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SUL-X Beamline

The X-ray beamline of the Sychrotron Laboratory for Environmental Studies (Synchrotron Umwelt-Labor) combines diffraction, absorption and fluorescence measurements on environmentally relevant materials with microfocusing capabilities.

Sources of pollution, path of contaminants, and the contribution of synchrotron radiation based techniques via Molecular Environmental Science (MES) to enviornmnetal questions are the main tasks of this beamline.
Umwelt

 

 

The SUL X beamline is major part of the Synchrotron Laboratory for Environmental Studies supported by the German governments (BMBF and state Baden Württemberg) for dealing environmental questions with synchrotron radiation methods. Therefore this beamline is designed for combined measurements with a microfocusing capability.

Initially utilising a wiggler source the beamline will be upgraded at a later date with a superconducting undulator.

Environmental samples are generally complex (e.g., contaminated soils, mining dump sediments), consisting of mixtures of mineral phases (amorphous, crystalline, with micrometer or nano-scale particle sizes), microbes, and in some cases vegetable material. Spatial distribution, speciation, and phase association of trace levels of contaminants are the basis for risk assessment and development of remediation strategies (e.g. arsenic speciation and distribution in groundwater related sediments). This problem is best addressed by synchrotron based techniques capable of providing spatial resolution in the micrometer range while allowing the combination of microfocused techniques (XRF, XAS, XRD, IR), as foreseen in the SUL concept.

Team SUL-X
name title function area of activity e-mail
Ralph Steiniger Dr. Beamline Scientist - SUL-X Hard X-ray Spectroscopy ralph steiningerVmx4∂kit edu
Jörg Göttlicher Dr. Beamline Scientist - SUL-X Hard X-ray Spectroscopy joerg goettlicherEcn7∂kit edu

SUL-X Beamline

SUL-X

Schematic Beamline Layout

      

Optic components

 Bilder-SULX-webpage-Optik-M1  Bilder-SULX-webpage-Optik-M2uDCM  Bilder-SULX-webpage-Optik-KBM
Front-End with first, horizontal, focusing mirror (M1) First part of the otic hutchwith double crystal monochromator (DCM) and second, vertical, focusing mirror (M2)

End of the optic in experiemntal hutch with the Kirckpatrick -Baez mirror system (KBM)

Experimente an der SUL-X Beamline

Experimental station - 3D model (under construction)


 Messplatz


SUL-X21


Experimental station - Detectors


   Detector  Type  Main specification
 D1  Fluorescence 7 element Si(Li) (Gresham, now e2v)

Resolution (averaged over all elements, optimum peaking time):
<140 eV (at 5.9 keV, 1000 cps)
<310 eV (at 5.9 keV, 100.000 cps)

Area per element 30 mm2

 D2  Absorption 3 ionisation chamber (Oxford Instruments, IC-Plus type)  Active lenght 5cm, Kapton windows 6 µm thick
 D3  Diffraction CCD detector (Photonic science)

Active area 80x120mm2 (hor. x vert.)

Fiber optic 3.46:1 scaling down pixels 2048x2048, 16 bit dynamic through fusion mode

Readout time 3.3s – 21s
Vacuum compatible

 D4  Selection of sample spots Optical microscope (TSO Spezialoptik)

Resolution 2µm,

Transmitted and reflected light, Vacuum compatible



Experimental station - Sample stage

   Movement  Range
 S1  z stage  105 mm
 S2  x/y stage  100mm / 40mm
 S3  phi circle  360°
 S4  chi cradle  10°
 S5  theta circle 360°
 S6  2 theta circle   -160° to +15°

 

 

 

 

 

 

 

 

 

 

 

7 Element Si(Li) fluorescence detector (Gresham)

detectorintestdetector  

 

In-vacuum CCD detector (Photonic Science)

139_3948cc
CCD-Detector-SeitenansichtAnschluesse-139_3950cc
 

 

