Fluorescence spectroscopy sample preparation

See also Environmental and Agricultural Applications of Atomic Spectroscopy Environmental Applications of Electronic Spectroscopy Geology and Mineralogy, Applications of Atomic Spectroscopy Inorganic Compounds and Minerals Studied Using X-Ray Diffraction IR and Raman Spectroscopy Studies of Works of Art IR Spectroscopy Sample Preparation Methods MRI of Oil/Water in Rocks X-Ray Fluorescence Spectrometers. 

The performance of microwave-assisted decomposition of most difficult samples of organic and inorganic natures in combination with the microwave-assisted solution preconcentration is illustrated by sample preparation of carbon-containing matrices followed by atomic spectroscopy determination of noble metals. Microwave-assisted extraction of most dangerous contaminants, in particular, pesticides and polycyclic aromatic hydrocarbons, from soils have been developed and successfully used in combination with polarization fluoroimmunoassay (FPIA) and fluorescence detection. 

For the preparation of samples for X-ray fluorescence spectroscopy, lithium metaborate is the preferred flux because lithium does not give rise to interfering X-ray emissions. The fusion may be carried out in platinum crucibles or in crucibles made from specially prepared graphite these graphite crucibles can also be used for the vacuum fusion of metal samples for the analysis of occluded gases. 

The limit of detection by Raman spectroscopy was 3-5 weight % for the oxime ester and methacrylonitrile for these samples. The shorter time required to reduce background fluorescence in those samples filtered through activated charcoal indicates that more careful sample preparation and purification would lower this limit. 

Raman spectroscopy can offer a number of advantages over traditional cell or tissue analysis techniques used in the field of TE (Table 18.1). Commonly used analytical techniques in TE include the determination of a specific enzyme activity (e.g. lactate dehydrogenase, alkaline phosphatase), the expression of genes (e.g. real-time reverse transcriptase polymerase chain reaction) or proteins (e.g. immunohistochemistry, immunocytochemistry, flow cytometry) relevant to cell behaviour and tissue formation. These techniques require invasive processing steps (enzyme treatment, chemical fixation and/or the use of colorimetric or fluorescent labels) which consequently render these techniques unsuitable for studying live cell culture systems in vitro. Raman spectroscopy can, however, be performed directly on cells/tissue constructs without labels, contrast agents or other sample preparation techniques. 

Preparation of an ultrasonic slurry of the sample is occasionally used, as for example in the determination of cobalt, nickel and copper [200], selenium [39] and arsenic and antimony [40]. Extraction of leaves with a chloroform solution of xanthate completely extracted cadmium [41,103]. X-ray fluorescence spectroscopy is a nondestructive method of analysing plant materials if they can be converted into a suitable form for presentation to the instrument. 

In this work we utilized FTIR methods to examine the SA monolayers on flat, polar solid surfaces prepared from nonpolar solutions. We used ATR and GI FTIR measurements to characterize the material and bonding of the S A monolayers, and used transmission and ATR FTIR to monitor the dynamics of the SA adsorption process. With reference to measurements on standard Langmuir-Blodgett monolayer samples, we were able to quantify the S A kinetic results. We also used fluorescence spectroscopy of incorporated pyrene probes in S A mixed monolayer films as a simple method for the determination of the relative adsorption and thermodynamic constants. 

Bulk spectroscopic techniques such as x-ray fluorescence and optical and infrared spectroscopies involve minimal sample preparation beyond cutting and mounting the sample. These are discussed in Section 9.2.1. Spectroscopic techniques such as wavelength dispersive spectroscopy (WDS) and energy dispersive spectroscopy (EDS) are performed inside the SEM and TEM during microscopic analysis. Therefore, the sample preparation concerns there are identical to those for SEM and TEM sample preparation as covered in Section 9.3. Some special requirements are to be met for surface spectroscopic techniques because of the vulnerability of this region. These are outlined in Section 9.5. 

Overall methods using either different or no sample preparation procedures and various detection techniques have also been compared. Thus, fine ambient aerosol was analysed for 11 elements by using US-assisted slurry formation for 15 min prior to AAS, as well as by X-ray fluorescence spectroscopy and laser ablation ICP-MS. Sample treatments were found to provide similar results. However, the detection techniques compared the number of target analyte elements to be determined, detection limits and purchase costs [10],... 

These techniques fall into two categories those considered as routine (e.g. atomic absorption and emission spectroscopy, X-ray fluorescence) and a growing number of microanalytical surface techniques (e.g. laser microprobe mass analysis [LAMMA] and sensitive high-resolution ion microprobe [SHRIMP]). Each analytical technique requires specific sample preparation prior to analysis, as summarised in Table 13.1. 

The second method (ASTM D-4294, IP 477) uses energy-dispersive X-ray fluorescence spectroscopy, has slightly better repeatability and reproducibility than the high-temperature method, and is adaptable to field applications but can be affected by some commonly present interferences such as halides. In this method, the sample is placed in a beam emitted from an X-ray source. The resultant excited characteristic X radiation is measured, and the accumulated count is compared with counts from previously prepared calibration standard to obtain the sulfur concentration. Two groups of calibration standards are required to span the concentration range, one standard ranges from 0.015% to 0.1% w/w sulfur and the other from 0.1% to 5.0% w/w sulfur. 

Photo-acoustic spectroscopy has been used for ultratrace levels of Hg in air and snow (de Mora etal. 1993). X-ray fluorescence is nondestructive, rapid, requires minimal sample preparation, and was, for example, used successfully to determine the maximal level of mercury in maternal hair to assess fetal exposure (Toribora et al. 1982). However, the procedure is less sensitive compared to AAS and INAA if no pre-concentration is used. Electrochemical methods have been replaced as detectors in chromatography by other instrumental techniques because of poorer detection limits. High-performance liquid chromatography (HPLC) with reductive amperometric electrochemical reduction, however, was shown to be capable of speciating Hg(II), methyl- ethyl- and phenylmercury, with detection limits <2pgL (Evans and McKee 1987). 

The method to be employed for measurement of the analytical signal largely determines the form of the sub-sample and, consequently, the extent and type of sample preparation required. Nuclear activation methods, x-ray fluorescence techniques, graphite furnace atomic absorption, classical emission spectroscopy and many mass spectrome-... 

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