Deuterium standard

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Heavy water is deuterium oxide, D20. The standard reaction Gibbs free energy for the autoprotolysis of pure deuterium oxide is +84.8 kj-mol 1 at 298 K. (a) If pD is defined analogously to pH, what is the pD of pure D20 at 298 K ... 

The two most common isotopes of oxygen are and 0, and the two natural isotopes of hydrogen are and or D (deuterium). If a sample of carbonate contains Cis moles of and Ci6 moles of then define the heavy light ratio as Ris = Cia/Cie- Similarly, natural water molecules are mostly of three types H O, H] 0, and HD O. For a given sample of water, call the number of moles of each W, W g, and Wq, respectively. Then define the heavyriight ratios as ki8 = Wig/VV and Rp = WqIW. For either water or carbonate, the 5 are defined as deviations of these ratios from standard values for these ratios (call the ratios of the standards Sig and Sq) ... 

When [ H]-labeled precursors are employed the resulting compounds can be used as internal standards for analysis, especially by utilization of mass spectrometric methods. Appropriate deuterated standards are shown in Fig. 7. The introduction of deuterium into the A9-THC precursors can be done with Grignard reagents such as C[ H3]MgI or reducing substances such as LiAl[ H4]. The general procedures for the synthesis with these [ Hj-labeled precursors are the same as described above for the unlabeled compounds [76,78]. 

The method using GC/MS with selected ion monitoring (SIM) in the electron ionization (El) mode can determine concentrations of alachlor, acetochlor, and metolachlor and other major corn herbicides in raw and finished surface water and groundwater samples. This GC/MS method eliminates interferences and provides similar sensitivity and superior specificity compared with conventional methods such as GC/ECD or GC/NPD, eliminating the need for a confirmatory method by collection of data on numerous ions simultaneously. If there are interferences with the quantitation ion, a confirmation ion is substituted for quantitation purposes. Deuterated analogs of each analyte may be used as internal standards, which compensate for matrix effects and allow for the correction of losses that occur during the analytical procedure. A known amount of the deuterium-labeled compound, which is an ideal internal standard because its chemical and physical properties are essentially identical with those of the unlabeled compound, is carried through the analytical procedure. SPE is required to concentrate the water samples before analysis to determine concentrations reliably at or below 0.05 qg (ppb) and to recover/extract the various analytes from the water samples into a suitable solvent for GC analysis. 

Analytical accuracy. The mixture of all deuterium-labeled internal standards is added to each water sample before extraction. This does not prevent the loss of the unlabeled herbicides from the sample in subsequent processing steps, but a proportional loss of the deuterated internal standard precludes the need to correct for recovery. Although referring to recovery in this type of analysis is inappropriate, the accuracy of this method should be monitored. 

At Bayer CropScience, the use of a stable isotope IS has become common practice to eliminate the effects of matrix suppression on instrument signals. The stable isotopes are synthesized by deuterium exchange reactions on authentic native standards or the... 

Solution 10% in deuterium oxide, with 1,4-dioxane as the internal standard.b See Ref. 19.c See Refs. 82 and 83. d These assignments may have to be interchanged. 

Spectroscopic Analysis. Infrared (IR) spectroscopic analysis was performed on a Beckman Microlab 620 MX computing spectrometer. Samples were cast on a sodium chloride pellet or made into a pellet with potassium bromide. and 13C NMR spectra were obtained using a JEOL HNM-FX 270 MHz Fourier transform NMR spectrometer. Samples were dissolved in deuterium chloroform and chemical shifts were referenced to an internal standard of tetramethylsilane. 

Fig. 2. Stochastic accretion models for an open system. The infalling gas is assumed to be extragalactic material with standard Big Bang nucleosynthetic abundances (Xo = 0.758, Yo = 0.242, 2D=6.5xlCP5, SBBN) and zero metals, (a) Star formation rate vs. time for the thin disk. From the top to the bottom the curves refer to 44%, 10%, 5%, 1% and no mass added, (b) Metallicity vs. time for the thin disk. From the top to the bottom the curves refer to standard case (no mass added), 1%, 5%, 10%, 44% of mass added. The metallicity evolution curve illustrates the relatively weak dilution effects that are offset by continuing star formation. Details for the Deuterium abundances are shown in Fig. 3...

There is some disagreement in the literature as to the value of the (4He, H) elastic scattering cross section. Values differing by almost a factor of two have been reported, as reviewed by Paszti et al. (1986). The cross section is strongly non-Rutherford, but ab initio calculations have been reported that agree well with the trend of experimental data and could be used in simulation calculations (Tirira et al., 1990). The cross section for deuterium analysis has a resonance near a 4He+ energy of 2.15 MeV, which allows enhanced sensitivity. Detailed measurements of this cross section have been reported by Besenbacher et al. (1986). In practice, rather than calculate an experiment s calibration from first principles, calibration standards are usually used hydrogen-implanted silicon standard are the norm. 

Sections I-V of this chapter deal with the syntheses of unsaturated organic compounds playing an essential role in biochemical processes of life. Numerous polyunsaturated compounds have been synthesized in order to elucidate their physiological role, for instance in brain. However, the main impact on permanent searches for new improved methods of synthesis of isotopically labelled dienes and polyenes comes from nuclear medicine and nuclear pharmacy. The deuterium and carbon-13 labelled polyunsaturated compounds are needed as internal standards in mass spectral determinations of very low concentrations of biologically active substances in biological fluids. 

Craig, H., Standard for Reporting Concentrations of Deuterium and 0xyqen-18 in Natural Waters. Science, 1961, 133, 1833-1834. 

The carbon-13 NMR spectrum of griseofulvin (Figure 3) was obtained at ambient temperature in DMSO-d containing TMS as internal reference utilizing Varian Associates XL-100-15 spectrometer equipped with Fourier accessories The system was locked to the deuterium resonance frequency of the solvent, and operated at a frequency of 25.2 MHz for carbon-13. The chemical shifts are reported ( c, ppm.) from the Internal standard TMS. 

The nuclear magnetic resonance spectrum of sodium valproate as shown in Figure 3 was obtained on a Varian Associates T-60 NMR Spectrometer in deuterium oxide containing tetramethylsilane as the internal standard. The spectral peak assignments (2) are presented in Table I. 

Because most common solvents, including water, contain protons, and most NMR analyses involve the measurement of protons, a solvent without protons is generally used in NMR spectroscopy. Commonly, solvents in which the hydrogen atoms are replaced with deuterium (i.e., solvents that have been deuterated) are used, the most common being deuterochloroform. In addition, an internal standard, most commonly tetramethylsilane (TMS), is added to the sample in the NMR sample tube (see Figure 14.3, D) and all absorption features are recorded relative to the absorption due to TMS. 

Craig, H. (1961). Standards for reporting concentrations of deuterium and oxygen-18 in natural waters. Science 133 1833-1834. 

N.m.r. spectroscopy T.l.c.-m.s. analysis of oligosaccharides coupled to a lipid amine (neoglycolipids) H n.m.r. spectrum in D20 after exchange of free protons with deuterium Experiments conducted at 295 K, with acetone as the internal standard (set at 2.225 p.p.m. from 4,4-dimethyl-4-silapentane-1-sulfonate) Results compared, to within 0.005 p.p.m. (laboratory-to-la-boratory variation) of data in the literature Conformational studies by n.O.e. experiments Natural-abundance-13C analysis Chemical-shift assignment by 2D H- H and H-13C n.m.r. spectroscopy... 

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