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1.
肝中茚满二酮类杀鼠剂固相萃取-紫外导数光谱检测法 总被引:2,自引:0,他引:2
报道了肝中敌鼠,氯敌鼠,杀鼠酮三种茚满二酮类杀鼠剂的题示检测方法。肝匀浆先用乙腈或二甲基甲酰胺浸提,浸提液用6%高氯酸溶液或0.1mol/L氢氧化钠溶液稀释,然后加入GDX101大孔树脂萃取,肝中杀鼠剂萃取率约80%,检出限为1μg/g以下 相似文献
2.
氯化三辛基甲基胺萃取原子吸收法测定微量锑的研究 总被引:1,自引:1,他引:0
本文在KI-H2SO4体系中,研究了锑的碘络阴离子的萃取行为,并结合火焰原子吸收法测定了微量锑,萃取体积比(V水/V有)为20,线性范围为0-2μg/ml,锑的特征浓度为0.5μg/ml/1%吸收,检出限为0.1μg/ml。 相似文献
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固相萃取—紫外导数光谱法测定血中茚满二酮类抗凝血杀鼠剂 总被引:3,自引:1,他引:3
报道了血中敌鼠、氯敌鼠、杀鼠酮的题示测定方法。该法操作简便快速、回收率高,灵敏度较高,萃取使用国产高分子多孔微球GDX301,价廉易得。三种杀鼠剂以10mg/L量分别加于血中,回收率依次为100.5%±2.9%、101.5%±1.3%及99.3%±1.5%;血中三种杀鼠剂检出限分别为0.4、0.6及0.4mg/L。 相似文献
4.
萃取—缝管原子捕集原子吸收法测定水中碲(Ⅳ)和磅(Ⅵ) 总被引:8,自引:0,他引:8
研究了碲(Ⅳ)和碲(Ⅵ)在DDTC-CCl4体系中的萃取和反萃取行为,并用缝管原子捕集技术结合火焰原子吸收法测定了水样中的碲(Ⅳ)和碲(Ⅵ),特征浓度为1.2g/L/1%吸收,检出限0.2μg/L,相对标准偏差1.7%,富集倍中达100%。 相似文献
5.
PBA光纤化学传感器在线监测家兔口服呋喃妥因的尿药浓度 总被引:1,自引:0,他引:1
芘丁酸光纤化学传感器(PBA—FOCS)用于在线测定家兔口服呋喃妥因后排出尿液中的药物浓度。方法的检出限为1.3μg/mL,线性范围1~100μg/mL,精密度(RSD)1.5~3.5%,回收率在95.0~100%之间。4只雄性家兔的尿药浓度—时间曲线显示达峰时间为3.5h,6h累积尿药排出百分率为21%。实验结果显示传感器、测定池和仪器系统设计合理。可实时、在线测定生物体液中的药物浓度并达到实用水平。 相似文献
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2,3—二氨基萘荧光分光光度法测定环境水样中的痕量亚硝酸盐 总被引:1,自引:0,他引:1
本文描述了用2,3-二氨基萘荧光分光光度法测定水样中亚硝酸盐的最佳测定条件,并测定了井水和湖水中的亚硝酸盐,测定样品的检出限为0.4μg/L,线性范围是1.0-1500μg/L相对标准偏差为1.6%,加标回收率为95%-106%。本法简便,快速,准确度高,共存离子干扰小,样品无须萃取步骤。 相似文献
8.
碱性氢化物发生—火焰原子吸收光谱法测定锡 总被引:7,自引:2,他引:7
对Sn-NaOH-KBH4体系进行了系统研究,采用三乙醇胺-EDTA联合干扰抑制剂,可消除一定量铁及合金元素的干扰,对于锡含量小于0.01%的试样,用苯萃取锡后所有元素不干扰测定。测定液中锡量为0-4μg/10ml,呈线性关系,灵敏度为0.004mg/L/1%,检出限为0.008mg/L,测定钢中大于0.001%锡,结果满意。 相似文献
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氢化物发生电感耦合等离子体原子发射光谱法同时测定水和生物样品中… 总被引:13,自引:0,他引:13
研究了一种小型同心氢化物发生配置一个气液分离器后与多道ICP-AES联用,同时测定水和生物样品中砷、铋、锑、硒的方法。检出限为砷0.4μg/L,铋0.5μg/L,锑1.4μg/L,硒0.5μg/L,相对标准偏差为砷2.7%,铋1.5%,锑2.7%,硒1.9%。用本法测定美国和国家标准物质中的氢化元素,结果满意。 相似文献
11.
