Identification of species’ blood by attenuated total reflection (ATR) Fourier transform infrared (FT-IR) spectroscopy

Blood is one of the most common and informative forms of biological evidence found at a crime scene. A very crucial step in forensic investigations is identifying a blood stain’s origin. The standard methods currently employed for analyzing blood are destructive to the sample and time-consuming. In this study, attenuated total reflection (ATR) Fourier transform infrared (FT-IR) spectroscopy is used as a confirmatory, nondestructive, and rapid method for distinction between human and animal (nonhuman) blood. Partial least squares-discriminant analysis (PLS-DA) models were built and demonstrated complete separation between human and animal donors, as well as distinction between three separate species: human, cat, and dog. Classification predictions of unknown blood donors were performed by the model, resulting in 100 % accuracy. This study demonstrates ATR FT-IR spectroscopy’s great potential for blood stain analysis and species discrimination, both in the lab and at a crime scene since portable ATR FT-IR instrumentation is commercially available.     

Rapid and quantitative detection of the microbial spoilage in milk using Fourier transform infrared spectroscopy and chemometrics

Microbiological safety plays a very significant part in the quality control of milk and dairy products worldwide. Current methods used in the detection and enumeration of spoilage bacteria in pasteurized milk in the dairy industry, although accurate and sensitive, are time-consuming. FT-IR spectroscopy is a metabolic fingerprinting technique that can potentially be used to deliver results with the same accuracy and sensitivity, within minutes after minimal sample preparation. We tested this hypothesis using attenuated total reflectance (ATR), and high throughput (HT) FT-IR techniques. Three main types of pasteurized milk - whole, semi-skimmed and skimmed - were used and milk was allowed to spoil naturally by incubation at 15 degrees C. Samples for FT-IR were obtained at frequent, fixed time intervals and pH and total viable counts were also recorded. Multivariate statistical methods, including principal components-discriminant function analysis and partial least squares regression (PLSR), were then used to investigate the relationship between metabolic fingerprints and the total viable counts. FT-IR ATR data for all milks showed reasonable results for bacterial loads above 10(5) cfu ml(-1). By contrast, FT-IR HT provided more accurate results for lower viable bacterial counts down to 10(3) cfu ml(-1) for whole milk and, 4 x 10(2) cfu ml(-1) for semi-skimmed and skimmed milk. Using FT-IR with PLSR we were able to acquire a metabolic fingerprint rapidly and quantify the microbial load of milk samples accurately, with very little sample preparation. We believe that metabolic fingerprinting using FT-IR has very good potential for future use in the dairy industry as a rapid method of detection and enumeration.     

FT-IR surface analysis of poly [(4-hydroxybenzoic)-ran-(2-hydroxy-6-naphthoic acid)] fiber – A short review

Instrumental techniques such as Fourier Transform Infrared Spectroscopy (FT-IR) constitute well-studied methodologies for polymer characterization, including polymeric fibers. However, a relatively short number of scientific publications involve the characterization of commercial Poly [(4-hydroxybenzoic)-ran-(2-hydroxy-6-naphthoic acid)] (Vectran™) fiber and its surface species. The majority of the published infrared studies uses the medium infrared region (MIR) associated to the Attenuated total reflection (ATR) method. In this scenario, this short review addresses the characteristics of Vectran™ fiber, sample depth data of each FT-IR spectrum mode, reflection and photo-acoustic spectroscopy (PAS), including near infrared (NIR) analysis. This paper addresses also researches on the characterization of Vectran™ by several FT-IR analysis conditions aiming to contribute to future studies. This brief review deals with methodologies developed in the last decade and published by several scientific research groups, emphasizing studies conducted in the last five years. A critical assessment and trends are also included.     

Helical polyurethane@attapulgite nanocomposite: Preparation, characterization and study of optical activity

Helical polyurethane@attapulgite (BM-ATT) based on R-1,1′-binaphthyl-2′,2-diol (R-BINOL) composite was prepared after the surface modification of attapulgite (ATT). BM-ATT was characterized by Fourier-transform infrared (FT-IR) spectroscopy, X-ray diffraction (XRD), thermogravimetric analysis (TGA), scanning electron microscopy (SEM), transmission electron microscopy (TEM), high resolution transmission electron microscopy (HTEM) and vibrational circular dichroism (VCD) spectroscopy. FT-IR and XRD analyses indicate that the helical polyurethane has been successfully grafted onto the surfaces of the modified ATT without destroying the original crystalline structure of ATT. BM-ATT exhibits the rod-like structure by SEM, TEM, and HTEM photographs. BM-ATT displays obvious Cotton effect for some absorbance in VCD spectrum, and its optical activity results from the singlehanded conformation of helical polyurethane.     