Available Methods, Obtainable Parameters

The SUL X-ray beamline closes the spectral gap between soft and hard X-ray spectroscopy, and offers to investigate samples - without remounting them - sequentially
with the following methods and modes:

Fluorescence Spectroscopy:

  •     elemental mapping of an extended sample :e.g. thin section of a contaminated soil sample
        (microfocused beam size mode)
  •     high sensitivity to low concentrations (primary “white light” beam with its high flux mode)


Absorption spectroscopy for all elements between S(Al) and U:

  •     information about the local atomic geometry (EXAFS)
  •     chemical state of the absorbing atom (XANES)
  •     investigations on ordered (crystalline) and disordered (amorphous, liquid) materials
  •     dilute species and light elements (fluorescence mode of XAS)


Diffraction experiments (powder and aggregates of crystals):

  •     location of pollutant atoms within a crystalline mineral matrix
  •     investigation of sample concentrations, chemical states of elements and their associations
        mineral phases
        down to the μm scale
  •     essential key parameters for environmental and health risk assessment

Advantages

  •     Nondestructive, Surface / volume sensitive
  •     Three X-ray techniques with microfocus without sample remounting
  •     Spectroscopy from light elements S(Al) to U at a single beamline


Purpose, summarized

  •     Environmental science, material science, biology
  •     Focus on inhomogeneous, complex samples
  •     Spatial element distribution, speciation, and mineral phase determination

 

Key parameters of the beamline

Energy range

2.3 kev - 19 keV (S K-edge, U L3-edge), later 1.4 keV (Al K-edge)

Energy resolution (DE/E)

Si(111) 2x10-4; Si(311) 1x10-4; YB66(004) 5x10-4;

 

(theoretical values) 

Source

Wiggler (27 pole each 74 mm), later upgrade undulator (100 pole each 14mm)

Optics (sorted in beam direction)

Toroidal mirror, horizontally focusing, vertically collimating

DCM with Si(111), Si(311), YB66(400) and mirror (white light)

Cylindrical mirror with three coatings, low energy band path, vertically focusing

Precise slit in focus, defining a “new” source with adjustable size

Elliptical Kirkpatrick Baez mirror system, focusing “new” source

Monochromatic or “white light” beam path, selectable.

Beam size at sample position

1 mm (hor) x 1mm (vert) down to 30 µm x 25 µm

(later down to 10 µm x 10 µm)

Flux at sample position

4 x 1010 (5keV), 3 x 1010 (10kev), 3 x 1010 (20keV) ph/s / 100mA e- current in spot size (FWHM) 0.2 mm (hor) x 0.1 mm2

Experimental station

 

Sample diffractometer with theta, phi circle and chi cradle (10°), xyz linear stages

CCD detector on 2theta arm for diffraction

3 retractable ionization chambers for absorption

7 element Si(Li) fluorescence detector for fluorescence

Optical microscope

Diffractometer and detectors all in vacuum vessel

Sample environment

Chambers for different environments (gases, liquids, T-controlled) are planned; low temperature environment down to -5 °C (small samples, peltier cooled), and down to -20 °C (flat samples, N 2 cryostream) available.

 

Publications since 2010
Title Author Source Date Link

A. Fiege, H. Behrens, F. Holtz, F. Adams 

Geochimica et Cosmochimica Acta 125, 241–264 

2014 PDF

I. Jerzykowska, J. Majzlan, M. Michalik, J. Göttlicher, R. Steininger, A. Błachowski, K. Ruebenbauer

Chemie der Erde - Geochemistry 74, 393-406

2014

PDF

J. Morales, J. M. Astilleros, A. Jiménez, J. Göttlicher, R. Steininger, L. Fernández-Díaz 

Applied Geochemistry 40, 89-96 

2014 PDF

S. Paikaray, J. Essilfie-Dughan, J. Göttlicher, K. Pollok, S. Peiffer 

Journal of Hazardous Materials 265, 208-216 

2014 PDF

A.Voegelin, R. Kaegi, M. Berg, K.S.Nitzsche, A. Kappler, V.M. Lan, P.T.K. Trang, J. Göttlicher, R. Steininger

