New Frontiers in Application of FTIR Microscopy for Characterization of Cultural Heritage Materials

We present an overview of recent advances in the application of Fourier Transform Infrared (FTIR) microscopy for analysis of complex, multicomponent, and multilayer samples such as those typically encountered in the field of heritage materials. This technique is particularly useful since it allows identification and localization of both organic and inorganic (if IR active) compounds. New improvements have been possible thanks to the introduction of ad hoc sample preparation methods to obtain either thin or cross sections that allow both avoidance of contamination from organic embedding resin and improvement of the quality of the acquired spectra. Moreover, integrated use of spectra registered in the near-infrared (NIR) and mid-infrared (MIR) regions allows better comprehension of cross section composition. Data interpretation has been improved thanks to the development of chemometric methods for elaboration of hyperspectral data. A new and very promising field is the development of enhanced FTIR methods for detection of trace components in microextracts. These systems, allowing detection of extractable organic compounds from about 0.1 mg of sample, will be extremely useful in the future for analysis of natural and synthetic colorants, varnishes extracted, for instance, from cotton swabs used during cleaning of paintings, and organic residues on archeological remains.

[1]  Y. Saito,et al.  A Simple Chemical Method for the Preparation of Silver Surfaces for Efficient SERS , 2002 .

[2]  Miguel Valcárcel,et al.  Vanguard-rearguard analytical strategies , 2005 .

[3]  C. Cardell,et al.  Validating chemical and structural changes in painting materials by principal component analysis of spectroscopic data using internal mineral standards , 2013 .

[4]  Michael D. Morris,et al.  Microscopic and Spectroscopic Imaging of the Chemical State , 1993 .

[5]  Josse De Baerdemaeker,et al.  A review of the analytical methods coupled with chemometric tools for the determination of the quality and identity of dairy products , 2007 .

[6]  Costanza Miliani,et al.  Multivariate chemical mapping of pigments and binders in easel painting cross-sections by micro IR reflection spectroscopy , 2011, Analytical and bioanalytical chemistry.

[7]  Lucia Toniolo,et al.  The analysis of polychrome works of art: 40 years of infrared spectroscopic investigations , 2001 .

[8]  L. Bertrand,et al.  Insights into the varnishes of historical musical instruments using synchrotron micro-analytical methods , 2008 .

[9]  Loïc Bertrand,et al.  Identification of the finishing technique of an early eighteenth century musical instrument using FTIR spectromicroscopy , 2011, Analytical and bioanalytical chemistry.

[10]  M. Papiz,et al.  Identification of copper-based green pigments in Jaume Huguet's Gothic altarpieces by Fourier transform infrared microspectroscopy and synchrotron radiation X-ray diffraction. , 2002, Journal of synchrotron radiation.

[11]  N. S. Baer,et al.  APPLICATION OF INFRARED FOURIER TRANSFORM SPECTROSCOPY TO PROBLEMS IN CONSERVATION , 1977 .

[12]  S. Asahina,et al.  Surface Preparation of Cross Sections of Traditional and Modern Paint Using the Argon Ion Milling Polishing CP System , 2006, Microscopy and Microanalysis.

[13]  Joyce Plesters,et al.  Cross-sections and chemical analysis of paint samples , 1956 .

[14]  Ludovic S. Live,et al.  Nanohole arrays in chemical analysis: manufacturing methods and applications. , 2010, The Analyst.

[15]  I. V. Berghe,et al.  High-performance liquid chromatography and non-destructive three-dimensional fluorescence analysis of early synthetic dyes. , 2007, Journal of chromatography. A.

[16]  L. Litti,et al.  Use of nano gold obtained by laser ablation for SEIRA analyses of colorants , 2014, Heritage Science.

[17]  Aviva Burnstock,et al.  Non-invasive in-situ investigations versus micro-sampling: a comparative study on a Renoirs painting , 2007 .

[18]  Cristiana Lofrumento,et al.  SERS detection of red organic dyes in Ag-agar gel , 2013 .

[19]  C. Miliani,et al.  FT-NIR spectroscopy for non-invasive identification of natural polymers and resins in easel paintings , 2009, Analytical and bioanalytical chemistry.

[20]  Mauro Bacci,et al.  A study of the blue colors used by Telemaco Signorini (1835–1901) , 2009 .