Preparation and Characterization of NiO Nanoparticles Via Solid-State Thermal Decomposition of Nickel(II) Schiff Base Complexes [Ni(salophen)] and [Ni(Me-salophen)]

This study focuses on the preparation and characterization of nickel oxide nanoparticles from nickel(II) Schiff base complexes as new precursors. At first nickel(II) complexes [Ni(salophen)] and [Ni(Me-salophen)] were synthesized and characterized by elemental analyses and FT-IR spectroscopy. Then NiO nanoparticles were prepared by solid-state thermal decomposition at 550 ºC for 3.5 h. The FT-IR spectrum confirmed the composition of products. The crystalline structures and morphology of products were studied by X-ray powder diffraction (XRD), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). XRD results revealed that the obtained products were nickel oxide. SEM and TEM images demonstrated that the NiO nanoparticles have uniform shape with size between 35 and 70 nm.     

介孔Ce-MCM-48的合成及其可见光催化性能研究

分别利用十六烷基三甲基溴化铵(CTAB)、正硅酸乙酯(TEOS)为模板剂和硅源,合成了高度有序的MCM-48材料。通过浸渍法制备了Ce含量不同的MCM-48(Ce-MCM-48s)材料。采用TG-DTA、小角XRD、N2吸-脱附、FT-IR、TEM、XPS和UV-vis等对Ce-MCM-48s进行了表征。XRD、N2吸-脱附和TEM证明Ce-MCM-48s具有与MCM-48相似的三维螺旋立体结构;FT-IR和XPS表明MCM-48孔道及其表面已被Ce氧化物所覆盖。可见光催化降解罗丹明B的实验证明,10%Ce-MCM-48的催化降解效率好于纯CeO2,商用TiO2(P125),5%Ce-MCM-48和15%Ce-MCM-48的。     

Diffusion and structure of water in polymers containing N-vinyl-2-pyrrolidone

Poly(N-vinyl-2-pyrrolidone) (PVP), a water-soluble polymer, is known for its excellent biocompatibility. It is generally recognized that the properties of polymers may be profoundly affected by the structure of water absorbed in them. In this study, Fourier transform infrared (FT-IR) in attenuated total reflection (ATR) and transmission mode was performed to examine the diffusion and structure of water in PVP and its copolymers. The obtained spectra were analyzed using two-dimensional (2D) IR with the aid of density functional theory (DFT) calculations. The 2D IR of time-resolved FT-IR/ATR spectra shows that type II water between 3300 and 3500 cm(-1) occurs earlier during the water absorption process, which is also demonstrated by transmission FT-IR at the initial stage of water absorption. Conversely, type II water changes last when desorption takes place. Results from DFT calculations indicate that type II water might be monomeric or dimeric water molecules interacting with a carbonyl group in the pyrrolidone moiety. Furthermore, it is found that vibrations less than 3300 cm(-1) (type I water) arise from water molecules involved in a carbonyl group interacting with more than two water molecules. It is reasonable that the transmission FT-IR spectra of film with an extra low water amount hardly show vibration bands below 3300 cm(-1); however, this region is distinct in the FT-IR/ATR spectra of fully swollen film. In addition, vibration bands between 3800 and 3500 cm(-1) (type III water) are assigned to free water or water with relatively weak hydrogen bonding, as supported by the transmission FT-IR spectra of polyacrylonitrile (PAN) and the calculation results. Therefore, the diffusion process and the structures of water in PVP and its copolymers can be successfully accessed on the basis of the 2D IR analysis and DFT calculations.     

