No abstract

The qualitative analysis of nanodiamonds by FTIR spectrometry as photoacoustic (FTIR–PAS), diffuse-reflectance (DRIFT), and attenuated total reflection (ATR) modalities was evaluated for rapid and nondestructive analysis and comparison of nanodiamonds. The reproducibility and signal-gathering depth of spectra was compared. The assignment of characteristic bands showed that only six groups of bands were present in spectra of all the modalities with appropriate sensitivity: 1760 (C=O stretch, isolated carboxyl groups); 1640–1632 (H–O–H bend, liquid water); 1400–1370 (non-carboxyl C–O–H in-plane bend and CH2 deformation); 1103 (non-carboxyl C–O stretch); 1060 (in-plane C–H bend, non-aromatic hydrocarbons and carbohydrates); 940 cm−1 (out-of-plane carboxyl C–O–H bend). DRIFT provides the maximum number of bands and is capable of measuring hydrogen-bonded bands and CHx groups. ATR provides the good sensitivity for water and C–H/C–C bands in the range 2000–400 cm−1. FTIR–PAS reveals less bands than DRIFT but more intense bands than ATR–FTIR and shows the maximum sensitivity for absorption bands that do not appear in ATR-IR spectra and are expedient for supporting either DRIFT or FTIR–PAS along with depth-profiling. Thus, all three modalities are required for the full characterization of nanodiamonds surface functional groups.

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Granulometric fractionation as a source of additional information on organic-matter and inorganic matrix components of soils using FTIR–photoacoustic spectroscopy (FTIR–PAS) supported by attenuated–total reflection FTIR spectroscopy (ATR–FTIR) for a wide range of aggregate fractions (10–5000 μm) was used to compare the sensitivity, reproducibility, information contents, and representativity of fractionated samples. For chernozem and sod-podzolic soils and different agricultural-use chernozem samples, differences in the composition were found, manifested in normalized spectra of microaggregate fractions, with the range of 10–100 μm bearing the complete information. Most changes are observed in the soil organic matter range (1900–1340 cm–1), although these changes are slight, and in the soil-matrix region (550–300 cm–1). The latter region increases the intensity of bands corresponding to amorphous silica and clay minerals in fine fractions, while the intensity of bands attributed to quartz lattice vibrations decreases. FTIR–PAS spectra do not differ considerably at high interferometer modulation frequencies as the signal-penetration depth is comparable with particle sizes. The soil fractions below 20 μm result in the maximum sensitivity, reproducibility, and signal-to-noise ratio, showing no changes from coarser fractions by the information content and, thus, providing representative samples for analysis. The fractionation shows more differences in the sod-podzolic and chernozem soil fractions than the whole soil spectra. FTIR–PAS provides better sensitivity and reproducibility in the 4000–2000 cm–1 region and ATR–FTIR in the 2000–100 cm–1 region.

The qualitative analysis of nanodiamonds by FTIR spectrometry as photoacoustic (PAS), diffuse-reflectance (DRIFT), and attenuated total reflection (ATR) modalities was evaluated for rapid and nondestructive analysis and comparison of nanodiamonds. The spectra reproducibility and signal-gathering depth was compared. The assignment of characteristic bands showed that only six groups of bands were present in spectra of all the modalities with appropriate sensitivity: 1760 (C=O stretch, isolated carboxyl groups); 1640–1632 (H–O–H bend, liquid water); 1400–1370 (non-carboxyl C–O–H in-plane bend and CH2 deformation); 1103 (non-carboxyl C–O stretch); 1060 (in-plane C–H bend, non-aromatic hydrocarbons and carbohydrates); and 940 cm–1 (out-of-plane carboxyl C–O–H bend). DRIFT provides the maximum number of bands and is capable of measuring hydrogen-bonded bands and CHX groups. ATR provides the good sensitivity for water and C–H/C–C bands in the range 2000–400 cm–1. PAS-FTIR reveals less bands than DRIFT but more intense bands than ATR-FTIR and shows the maximum sensitivity for absorption bands that do not appear in ATR-IR spectra and are expedient for supporting either DRIFT or PAS along with depth-profiling. Thus, all three modalities are required for full characterization of nanodiamonds surface functional groups.