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Microprobe X-ray fluorescence Beamline (BL-16) [an error occurred while processing this directive]

Introduction

Owing to numerous advantages of a synchrotron based X-ray fluorescence (XRF) technique, we have setup a microprobe XRF beamline (BL-16) on Indus-2 synchrotron radiation facility. The beamline has now become operational. A user can access this beamline by submitting a user beamtime proposal. The beamline works in the x-ray energy range of 4-20 keV. Using the micro-focused mode of the beamline it is possible to examine a specimen for spatial distribution of elements. Various parameters of the microprobe XRF beamline (BL-16) are summarized in Table 1.

The beamline has wide range of usages - both from research laboratories and industries; and for researchers working in diverse fields. Apart from the fields of pure sciences like physics and chemistry, the beamline also provides an attractive platform to exercise interdisciplinary applied sciences like medical, forensic and environmental studies etc. The beamline allows a user to perform x-ray fluorescence and total reflection x-ray fluorescence characterization of materials at micro and trace level. Apart from the elemental mapping, the beamline also provides other modes of XRF characterization, viz. grazing incidence x-ray fluorescence (GIXRF) analysis, chemical speciation, and near-edge absorption spectroscopy etc.

Major applications fields of the beamline

  1. XRF bulk elemental analysis (un-focused mode).
  2. Microprobe XRF – scanning multi-element analysis at a ppm levels with ~ 5 µm spatial resolution (focused mode).
  3. TXRF (Total reflection x-ray fluorescence) spectrometry – for ultra trace element analysis in the femtogram region.
  4. GIXRF (Glancing incidence x-ray fluorescence) spectrometry – a novel technique for depth profiling of impurities in thinfilms and surfaces.
  5. SIXES (Selectively induced x-ray fluorescence emission spectrometry) – to infer chemical state from the chemical shift of the absorption edge (chemical speciation)
  6. Absorption contrast x-ray imaging.

Beamline layout

Beamline Layout

Beamline parameters

Table 1

 
Beamline Optics
 
 
Photographs of the µ-XRF experimental setup and beamline shielding hutch
Experimental Setup and beamline shielding hutch
 
Photograph of the beamline inside optics shielding hutch
Photograph of the beamline inside optics shielding hutch
 
 

Experimental stations

The BL-16 beamlinme has two experimental stations:

  1. 5-axis sample manipulator: For µ-probe XRF mapping/ Imaging of multielement samples
  2. 2-circles goniometer: For grazing incidence XRF/XRR characterization

Beamline performance

Micro-focus x-ray beam

BL-16 beamline provides microfocus x-ray beam spot at the scanning experimental station of the beamline using elliptical bent Kirkpatrick-Baez focusing mirrors. Figures show the measured focus beam size and the X-ray intensity distribution. This micro focused X-ray beam can be used to map the elemental heterogeneity in a specimen.

Recorded CCD Image of microfocused beam at BL-16 experimental station
Recorded CCD Image of microfocused beam at BL-16 experimental station

Measurements for the focused beam

Measured focused beam size at the experimental station was found to be ~ 4.3 µm (V) x 7.5 µm

Few examples

X-ray fluorescence measurements

X-ray fluorescence measurements

Measured SRXRF spectrum from a NIST 610 standard sample (trace elements in glass matrix) at excitation energy of 15 keV. The minimum detection sensitivities for various elements were found to be in ppb range.

Micro-XRF scanning

Micro-XRF scanning
Measured fluorescence micrograph of a Cu grid structure using the BL-16 microfocus beam.

Recent users of the BL-16 beamline (2012-13)

    1.

    2012
    August

    Dr. P. Subramania Athray

    Space Astronomy and Instrumentation Division, ISRO Satellite Center, Vimanapura, Bangalore.

    Vacuum assisted EDXRF analysis of Lunar simulant JSC1-A (soil) samples.

    2. 

    2012
    September 9-15

    Ms. Gurpreet Kaur and Ms. Himani Bansal

    Punjabi University, Patiala

    Measurements of  M shell fluorescence of heavy elements

    3. 