Environ. Chem. 11, 566-578

2014

PDF

B. D. Belviso, F. Italiano, R. Caliandro, B. Carrozzini, A. Costanza, M. Trotta 

BioMetals 26, 693-703 

2013 PDF

R. M. Bolanz, M. Wierzbicka-Wieczorek, M. Čaplovičová, P. Uhlík, J. Göttlicher, R. Steininger, J. Majzlan 

Environ. Sci. Technol. 47, 9140-9147 

2013

PDF

J. Czapla, W. M. Kwiatek, J. Lekki, J. Dulińska-Litewka, R. Steininger, J. Göttlicher 

Radiat. Phys. Chem. 93, 154-159 

2013 PDF

J. Czapla, W. M. Kwiatek, J. Lekki, A. Kisiel, R. Steininger, J. Goettlicher 

J. Phys.: Conf. Ser. 430, 012040 

2013 PDF

M. Fischer, D. N. Thomas, A. Krell, G. Nehrke, J. Goettlicher, L. Norman, K. M. Meiners, C. Riaux-Gobin, G. S. Dieckmann 

Antarctic Science 25, 421-432 

2013 PDF
P. Gamaletsos, A. Godelitsas, E. Dotsika, E. Tzamos, J. Göttlicher, A. Filippidis The Handbook of Environmental Chemistry, DOI 10.1007/698_2013_230   2013 PDF

J. Goettlicher, A. Kotelnikov, N. Suk, A. Kovalski, T. Vitova, R. Steininger 

Z. Kristallogr. 228, 157-171 

2013 PDF

E. Hiller, M. Petrák, R. Tóth, B. Lalinská-Voleková, L. Jurkovič, G. Kučerová, A. Radková, P. Šottník, J. Vozár 

Environ. Sci. Pollut. Res. 20, 7627-7642 

2013 PDF

D. Issenmann, S. Ibrahimkutty, R. Steininger, J. Göttlicher, T. Baumbach, N. Hiller, A-S. Müller, A. Plech 

J. Phys.: Conf. Ser. 425, 092007 

2013 PDF

S. P. Kilias, P. Nomikou, D. Papanikolaou, P. N. Polymenakou, A. Godelitsas, A. Argyraki, S. Carey, P. Gamaletsos, T. J. Mertzimekis, E. Stathopoulou, J. Goettlicher, R. Steininger, K. Betzelou, I. Livanos, C. Christakis, K. Croff Bell, M. Scoullos 

Scientific Reports 3, 2421 

2013 PDF

S. Mangold, R. Steininger, T. dos Santos Rolo, J. Göttlicher 

J. Phys.: Conf. Ser. 430, 012130 

2013 PDF

S. Mangold, R. Steininger, T. Spangenberg 

J. Phys.: Conf. Ser. 430, 012022 

2013 PDF

O. Noked, A. Melchior, R. Shuker, T. Livneh, R. Steininger, B.J. Kennedy, E. Sterer 

J. Solid State Chem. 202, 38-42 

2013 PDF

V. Veselská, J. Majzlan, E. Hiller, K. Petková, L. Jurkovic, O. Ďurža, B. Voleková-Lalinská 

Applied Geochemistry 33, 153-164 

2013 PDF

T. Vitova, M. A. Denecke, J. Göttlicher, K. Jorissen, J. J. Kas, K. Kvashnina, T. Prüßmann, J. J. Rehr, J. Rothe 

J. Phys.: Conf. Ser. 430, 012117 

2013 PDF

L. H. E. Winkel, B. Casentini, F. Bardelli, A. Voegelin, N. P. Nikolaidis, L. Charlet 

Geochimica et Cosmochimica Acta 106, 99-110 

2013 PDF

S. Ziegler, K. Dolch, K. Geiger, S. Krause, M. Asskamp, K. Eusterhues, M. Kriews, D. Wilhelms-Dick, J. Goettlicher, J. Majzlan, J. Gescher 