Comparison of diffuse-reflectance absorbance and attenuated total reflectance FT-IR for the discrimination of bacteria

A collection of bacteria belonging to the genus Bacillus were analysed by diffuse reflectance absorbance and attenuated total reflectance Fourier transform infrared (FT-IR) spectroscopy in the mid-infrared. The diffuse reflectance absorbance method is a rapid whole organism fingerprinting method, which generates a biochemical profile of the bacteria, where samples are presented to the FT-IR spectrometer dried on a metal carrier. The attenuated total reflectance FT-IR used in conjunction with a diamond attenuated total reflectance (ATR) accessory produces a biochemical profile of the surface chemistry of bacteria directly without the need for drying, and has not previously been used in the discrimination of bacteria. Principal component, discriminant function and hierarchical cluster analysis were performed on the data to discriminate the bacteria. The differentiation of the bacteria to species level was observed in both analyses however, it was concluded that the ATR FT-IR illustrated better sub-species differentiation of the microorganisms. This may imply that the total biochemical profiling infers discrimination to species level whereas strain specific markers are present on the cell surface chemistry.     

超声合成Fe3O4@SiO2复合纳米磁性粒子用于质粒DNA的提纯

用超声合成了Fe3O4@SiO2复合纳米磁性粒子, 并用于质粒DNA的提取. 用透射电镜(TEM)、红外光谱(FT-IR)、震动样品磁场计(VSM)、X光电子能谱仪(XPS)等方法对合成的复合磁性粒子的表面形貌、结构、磁性质等进行了表征, 合成的复合磁微粒粒径分布均匀, 在15～20 nm, 磁响应性好. 用该复合磁微粒提取DNA的纯度能达到A260/A280＝ 1.8±0.1, 琼脂糖电泳证明质粒DNA结构基本没有被破坏, 主要为超螺旋结构, 能满足PCR等后续分子生物学操作的要求.     

染料掺杂聚吡咯微纳米管的合成及其影响因素研究

以水溶性染料酸性红G为掺杂剂, 以三氯化铁为氧化剂, 采用无模板自组装方法制备得到了聚吡咯微/纳米管. 利用FTIR, XRD, SEM, TEM对所合成的聚吡咯微/纳米管的结构形貌进行了表征. 结果表明, 搅拌条件下, 酸性红G原位掺杂得到的聚吡咯管直径在100～910 nm之间, 管长大于50 μm. XRD表明所得聚吡咯微/纳米管为无定形态. 研究了反应时间、反应温度、吡咯浓度、掺杂剂与吡咯浓度比、氧化剂滴加速度等对聚吡咯管形貌的影响, 获得了最佳的反应条件.     

油溶性Ag纳米微粒的制备及表征

Surface modified silver nano particles were synthesized in a mixture solvent of water-alcohol with Pyridinium di-n-octadecyldithio phosphate(PyDDP) as a modification agent. Themorphology and structure of DDP-coated Ag (Ag-DDP) nanoparticles were characterized using X-ray powder diffraction(XRD), Transmission electron microscopy(TEM), Fourier transform infrared spectrum (FT-IR) and Thermo gravimetric analysis(TGA). Anti wear properties of Ag-DDP nano particles were tested using a four-ball tribological testing machine. The disperse properties of Ag-DDP nanoparticles were evaluated in solvents such as chloroform, benzen, toluene, liquid paraffin, distilled water and ethanol. The results show that Ag-DDP nanoparticles disperse in organic solvents, but they don’t disperse in water or ethanol. The good disperse properties in organic solvents enable Ag-DDP nanoparticles to be used as oil additives. The XRD pattern of Ag-DDP nanoparticles indicates that they have fcc crystal structure, and the modification layer can prevent the oxidation of Ag nanocores. TEM graphs show that Ag-DDP nanoparticles have a homogeneous grain distribution; the average diameter is about 15nm. FT-IR and TGA curves indicate that the existence of modification layer can prevent the adsorption of water on the surface of nanoparticles. Tribological tests show that Ag-DDP nanoparticles have good anti-wear properties in liquid paraffin, and they can improve the applied load of base oil.     