H. Schumann 《Angewandte Chemie (International ed. in English)》1969,8(12):937-950
The preparation, properties, and reactions of the compounds named in the title are described, with particular reference to the possible participation of (p→d)π components in the bonding between the group IVB and the group VB elements. 相似文献
12.
Dr. Wenlong Yang Dr. Jorge H. S. K. Monteiro Prof. Ana de Bettencourt‐Dias Prof. Vincent J. Catalano Prof. Wesley A. Chalifoux 《Angewandte Chemie (International ed. in English)》2016,55(35):10427-10430
The design of a relatively simple and efficient method to extend the π‐conjugation of readily available aromatics in one‐dimension is of significant value. In this paper, pyrenes, peropyrenes, and teropyrenes were synthesized through a double or quadruple benzannulation reaction of alkynes promoted by Brønsted acid. This novel method does not involve cyclodehydrogenation (oxidative aryl–aryl coupling) to arrive at the newly incorporated large arene moieties. All of the target compounds were synthesized in moderate to good yields and were fully characterized with the structures unambiguously confirmed by X‐ray crystallography. As expected, photophysical characterization clearly shows increasing red‐shifts as a function of extended conjugation within the fused ring systems. 相似文献
13.
C. Peter Sebastian Constanze Fehse J. Paul Attfield Sudhindra Rayaprol Rainer Pöttgen 《Journal of solid state chemistry》2006,179(8):2376-2385
The rare earth-silver-stannides YAgSn, TmAgSn, and LuAgSn were synthesized from the elements by arc-melting and subsequent annealing. The three stannides were investigated by X-ray powder and single-crystal diffraction: NdPtSb type, P63mc, Z=2, a=468.3(1), pm, wR2=0.0343, 353 F2 values, 12 variables for YAgSn, and ZrNiAl type, P6¯2 m, a=726.4(2), , wR2=0.0399, 659 F2 values, 15 variables for TmAgSn, and a=723.8(2), , wR2=0.0674, 364 F2 values, 15 variables for LuAgSn. Besides conventional laboratory X-ray data with monochromatized Mo radiation, the structures were also refined on the basis of synchrotron data with , in order to clarify the silver-tin ordering more precisely. YAgSn has puckered, two-dimensional [AgSn] networks with Ag-Sn distances of 278 pm, while the [AgSn] networks of TmAgSn and LuAgSn are three-dimensional with Ag-Sn distances of 279 and 284 pm for LuAgSn. Susceptibility measurements indicate Pauli paramagnetism for YAgSn and LuAgSn. TmAgSn is a Curie-Weiss paramagnet with an experimental magnetic moment of 7.2 μB/Tm. No magnetic ordering is evident down to 2 K. The local environments of the tin sites in these compounds were characterized by 119Sn Mössbauer spectroscopy and solid-state NMR (in YAgSn and LuAgSn), confirming the tin site multiplicities proposed from the structure solutions and the absence of Sn/Ag site disordering. Mössbauer quadrupolar splittings were found in good agreement with calculated electric field gradients predicted quantum chemically by the WIEN2k code. Furthermore, an excellent correlation was found between experimental 119Sn nuclear magnetic shielding anisotropies (determined via MAS-NMR) and calculated electric field gradients. Electronic structure calculations predict metallic properties with strong Ag-Sn bonds and also significant Ag-Ag bonding in LuAgSn. 相似文献
14.
Piers WE Bourke SC Conroy KD 《Angewandte Chemie (International ed. in English)》2005,44(32):5016-5036
Boron cations are elusive and highly electrophilic species that play a key role in the chemistry of boron. Despite early interest in the chemistry of boron cations, until recently they have largely remained chemical curiosities. However, hints at harnessing their potential as potent electrophiles have begun to appear and developments in weakly coordinating anion technology suggest that this is an area of research that is ripe for exploration. It has been nearly 20 years since the last major review on boron cations; herein we summarize the progress in the area since that time. 相似文献
15.
