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吴诚 《理化检验(化学分册)》2007,43(8):705-706
第三次沉淀是草酸沉淀,经过前两次分离,干扰稀土(Ⅲ)最终以草酸盐沉淀的共存元素已经除去。这次沉淀是以草酸盐的形式得到稀土的沉淀并最终得到符合化学计量要求的稀土氧化物。应予说明,试样如含有钇及钪,在整个分离过程中均与稀土元素在一起,故最终也包括在总稀土的含量之中。 相似文献
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吴诚 《理化检验(化学分册)》2006,42(3):235-236
2.1.2 沉淀草酸稀土时草酸的加入量及溶液的酸度条件与稀土的氢氧化物和氟化物相比,草酸稀土沉淀的溶解度相对较大,因此,溶液体积不宜太大和稀土离子的量不宜太少是进行草酸稀土沉淀时的两项基本要求。为使草酸稀土的沉淀尽可能地完全,一般要求 相似文献
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吴诚 《理化检验(化学分册)》2006,42(2):151-152
2金属材料中稀土元素的测定2.1重量测定法重量测定法常应用于稀土元素含量较高的合金的分析。可用稀土-硅-镁中间合金作为例子说明稀土总量的重量测定法在这种合金的分析中的应用。稀土硅镁之间合金的主成分是硅、稀土、铁和镁,同时还含少量或微量的钙、锰、钛、铝、磷等元素。此外,由于稀土矿源不同,可能会含有某些特殊元素。例如包头稀土矿还给合金带入一定量的钍。表1中列举了几种稀土-硅-镁合金标准物质的组份,供参考。根据这一合金的组成,在最终进行稀土元素的沉淀、灼烧及称量之前必须先使稀土与共存的干扰测定的元素分离,然后选择一… 相似文献
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吴诚 《理化检验(化学分册)》2005,41(4):300-301,304
(8)钨酸沉淀重量法测定钨的一项缺点是所得到的钨酸虽经多次洗涤仍然吸附带人一定量的其他共存元素,如硅、铁、钛、铬、钼、钒、铌、钽等,因而随后灼烧所得的三氧化钨是不纯的,其中夹杂了上述元素的氧化物。因此,在最终取得钨的测定结果之前要用各种方法将夹杂在三氧化钨中的其他元素的氧化物一一测定,将所测得的结果换算成氧化物的质量从不纯三氧化钨的质量中减去。几种主要的国内外标准方法中所用的测定这些夹杂元素的方法可大致归纳如下。 相似文献
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吴诚 《理化检验(化学分册)》2008,44(2):196-196,201
(2)草酸盐沉淀重量法测定铝合金中稀土总量(详见GB/T 6987.32-2001). 此方法适用于含稀土总量ω(RE)≥1.5%~10%的铝合金. 相似文献
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《分析试验室》2016,(11)
试样经酸分解后,加氢氟酸沉淀稀土,分离除去Ni,Mn,Fe,Co等元素;用硝酸和高氯酸破坏滤纸并溶解沉淀,经氨水分离再次沉淀稀土,过滤去除Ni,Co,M g等元素;用盐酸溶解沉淀,在p H 1.8~2.0的条件下用草酸沉淀稀土,以分残余离Ni,Co,Al等杂质,灼烧至恒重完成稀土总量测定。本方法适合稀土总量的测定范围为25.00%~45.00%,测定结果相对标准偏差在0.39%~0.44%之间,标准加入回收率为98.7%~102.3%。同时选择8家试验室进行数据比对,并将精密度数据进行正态分布检验、等精度检验和可疑值检验,检验结果均符合要求。采用本方法测定贮氢合金中的稀土总量准确、稳定,可用于仲裁判定。 相似文献
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Levuglandins (LGs) and isolevuglandins (isoLGs), formed by rearrangement of endoperoxide intermediates generated through the cyclooxygenase and free radical induced oxidation of polyunsaturated fatty acids (PUFAs), are extraordinarily reactive, forming covalent adducts incorporating protein lysyl ε-amino groups. Because they accumulate, these adducts provide a dosimeter of oxidative injury. This review provides an updated and comprehensive overview of the generation of LG/isoLG in vitro and in vivo and the detection methods for the adducts of LG/isoLG and biological molecules in vivo. 相似文献
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Journal of Solution Chemistry - Enthalpies of solution of purine and adenine in water and in demethylsulfoxide were measured calorimetrically in the temperature range 25–40°C. ΔH s... 相似文献
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Héloïse Thérien‐Aubin Ariella Lukach Natalie Pitch Prof. Eugenia Kumacheva 《Angewandte Chemie (International ed. in English)》2015,54(19):5618-5622
The entropically driven coassembly of nanorods (cellulose nanocrystals, CNCs) and nanospheres (dye‐labeled spherical latex nanoparticles, NPs) was studied in aqueous suspensions and in solid films. In mixed CNC‐latex suspensions, phase separation into an isotropic latex‐NP‐rich and a chiral nematic CNC‐rich phase took place; the latter contained a significant amount of latex NPs. Drying the mixed suspension resulted in CNC‐latex films with planar disordered layers of latex NPs, which alternated with chiral nematic CNC‐rich regions. In addition, fluorescent latex NPs were embedded in the chiral nematic domains. The stratified morphology of the films, together with a random distribution of latex NPs in the anisotropic phase, led to the films having close‐to‐uniform fluorescence, birefringence, and circular dichroism properties. 相似文献
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Determination of diazepam and nordazepam in milk and plasma in the presence of oxazepam and temazepam 总被引:1,自引:0,他引:1
