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71.
meso-四(3,5-二溴-4-羟基苯基)卟啉[T(DBHP)P]二阶导数光度法同时测定废水中锌和铅的研究 总被引:2,自引:0,他引:2
本文研究了meso-四(3,5-二溴-4-羟基苯基)卟啉与铅,锌显色反应的二阶导数光谱行为,建立了同时测定电镀废水中锌和铅的二阶导数光度法。在硼砂-氢氧化钠碱性介质中,沸水浴上加热3min,锌、铅的显色反应即可定量完成。比耳定律范围分别为:0~10μg/25mLZn ̄(2+),0~10μg/25mLPb ̄(2+);检出限为:c_(L、Zn) ̄(2+)=5.6ng/mL,c_(LPb) ̄(2+)=4.0ng/mL。 相似文献
72.
以天然水菱镁矿为原料,通过"煅烧-水化-煅烧"的简单方法制备了高比表面积介孔网状MgO,且实验过程中无须加入任何试剂。系统性研究了氧化镁用量、吸附时间、吸附温度及pH对氧化镁吸附模拟废水中铅离子吸附性能的影响,揭示了吸附机理,并考察了氧化镁对多种离子的吸附效果。结果表明:该氧化镁吸附剂具有188 m2·g-1的高比表面积和0.85 cm3·g-1的高孔体积,平均孔径为12.33 nm,其吸附动力学和等温线数据与伪二级模型和Langmuir模型高度吻合,表明重金属离子在氧化镁上为单层化学吸附。MgO介孔网状结构表现出对Pb(Ⅱ)的高吸附性能,最大吸附量为7 431.5 mg·g-1,该数值远高于其他报道的基于MgO吸附剂的数值,铅去除率高达99.8%以上。介孔网状MgO的吸附机理主要是羟基官能团以及Mg(Ⅱ)与MgO表面重金属离子之间的离子交换所致。另外,该氧化镁可同时吸附多种离子,对Cd、Cr、Ni、As、Co、P、Se、Be、Bi、Cu、Fe、Mn、V、Zn、Al离子均具有优异的吸附性能。 相似文献
73.
本文用两相滴定法研究了1-苯基-3-甲基-4-苯甲酰基-5-吡唑酮(PMBP,简写为HA)与甲基膦酸二(1-甲基庚基)脂(P350,简写为B)对Pb2+、Cd2+和Cu2+离子在不同的有机溶剂中的萃取机理.确定了萃合物的组成分别为:MA2(M=Pb2+、Ca2+、Cu2+);MA2·HA(M=Cd2+);MA2·B(M=Pb2+、Cd2+)和MA2·2B(M=Cd2+),同时求得了相应的萃合常数β值. 相似文献
74.
Wiesława Nocuń-Wczelik 《Journal of Thermal Analysis and Calorimetry》2007,88(1):291-294
The effect of PbO on cement hydration kinetics by calorimetric method
was evaluated as a first step in this project. Substantial retardation of
reaction with water at early stages with subsequent intensification of the
process was found. As the next step, the model systems covering pure cement
minerals and their mixtures of various composition as well as soluble Pb salts
were taken into account to elucidate the mechanism of delayed, by quite good
formation of products in the so-called post-induction period. The precipitation
of sulphate, forming very thin impermeable layer seems to be responsible for
this delaying effect in case of cement, however the other reactions of Pb
compounds in alkaline environment of hydrating calcium silicate are not out
of importance. In order to prove this, the studies of chemical composition
in small areas were also carried out. 相似文献
75.
Noel V. Stanton Tracy Fritsch Ciaran Geraghty Mary Frances Verostek Bruce Weiner Patrick J. Parsons 《Accreditation and quality assurance》2006,11(11):590-592
Following implementation of the CLIA ‘88 laboratory regulations, the primary role of proficiency testing (external quality assessment, PT) in the U.S. has been widely viewed as one of assuring regulatory compliance. PT can also be an effective tool for detecting widespread analytical problems, subject to limitations based on the method of PT assigned value determination. A recent case study describes the role of two PT programs in detecting and resolving a calibration bias in the LeadCare blood lead analyzer, and illustrates the limitations of peer-group target determination in fulfilling that PT role. 相似文献
76.
Feth Martin P. Weber Achim Merkle Rotraut Reinöhl Ulrich Bertagnolli Helmut 《Journal of Sol-Gel Science and Technology》2003,27(2):193-204
Two solid solutions of lead zirconium titanates PbZr
x
Ti1 – x
O3 (x = 0.1 and 0.35) as well as the reference compounds lead titanate and lead zirconate were prepared from zirconium and titanium n-propoxide, dissolved in 2-methoxyethanol, by sol-gel process. The amorphous products after pyrolysis of the dried gels and the crystalline phases were studied by EXAFS spectroscopy to monitor the structural changes from the amorphous oxide mixture to the crystalline ceramics after calcination. Additionally, the crystalline phases were identified by X-ray diffraction (XRD).It follows from the analysis of the EXAFS data that the local order of the amorphous phases seems to be completely different from that of the crystalline phase. There is no indication of a preformation of the local order of the perovskite structure. The analysis of our EXAFS spectra can be interpreted very consistently with the assumption that in the amorphous samples a segregation exists on molecular level and the low crystallisation temperatures are a consequence of very short diffusion paths. 相似文献
77.