The ISME Journal 7, 1725-1737 

2013 PDF

L. Bertrand, M. Cotte, M. Stampanoni, M. Thoury, F. Marone, S. Schöder 

Physics reports-Review section of physics letters 519 (2012) 51-96 

2012 PDF

R. M. Bolanz, J. Majzlan, L. Jurkovic, J. Göttlicher

Fuel, 94, 125

2012

PDF

N. V. Chukanov, S. M. Aksenov, R. K. Rastsvetaeva, D. I. Belakovskiy, J. Göttlicher, S. N. Britvin, S. Möckel

Novye dannye o mineralakh, 47, 33–42 (in English)

2012

N. V. Chukanov, D. A. Varlamov, F. Nestola, D. I. Belakovskiy, J. Göttlicher, S. Britvin, A. Lanza, S. Jancev 

Journal of Mineralogy and Geochemistry 189 (2012) 275-286 

2012 PDF

J. Czapla, W. M. Kwiatek, J. Lekki, R. Steininger, J. Göttlicher 

Acta Physica Polonica A 121 (2012) 497-501 

2012 PDF

A. Diener, R. Köppe 

Journal of Crystal Growth 349 (2012) 55-60 

2012 PDF

C. E. Farnsworth, A. Voegelin, J. G. Hering 

Environmental Science & Technology 46 (2012) 277-284 

2012 PDF

B. Lalinska, J. Majzlan, T. Klimko, M. Chovan, G. Kucerova, J. Michnova, R. Hovoric, J. Göttlicher, R. Steininger 

Canadian Mineralogist 50 (2012) 481-500 

2012 PDF

L. M. Och, B. Müller, A. Voegelin, A. Ulrich, J. Göttlicher, R. Steininger, S. Mangold, Vologina E.G., M. Sturm 

Chemical Geology 330 (2012) 244-259 

2012 PDF

S. Paikaray, J. Göttlicher, S. Peiffer 

Chemosphere 86 (2012) 557-564 

2012 PDF

I. V. Pekov, N. V. Chukanov, S. N. Britvin, Y. Kabalov, J. Göttlicher, V. Yapaskurt, A. E. Zadov, S. Krivovichev, W. Schüller, B. Ternes 

Mineralogical Magazine 76 (2012) 1133-1152 

2012 PDF

L. Shen, S.-W. Yang, S. Xiang, T. Liu, B. Zhao, M. F. Ng, J. Goettlicher, J. Yi, S. Li, L. Wang, J. Ding, B. Chen, S.-H. Wei, Y. P. Feng 

Journal of the American Chemical Society 134 (2012) 17286-17290 

2012 PDF

A. Tampieri, T. D'Alessandro, M. Sandri, S. Sprio, E. Landi, L. Bertinetti, S. Panseri, G. Pepponi, J. Goettlicher, M. Banobre-Lopez, J. Rivas 

Acta Biomaterialia 8 (2012) 843-851 

2012 PDF

M. West, A. T. Ellis, P. J. Potts, C. Streli, C. Vanhoof, D. Wegrzynek, P. Wobrauschek 

Journal of Analytical Atomic Spectrometry 27 (2012) 1603-1644 

2012 PDF

P. Gamaletsos, A. Godelitsas, T. J. Mertzimekis, J. Goettlicher, R. Steininger, S. Xanthos, J. Berndt, S. Klemme, A. Kuzmin, G. Bardossy 

