A high-precision exact-matching quadruple isotope dilution method (ID4MS) was employed for the quantitation of nitrate in an air-dried spinach powder Certified Reference Material (CRM). The analyte was extracted in hot water following addition of 15NO\({}_{3}^{-}\) internal standard. The blend was then treated with sulfamic acid to remove nitrite and with triethyloxonium tetrafluoroborate to promote aqueous conversion of nitrate into volatile EtONO2. The derivative was analyzed by headspace GC–MS with 3-min elution time. The method performance was validated with a series of tests which demonstrated adequate selectivity and ruggedness. This method supported the development of novel SPIN-1 CRM giving a modest contribution to its uncertainty (uchar = 0.85%). With respect to previous attempts, the SPIN-1 was proven stable, homogeneous (uhom = 0.44%), and suitable for spinach monitoring under EU regulations. On dried basis, the nitrate content of SPIN-1 was found to be 22.53 ± 0.43 mg/g (Uc = 1.9%, k = 2). The material was also used in an inter-laboratory study where four laboratories employed a total of ten measurement methods.
A novel two-step method for the preparation of ( E )-2-chlorovinylthioarenes (or hetarenes) from thiols and 1,1,2-trichloroethane in the phase transfer catalytic systems solid K 2 CO 3 /solid KI/18-crown-6/xylene and solid KOH/18-crown-6/toluene has been developed. ( E )-2-chlorovinylthioarenes were isolated in yields up to 98%. Utilization of ( E )-2-chlorovinylthioarenes in the Heck and Stille reactions has been shown. 相似文献
Kirchberg asked in 2004 whether the commutant of L(H) in its (norm) ultrapower is trivial. Assuming the Continuum Hypothesis, we prove that the answer depends on the choice of
the ultrafilter. 相似文献
Classical molecular dynamics simulations have been performed for crystalline germanium with the aim to estimate the thermal
effects within the first three coordination shells and their influence on the single-scattering and multiple-scattering contributions
to the Ge K-edge extended x-ray absorption fine structure (EXAFS). 相似文献
It is shown to be consistent with set theory that the uniformity invariant for Lebesgue measure is strictly greater than the corresponding invariant for Hausdorff r-dimensional measure where 0<r<1. 相似文献