13C CP-MAS NMR spectroscopy is a technique that has proved to be useful in studying soil organic matter (SOM). Nevertheless, NMR spectra exhibit a weak signal and have very low resolution due to: the low natural abundance of 13C (1.1 % of C) in SOM, the generally low SOM content of soils, and the presence of paramagnetic impurities. This paper studies the effects of soil chemical pre-treatments on 13CP-MAS NMR spectra quality and spectra representativity i.e. soil C mass balance.
After chemical pre-treatment to increase total organic carbon (TOC) content and C/Fe ratio, eight soils characterized by different levels of organic carbon content and C/Fe ratios were studied using 13CP-MAS NMR. Moreover, where chemical treatments were not applicable due to high carbon losses, the number of 13CP-MAS NMR scans was increased in order to obtain satisfactory spectra.
Results show that chemical pre-treatment of soils with C/Fe > 1 caused high C losses. Bulk soils were therefore studied by increasing the number of 13CP-MAS NMR scans. Acceptable spectra were obtained from 8K scans (1K = 1024 transient). On the other hand, even when a large number of scan (32K) are used, soil with C/Fe < 1 cannot be studied. As these soils are characterized by low C losses after HCl treatments (range of 2.9–25.4%), a pre-treatment of at least 1.39 mol l−1 HCl removes excess Fe and at the same time increases C/Fe ratio resulting in 32K scans providing good spectra. 相似文献
A solid phase extraction method for the determination of gold(III) at trace levels by flame atomic absorption spectrometer
(FAAS) was developed. The method was based on retention of gold as chloro complexes through the Amberlite XAD-2000. The effect
of some analytical parameters including hydrochloric acid concentration, sample volume, sample and eluent flow rates, eluent
volume, eluent concentration and interfering ions on the recovery of gold(III) was investigated. The retention of gold(III)
from 1.5 mol l−1 HCl solution and the recovery of gold with 0.07 mol l−1 NH3 solution were quantitative (≥95%). The relative standard deviation (RSD) was calculated as 3.2% (n = 10). The detection limit for gold was 2 μg l−1. The accuracy was checked with the determination of gold spiked an artificial seawater and a pure copper samples. 相似文献
Cellulose nitrate membrane filter was used for the preconcentration-separation of Cu, Co, Cd, Pb and Cr ions. The analyte
ions were collected on the membrane filter by the aid of carmine. Then membrane filter was dissolved by using nitric acid.
The levels of the analytes in the final solutions were determined by flame atomic absorption spectrometry (FAAS). The analytical
parameters including pH, amounts of carmine, sample volumes etc. have been optimized. No influences have been observed from
the matrix ions. The detection limits for analytes were in the range of 0.08 μg/l-0.93 μg/l. The validation of the procedure
was checked by the analysis of standard reference sediment (GBW 07309). The present method has been successfully applied for
the FAAS determinations of analyte ions in real samples including black tea and magnesium salts. 相似文献
Growth, accumulation and intracellular speciation and distribution of copper (Cu) in Sesbania drummondii was studied using scanning-electron microscopy (SEM), X-ray absorption near edge structure (XANES) and extended X-ray absorption fine structure (EXAFS). The growth of seedlings was assessed in terms of biomass accumulation. The growth of the seedling was enhanced by 73.5% at a low Cu concentration (50 mg l−1) compared to the control treatment. Additionally, seedling growth was inhibited by 18% at 300 mg l−1 Cu with respect to the control. Copper concentration in roots and shoots was increased with increasing Cu concentration in the growth solution. The accumulation of Cu was found to be higher in roots than in the shoots. At a concentration of 300 mg l−1 Cu, the roots accumulated 27,440 mg Cu kg−1 dry weight (dw) while shoots accumulated 1282 mg Cu kg−1 dw. Seedlings were assessed for photosynthetic activity by measuring chlorophyll a fluorescence parameters: Fv/Fm and Fv/F0 values. Photosynthetic integrity was not affected by any of the Cu treatments. The X-ray absorption spectroscopic (XAS) studies showed that Cu was predominantly present as Cu(II) in Sesbania tissue. In addition, from the XAS studies it was shown that the Cu exists in a mixture of different coordination states consisting of Cu bound to sugars and small organic acids with some possible precipitated copper oxide. From the EXAFS studies, the coordination of Cu was determined to have four equatorial oxygen(nitrogen) ligands at 1.96 Å and two axial oxygen ligands at 2.31 Å. Scanning-electron microscopy studies revealed the distribution of Cu within the seedlings tissues, predominantly accumulated in the cortical and vascular (xylem) regions of root tissues. In the stem, most of the Cu was found within the xylem tissue. However, the deposition of Cu within the leaf tissues was in the parenchyma. The present study demonstrates the mechanisms employed by S. drummondii for Cu uptake and its biotransformation. 相似文献
The effect of long-term exposure to high frequency electromagnetic field (HF EMF) on some somatic and neural characteristics
was studied in neurodefective Lurcher mutant (+/Lc) and normal wild type mice (+/+). Both newborn and young adult (3 months)
animals derived from two strains (C3H, B6CBA) were exposed to HF EMF (870 MHz) from 1st to 21st day or from 91st to 120th
day respectively. In animals of both groups and controls we observed the development of body weight. Moreover, in the HF EMF
exposed adult B6CBA animals we studied spatial learning ability, motor functions and the CNS excitability. To investigate
specific energy absorption rate (SAR) in experimental animals we have done the basic 3D calculations of the electromagnetic
energy distribution in the simplified model of the mouse. The HF EMF exposed animals exhibited mild differences of body weight
between them and unexposed controls. The long-term exposure to HF EMF did not significantly influence the ability to learn
in the Morris water maze. However, significant lower swimming speed was found in the irradiated +/Lc as well as lower motor
activity of +/+ in the open field when compared to controls. No significant differences were found between HF EMF irradiated
animals and controls in examination of the CNS excitability and motor functions. 相似文献