tz2 1 tz2 1 21 5000 tz2 midp Or press F3 gt tz2d midp The variable tz2d now contains the actual position of the direct beam This too is needed to determine the actual incident angle with respect to the horizontal Now move the sample back into the beam and the detector to look at the reflected beam gt tzs tzs 2 tz2 tz2r ro2 ro2 cout gt QTRU calculates from the height difference tz2d tz2r and the detector to sample distance LEN4 the actual incident angle with respect to the horizontal QTRUE is in units of Qc QO gt qpri QTRUE O qpri 0 85 0 prints the calculated and actual motor positions for the actual incident angle QTRUE and for the nominal incident angle Q1 0 85 and Finally if you are sure you know what you are doing gt qcap QTRUE O This is the critical command in the alignment where the zero positions of all motors are REMOed This command expects that all motors are in their optimal positions in the reflection geometry as determined by the previous scans No individual motor remo commands are necessary Now the diffractometer is ready for reflectivity measurements June 14 2006 16 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 8 5 a complete vertical alignment Be careful these commands move a lot of motors Understand what goes on and consider how much of this needs to be done 1 gt qi 0 85 qtoa 2 gt rtzm 2 5
14. http www fys ku dk krkj BW1 BW1 liquid surface manual pdf A SHORT USER MANUAL FOR THE LIQUID SURFACE DIFFRACTOMETER AT BEAMLINE BW1 in HASYLAB AT DESV by Jens Pittler lt jpitt physik uni leipzig de gt with some modifications by Kristian Kj r lt kristian kjaer nbi ku dk gt University of Leipzig Soft Matter Physics Dept Leipzig Germany Niels Bohr Institute University of Copenhagen Denmark E l XR A d a q 2ksina R 4 Re ae js a eras k monolayer ji subphase aq k k a k jA D2 D1 qz sina sin ar ksinar erase Rod Tene gz x T ap bi Fae qz hk E hk dzy ky cos ay cos ap 2 cos o cos ar COS 20 1 ky 1 cos ar 2 cos 04 cos 20 1 2k sin 20 Order a ji LEE gq K sina sina 5 i ksinar Nal A1 Beam sox Monit a er lt Monochromator Monochromatieffil Beam C speculariv reflected Intensity N T R Jensen and K Kjaer p 205 254 in Cc Novel methods to study interfacial layers ww Studies in interface science 11 Elsevier 2001 June 14 2006 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf Contents 1 preamble 2 login and startup 3 some useful main commands 4 starting a new sample 5 measuring an isotherm 6 reflectivitv scan 7 diffraction scan 8 alignment 8 1 alignment procedures 0 00 827 Sami ple alignments o
15. pska last_bwi 2 pdf June 14 2006 4 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf 3 some useful main commands gt shut gt open gt go home gt go refl gt go difr gt go vert gt go_dir gt new_monolayer gt all 0 8 gt ql 0 85 q2 0 qtoa gt qc 0 021764 q0 qc gt lt Variable gt gt PRES lt VALUE gt gt PRSC lt VALUE gt CONTROL C June 14 2006 closes the mini shutter to save the sample from beam damage opens the mini shutter to move to the home position i e the same as gt qi 0 85 q2 0 qtoa go_vert to move to reflection mode to move to diffraction mode to use the indirect vertical detector in reflection mode to use the direct detector in reflection mode to make a comment in the log print assign dfit and move tls back to 15 sets the aluminium absorber 0 8 mm is the maximum value used moves motors to incident and exit angles inan exan 0 85 thtc 0 1099 DEG for lam 1 3037 A i e to a vertical vector of length 0 85 QO are the values for a pure water subphase prints the value of Variable on the screen assign the pre set counting limit select the type of counting prsc 0 Counting for PRES seconds prsc 1 Counting up to PRES monitor counts prsc 2 Counting up to PRES counts in the I detector the PSD prsc 3 Counting up to PRES counts in the AUX detector interrupt a scan or movement http www fys ku dk
