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991.
The microwave acid digestion method was applied to the decomposition of rock samples and optimum conditions were investigated. Samples of 10–100 mg were decomposed by changing the amount and composition of acid, heating time and number of reheating steps and then the concentrations of Si, Fe, Mn, Na, K and Mg in these samples were measured. The concentrations agreed with reported values when 10 mg of sample were decomposed by heating for 60 s with 0.3 ml of concentrated HNO3 and 0.1 ml of concentrated HF. Similarly, 100 mg of sample were also decomposed successfully by heating for 45–110 s with 0.3–1.0 ml of concentrated HNO3 and 0.4–0.7 ml of concentrated HF. It is concluded that the microwave acid digestion method decomposes rock samples with a very short heating time and with small amount of reagents compared with methods using conventional sealed PTFE vessels, which require several hours for the heating step and several millilitres of reagents. 相似文献
992.
V. Yu. Korotaev Yu. A. Skorik A. Yu. Barkov M. I. Kodess A. Ya. Zapevalov 《Russian Chemical Bulletin》2005,54(11):2545-2549
3,3,3-Trifluoro-N′-(3-trifluoromethylphenyl)-1,2-propanediamine (5) was synthesized by the reaction of 2-diazo-1,1,1-trifluoro-3-nitropropane or 3,3,3-trifluoro-1-nitropropene with 3-aminobenzotrifluoride
followed by the reduction of the nitro group. The Michael 1,4-addition of diamine 5 to acrylic acid occurs only at the N(1) atom and affords N-mono-or N,N-dicarboxyethyl derivatives 6 and 7, depending on the reactant ratio. Protolytic equilibria 5–7 in aqueous solutions were studied by pH-potentiometry and UV spectroscopy. Only the aliphatic amino group can be protonated
in an aqueous solution, while the aromatic amino group remains unprotonated even in 12 M HCl. The stability constants of transition metal (Cu2+, Ni2+, Zn2+) complexes with ligands 5–7 were determined by pH-potentiometric titration. The stability of the complexes and selectivity of the ligands toward Cu2+ ions increase with an increase in the number of N-carboxyethyl groups.
Published in Russian in Izvestiya Akademii Nauk. Seriya Khimicheskaya, No. 11, pp. 2465–2469, November, 2005. 相似文献
993.
Sánchez-Machado DI López-Cervantes J López-Hernández J Paseiro-Losada P Simal-Lozano J 《Biomedical chromatography : BMC》2004,18(2):90-97
A high-performance liquid chromatographic (HPLC) method is described for determination of the ratio of beta-d-mannuronic acid to alpha-l-guluronic acid (M/G ratio) in dietary fibre of edible seaweeds. Total dietary fibre (TDF) content was determined gravimetrically. The TDF fraction was hydrolysed with 12 m and 1 m H(2)SO(4), then neutralized with AG 4 x 4 resin. The uronic acids were separated in a Tracer Extrasil SAX 5 micro m column (25 cm x 4 mm) at 35 degrees C, with 2 mm KH(2)PO(4) containing 5% methanol as mobile phase at a fl ow rate of 1.5 mL/min. The detection wavelength was UV 210 nm. The chromatographic identifications of beta-d-mannuronic acid and alpha-l-guluronic acid were confirmed by liquid chromatography-mass spectrometry (LC-MS). The method precision was 1.4% for beta-d-mannuronic acid and 3.5% for alpha-l-guluronic acid. The method was used to determine M/G ratio in canned seaweeds (Saccorhiza polyschides and Himanthalia elongata) and in dried seaweeds (H. elongata, Laminaria ochroleuca, Undaria pinnatifida, Palmaria sp. and Porphyra sp.). 相似文献
994.
铜(Ⅱ)-邻菲咯啉-(邻菲咯啉-5,6-二酮)络合物的合成及其同脱氧核糖核酸的作用 总被引:9,自引:0,他引:9
以邻菲咯啉(phen)、邻菲咯啉-5,6-二酮(dione)为配体首次合成了高氯酸邻菲咯啉-邻菲咯啉-5,6-二酮(Ⅱ)。用荧光光谱,摩尔比,粘度,MLCT减色效应,平衡常数以及荧光能量转移研究了各合物与鱼精子DNA的结合情况,证实了该络合物与DNA存在插入作用。基于络合物对DNA能量转移造成荧光量子产率比值(Φλ/Φ320)的降低,解释了不同波长激发光下,荧光发射峰在加入DNA后产生猝灭和增强两种绝然不同的现象。 相似文献
995.