Nuclear Instruments and Methods in Physics Research B 269 (2011) 3067-3073 

2011

PDF

A. Godelitsas, P. Nastos, T. J. Mertzimekis, K. Toli, R. Simon, J. Göttlicher 

Nuclear Instruments and Methods in Physics Research B 269 (2011) 3077-3081 

2011

PDF

J. Göttlicher, S. Marks, R. Simon, R. Steininger, A. Platte, S. Niggemann 

Mineralogical Magazine 75(3) (2011) 925 

2011

PDF

M. Kersten, T. Y. Reich, K. H. Liu, G. T. Schmidt, J. Goettlicher 

Soil Science Society of America Journal 75 (2011) 509-520 

2011

PDF

J. Majzlan, B. Lalinska, M. Chovan, U. Blass, B. Brecht, J. Goettlicher, R. Steininger, K. Hug, S. Ziegler, J. Gescher 

American Mineralogist 96 (2011) 1-13 

2011

PDF

F. Meirer, B. Pemmer, G. Pepponi, N. Zoeger, P. Wobrauscheck, S. Sprio, A. Tampieri, J. Goettlicher, R. Steininger, S. Mangold, P. Roschger, A. Berzlanovich, J. G. Hofstaetter, C. Streli 

Journal of Synchrotron Radiation 18 (2011) 238-244 

2011

PDF

S. Paikaray, J. Goettlicher, S. Peiffer 

Chemical Geology 283 (2011) 134-142 

2011

PDF

M. Saheb, D. Neff, C. Bataillon, E. Foy, P. Dillmann 

Corrosion Science 53 (2011) 2201-2207 

2011

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J. Stelling, H. Behrens, M. Wilke, J. Goettlicher, E. Chalmin-Aljanabi 

Geochimica et Cosmochimica Acta 75 (2011) 3542-3557 

2011

PDF

A. Al-Ebraheem, J. Göttlicher, K. Geraki, S. Ralph, M. J. Farquharson 

X-Ray Spectrometry 39 (2010) 332-337 

2010

PDF

N. V. Chukanov, J. Göttlicher, S. Möckel, Z. Sofer, K. V. Van, D. I. Belakovskiy 

New Data on Minerals 45 (2010) 17-22 

2010

PDF

G. S. Dieckmann, G. Nehrke, C. Uhlig, J. Goettlicher, S. Gerland, M. A. Granskog, D. N. Thomas 

Cryosphere 4 (2010) 227-230 

2010

PDF

K. Janssens, W. De Nolf, G. Van Der Snickt, L. Vincze, B. Vekemans, R. Terzano, F. E. Brenker 

TrAC Trends in Analytical Chemistry 29 (2010) 464-478 

2010

PDF

A. L. Soldati, J. Goettlicher, D. E. Jacob, V. Vicente Vilas 

Journal of Synchrotron Radiation 17 (2010) 193-201 

2010

PDF

R. Terzano, A. Santoro, M. Spagnuolo, B. Vekemans, L. Medici, K. Janssens, J. Goettlicher, M. A. Denecke, S. Mangold, P. Ruggiero 

Environmental pollution 158 (2010) 2702-2709 

2010

PDF

E. Hiller, L. Jurkovic, J. Kordik, I. Slaninka, M. Jankular, J. Majzlan, J. Gottlicher, R. Steininger

Applied Geochemistry, 24 (11), 2175-2185

2009

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T. Spangenberg, J. Göttlicher, R. Steininger

AIP Conf. Proc., 1092, 93

2009

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S. Ziegler, S. Ackermann, J. Majzlan, J. Gescher

Environmental Microbiology, 11 (2), 2329-2338

2009

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L. Backnaes, J. Stelling, H. Behrens, J. Göttlicher, S. Mangold, O. Verheijen, R. G. C. Beerkens, J. Deubener

Journal of the American Ceramic Society, 91 (3), 721-727

2008

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G. S. Dieckmann, G. Nehrke, S. Papadimitriou, J. Göttlicher, R. Steininger, H. Kennedy, D. Wolf-Gladrow, D. N. Thomas

Geophysical Research Letters, 35 (8), art.no.-L08501

2008

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V. Hurai, J. Göttlicher, J. Majzlan, M. Huraiova

Canadian Mineralogist, 46, 1173-1181

2008

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J. Majzlan, B. Lalinska, M. Chovan, L. Jurkovic, S. Milovska, J. Göttlicher

Geochimica et Cosmochimica Acta, 71 (17), 4206-4220

2007

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