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31.
A technique for the separation and preconcentration of Cr(VI) and Cr(III) in fresh waters is presented. The analytical procedure involves the use of anion- and cation-exchange columns. The columns are eluted and the eluate is analysed for chromium using a graphite furnace atomic absorption spectrometer. The recovery of Cr(VI) and Cr(III) is 97.86 ± 1.31% and 102.36 ± 1.25% (95% confidence), respectively. The detection limits are 0.019 and 0.020 μg 1?1 for 200 ml of sample (twice the standard deviation of eleven replicate blanks). The method is rapid and the need for minimum sample handling avoids contamination problems. 相似文献
32.
磷酸三丁酯萃取原子吸收光谱法测定微量Cr(Ⅲ)和Cr(Ⅵ) 总被引:2,自引:0,他引:2
常用的 APDC-MIBK 和 DDTC-MIBK 萃取原子吸收法一般只能测至十几个ppb 浓度的铬,且需在较高温度下进行萃取.本文报道一种用磷酸三丁酯(TBP)萃取原子吸收光谱法测定微量 Cr(Ⅲ)和 Cr(Ⅵ)的方法.实验表明,Cr_2O_7在盐酸介质中可与 TBP 形成 Cr(Ⅵ)-TBP-Cl-溶剂化合物,借此可测定0-0.25μg·ml~(-1)浓度范围内的 Cr(Ⅵ).若用 KMnO_4将平行试样中的 Cr(Ⅲ)氧化为 Cr(Ⅵ),测得总铬量,通过差减法即可算出Cr(Ⅲ)的含量.本法灵敏度高,准确度好. 相似文献
33.
Density functional calculations were performed on bonding and structural features of [(ηn-BH4)TM(CO)4]− (n = 1, 2, 3; TM = Cr, Mo) complexes. Calculations show that the ground state is bidentate which is in good agreement with experimental results. It has been found that the bridge and terminal hydrogen atoms will interchange by two pathways: (i) twist of BH4 about one of the bridge B-H and (ii) twist of BH4 about one of the terminal B-H. The molecular orbital calculations and natural bond orbital methodologies for different isomers of these complexes have been evaluated. The final results indicate that case (i) is more preferable relative to another case. 相似文献
34.
Cr(Ⅲ)—5—Br—PADAP—Triton X—100析相光度法测定微量铬的研究 总被引:1,自引:0,他引:1
研究Cr(Ⅲ)-5-Br-PADAP-Triton X-100析相显色体系,建立测定微量铬的析相光度法。在pH 4.5乙酸-乙酸钠介质中,Cr(Ⅲ)、5-Br-PADAP、Triton X-100加热形成的配合物,于95℃恒温浴中析相1h,即被Triton X-100相完全富集,最大吸收峰为593nm,铬含量在0~10μg/5ml服从比耳定律,以硫脲、锰-EDTA、柠檬酸钠、氟化钾为掩蔽剂,测定水样中微量铬,获得满意结果。 相似文献
35.
The reactivity of a Cr‐Te multilayer film consisting of 326 Cr/Te double‐layers with about 88(3) at% Te was investigated with in‐situ X‐ray diffraction. The occurrence of a superstructure reflection caused by the multilayer system is observed. During the annealing procedure between 80 and 90 °C the layer‐by‐layer arrangement is destroyed and elemental Te crystallizes. After 6 h isothermal annealing at 140 °C CrTe3 starts to crystallize. The amount and the crystal size of CrTe3 increase with raising temperature and Te is consumed during the growth process. At 220 °C the formation of crystalline Cr2Te3 is observed and between 220 and 260 °C CrTe3 is completely decomposed into Cr2Te3. The two Cr tellurides grow as highly textured materials. The size of CrTe3 crystals is significantly larger than that of Cr2Te3. For a co‐deposited Cr‐Te film with composition 77(3) at% Te the tri‐telluride and elemental Te crystallize simultaneously. The texture of CrTe3 is less pronounced and different reflections of the tri‐telluride occur besides the (h00)‐reflections. Up to 160 °C a pronounced increase of the crystallite size is observed and the crystals are significantly larger than those obtained with the multifilm sample. At 130 °C the crystallization kinetics seem to be controlled by nucleation. 相似文献
36.
Toshikatsu Takanami 《Tetrahedron letters》2005,46(16):2893-2896
The catalytic Z-selective Claisen rearrangement of simple aliphatic allyl vinyl ethers can be achieved using a chromium(III) porphyrin complex, Cr(TPP)Cl, as a catalyst: Cr(TPP)Cl significantly enhances reversal of E-Z selectivity in the thermal Claisen rearrangement of allyl vinyl ethers, especially, 4,5- and 4,6-disubstituted derivatives, at low catalyst loading. 相似文献
37.