[21]  Rocco Mazzeo,et al.  Performance evaluation of mapping and linear imaging FTIR microspectroscopy for the characterisation of paint cross sections , 2010, Analytical and bioanalytical chemistry.

[22]  D. Fabbri,et al.  Application of ATR-far-infrared spectroscopy to the analysis of natural resins , 2011, Analytical and bioanalytical chemistry.

[23]  Dusan Stulik,et al.  Infrared Spectroscopy in Conservation Science , 2000 .

[24]  Naoki Matsuda,et al.  Charge transfer resonance Raman process in surface-enhanced Raman scattering from p-aminothiophenol adsorbed on silver: Herzberg-Teller contribution , 1994 .

[25]  A. Savitzky,et al.  Smoothing and Differentiation of Data by Simplified Least Squares Procedures. , 1964 .

[26]  Charlotte Martin de Fonjaudran,et al.  Stratigraphic analysis of organic materials in wall painting samples using micro-FTIR attenuated total reflectance and a novel sample preparation technique , 2008, Analytical and bioanalytical chemistry.

[27]  D. Gastaldi,et al.  Identification of dyestuffs in historical textiles: Strong and weak points of a non-invasive approach , 2013 .

[28]  J. Lombardi,et al.  Sample treatment considerations in the analysis of organic colorants by surface-enhanced Raman scattering. , 2012, Analytical chemistry.

[29]  M. Milosevic,et al.  Internal Reflection and ATR Spectroscopy , 2004 .

[30]  Costanza Miliani,et al.  Reflection infrared spectroscopy for the non-invasive in situ study of artists’ pigments , 2012 .

[31]  M. Manfait,et al.  Characterization of island films as surface-enhanced Raman spectroscopy substrates for detecting low antitumor drug concentrations at single cell level. , 1998, Biospectroscopy.

[32]  A. Hartstein,et al.  Enhancement of the Infrared Absorption from Molecular Monolayers with Thin Metal Overlayers , 1980 .

[33]  Masatoshi Osawa,et al.  Surface-enhanced infrared absorption of p-nitrobenzoic acid deposited on silver island films: contributions of electromagnetic and chemical mechanisms , 1991 .

[34]  Costanza Miliani,et al.  On the Use of Overtone and Combination Bands for the Analysis of the CaSO4—H2O System by Mid-Infrared Reflection Spectroscopy , 2010, Applied spectroscopy.

[35]  P. Oliveri,et al.  Evaluation of the effect of six different paint cross section preparation methods on the performances of Fourier Transformed Infrared microscopy in attenuated total reflection mode , 2012 .

[36]  H. Emerich,et al.  Identification of reaction compounds in micrometric layers from gothic paintings using combined SR-XRD and SR-FTIR. , 2009, Talanta.

[37]  Jean Susini,et al.  Applications of synchrotron-based micro-imaging techniques to the chemical analysis of ancient paintings , 2008 .

[38]  P. Oliveri,et al.  FT-NIR microscopy: An advanced spectroscopic approach for the characterisation of paint cross-sections , 2014 .

[39]  R. Laursen,et al.  Development of mild extraction methods for the analysis of natural dyes in textiles of historical interest using LC-diode array detector-MS. , 2005, Analytical chemistry.

[40]  S. Hardman,et al.  The mineralization of fibres in burial environments , 1994 .

[41]  E. Manzano,et al.  Benefits of applying combined diffuse reflectance FTIR spectroscopy and principal component analysis for the study of blue tempera historical painting. , 2008, Analytica chimica acta.

[42]  R. C. Reeder,et al.  Fourier transform spectroscopic imaging using an infrared focal-plane array detector. , 1995, Analytical chemistry.

[43]  Lucia Toniolo,et al.  Spectrochemical characterization by micro-FTIR spectroscopy of blue pigments in different polychrome works of art , 1999 .

[44]  Peter R. Griffiths,et al.  Fourier Transform Infrared Spectrometry, Second Edition , 2007 .

[45]  A. C. Jones,et al.  Infrared Spectroscopy of Surface Coatings in Reflected Light , 1960 .

[46]  Jia-sun Tsang,et al.  SOME IMPROVEMENTS IN THE STUDY OF CROSS SECTIONS , 1991 .