Michael Chariss Andrea Zickgraf Heike Stenger Elmar Bru Cristelle Desmarquet Martin Drger Silke Gerstmann Dainis Dakternieks James Hook 《Polyhedron》1998,17(25-26)
44 members of thecompound series Ph4−nMRn (M=Si, Ge, Sn, Pb; R=o-, m-, p-Tol; n=0–4) were synthesized (15 newcompounds). The crystal structures of Ph3Sn (o-Tol) and PhSn (o-Tol)3 were determined and compared to 16 known structures. Subject to the distanced (M–C), an interplay between through-space π–π repulsion and π–σ attraction leads to either elongated or compressed tetrahedral geometry. 29 Si-, 119 Sn- and 207 Pb-NMR chemical shifts were determined in solution and in the solid state. 73 Ge chemical shifts were measured only in solution. Anupfield or downfield sagging of the chemical shifts along each series is rationalized in terms of a π–σcharge transfer which is constrained by torsion of the aromatic groups. 相似文献
78.
Orhan Acar 《Mikrochimica acta》2005,151(1-2):53-58
Lead, Cr, Mn and Zn in slurries of botanic and biological samples were determined by electrothermal atomic absorption spectrometry (ETAAS) using W, Ir, NH4H2PO4, W and NH4H2PO4, Ir and NH4H2PO4, W and Ir, and W + Ir + NH4H2PO4 chemical modifiers in an 0.2% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture. Zeeman effect background correction was performed and platforms inserted into graphite tubes were used. Comprehensive comparative studies were carried out with respect to pyrolysis and atomization temperatures, atomization and background absorption profiles, characteristic masses, detection limits and accuracy of the determinations in the presence and absence of modifiers. The mixture of W + Ir + NH4H2PO4 was found to be preferable for the determination of Pb, Cr, Mn and Zn in slurry samples. The pyrolysis temperatures of the analytes were increased up to 1250 °C for Pb, 1000 °C for Zn, 1400 °C for Cr and Mn by using W + Ir + NH4H2PO4 with an 0.2% (v/v) Triton X-100 plus 0.2% (v/v) nitric acid mixture used as diluent solution. The optimum masses of the mixed modifier components were found to be 20 µg W + 4 µg Ir + 50 µg NH4H2PO4. The characteristic masses of Pb, Cr, Mn and Zn obtained are 16.3, 5.6, 0.1 and 1.1 pg, respectively. The detection limits of Pb, Cr, Mn and Zn based on integrated absorbance for 0.5% (m v−1) slurries were found to be 0.14, 0.06, 0.02 and 0.01 µg g−1, respectively. The slurries of botanic and biological certified and standard reference materials were analyzed with and without the modifiers. Depending on the sample type, the percent recoveries increased from 63 up to 104% for analytes when using the proposed modifier mixture. 相似文献
79.
采用物理涂附法将单链DNA固定到金表面得到ssDNA/Au修饰电极。研究表明,该电极在pH 5,0.2 mol/L NaAc-HAc缓冲底液中,可用于测定水中痕量Pb2 。Pb2 以Pb-DNA络合物的形式吸附在电极上,以示差脉冲伏安法测定Pb2 ,在0.15 V(vsSCE)处有灵敏的氧化峰,其峰电流与Pb2 浓度在5.0×10-8~1.0×10-6mol/L范围内呈良好的线性关系,此法的检测限为2.0×10-8mol/L,该修饰电极的稳定性和抗干扰性都较好。用该电极对饮用水中的Pb进行检测,得到了满意的结果。 相似文献
80.
Bernd BrodbeckBernd Püllmann Sébastien SchmittMatthias Nettekoven 《Tetrahedron letters》2003,44(8):1675-1678
The parallel iterative solution-phase synthesis of 5-amino-1-aryl-[1,2,4]triazolo[1,5-a]pyridine-7-carboxylic acid amide derivatives is described. The key intermediate 2,6-bis-aminopyridine-4-carboxylic acid methyl ester was synthesised in a two step procedure in 64% overall yield and elaborated to a variety of triazolopyridine-5-carboxylic acid methyl ester by selective pyridine-N-amination, condensation of the adduct with a wide selection of aldehydes and subsequent cyclisation and oxidation. The desired esters were obtained in yields up to 70%. The final transformation to the amide derivatives was accomplished by application of carefully optimised reaction conditions thus giving access to a library of total 500 triazolopyridine amide derivatives. Iterative synthetic cycles (12-48 library members each) allowing for maximal flexibility in chemistry and maximal efficiency in in vitro biological activity optimisation guided by molecular modelling efforts constitute a synergistic procedure for rapid lead optimisation. 相似文献