Photoluminescence, absorption and excitation spectra of K2LiAlF6 single crystals doped with 1% of Cr3+ are presented. The near-infrared photoluminescence observed at room temperature, 77 and 4 K are attributed to the zero-phonon spin-allowed 4T2(4F)→4A2(4F) transition of Cr3+ octahedrally coordinated by F− ions. Lifetimes are obtained. The 4 K emission broad band was described in terms of normal modes of the octahedral complex [CrF6]3−. The Racah, crystal-field and Huang-Rhys parameters are calculated and the quantum efficiency and thermal quenching estimated and compared with Cr3+ properties in different environments. 相似文献
38.
二溴羟基苯基荧光酮—乳化剂OP荧光熄灭法测定微量铬(Ⅵ) 总被引:11,自引:3,他引:11
本文基于Cr(Ⅵ)-二溴羟基苯基荧光酮(DBH-PF)-OP体系的荧光熄灭效应,提出一种测定痕量铬(Ⅵ)的新荧光方法。在pH2.4-4.1的HCl-NaAc缓冲介质和OP存在下,Cr(Ⅵ)与DBH-PF形成1:2的橙红色络合物,络合物的最大激发发工和发射波长分别是365mm和528nm。铬(Ⅵ)量在0.05-1.5μg/25ml范围内与△F呈线性关系,检测限是2.0ng/ml。方法用于电镀废液,废 相似文献
39.
Removal of humic matter interference in the determination of Cr(VI) in soil extracts by the diphenylcarbazide method 总被引:1,自引:0,他引:1
Alkaline digestion of soil samples, which is recommended for minimizing Cr(III)–Cr(VI) interconversions during the extraction of Cr(VI), may also solubilize humic matter (HM). The latter is responsible for both positive and negative interference in the analysis of Cr(VI) in the extract by the diphenylcarbazide (DPC) method. Humic compounds indeed absorb light at 540 nm as the Cr-DPC product and are also able to rapidly reduce Cr(VI) under the pH conditions of the standard DPC method. To prevent any risk of interference and make the DPC method applicable to soil extracts, a new protocol is proposed. This consists of three successive steps: (1) extraction of Cr(VI) by the U.S.EPA method 3060A in the presence of Mg2+; (2) batch removal of solubilised HM by the XAD-7 sorbent at pH 3.0 ± 0.1 with 3–5 min contact time; (3) analysis of Cr(VI) with the DPC method at pH 3.0 ± 0.1. The application of this new protocol to the soil product SQC-012 Lot 4 certified by R.T. Corporation (RTC, USA) gave significantly lower Cr(VI) concentrations and smaller variability compared to certified values (46.5 ± 2.3 instead of 153 ± 32.6 mg/kg). The new protocol was validated by Cr(VI) and Cr(III) spikes either to the soil/extractant suspension or to the exctract. Cr(VI) results in the wide range of acceptance limits (104–202 mg/kg) reported by RTC were only obtained when the U.S.EPA method 3060A without the addition of Mg2+ and DPC analysis at pH 1.0 were applied. The latter procedure appears questionable since it leads to largely variable results which reflect the complex role played by humic matter in the determination of Cr(VI) and the instability of Cr(III) during the extraction. 相似文献
40.
A method for the determination of trace Cr(III) in aqueous solution by solid-phase microextraction (SPME) coupled with gas chromatography (GC)-flame photometric detection (FPD) was developed. Aqueous Cr(III) was first converted to the volatile chromium trifluoroacetylacetonate (Cr(tfa)3) by derivatization with 1,1,1-trifluoroacetylacetone (Htfa), followed by SPME extraction using a polyimide-coated silica fiber. The distribution constants (K) of derivatized cis- and trans-Cr(tfa)3 between the polyimide phase and aqueous phase were 2012 and 2214, respectively. The two Cr(tfa)3 isomers extracted can be efficiently separated by a DB-210 GC column within 9 min. Selective detection of Cr was performed by a FPD equipped with a 385-nm long-pass filter. Linearity (r> 0.99) over the concentration range 5-300 ng ml(-1) Cr was obtained and the limit of detection was 2 ng ml(-1) Cr. The relative standard deviation was 7% at 10 ng ml(-1) Cr (n = 5). Applicability of this method to water analysis was tested by analyzing the chromium content in a reference standard water sample and an industrial effluent. 相似文献