For studies on the excretion of drugs into milk a sensitive high-performance liquid chromatographic assay was developed to quantitate diazepam and nordazepam in the milk and plasma of humans and rabbits in the presence of their major metabolites, oxazepam and temazepam. Flurazepam was used as an internal standard. The assay involves extractions with diethyl ether and an additional acid clean-up step. Chromatographic separation was achieved by a LiChrospher 60 RP-select B (5 microns) column and KH2PO4- acetonitrile (69:31, v/v) adjusted to pH 2.80 as a mobile phase. The same extraction and chromatographic conditions were suited to both types of samples, milk and plasma. The limits of determination using ultraviolet detection at 241 nm was for diazepam 20 ng/ml and for nordazepam 15 ng/ml. The absolute recoveries of diazepam, nordazepam and flurazepam in human milk were 84, 86 and 92% and in human plasma 97, 89 and 94%, respectively. The within- and between-day accuracy and precision for diazepam and nordazepam in milk and plasma at all concentrations tested (20-1500 ng/ml) were better than 8%. The high fat content which occurs in rabbit milk presented no limitation for the extraction of lipophilic diazepam: the method was successfully used to monitor milk and plasma concentrations of diazepam and nordazepam in lactating New Zealand White rabbits during 26-h infusions of diazepam (1.4 mg/h). 相似文献
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Nagaraju M. Patro Azmi Sultana Keiji Terao Daisuke Nakata Ayako Jo Akihito Urano Yoshiyuki Ishida Raghu N. Gorantla Vinay Pandit Kshama Devi Shishir Rohit Baljinder K. Grewal Elizabeth M. Sophia Anand Suresh Vineeth K. Ekbote Sarasija Suresh 《Journal of inclusion phenomena and macrocyclic chemistry》2014,78(1-4):471-483
In the present study investigated the effect of curcumin (CUR) alpha (α), beta (β) and gamma (γ) cyclodextrin (CD) complexes on its solubility and bioavailability. CUR the active principle of turmeric is a natural antioxidant agent with potent anti-inflammatory activity along with chemotherapeutic and chemopreventive properties. Poor solubility and poor oral bioavailability are the main reasons which preclude CUR use in therapy. Extent of complexation was β-CD complex (82 %) > γ-CD (71 %) > α-CD (65 %). Pulverization method resulted in significant enhancement of CUR (0.002 mg/ml) solubility with CUR α-CD complex (0.364 mg/ml) > CUR β-CD complex (0.186 mg/ml) > CUR γ-CD complex (0.068 mg/ml). Gibbs-free energy and in silico molecular docking studies favour formation of α-CD complex > β-CD complex > γ-CD complex. With reference to CUR, relative bioavailability of CUR α-CD, CUR β-CD and CUR γ-CD complexes were 460, 365 and 99 % respectively. CUR–CD complexes exhibited increased bioavailability with an increase in t½, tmax, Cmax, AUC, Ka, and MRT; and a decrease in Ke, clearance and Vd values. AUC increase was CUR α-CD complex > CUR β-CD complex > CUR γ-CD complex. Significant difference (p < 0.05) was observed between CUR α-CD complex and CUR γ-CD complex by one-way ANOVA and Dunnett’s post hoc test for multiple comparison analysis. Correlation observed between in vitro, in vivo and in silico methods indicates potential of in silico and in vitro methods in CD selection. 相似文献
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Electrochemical Fluorination of Benzamide and Acetanilide in Anhydrous HF and in Acetonitrile 总被引:1,自引:0,他引:1
Shainyan B. A. Danilevich Yu. S. Grigor’eva A. A. Chuvashev Yu. A. 《Russian Journal of Organic Chemistry》2004,40(4):513-517
Electrochemical fluorination of benzamide in anhydrous hydrogen fluoride does not involve the amide group but occurs exclusively at the aromatic ring, yielding isomeric fluoro- and difluorobenzamides and 3,3,6,6-tetrafluoro-1,4-cyclohexadienecarboxamide. Electrochemical fluorination of benzamide in acetonitrile as solvent gives the same products, as well as benzonitrile and its fluorinated derivatives and products of hydrolysis and fluorination of acetonitrile. Electrochemical fluorination of acetanilide in anhydrous HF leads to complete tarring of the reaction mixture, while its fluorination in acetonitrile results in selective formation of m-fluoroacetanilide. 相似文献
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M. Yu. Antipin Yu. T. Struchkov I. F. Shishkov A. V. Golubinskii T. L. El'fimova L. V. Vilkov A. A. Bredikhin A. N. Vereshchagin S. M. Ignatov V. F. Rudchenko R. G. Kostyanovskii 《Russian Chemical Bulletin》1986,35(10):2040-2046
Conclusions It has been established by the methods of x-ray diffraction analysis and electron diffraction analysis and measurements of the dipole moments and the birefringence that in the crystalline and gaseous phases, as well as in solution, N,N-dimethoxyamine has a gauche-gauche conformation, which is stipulated by a stabilizing nO-N-O* orbital interaction. The geometric parameters of the molecule have been determined.Translated from Izvestiya Akademii Nauk SSSR, Seriya Khimicheskaya, No. 10, pp. 2235–2242, October, 1986. 相似文献