A PROTOCOL FOR ANALYSIS

In this section, a protocol for analysis of cementitious materials by nitrogen adsorption is proposed and degassing conditions for preserving the microstructure of anhydrous and hydrated cement samples are described. When using these recommended sample preparation conditions, the obtained values have shown to be reproducible and reliable. 

Rossbach M, Ostapczuk P, Emons H (1998) Microhomogeneity of candidate reference materials Comparison of solid sampling Zeeman-AAS with INAA. Fresenius J Anal Chem 360 380-383. Rossbach M, Stoeppler M (1987) Use of CRMs as mutual calibration materials and control of synthetic multielement standards as used in INAA. J Radioanal Nud Chem Artides 113 217-223. Sargent M (1995) Development and application of a protocol for quality assurance of trace analysis. Anal Proc 32 71-76. 

There have been very few method development processes proposed for 2DLC. One study (Schoenmakers et al., 2006) is titled A protocol for designing comprehensive two-dimensional liquid chromatography separation systems. This study advocates that one initially chooses the first-dimension maximum acceptable analysis time, the first-dimension maximum workable pressure drop, and the smallest first-dimension column diameter. The first two variables are then used to construct a Poppe plot (Poppe, 1997)—pronounced Pop-puh (Eksteen, 2007). 

J. Gobom, M. Schuerenberg, M. Mueller, D. Theiss, H. Lehrach, and E. Nordhoff. a-Cyano-4-hydroxycinnamic Acid Affinity Sample Preparation. A Protocol for MALDI-MS Peptide Analysis in Proteomics. Anal. Chem., 73(2001) 434-438. 

Shah AJ, de Biasi V, Taylor SG, Roberts C, Hemmati P, et al. 1999. Development of a protocol for the automated analysis of amino acids in brain tissue samples and microdialy-sates. J Chromatogr B 735 133-140. 

Figure 3 shows a flow chart that outlines the protocol for analysis both of synthetic wastewater and waters encountered in field tests at Ft. Eustis, Va. 

The philosophy of a preliminary survey analysis is used to help define the extent of potential risk (Level I analysis). Data gathered in the Level I survey analysis is used as a protocol for more detailed analysis (Level II). At Level III, a detailed analysis is made as a function of system parameters and time. 

A class of statistical methods frequently used to analyze kinetic and thermodynamic data. Most of these methods require a preliminary estimate of the constants followed by cycles of iterative calculations that converge on a final value(s). Cleland has presented a protocol for the statistical estimation of kinetic data. A nonlinear analysis has also been applied to progress curves. ... 

The CPMP (2001) Points to Consider on Application with 1. Meta-Analysis 2. One Pivotal Study indicates that it is good practice to write a protocol for the meta-analysis ... 

We conclude that developing a protocol for efficient population transfer between a subset of states in a physical system requires a careful examination of the influence of background states. An analysis that is based only on the properties of a small subset of states may not be robust when those states are embedded in a dense manifold of other states. 

Busch, Kenneth A. Memoranda to Deputy Director, DLCD, Dated 1/6/75, 11/8/74, Subject "Statistical Protocol for Analysis of Data from Contract CDC-99-74-45."... 

If sample analysis is to be conducted by a commercial analytical laboratory, the investigator and the laboratory personnel should jointly review available sampling techniques to select the best sampling strategy and establish a protocol for the delivery and storage of collected samples. 

The core technology used in the analysis of aroma chemicals is gas chromatography (GC) therefore, foods must be sampled so they can be introduced on to a GC column. For liquid samples it is possible to inject them into split, splitless, or on-column injectors directly. This is the preferred method for the analysis of synthetic aromas, essential oils, and aroma standards however, solid or dilute liquid samples need to be extracted, distilled, or gas-phase generated in order to obtain useful results. This unit begins with simple direct analysis of a synthetic flavor (see Basic Protocol 1) followed by the analysis of a dilute liquid sample by solvent extraction (see Basic Protocol 2). It ends with a protocol for determining retention indices (see Support Protocol). 

Lu, F., and Ralph, J., 1997, Derivatization followed by reductive cleavage (DFRC method), a new method for lignin analysis protocol for analysis of DFRC monomers, J. Agr. Food Chem. 45 2590-2592. 