    2013
    Sept. 24-25

    Dr. Rakesh Verma

    Analytical Chemistry Division
    BARC, Mumbai

    Measurements  of Cl in Graphite

    4.

    2012
    October  9-12

    Dr.  S . B. Roy

    RRCAT, Indore

    Near edge measurements  of pure Nb samples (1st measurement was done to evaluate the feasibility of the experiment)

    5.

    Nov. 2012

    Sushmita Bhartiya

    Target lab LMDD, RRCAT, Indore

    Analysis of  Arsenic in water

    6.

    Dec. 2012

    Dr. S M Oak

    SSLD, RRCAT, Indore

    Analysis of Cl compounds

    7.

    Jan. 2013

    Dr. R V Nandedkar

    IPS Academy, Indore

    Analysis of  Arsenic in water treated with metal nano-particles 

    8.

    Feb. 2013

    Sh. Vishal Dhamgaya

    ISUD, RRCAT, Indore

    X-ray testing of  CRLs

    9.

    March 2013

    Dr.  S . B. Roy

    RRCAT, Indore

    Mixro-XRF measurements of Nb samples

    10.

    April 2013

    Dr. R V Nandedkar

    IPS Academy, Indore

    Analysis of  Arsenic in water treated with metal nano-particles (another sample set)

    11. 

    April 2013

    B. K Shinda

    UHV Division, RRCAT

    Material composition Stainless steel

    12. 

    April 2013

    Dr. Debdutta Lahiri

    High pressure & synchrotron radiation Division., BARC, Mumbai

    Analysis of HgS based Ayurvaid Bhasma samples

    13.

    April 2013

    Dr. Alok Dube

    LABID, RRCAT

    X-ray fluorescence analysis of Chlorine p6-copper iodide compounds

    14. 

    May 13-7 Jun 2013

    Sh. Vishal Dhamgaya

    ISUD, RRCAT, Indore

    X-ray testing of  CRLs in SU-8 materials

    15. 

    Jun 2013
    10-14

    Dr. anil Kumar Sharma and Dr. Sanjiv Puri

    Punjabi University, Patiala

    Measurements of L shell fluorescence and CK yield for Re, and Os.

    16.

    Jun 2013

    Dr. A. S. Joshi

    Plasma Physics Division RRCAT

    Determination Pt impurity in Glass samples

    17.

    Jun 2013
    17-19

    Sushmita Bhartiya

    Target lab LMDD, RRCAT, Indore

    TXRF Analysis of  Arsenic in water

    18.

    Jun 2013
    20-21

    Dr. Alok Dube

    LABID, RRCAT

    TXRF X-ray fluorescence analysis of Chlorine p6-copper iodide compounds in cells

    19.

    2013
    Jun 24-28

    Dr. Rakesh Verma

    Analytical Chemistry Division
    BARC, Mumbai

    Measurements  of Cl in Graphite

    20. 

    2013, 3-5 July

    Dr. Sunil Verma

    Laser Materials Development and Devices Division

    Impurities in KDP crystals

    21. 

    2013, 8-10 July

    Dr. N L Misra

    FCD, BARC, Mumbai

    U- trace analysis

    22. 

    2013, 22-26 July

    Dr. K V. G. Kutty

    IGCAR, Kapakkam

    Analysis of Trace elements liquid sample

    23. 

    2013, 29-31 July

    Dr. Sanjieev

    IIT Mumbai

    TXRF analysis of Blood samples

    24. 

    2013,5-8 August

    Raj Mittal Singla

    Panjabi University, Patiala

    M-shell XRF cross section measurements

    25. 

    2013, 19-23 August

    Prof. N.M. Badiger

    Karnataka University, Dharwad

    Resonant Raman X-ray scattering cross section measurements

    26. 

    2013, 2-20 September

    Vishal Dhamgaye

    RRCAT, Indore

    Characterization of micro X-ray lens

    27.

    2013, 23-27 September

    Rajiv Jain

    RRCAT, Indore

    Testing of DCM Energy calibration of BL-16 beamline

    28. 

    2013, 1-4 October

    Dr. A. S. Joshi

    RRCAT, Indore

    XRF analysis laser glass substrate

    29. 

