Microprobe X-ray fluorescence beamline

Beamline overview

X-ray fluorescence (XRF) spectroscopy is a powerful non-destructive method for micro and trace elemental characterization of materials. The technique is used in a range of domains, including geology, archaeology, biomedical science, and material science, etc. The BL-16 beamline allows a variety of re-configurable operational modes (normal XRF, TXRF, and micro-XRF modes) with minimal set-up time. It provides an attractive platform for researchers to conduct a wide range of research activities, particularly in the fields of archaeology, earth science, and environmental applications, etc.

The Beamline

Beamline parameters & Optical layout

SourceBending magnet
Energy Range5-20 keV
Beam acceptance 1 mrad (h) × 0.2 mrad (v)
Energy resolution(ΔE/E)~ 10-3-10-4
Beam spot size (at sample position)~ 7.5 µm (h) × 4.3 µm (v) [Focused mode]
~ 22 mm (h) × 5 mm (v) [Unfocused mode]
MonochromatorSi (111) double-crystal monochromator
Photon Flux [at 10 keV X-rays/ 100 mA ring current]~ 2 × 107 photons/sec [Focused mode]
~ 1 × 108 photons/sec/mm2 [Unfocused mode]
Beamline parameters & Optical layout
BL-16 Beamline optical layout
  1. The BL-16 beamline uses a fixed-exit double crystal monochromator (DCM) (FMB, Berlin, Germany) with a pair of symmetric and asymmetric Si (111) crystals (mounted side-by-side).
  2. The beamline utilises various types of slit systems (water cooled and un-cooled) for controlling the final beam size available at the experimental station, as per the user requirements.
  3. The beamline also utilises a Kirkpatrick–Baez (KB) optics (Xradia, USA), comprising of two elliptical bendable mirrors for focusing of the synchrotron X-ray beam.
  4. The beamline offers minimum micro focus beam dimensions ~ 5 μm (V) × 8 μm (H) for microfluorescence mapping applications.
  5. The BL-16 beamline also includes a third experimental station for analysis of thin layered materials using X-ray reflectivity (XRR) and grazing incidence X-ray fluorescence (GIXRF) measurements.

Experimental station

The BL-16 beamline allows various re-configurable experimental stations (for normal XRF, TXRF, micro-XRF, XRR and GIXRF measurements) with a minimal set-up time, which allows a user to perform a wide range of experiments.

An inside view of the experimental hutch of the BL-16 Beamline
An inside view of the experimental hutch of the BL-16 Beamline
Experimental facilities

1) XRF-TXRF chambers

This setup is used for the XRF and TXRF analysis of different types of samples (i.e. bulk, liquid and powder forms).

XRF-TXRF chambers
XRF-TXRF chambers
XRF-TXRF chambers
2) Two-Circle Goniometer

This setup is used for simultaneous X-Ray Reflectivity (XRR) and Grazing Incidence X-ray Fuorescence (GIXRF) of thinflims, multilayers and nano structured materials.

A photograph of the BL-16 Goniometer setup
A photograph of the BL-16 Goniometer setup
3. MicroXRF

This setup is used for the elemental mapping of heterogeneous multi-element samples using micro focused X-ray beam. A five-axis sample manipulator stage is used for mounting of the sample.

3. MicroXRF
A photograph of the BL-16 MicroXRF sample manipulator system
A photograph of the BL-16 MicroXRF sample manipulator system

Application Areas

The different experimental stations of the beamline provide an attractive platform for conducting a wide range of research activities, particularly in the fields of archaeology, earth science and environmental applications, and materials science. Some of the research fields are given below.

  1. Materials and Engineering
  2. Thin films, multilayers and nanoparticles
  3. Elemental analysis of Medicines
  4. Environmental monitoring and toxicity
  5. Life science
  6. Food, Agricultural & Geological materials
  7. Forensic applications

1. Improvement of limit of detection sensitivities in the parts per billion range using conventional geometry synchrotron radiation excited EDXRF measurements
Md. Akhlak Alam, M.K. Tiwari, Ayushi Trivedi, Ajay Khooha and A. K. Singh J. Anal. At. Spectrom., Vol. 37, pp 575–583 (2022). DOI: 10.1039/d2ja00016d
2. Depth profiling of energetic Au ions inside P-type Si〈100〉substrate
Md. Akhlak Alam, Ayushi Trivedi, M.K. Tiwari, Devarani Devi, Sanjay Rai, Mukul Gupta, D.K. Avasthi
Applied Surface Science, Vol. 579,152173 (2022).
3. Serum Elemental Analysis of Type 2 Diabetes Patients Using SRXRF
N. Srinivasa Rao, G. J. Naga Raju, M. K. Tiwari, B. G. Naidu, P. Sarita Biological Trace Element Research, volume 200, pp 1485–1494 (2022).

