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801.
Double Pore Silica Gel Monolith Applied to Liquid Chromatography 总被引:2,自引:0,他引:2
K. Nakanishi H. Minakuchi N. Soga N. Tanaka 《Journal of Sol-Gel Science and Technology》1997,8(1-3):547-552
Silica gels retaining double pore structure in the size ranges of micrometer and nanometer have been applied to the rod-shaped
monolithic column for liquid chromatography. The macropore structure was designed by controlling the phase separation process
induced by the hydrolysis and polycondensation of alkoxysilane, whereas the mesopore structure was tailored by the solvent
exchange treatments on wet gels. The size exclusion chromatograms on polystyrene standards exhibited almost similar features
for octadecyl-modified rod and conventional packed beads columns. The dependence of plate height on the velocity of mobile
phase determined for amylbenzene was by far weaker in the rod column than in the packed beads column, suggesting that additional
geometrical factors should be considered in describing the separation mechanism in the rod column. 相似文献
802.
The sensitive detection of sulfur-containing analytes is of interest in many industrial applications; selective detection is also desirable since these compounds are usually present at trace levels in difficult matrixes. The purpose of this article is to review the use of the Sievers® ozone-based sulfur chemiluminescence detector, and its coupling with gas chromatography, supercritical fluid chromatography, and high performance liquid chromatography. Detection limits, linearity, response factors, and selectivity are discussed for each of these techniques. Critical operational parameters for the SCD are also described. The use of other sulfur selective detectors for SFC and HPLC is also briefly summarized. 相似文献
803.
804.
Yozo Kosaka Toshiyuki Uryu 《Journal of polymer science. Part A, Polymer chemistry》1995,33(13):2221-2232
Side-chain liquid-crystalline copolymers and polymer blends containing an electron-donating (carbazolylmethylene)aniline group and electron-accepting nitrophenyl groups with various central linking groups between aromatic groups in the mesogenic units, i.e., N?CH, CH?CH, N?N, and COO, were prepared to examine effects of the mesogenic structure on thermal behaviours. The most remarkable effects of the central linking group on the thermal properties and the miscibility were observed for the polymer blends. The 1:1 miscible polymer blends were prepared from the electron-donating polymer containing (carbazolylmethylene)aniline group (PM6Cz) and the electron-accepting polymers with similar central linking groups, i.e., N?CH, CH?CH, and N?N. For example, the 1: 1 polymer blend of PM6Cz and the electron-accepting polymer containing the nitrostilbene group induced a smectic phase from 73 to 207°C. This isotropic temperature was 46°C higher than the calculated value (161°C) based on the composition without the electron donor-acceptor interaction. On the other hand, the 1: 1 polymer blend of PM6Cz and the electron-accepting polymer containing the nitrophenylbenzoate group showed phase separation. Thus, the remarkable thermal stability and the miscibility of the polymer blends containing the electron donor and acceptor groups might be caused by planar structures between the mesogenic side groups which have similar central linking groups through the electron donor-acceptor interaction. A similar tendency was seen for copolymers and binary mixtures of both low-molecular-weight compounds containing the same mesogenic groups. © 1995 John Wiley & Sons, Inc. 相似文献
805.
Summary There are a number of reagents available for fluorescent labelling of primary amines. These include dansyl chloride, o-phthalaldehyde,
fluorescamine, and a new reagent, 9-fluorenylmethylchloroformate (FMOC), reported recently. This paper describes a reversed-phase
HPLC procedure for the separation and fluorescence detection of polyamines following pre-column derivatization with FMOC.
The polyamines studied by this method include putrescine, cadaverine, spermidine, and spermine. Experiments were carried out
to determine maximum fluorescence excitation and emission wavelengths, optimum reaction pH, linear ranges, and minimum detection
limits for each of the polyamines. The HPLC method includes a gradient program which provides complete separation from serum
hydrolysate components and specificity for the four polyamines with detection limits ranging from 2 to 9 pg. This procedure
was applied to hydrolyzed serum samples. 相似文献
806.
Summary A high-performance liquid chromatographic method, with 9-anthryldiazomethane as derivatizing agent, has been developed for
the simultaneous determination ofN-carbamoyl aspartate andl-dihydroorotate in serum. Sample preparation for 1 mL serum was by simple liquid-liquid extraction and then derivatization.
The compounds were separated on a Luna C18(2) column by use of a gradient prepared from acetonitrile and 10 mM sodium acetate
buffer, pH 6.0, and fluorimetric detection was performed at excitation and emission wavelengths of 365 nm and 412 nm, respectively.
The response was found to be linearly dependent on concentration between 0.8 and 60 μg mL−1 forl-dihydrooratate and between 0.9 and 90 μg mL−1 forN-carbamoyl aspartate; the mean recovery rates were 50 and 51%, respectively. The limits of detection and quantification were
0.33 μg mL−1 and 0.6 μg mL−1, respectively, forl-dihydroorotate and 0.4 μg mL−1 and 0.7 μg mL−1 forN-carbamoyl aspartate. This method can be used to assess accumulation ofN-carbamoyl aspartate andl-dihydroorotate in body fluids in situations where cellular pyrimidine de novo synthesis is impaired. 相似文献
807.