16. t positions of incident beam SH1 SH2 the heights of the slits given by the motor positions of TZ1 and RO1 and L1 L2 the distances from the monochromator to the slits gt ssli 1 5 1 5 16 1 scans monitor counts so a fixed time gt PRSC 0 is used versus the absolute vertical position of slit 1 This requires combined movement of TZ1 and RO1 so no simple motor scan can be used gt ssls midp sh2 moves slit 1 to the center of the peak and keeps slit 2 at its position gt smon tz1 tzi 1i tzi 1 21 1 scans the vertical height of the monochromator arm relative to its present position gt tzl midp puts slit2 in the center of the beam gt cout counts and outputs prints the result 8 4 alignment of the detector Alignment of the rotation of the detector arm gt saux ro2 ro2 0 4 ro240 4 17 5000 gt ro2 midp cout Alignment of the height of the detector arm gt saux tz2 tz2 1 tz241 21 5000 tz2 midp This command is stored in function key F3 gt tz2r midp The variable tz2r now contains the actual position of the reflected beam This is needed to determine the actual incident angle with respect to the horizontal Moving TZ2 to the expected position of the direct beam and the sample TZS 2 mm down gt ptz2d gt ro2 ro2 gt cout June 14 2006 15 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf The detector now looks into the direct beam Alignment of the height of the dete
17. the command tascom if tascom is not already running Otherwise locate the window with the running instance of tascom Before you do any scans you must set your own data directory To set the data directory use gt data_dir lt DIRECTORY gt All data filenames are ASCII files and end with dat the file names are constructed from a root string and a segment number The variables involved are data_dir fina and segn The convention at BW1 is to use systematic names 9 gt data dir aprjun2004 lena fina lena segn 0 Or gt data dir aprjun2004 lenb fina lenb or gt data dir aprjun2004 lenc fina lenc Thus the data file names will be composed of four letters and a four digit number With gt segn lt NUMBER gt lnttp www risoe dk afm external pska last_bw1 2 pdf nttp www risoe dk afm external pska Tascom_manuals htm June 14 2006 3 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf you can specify the starting number of the first file Set segn 0 only before the first scan in a run as in the example given for lena SEGN is automatically incremented with each scan With the command gt dfit lt Comment gt you can define a comment that is added to the header of each file With the command gt log any text you can write anv text on the log printer Set dialog 1 logp 1 and logF 1 cf the tascom manual Shttp www risoe dk afm external
18. value where mot is a motor name from the following table and value is any real number These motor positions can also be used as variables in calculations By contrast assignment of non motor variables causes no action the value is merely stored In the case of the variables sH1 sH2 Q1 Q2 InAn ExAn ExAn3 and S3Ho that in fact represent motor movements this will not be what you want For some action motor movement to occur a command must additionally be given Examples are gt sHi midp sH2 sH2 Wrong gt SIPo midp sH2 Right gt gt S3Ho 3 Wrong gt set_S3Ho 3 Right gt gt ExAn3 12 Wrong gt ARDX 12 Right gt gt Q1 0 85 Q2 0 A mistake most probably gt Q1 0 85 Q2 0 QtoA Right gt gt InAn 0 109964 ExAn InAn A mistake most probably gt InAn 0 109964 ExAn InAn Atoq Right The motor AL1 aluminium absorber wheel is in a sense a special case Assignments such as gt AL1 0 8 or gt AL1 0 0 cause the motor to move to the expected aluminium absorber thickness in mm Such is the calibration of this motor However as inspection of the device should convice the reader assignments such as gt AL1 0 75 or gt AL1 0 1 June 14 2006 19 http www fys ku dk krkj BW1 BW1 liquid surface manual pdf will not give the corresponding absorber thicknesses Concerning AL1 though completely unrelated to the issues discussed above note that working with
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