1. Near edge absorption studies of pure and impure NbSe2; theory and experiment
Soumyadeep Ghosh, Rukshana Pervin, Haranath Ghosh, M. K. Tiwari, Parasharam Shirage
Journal of Materials Science, Vol. 56, 17062–17079 (2021).
2. Assessment of the Elemental Profile of Leafy Vegetables by Synchrotron -Radiation Induced Energy Dispersive X-Ray Fluorescence Spectroscopy
AS Bharti, S Sharma, A K Singh, M K Tiwari, K N Uttami
Journal of Applied Spectroscopy Vol. 88, 653-661, (2021).
3. Synchrotron Based TXRF for Assessment of Treated Waste water
VK Garg, AL Srivastav, MK Tiwari, A Sharma, VS Kanwar
Nature Environment and Pollution Technology , Vol 20 (2), 743-746 (2021)

1. Elemental analysis of Arsenicum album 30
KA K Dwivedi and M K Tiwari
International Journal of Homoeopathic Sciences, Vol. 4(4), pp 135-137 (2020).
2. Solar X-Ray Monitor on Board the Chandrayaan-2 Orbiter: In-Flight Performance and Science Prospects
N. P. S. Mithun et. al.
Solar Physics, Vol. 295 , Article number: 139 (2020) .
3. Measurement of L subshell fluorescence yield ratios of some high Z elements by selective excitation method
G. B. Hiremath, A. S. Bennal, M. M. Hosamani, N. M. Badiger, A. Trivedi, M. K. Tiwari
X-Ray Spectrometry , Vol 50, Issue1, pp 37-44 (2021)
https://doi.org/10.1007/s11207-020- 01712-1
4. Surface-interface investigations of an ultrathin pulsed laser deposited NiO/ZnO bilayer structure
Ayushi Trivedi, Ram Janay Choudhary, Arijeet Das, Sanjay Kumar Rai, Manoj Kumar Tiwari, Anil Kumar Sinha,
Surface Interface Analysis ,Vol 52, pp 533 –540 (2020)
5. Study of the solid-state effect on L3 subshell fluorescence yield for high Z targets using Indus-2 synchrotron radiation
Gangadharayya B. Hiremath, A.S. Bennal, Santosh Mirji, M.M. Hosamani, N.M. Badiger, and M. K. Tiwari,
Canadian Journal of Physics, Vol. 98(5):470–473 (2020).

1. Prompt Screening of the Alterations in Biochemical and Mineral Profile of Wheat Plants Treated with Chromium Using Attenuated Total Reflectance Fourier Transform Infrared Spectroscopy and X-ray Fluorescence Excited by Synchrotron Radiation
Sweta Sharma, A. K. Singh, M. K. Tiwari & K. N. Uttam.
Analytical Letters, Vol 53:3, 482-508 , (2019).
2. Interface sharpening in miscible and isotopic multilayers: Role of short-circuit diffusion
A. Tiwari, M. K. Tiwari, M. Gupta, H.-C. Wille,and A. Gupta,
Phys. Rev. B , Vol. 99, 205413 , (2019).

3. Morphological and elemental mapping of gallstones using synchrotron microtomography and synchrotron X‐ray fluorescence spectroscopy
Mohana Bakthavatchalam, Jayanthi Venakataraman, Ramya J Ramana,Mayank Jain, Balwant Singh, Arul K Thanigai, Vaithiswaran Velyoudam, Saravanan Manickam Neethirajan, Manoj K Tiwari, Ashish K Agarwal,and Narayana S Kalkura
Journal of gastroenterology and hepatology 3, pp 381-387 , (2019).

4. Multivariate analysis of trace elemental data obtained from blood serum of breast cancer patients using SRXRF
B. Gowri Naidu, P. Sarita, G.J. Naga Raju, M.K. Tiwari
Results in Physics, Vol. 12, pp 673–680, (2019).
5. Study the effect of crystal structure on radiative vacancy transfer probabilities from L3to Mi,Ni and Oi subshells
Gangadharayya B. Hiremath, Santosh Mirji, M.M. Hosamani, N.M. Badiger, M.K. Tiwari
Chemical Physics Letters, Vol. 715, pp 317-322, (2019).

1. Effect of manganese stress on the mineral content of the leaves of wheat seedlings by use of X-ray fluorescence excited by synchrotron radiation
Sweta Sharma, Abhi Sarika Bharti, M. K. Tiwari, and K. N. Uttam
Spectroscopy Letters Vol. 51, Issue 6, pp 302-310 , (2018).
2. Fabrication and characterization of Er, Nd codoped Y2O3 transparent ceramic: A dual mode photoluminescence emitter
Pratik Deshmukh, S. Satapathy, Anju Ahlawat, M.K. Tiwari, A.K. Karnal
Journal of Alloys and Compounds, Vol. 754, pp 32-38, (2018)
3. Total reflection X-ray Fluorescence determination of interfering elements rubidium and uranium by profile fitting
Sangita Dhara, Ajay Khooha, Ajit Kumar Singh, M.K. Tiwari, N.L. Misra
Spectrochimica Acta Part B , Vol. 144, pp 87–91, (2018).
4. Recent trends in X-ray fluorescence spectrometry: precise investigation of Nanomaterials
M K Tiwari
Spectroscopy Europe ,Vol. 30, No. 1, pp. 15-19 (2018)
5. M sub-shell X-rayfluorescence cross-section measurements for six elements in the range Z=78–92 at tuned synchrotron photon energies5, 7 and 9 keV
Himani Bansal, M.K. Tiwari, Raj Mittal
Journal of Quantitative Spectroscopy & Radiative Transfer,Vol. 204,232–241, (2018).
6. An IAEA multi-technique X-ray spectrometry end station at Elettra Sincrotrone Trieste: bench-marking results and interdisciplinary applications
Andreas Germanos Karydas, et al.
J. Synchrotron Rad., Vol. 25, pp 189–203, (2018).
7. Development of multilayer mirrors for space-based astronomical X-ray optics
Singam S. Panini, M. Nayak, K. C. Shyama Narendranath, P. C. Pradhan, P. S. Athiray, P. Sreekumar, G. S. Lodha, M. K. Tiwari
Journal of Optics,Vol.47, Issue 1, pp 91–95, (2018).