B.V. Timokhin A. I. Golubin O. V. Vysotskaya V. A. Kron L. A. Oparina N. K. Gusarova B. A. Trofimov 《Chemistry of Heterocyclic Compounds》2002,38(8):981-985
Non-catalytic addition of 1,2,4-triazole to vinyl ethers and esters occurs on heating (65-175°C, 4-20 h) to give Markovnikov adducts (yield 30-100%). Electron-deficient alkenes (acrylonitrile, acrylic acid, 4-phenyl-3-buten-2-one) react with 1,2,4-triazole (78-190°C, 4-20 h) to give anti-Markovnikov adducts in yields of 45-83%. 相似文献
996.
在水溶液中培养了镨、钕、钇与甘氨酸形成的三元配合物。元素分析和热分析表明,该配合物可用Pr_xNd_yY_z(Gly)_6(H_2O)_4(ClO_4)_6·5H_2O(X+y+z=2)表示其分子式。X射线衍射方法测定了其单晶结构,结果表明,该晶体属三斜晶系,空间群P1,化学式Pr_(0.775)Nd_(0.700)Y_(0.525)Cl_6O_(45)N_6C_(12)H_(48),M_r=1466.09,晶胞参数如下:a=11.564(1),b=14.118(3),c=15.668(2)A,α=96.99(1),β=102.72(1),γ=105.33(1)°,晶胞体积V=2362(1)A~3,Z=2,D_c=2.060g/cm~3,结构偏离因子R=0.032,R_w=0.048。晶胞中存在两个络合单元,每个单元可用M_1M2(Gly)_6(ClO_4)_6(H_2O)_4.5H_2O表示,M_1=0.4Pr+0.375Nd+0.225Y,M2=0.375Pr+0.325Nd+0.30Y。三种稀土元素按一定比例统计性地占有两个格位。羧基以桥式联结金属离子,形成一维链式聚合物结构。在络合单元中,一个稀土离子是9配位,其配位多面体为畸变? 相似文献
997.
Cengiz Soykan Ramazan Coskun Ali Delibas Ertan Sahin 《高分子科学》2007,(5):491-500
2-Acrylamido-2-methy1-1-propanesulfonic acid(AMPS),and maleic acid(MA)copolymerized with different feed ratios using N,N-dimethylformamide as a solvent and benzoyl peroxide(Bz_2O_2)as an initiator at 70℃.Structure and composition of copolymers for a wide range of monomer feed were determined by elemental analysis(content of N for AMPS-units).Monomer reactivity ratios for AMPS(M_1)-MA(M_2)pair were determined by the application of conventional linearization methods such as Fineman-Ross(F-R),Kelen-Tüd(?)s(KT)and Extended Kelen-Tüds(EKT)and a nonlinear error invariable model method using a computer program RREVM.The characterizations were done by Fourier transform infrared spectroscopy(FTIR),differential scanning calorimetry(DSC)thermal gravimetry analysis(TGA),and and X-ray diffraction.The antimicrobial effects of polymers were also tested on various bacteria,and yeast. 相似文献
998.
将含有1.0%普鲁士蓝的碳黑与固体石蜡按2.5∶1(质量比)混合后装入φ0.2mm的石英毛细管中,在其上端插入一铂丝并抛光后即制成普鲁士蓝修饰碳黑微电极.对多巴胺(DA)及抗坏血酸(VC)在此电极上的电化学行为及应用此电极测定两组分的最佳条件进行了研究,在定量测定中采用二次微分线性扫描伏安法.在最佳条件下,DA与VC的峰电流(i″p)分别与各自的浓度保持如下线性关系DA为4.0×10-6~8.0×10-4mol·L-1,VC为6.0×10-5~1.0×10-3mol·L-1;检出限(3σ)依次为2.0×10-6mol·L-1及1.0×10-5mol·L-1.应用此方法分析了3种含DA及VC的混合溶液,测得结果的相对标准偏差(n=8)依次小于2.0%及3.0%,回收率范围依次为96.5%~101.0%及95.0%~102.5%. 相似文献
999.
Johannes Häusler 《Monatshefte für Chemie / Chemical Monthly》1982,113(10):1213-1216
Meldrum's acid (2) is acylated by diketen affording the acylMeldrum's acid3. In aqueous bicarbonate its 3-oxogroup is selectively reduced by sodium tetrahydroborate giving the alcohol4, which readily undergoes cyclization in refluxing dioxane leading to the title pyrone7. Under identical conditions3 produces the pyrone6 with the pyrone carboxylic acid5 as intermediate. 相似文献
1000.
本文对不同立构的聚甲基丙烯酸(PMAA)进行了热表征。实验结果表明,在30℃~200℃内未出现玻璃化转变。间同PMAA分别在-245℃和-280℃发生脱水反应和脱羧,而全同PMAA只在-185℃观察到脱水反应。这种热稳定性的明显差别与不同立构PMAA链上相邻羧酸距离有关。实验数据证实PMAA脱水反应为无规反应,服从一级动力学反应方程。脱水温度和间同立构含量成正比,脱水反应活化能间同PMAA比全同PMAA高~7Kcal/mol。 相似文献