多孔纳米Ce-M-O (M＝Pr, La)粉末的微波诱导燃烧合成及其表征

使用Ce(NO₃)₃•6H₂O, Pr(NO₃)₃•6H₂O, La(NO₃)₃•6H₂O, 尿素为原料, 利用微波引诱燃烧法合成了多孔纳米Ce-M-O (M＝Pr, La)固溶体. 使用XRD, X光电子能谱仪(XPS), Raman光谱仪, 红外光谱仪(FT-IR), 透射电镜(TEM), 场发射扫描电镜(FE-SEM)等仪器对纳米粉体进行了表征. XRD分析显示Ce-M-O粉体的粒径在20～50 nm之间, 且所有样品均具有萤石结构. XPS证明在Ce-Pr-O固溶体中Pr以＋3和＋4两种形式存在. Raman光谱表明随着M^3＋的掺杂, 在CeO₂晶格中产生氧缺陷, 且缺陷浓度随掺杂量增加不断提高. 红外光谱证明Ce—O键的吸收峰在1400 cm^－1左右, 且由于M^3＋的掺杂在2346 cm^－1的吸收峰消失. TEM照片说明样品具有类盘状的网络纳米微晶结构. 扫描图像说明产物具有多孔的外貌特征, 且孔径分布在2～40 nm之间.     

STUDY ON THE SURFACE MODIFICATION OF NANO-TiO2 BY GRAFTING PMMA／PBMA AND ITS THERMAL STABILITY

The surface of nano-TiO2 was encapsulated with hydroxyl-propyl-methyl cellulose (HPMC), and then cografted with acrylates. Conditions of absorbing and grafting have been studied. Modified nano-TiO2 particles were characterized by FT-IR spectra, TEM and TG analysis. It was convinced from FT-IR studies that both methyl methacrylate (MMA) and butylmethacrylate (BMA) were co-grafted onto the surface of nano-TiO2 particles. TEM images show that the surface of nano-TiO2 particles was successfully modified by a thick layer of film-like polymer. TG results demonstrate that the decomposition temperature of HPMC-g-PMMA/PBMA, which has been grafted onto the surface of nano-TiO2, is 56.9 K higher than that of HPMC-g-PMMA/PBMA.     

硬脂酸Langmuir Blodgett膜的FTIR研究

本文首次测得3—11层硬脂酸LB膜的FTIR-T光谱与测得的1—11层LB膜FTIR-ATR光谱对照表明, 透射技术简便易行, 两种技术研究LB脂结构, 可以起到相互补充的作用, 对于复杂体系LB膜, 两种方法对应的谱带强度比是获得分子片断取向的重要手段。     

Characterization of radix rehmanniae processing procedure using FT-IR spectroscopy through nonnegative independent component analysis

A method is proposed for monitoring the radix rehmanniae proparate processing procedure and determining the endpoint of the process using attenuated total reflectance (ATR) FT-IR through nonnegative independent component analysis (ICA). In the proposed method, ATR FT-IR spectra of the samples were firstly measured at different steaming periods. Then, nonnegative ICA was used for direct estimation of the feature spectra of the pure components in the mixture without pre-separation and other prior information. The estimated independent components (ICs) and their variation of the relative concentrations were used to characterize the processing procedure and determine the endpoint. The results show that the estimated three ICs are consistent with that of the chemical components in the mixtures, i.e. catalpol/rehmaionoside, glucose, and other compounds that nearly keep invariant during the processing procedure. The endpoint determined by the IR-ICA method is 15 h, which was located in the range obtained by expert sensory analysis, whereas the endpoint determined by the traditional sensory analysis is 14 ∼ 17 h and even 14 ∼ 20 h, which showed the significant deviation of the endpoints determined by different operators. Figure Characterisation of radix rehmanniae processing procedure using FT-IR spectroscopy through nonnegative independent component analysis     

Preparation and characterization of gold nanoparticles capped by peptide-biphenyl hybrids

Gold nanoparticles were prepared using peptide-biphenyl hybrids (PBHs) as capping agents. AuNPs were characterized by different techniques including UV-Vis, TEM, EDX, FT-IR, elemental analysis, (1)H NMR and (13)C CP/MAS NMR spectroscopy. TEM analysis showed that AuNPs present diameters in the range of 1.8-3.7 nm, depending on the structure and the amount of the capping PBH used. FT-IR spectroscopy and solid-state (13)C NMR revealed that the carboxylic group of PBHs, especially in the case of the acid ligands, interacts with the gold surface (in the form of carboxylate). The results confirm that PBHs are excellent stabilizers of AuNPs, being one of the first examples on the use of peptidomimetics-gold hybrid materials.     