[47]  Luc Moens,et al.  Some ideas on the definition of Raman spectroscopic detection limits for the analysis of art and archaeological objects , 2012 .

[48]  J. Coello,et al.  Near-infrared spectroscopy in the pharmaceutical industry. , 1998, The Analyst.

[49]  Single-Reflection Attenuated Total Reflection of Organic Monolayers on Silicon , 2003, Applied spectroscopy.

[50]  R. J. Gettens.  Science in the art museum , 1952 .

[51]  M. Milosevic,et al.  Internal Reflection and ATR Spectroscopy: Milosovic/Internal Reflection , 2012 .

[52]  Rocco Mazzeo,et al.  Analysis of paint cross-sections: a combined multivariate approach for the interpretation of μATR-FTIR hyperspectral data arrays , 2012, Analytical and Bioanalytical Chemistry.

[53]  J. M. Chalmers,et al.  Specular reflectance: A convenient tool for polymer characterization by FTIR-microscopy? , 1996 .

[54]  K. Castro,et al.  Classification and identification of organic binding media in artworks by means of Fourier transform infrared spectroscopy and principal component analysis , 2011, Analytical and bioanalytical chemistry.

[55]  R. Aroca,et al.  A New Surface for Surface-Enhanced Infrared Spectroscopy: Tin Island Films , 1997 .

[56]  S. Badilescu,et al.  Enhanced Infrared ATR Spectra of O-, m-, and p-Nitrobenzoic Acid with Ag Films , 1989 .

[57]  Paolo Oliveri,et al.  Chemometric brains for artificial tongues. , 2010, Advances in food and nutrition research.

[58]  P. Griffiths,et al.  Preparation and characterization by surface-enhanced infrared absorption spectroscopy of silver nanoparticles formed on germanium substrates by electroless displacement , 2007, Analytical and bioanalytical chemistry.

[59]  P. Pivarnik,et al.  Colloidal gold filtrates as metal substrates for surface-enhanced infrared absorption spectroscopy. , 1999, Analytical chemistry.

[60]  G. Cinque,et al.  Optimal Sample Preparation for the Analysis of Micrometric Heterogeneous Samples. , 2015, Analytical chemistry.

[61]  Marco Leona,et al.  Identification of organic colorants in fibers, paints, and glazes by surface enhanced Raman spectroscopy. , 2010, Accounts of chemical research.

[62]  C. Pasquini.  Near Infrared Spectroscopy: fundamentals, practical aspects and analytical applications , 2003 .

[63]  R. Cubeddu,et al.  Assessment of the ageing of triterpenoid paint varnishes using fluorescence, Raman and FTIR spectroscopy , 2009, Analytical and bioanalytical chemistry.

[64]  Tom Fearn,et al.  Chemometric Space: Sensitivity and specificity , 2009 .

[65]  M. Cotte,et al.  The use of synchrotron radiation for the characterization of artists' pigments and paintings. , 2013, Annual review of analytical chemistry.

[66]  Costanza Miliani,et al.  An integrated spectroscopic approach for the non-invasive study of modern art materials and techniques , 2010 .

[67]  G. Downey,et al.  Recent technological advances for the determination of food authenticity , 2006 .

[68]  J. Lopes,et al.  Quality control of pharmaceuticals with NIR: From lab to process line , 2009 .

[69]  S Prati,et al.  Development of innovative embedding procedures for the analyses of paint cross sections in ATR FITR microscopy , 2012, Analytical and Bioanalytical Chemistry.

[70]  Rocco Mazzeo,et al.  Attenuated Total Reflection-Fourier transform infrared microspectroscopic mapping for the characterisation of paint cross-sections. , 2007, Analytica chimica acta.

[71]  C. Domingo,et al.  Ag nanoparticles prepared by laser photoreduction as substrates for in situ surface-enhanced Raman scattering analysis of dyes. , 2007, Langmuir : the ACS journal of surfaces and colloids.

[72]  C. Di Natale,et al.  Nonspecific sensor arrays ("electronic tongue") for chemical analysis of liquids (IUPAC Technical Report) , 2005 .

[73]  M. Cotte,et al.  Preparation of thin-sections of painting fragments: classical and innovative strategies. , 2014, Analytica chimica acta.