The molar enthalpies of the solid–solid and solid–liquid phase transitions were determined by differential scanning calorimetry
for pure TbCl3 and KTb2Cl7, RbTb2Cl7, CsTb2Cl7, K3TbCl6, Rb3TbCl6 and Cs3TbCl6 compounds. Both types of compounds, i.e. M3TbCl6 and MTb2Cl7 (M=K, Rb, Cs) melt congruently and show additionally a solid–solid phase transition with a corresponding enthalpy Δtrs
H
0 of 6.1, 7.6 and 7.0 kJ mol–1 for potassium, rubidium and caesium M3TbCl6 compounds andΔtrs
H
0 of 17.1 (rubidium) and of 12.1 and 10.9 kJ mol–1 (caesium) for MTb2Cl7 compounds, respectively. The enthalpies of fusion were measured for all the above compounds with the exception of Rb3TbCl6 and Cs3TbCl6. The heat capacities of the solid and liquid compounds have been determined by differential scanning calorimetry (DSC) in
the temperature range 300–1100 K. The experimental heat capacity strongly increases in the vicinity of a phase transition,
but varies smoothly in the temperature ranges excluding these transformations. C
p data were fitted by an equation, which provided a satisfactory representation up to the temperatures of C
p discontinuity. The measured heat capacities were checked for consistency by calculating the enthalpy of formation of the
liquid phase, which had been previously measured. The results obtained agreed satisfactorily with these experimental data.
This revised version was published online in August 2006 with corrections to the Cover Date. 相似文献
808.
Historically, due to the size and nature of the instrumentation, highly skilled laboratory professionals performed clinical
testing in centralized laboratories. Today’s clinicians demand realtime test data at the point of care. This has led to a
new generation of compact, portable instruments permitting ”laboratory” testing to be performed at or near the patient’s bedside
by nonlaboratory workers who are unfamiliar with testing practices. Poorly controlled testing processes leading to poor quality
test results are an insidious problem facing point of care testing today. Manufacturers are addressing this issue through
instrument design. Providers of clinical test results, regardless of location, working with manufacturers and regulators must
create and manage complete test systems that eliminate or minimize sources of error. The National Committee for Clinical Laboratory
Standards (NCCLS) in its EP18 guideline, ”Quality management for unit-use testing,” has developed a quality management system
approach specifically for test devices used for point of care testing (POCT). Simply stated, EP18 utilizes a ”sources of error”
matrix to identify and address potential errors that can impact the test result. The key is the quality systems approach where
all stakeholders – professionals, manufacturers and regulators – collaboratively seek ways to manage errors and ensure quality. We illustrate the use of one quality systems approach, EP18, as a means to advance the quality of test results at point of
care.
Received: 26 June, 2002 Accepted: 17 July 2002
Presented at the European Conference on Quality in the Spotlight in Medical Laboratories, 7–9 October 2001, Antwerp, Belgium
Abbreviations NCCLS National Committee for Clinical Laboratory Standards (formerly) · POCT point of care testing · QC quality control ·
HACCP hazard analysis critical control points · CLIA clinical laboratory improvement amendments (of 1988)
Correspondence to S. S. Ehrmeyer 相似文献
809.
R.K.B GoverN.D. Withers S. AllenR.L. Withers J.S.O. Evans 《Journal of solid state chemistry》2002,166(1):42-48
SnP2O7 is a member of the ZrP2O7 family of materials, several of which show unusual thermal expansion behavior over certain temperature ranges and which show a number of displacive phase transitions on cooling from high temperature. Here we describe the structural properties of SnP2O7 from 100 to 1243 K as determined by X-ray and neutron powder diffraction. These studies reveal that SnP2O7 shows two phase transitions in this temperature range. At room temperature the material has a pseudo-cubic 3×3×3× superstructure. Electron diffraction studies show that the symmetry of this structure is P213 or lower. On warming to ∼560 K it undergoes a phase transition to a structure in which the subcell reflections show a triclinic distortion; above 830 K the subcell reflections show a rhombohedral distortion. Significant hysteresis in cell parameters is observed between heating and cooling. The structure of SnP2O7 is discussed with references to other members of the AM2O7 family of materials. 相似文献
810.
本文通过XRD、SEM、EDS研究了Ti0.4Zr0.1V1.1Mn0.5Cr0.1Nix(x=0,0.2,0.4,0.6,0.8)合金的相结构和电化学性能。该合金系由BCC结构的V基固溶体主相和六方结构的C14 Laves第二相组成,Ni能够促进第二相的生成,Ni含量的增加导致了各相中的化学组成和晶格参数的变化,并通过电化学方法研究了Ni含量对0.4Zr0.1V1.1Mn0.5Cr0.1合金电极的最大放电容量、自放电性能、高倍率放电性能、循环稳定性能等的影响。 相似文献