SURFACE MODIFICATION OF POLYPROPYLENE MICROPOROUS MEMBRANE BY TETHERING POLYPEPTIDES

Two kinds of polypeptides were tethered onto the surface of polypropylene microporous membrane （PPMM） through a ring opening polymerization of L-glutamate N-carboxyanhydride initiated by amino groups which were introduced by ammonia plasma and y-aminopropyl triethanoxysilane treatments. X-ray photoelectron spectroscopy （XPS）, attenuated total reflectance Fourier transform infrared spectroscopy （FT-IR/ATR）, scanning electron microscopy （SEM）, together with water contact angle measurements were used to characterize the modified membranes. XPS analyses and FT-IR/ATR spectra demonstrated that polypeptides are actually grafted onto the membrane surface. The wettability of the membrane surface increases at first and then decreases with the increase in grafting degrees of polypeptide. Platelet adhesion and murine macrophage attachment experiments reveal an enhanced hemocompatibility for the polypeptide modified PPMMs. All these results give evidence that polypeptide grafting can simultaneously improve the hemocompatibility as well as reserve the hydrophobicity for the membrane, which will provide a potential approach to improve the performance of polypropylene hollow fiber microporous membrane used in artificial oxygenator.     

Synthesis and characterization of hollow LiNiO<Subscript>2</Subscript> fibers via sol-electrospinning method

Hollow LiNiO₂ fibers have been prepared with a capillary spinneret electrospinning technique combined with the sol–gel method, and the possible mechanism for the fabrication of the hollow fibers was discussed. The xerogel fibers and those calcined at different temperatures were characterized by thermogravimetric (TG) analysis, X-ray diffractometry (XRD), Fourier transform infrared (FT-IR) spectrum, transmission electron microscopy (TEM), scanning electron microscopy (SEM) and etc. The Polyvinyl Pyrrolidone (PVP) has an important role in the formation of hollow LiNiO₂ fibers.     

Effect of sequential layer-by-layer surface modifications on the surface energy of plasma-modified poly(dimethylsiloxane)

Surface-initiated grafting of N,N-dimethylacrylamide, styrenesulfonate (SS), and (ar-vinylbenzyl)trimethylammonium chloride (VBTAC) from microwave plasma carboxylated, initiator-functionalized poly(dimethylsiloxane) (PDMS) surfaces was accomplished utilizing reversible addition-fragmentation chain transfer (RAFT) polymerization. Surface spectroscopic attenuated total reflectance (ATR) FT-IR analysis and atomic force microscopy (AFM) measurements were utilized to determine surface grafting and morphological surface features. The VBTAC-grafted PDMS provided a smooth, hydrophilic cationic surface for creating layer-by-layer (LBL) surfaces via alternating deposition of well-defined poly(SS) and poly(VBTAC), also prepared via aqueous RAFT. Comparisons of the ATR FT-IR spectra of the LBL assemblies and those of respective anionic poly(SS) and cationic poly(VBTAC) components confirmed strong electrostatic complexation of a fraction of the sulfonate and quarternary ammonium species in the layers as well as the existence of noncomplexed species. AFM images of surface topology indicated the presence of domains, likely phase-separated segments of the respective homopolymers, as well as interlayer mixing. The employed LBL methodology results in formation of stable, highly hydrophilic surfaces on a PDMS substrate. To our knowledge, this is the first study that illustrates surface functionalization of PDMS using microwave plasma and RAFT polymerization, followed by LBL deposition of polyelectrolytes.     

On-line FT-MIR/NIR process analysis

FT-IR spectrometers designed for laboratory operation are generally not suited for plant production areas where ambient temperatures often exceed 120° F and noise levels are extremely high. The Nicolet Pro-IR 5 process FT-IR spectrometer can operate in hostile environments over the spectral range from 10 000 to 250 wavenumbers. We have evaluated the performance of this system using a set of commercial detergent samples and a wide range of gas mixtures. The detergent samples were simultaneously analyzed for twelve components using a sophisticated partial least-squares statistical analysis software package. The concentrations ranged from 0.1 to over 50 wt.-%, with water being the major component. A comparison will be made between the NIR and MIR results using flow-through ATR (attenuated total reflectance) and transmission cells.