[74]  S. Berets,et al.  Grazing Angle Attenuated Total Reflection Spectroscopy: Fields at the Interface and Source of the Enhancement , 2007, Applied spectroscopy.

[75]  Marika Spring,et al.  ATR-FTIR imaging for the analysis of organic materials in paint cross sections: case studies on paint samples from the National Gallery, London , 2008, Analytical and bioanalytical chemistry.

[76]  G. Lachenal.  Dispersive and Fourier transform near-infrared spectroscopy of polymeric materials , 1995 .

[77]  J. Perlo,et al.  Noninvasive testing of art and cultural heritage by mobile NMR. , 2010, Accounts of chemical research.

[78]  C. Domingo,et al.  Surface-Enhanced Infrared Spectroscopy , 2004, Applied spectroscopy.

[79]  Piotr Targowski,et al.  Optical Coherence Tomography: its role in the non-invasive structural examination and conservation of cultural heritage objects—a review , 2012 .

[80]  Marco Leona,et al.  Nondestructive identification of natural and synthetic organic colorants in works of art by surface enhanced Raman scattering. , 2011, Analytical chemistry.

[81]  S. Kazarian,et al.  New Opportunities in Micro- and Macro-Attenuated Total Reflection Infrared Spectroscopic Imaging: Spatial Resolution and Sampling Versatility , 2003, Applied spectroscopy.

[82]  Boris Mizaikoff,et al.  Surface enhanced infrared absorption spectroscopy (SEIRA) using external reflection on low-cost substrates , 1998 .

[83]  Paola Ricciardi,et al.  Mapping of egg yolk and animal skin glue paint binders in Early Renaissance paintings using near infrared reflectance imaging spectroscopy. , 2013, The Analyst.

[84]  Masatoshi Osawa,et al.  Surface-Enhanced Infrared Absorption , 2001 .

[85]  Andre J. Sommer,et al.  Attenuated Total Internal Reflection Microspectroscopy of Isolated Particles: An Alternative Approach to Current Methods , 1999 .

[86]  S. Hardman,et al.  The detection of dyes by FTIR microscopy , 1994 .

[87]  W. Gardner.  The Pigments and Mediums of the Old Masters , 1914, Nature.

[88]  Manfred Anders,et al.  Nondestructive analysis and dating of historical paper based on IR spectroscopy and chemometric data evaluation. , 2007, Analytical chemistry.

[89]  A. Polubotko.  About enhancement of infrared absorption by molecules adsorbed on rough surfaces , 1993 .

[90]  Bertrand Lavédrine,et al.  The nature of the extraordinary finish of Stradivari's instruments. , 2010, Angewandte Chemie.

[91]  M. Meneghetti,et al.  Controlled size manipulation of free gold nanoparticles by laser irradiation and their facile bioconjugation , 2007 .

[92]  Robert G. Messerschmidt,et al.  Infrared microspectroscopy : theory and applications , 1988 .

[93]  F. Hahn,et al.  Anodic oxidation of methane at noble metal electrodes: an ‘in situ’ surface enhanced infrared spectroelectrochemical study , 2001 .

[94]  P. Walter,et al.  Analysis of natural dyes in archeological textiles using TOF‐SIMS and other analytical techniques , 2014 .

[95]  C. Miliani,et al.  Fiber-Optic Fourier Transform Mid-Infrared Reflectance Spectroscopy: A Suitable Technique for in Situ Studies of Mural Paintings , 2007, Applied spectroscopy.

[96]  O. Chiantore,et al.  FTIR imaging investigation in MIR and in an enlarged MIR–NIR spectral range , 2012, Analytical and Bioanalytical Chemistry.

[97]  M. Cotte,et al.  Shades of green in 15th century paintings: combined microanalysis of the materials using synchrotron radiation XRD, FTIR and XRF , 2013 .

[98]  S. Berets,et al.  Enhanced sensitivity in single-reflection spectroscopy of organic monolayers on metal substrates (pseudo-ATR) , 2004 .

[99]  P. Griffiths,et al.  Surface-enhanced infrared absorption of CO on platinized platinum , 1999 .

[100]  S Prati,et al.  New advances in the application of FTIR microscopy and spectroscopy for the characterization of artistic materials. , 2010, Accounts of chemical research.