    2013,14-18 October

    Sunil Verma

    RRCAT, Indore

    XRF characterization of potassium dihydrogen sulphate single crystal

    30. 

    2013, 21-25 October

    Dr. N L Misra

    BARC, Mumbai

    U-L, and U-M TXRF analysis

    31. 

    2013, 28-31 October

    Vishal Dhamgaye

    RRCAT, Indore

    TXRF analysis of SU-8

     

Publications

2013

  1. “Experimental validation of XRF inversion code for Chandrayaan-1”
    P.S. Athiray, M. Sudhakar, M.K. Tiwari, S. Narendranath, G. S. Lodha, S. K. Deb, P. Sreekumar, S.K. Dash
    Planetary and Space Science 89 183–187 (2013).

  2. “M sub shell X-ray emission cross section measurements for Pt, Au, Hg, Pb, Th and U at 8 and 10 keV synchrotron photons”
    Gurpreet Kaur, Sheenu Gupta, M K Tiwari and Raj Mittal
    Nuclear Inst. and Methods in Physics Research, B 2013 (in press).

  3. “Development of high aspect ratio X-ray parabolic compound refractive lens at Indus-2 using X-ray lithography”
    V. P. Dhamgaye, M. K. Tiwari, C. K. Garg, P. Tiwari, K. J. S. Sawhney, G. S. Lodha
    Microsystem Technologies 2013 (in press).

  4. “A microfocus X-ray fluorescence beamline at Indus-2 synchrotron radiation facility”
    M. K. Tiwari, P. Gupta, A. K. Sinha, S. R. Kane, A. K. Singh, S. R. Garg, C. K. Garg, G. S. Lodha and S. K. Deb
    J. Synchrotron Rad. 20, 386–389 (2013).

  5. "A microprobe-XRF Beamline on Indus-2 Synchrotron Light Source"
    M. K. Tiwari, S. R. Kane, A. K. Sinha, C. K. Garg, A. K. Singh, P. Gupta, S. R. Garg, G. S. Lodha and S. K. Deb
    Journal of Physics: Conference Series 425, 072020 (2013).

  6. “Synchrotron-induced EDXRF determination of uranium and thorium in mixed uranium –thorium oxide pellets”
    N. L. Misra, M. K. Tiwari, S. Sanjay Kumar, Sangita Dhara, Ajit Kumar Singh, G. S. Lodha, S. K. Deb, P. D. Gupta and S. K. Aggarwal
    X-Ray Spectrom., 42, 4–7 (2013).

  7. “Synchrotron based micro-XRF study to assess the uniformity in solid pellets”
    N.L. Misra, M. K. Tiwari, BalGovind Vats, S. Sanjay Kumar, Ajit Kumar Singh, G. S. Lodha, S.K. Deb, P.D. Gupta and S.K. Aggarwal
    Presented in EXRS 2012 conference.

2012

  1. “A study on the effect of tantalum-impurity content on the superconducting properties of niobium materials used for making superconducting radio frequency cavities”
    S. B. Roy, L. S. Sharath Chandra, M. K. Chattopadhyay, M. K. Tiwari, G. S. Lodha and G. R. Myneni,
    Supercond. Sci. Technol. 25, 115020 (2012).

  2. “Peak energy shift with fertilization in mint plants:  EDXRF measurements with synchrotron photon source”
    Kamaldip Kaur, Kanan Deep, Meenakshi Bansal, M. K. Tiwari, Raj Mittal
    Arch. Appl. Sci. Res., 4 (5):2152-2160 (2012).

  3. “Commissioning of a Microprobe-XRF Beamline (BL-16) on Indus-2 Synchrotron Source”
    M. K. Tiwari, P. Gupta, A. K. Sinha, C. K.Garg, A. K. Singh, S. R. Kane, S. R.Garg and G. S.Lodha
    AIP Conf. Proc.1447, 499-500 (2012); doi: 10.1063/1.4710097

Contact Number : 244 2516/ 244 2123

Contacts:

Name Email Phone
Dr. M K Tiwari mktiwari(at)rrcat.gov.in 0731-2442124 (Beamline incharge)

Last Modification on : January 2014
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