Raw data generated by the Phenotype Pfinder protocol is maintained in a dedicated database. The database automatically graphs the data, generates statistical analyses of assays, and flags those assays which show a statistically significant difference between WT and KO mice. The data can be searched and viewed by either specific KO line or assay. The database also offers a tool for analysis of historically accumulated control data sorted by genetic background. 

Fluorescent and metal decorated viral nanoparticles for structural analysis Probe reactivity of carboxylates present on the solvent-exposed surface Addressability of tyrosines and a protocol for covalently stitching together adjacent subunits of the capsid Probing the addressability of CPMV and gaining structural information of the viral capsid... 

Once the material has been chosen for sampling and storage, it is important to establish a protocol for the collection of milk samples. The extraction will be achieved manually or by means of a plastic milk extractor, a new one for each sampling. The nipple and the skin around it should be cleaned with soap and distilled water before collection. The milk thus collected should then be stored in plastic containers previously decontaminated, as explained above. The containers should be labeled and kept at — 20°C until analysis. 

Even the least pernickety experimenter recognizes that all the basic details of laboratory procedures have to be planned well before putting hand to test-tube and yet it seems normal practice (especially among academics) that statistical analysis is the merest after-thought. The author recently reviewed a protocol for a postgraduate project that blithely asserted when all the data have been collected, a statistician will be consulted to show the results are significant . 

In this chapter, we provide protocols to determine the ability of a peptide to mediate DNA internalization in cultured human tumor cells. Fluorescence-assisted cell sorting (FACS) analysis is used to obtain quantitative data on the time and temperature dependence of macromolecular delivery. Confocal microscopy is used to study the subcellular localization in both fixed and live cells. Fluorescently labeled transferrin and dextran are used to label the clathrin-dependent (15) and the non-clathrin, non-caveolar (16) endocytic compartments, respectively. Expression of a caveolin-l-YFP fusion protein is used to label cell surface caveolae and intracellular caveosomes (17). Finally a protocol, for the overexpression of dominant-negative dynamin [GTPase deficient dynamin-2 containing the amino acid substitution K44A (18)] is provided to evaluate the dynamin dependence of the uptake mechanism. 

The analysis of acrolein in wastewater and water-miscible wastes or soils with low levels of contamination can be performed using EPA methods 603 and 8030, respectively (EPA 1982a, 1986b). In closely related techniques, an aliquot of water is subjected to a purge and trap protocol, and the sample is thermally desorbed onto a GC for analysis and quantitation. For waste samples not miscible with water or for soil samples with high levels of contamination, the sample can first be... 

Mueller, M., Theiss, D., Lehragh, H., Nordhoff, E. (2001). a-Cyano-4-hydroxycinnamic acid affinity sample preparation. A protocol for MALDI-MS peptide analysis in proteomics. Anal. Chem. 73, 434 38. 

Granado, F. Ohnedilla, B. Gil-Martinez, E. Blanco, 1.2001. A fast, reliable and low-cost saponification protocol for analysis of carotenoids in vegetables. J. Food Comp. Anal. 14 479 89. 

A protocol for risk assessment of unlisted migrants should be developed that is pragmatic, cost-effective and accepted by both industry and legislative authorities. In this protocol, exposure, toxicology and chemical analysis should be combined. A possible combination would be the approach described above of relating exposure to the threshold of toxicological concern (TTC) principle. This would determine the analytical boundaries for screening of... 

Does the contractor provide a protocol of analysis or a certificate of compliance for each lot of product at the time of shipment as well as copies of completed batch records ... 

Before any sample can be subjected to chromatography, some type of sample preparation is required, which can be as simple as filtration or an involved solid-phase extraction protocol. Sample preparation is that activity or those activities necessary to prepare a sample for analysis. The ultimate goal of sample preparation is to provide the component of interest in solution, free from interferences and at a concentration appropriate for detection. This entry will briefly discuss seven topic areas included in sample preparation standard methods, solid-phase extraction (SPE), matrix solid-phase dispersion (MSPD), solid-phase microextraction (SPME), microdialysis, ultraliltration (UF), and automated systems. 

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