1. Elemental Investigation of the Leaf and Seed of Coriander Plant by Synchrotron Radiation X-ray Fluorescence Spectroscopy
Abhi Sarika Bharti, Sweta Sharma, Nidhi Shukla, M. K. Tiwari, K. N. Uttam
National Academy Science Letters, Vol. 40, Issue 5, pp 373–377, (2017).
2. Depth resolved chemical speciation of a W-B4C multilayer structure
Gangadhar Das, A. G. Karydas, Haranath Ghosh, M. Czyzycki, A. Migliori, A. K. Sinha, M. K. Tiwari
Phys. Rev. B, Vol. 96, 155444, (2017).
3. Measurement of Coster-Kronig vacancy transfer factor of some lanthanides using monoenergetic X-ray photons
Krishnananda, Santosh Mirji, N.M. Badiger, M.K. Tiwari
Vacuum, Vol. 144, pp 160-163 ,(2017).
4. Determination of impurities in graphite using synchrotron radiation based X-ray fluorescence spectrometry
M. Ghosha, K.K. Swain, P.S. Remya Devia, T.A. Chavan, A.K. Singh, M. K. Tiwari, R. Verma
Applied Radiation and Isotopes, Vol. 128, pp 210–215 , (2017)
5. L X-ray intensity ratio measurements using selective L sub-shell photo- ionisation on synchrotron
Himani Bansal, M. K. Tiwari, Raj Mittal
Radiation Physics and Chemistry, Vol. 139, pp 22–26 , (2017).
6. Probing nanostructured materials using X-ray fluorescence analysis
Gangadhar Das, Ajay Khooha, Ajit Kumar Singh, M. K. Tiwari
X-Ray Spectrom. 2017, Vol .46(5), pp 448–453, (2017)
7. Measurement of L X-ray Fluorescence Cross-sections for 74W at Excitation Energies 12, 14, 15 and 16.5 keV with Synchrotron Radiation
R. Kumar, A. Rani, R.M. Singh, M.K. Tiwari, A.K. Singh
Radiation Physics and Chemistry, Vol. 131, pp. 79-85 , (2017).
8. Direct Determination of Oxidation States of Uranium in Mixed-Valent Uranium Oxides Using Total Reflection X-ray Fluorescence X-ray Absorption Near-Edge Spectroscopy
Kaushik Sanyal, Ajay Khooha, Gangadhar Das, M. K. Tiwari, and N. L. Misra
Anal. Chem. , Vol 89 (1), pp. 871–876 , (2017).
9. L sub-shell fluorescence cross-section measurements for elements, Z = 62–67, at tuned photon energies
Himani Bansal, M.K. Tiwari, Raj Mittal
Journal of Quantitative Spectroscopy and Radiative Transfer, Vol. 199, pp. 93–102 (2017).

Science Highlights

Science Highlights
Depth profiling of energetic Au ions inside P-type Si 〈100〉 substrate

Applied Surface Science 579, 152173 (2022) https://doi.org/10.1016/j.apsusc.2021.152173

Science Highlights
Structural investigation of Ayurveda Lauha (Iron) Bhasma

Journal of Ayurveda and Integrative Medicine, 14 100690 (2023)

Science Highlights
Improvement of limit of detection sensitivities in the parts per billion range using conventional geometry synchrotron radiation excited EDXRF measurements

Journal of Anal. At. Spectrom., 37, 575-583 (2022). https://doi.org//10.1039/d2ja00016d

Science Highlights
Serum Elemental Analysis of Type 2 Diabetes Patients Using SRXRF

Biological Trace Element Research, 200,1485–1494 (2022) https://doi.org/10.1007/s12011-021-02762-7.

Science Highlights
Surface-interface investigations of an ultrathin pulsed laser deposited NiO/ZnO bilayer structure

Surface Interface Analysis, 52, 533 –540 (2020). https://doi.org/10.1002/sia.6774

Team members

  1. Dr. M.K. Tiwari
  2. Mrs. Ayushi Trivedi
  3. Shri Ajit Kumar Singh
  4. Shri Ajay Khooha
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