Wenlong Yang Jorge H. S. K. Monteiro Ana deBettencourt‐Dias Vincent J. Catalano Wesley A. Chalifoux 《Angewandte Chemie (Weinheim an der Bergstrasse, Germany)》2016,128(35):10583-10586
The design of a relatively simple and efficient method to extend the π‐conjugation of readily available aromatics in one‐dimension is of significant value. In this paper, pyrenes, peropyrenes, and teropyrenes were synthesized through a double or quadruple benzannulation reaction of alkynes promoted by Brønsted acid. This novel method does not involve cyclodehydrogenation (oxidative aryl–aryl coupling) to arrive at the newly incorporated large arene moieties. All of the target compounds were synthesized in moderate to good yields and were fully characterized with the structures unambiguously confirmed by X‐ray crystallography. As expected, photophysical characterization clearly shows increasing red‐shifts as a function of extended conjugation within the fused ring systems. 相似文献
16.
A systematic quantum chemical investigation of mono-, di-, and triaminoborane, -alane, -gallane, and -indane is carried out to determine quantitatively the effects of pi bonding and negative hyperconjugation on structures, energetics, and rotational barriers in these systems. Pi bonding plays a significant role in the aminoborane compounds, but becomes rapidly less significant in the aminoalanes, -gallanes, and -indanes. For each main-group metal X investigated, X-N rotational barriers are found to be essentially equal depending only on the number of remaining in-plane amino groups. The contribution of negative hyperconjugation to reducing rotational barriers, as assessed from natural bond orbital (NBO) delocalization energies, is independent of the pyramidalization of the out-of-plane amino group, and is also dependent only on the number of rotated groups. Optimized tris[bis(trimethylsilyl)amino]-substituted structures of boron, aluminum, gallium, and indium are found to compare quite well with available experimental structural data, and exhibit X-N torsion angles that are independent of the central metal atom. 相似文献
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A new protocol for the Ullmann-type arylation process of different aromatic heterocycles without any transition-metal catalyst, implying the use of a combination of an excess of potassium hydroxide and dimethyl sulfoxide, is described. The reaction can be performed between a broad range of starting nucleophiles including phenol, alcohols, amines, nitrogen-containing five-membered systems such as pyrazoles, imidazoles, and indoles, and amides with haloarenes, iodide and bromide derivatives giving the best results, the possible pathway involving the in situ generation of the corresponding benzyne intermediate. When the reaction was performed with 2-iodoaniline and either carboxamides or isothiocyanato derivatives, the corresponding benzoazole derivatives were obtained. 相似文献
19.
V. V. Gavrilenko L. A. Chekulaeva I. A. Savitskaya I. A. Garbuzova 《Russian Chemical Bulletin》1992,41(11):1957-1959
A convenient and practical method is proposed for the synthesis of lanthanide and yttrium alkoxides. The method involves dissolving the metals or their hydrides in a solution of dry HCl in the corresponding alcohol, with subsequent dehalogenation of the LnCl3 solution by an equivalent amount of alkali metal (Na, Li), The rareearth alkoxides are easily converted into acetylacetonates Ln(acac)3 by the action of acetylacetone.A. N. Nesmeyanov Institute of Elementoorganic Compounds, Russian Academy of Sciences, 117813 Moscow. Translated fromIzvestiya Akademii Nauk, Seriya Khimicheskaya, No. 11, pp. 2490–2493, November, 1992. 相似文献
20.
Rolf W. Saalfrank Norbert Löw Bernhard Demleitner Dietmar Stalke Markus Teichert 《Chemistry (Weinheim an der Bergstrasse, Germany)》1998,4(7):1305-1311
Efficacious metal control of self-assembly of dialkylketipinate dianions leads to completely different supramolecular assemblies. The structures of grid 1 , double-decker 2 , triple-decker 3 , and metalla-spherand 4 were characterized by X-ray crystallographic analyses or by NMR spectroscopy. 相似文献