X-ray fluorescence spectrometry analysis for minerals with agaron gel for sample preparation

A mineral sample preparation with agaron gel used in X-ray fluorescence analysis was developed. Mineral samples were decomposed with aqua-regia. The sample solution mixed with agaron gel was heated to boiling and then it would become quasi-solid gel under normal temperature. The elements dispersed in gel medium could be detected by X-ray fluorescence spectrometry. The method has both advantages of the solution preparation method and the solid preparation method. In addition, this method was adapted in detecting high content ores due to its' avoiding the risk of using platinum crucibles. The method has been applied to the determination of lead, zinc and iron in zinc and lead concentrates successfully.     

P(VDF-HFP)基凝胶电解质染料敏化纳米TiO2薄膜太阳电池

采用循环伏安法(CV)研究了凝胶电解质中I₃-/I-氧化还原行为,凝胶电解质中I₃-/I-的表观扩散系数和相应的稳态扩散电流明显低于液体电解质.通过对阴/阳离子的结合能和孔穴阻塞作用的研究解释了凝胶电解质电导率较液体电解质发生变化的原因.制备的凝胶电解质电池具有较高的光电转换效率(6.6%),其短路电流密度(Jsc)仅比液体电解质电池低0.3-0.4 mA/cm²,电池效率也仅低约0.6%.     

Quantitative analysis of elements (C, N, O, Al, Si and Fe) in polyamide with wavelength dispersive X-ray fluorescence spectrometry

A wavelength dispersive X-ray fluorescence (WD-XRF) spectrometry combined with calibration curve method was established for simultaneously analyzing low-Z elements (C,N,O) and Al,Si,Fe in polyamide.To investigate the origin of plastic material causing deposition and blocking in instrument engines and pipelines,polyamide 6 (PA 6,an engineering plastic) was chosen as the study object on account of its common use in industry.The sample preparation with pressed powder disk has been developed for determination of six elements in PA 6.Pure Cu metal was used as the matrix and PA 6 was regarded as standard sample for C,N,O elements.PA 6 particles were firstly smashed to uniform powder in liquid nitrogen,and then mixed with inorganic standard powders (Fe2O3,Al2O3,SiO2,and Na 2 SiO 3).The mixture was ground to obtain homogeneous calibration materials for WD-XRF analysis.The quantitative property of the calibration curve method for each element was reliable.The limits of detection (S/N≤3) of C,N,O,Al,Si and Fe using WD-XRF were 249,120,101,6.2,3.3,and 1.8 μg/g,respectively.To confirm the accuracy of the proposed WD-XRF calibration curve method,inductively coupled plasma optical emission spectroscopy (ICP-OES) detection for Al,Si,Fe and elemental analyzer (EA) analysis for C,N,O were utilized.A good correlation of the WD-XRF results with the measurements of ICP-OES and EA was observed.     

A comparison of methods for the determination of platinum in ores

Fire-assay and wet-extraction methods of determining platinum in ores have been evaluated. The fire-assay procedure using lead as a collector was used in combination with flame and flameless atomic-absorption, emission spectroscopy and X-ray fluorescence. In this last method flattened silver beads were analysed directly, whereas for the other methods the beads were dissolved in aqua regia and the solutions made up with concentrated hydrochloric acid before analysis. The wet procedures involved treatment of the ores with acids and subsequent analysis by flame atomic-absorption or by spectrophotometry after treatment with tin(II) chloride. Chromatographic, ion-exchange and solvent-extraction procedures were used to isolate platinum from base metals, the other platinum metals and gold. Results for each ore by fire assay-flame atomic-absorption, fire assay-emission spectroscopy, and wet extraction combined with spectrophotometry, showed no difference at the 99% confidence level. X-Ray fluorescence and flameless atomic-absorption results tended to be high and low respectively. The most precise method was wet extraction followed by spectrophotometric determination. Emission spectroscopy and X-ray fluorescence generally yielded the poorest precision. Wet-extraction methods were time-consuming and since no advantage was gained in accuracy over the fire-assay methods, a combined fire assay-flame atomic-absorption system was the preferred method of analysis.     

Use of thiopropyl sepharose for preparation of 2-nitro-5-thiobenzoic acid

A simple method is described for preparation of 2-nitro-5-thiobenzoic acid (NTB), a compound with versatile applications but is commercially unavailable. In this method, NTB is produced by the reduction of 5,5′-dithiobis(2-nitrobenzoic acid) (DTNB) with thiopropyl sepharose, which is then separated from NTB by filtration. Two molecules of NTB can be generated from each molecule of DTNB when a large excess of thiopropyl sepharose is used. Thiopropyl sepharose is commercially available and can be readily regenerated for repeated use in the preparation of NTB. This method is simple and more effective than any other reported methods of NTB preparation.     

Photovoltaic performance of dye-sensitized solar cells assembled by in-situ chemical cross-linking

Quasi-solid state dye-sensitized solar cells (DSSCs) were assembled by in-situ chemical cross-linking of a gel electrolyte precursor containing liquid electrolyte. The DSSCs assembled with this cross-linked gel polymer electrolyte showed higher open circuit voltage and lower short-circuit photocurrent density than those of DSSCs with liquid electrolyte. Addition of SiO₂ nanoparticles into the cross-linked gel polymer electrolyte significantly improved the photovoltaic performance and long-term stability of the DSSCs. The optimized quasi-solid state DSSC showed high conversion efficiency, 6.2% at 100 mW cm^?2 with good durability.     

新型梳状共聚物在准固态染料敏化太阳能电池中的应用及其对电子复合的影响

合成了乙烯基咪唑碘盐(VImI)和聚乙二醇单甲醚甲基丙烯酸酯(PEGMA)的梳状共聚物.利用VImI/PEGMA共聚物制备了准固态聚合物电解质.通过光电流密度-电压(J-V)曲线和电导率测定以及电化学阻抗分析,探讨了基于此电解质的染料敏化太阳能电池的电荷传输与界面电子转移机制.结果表明,VImI/PEGMA共聚物可以有效抑制TiO2/电解质界面电子复合并提高TiO2导带能级,敏化电池的光伏性能并不完全取决于电解质的电导率.通过考察共聚物中VImI与PEGMA单元的摩尔比与开路电压的关系,发现共聚物对电子复合的抑制作用主要源于VImI链段.此外,开路电压衰减(OCVD)和瞬态光电流测试结果说明,共聚物能够提高TiO2薄膜的电子寿命,而且对陷阱电子能级的分布具有调节作用.当共聚物在电解质中的质量分数为50%,VImI与PEGMA的摩尔比为5.0时,准固态染料敏化太阳能电池于100mW·cm-2光强下获得了4.10%的光电转换效率.     

Solid Phase Extraction and Determination of Lead in Water Samples Using Silica Gel Homogeneously Modified by Thiosalicylic Acid

Abstract

Silica gel was modified by thiosalicylic acid via homogeneous routes to obtain immobilized silica gel sorbent (TSA‐immobilized silica gel). This new sorbent was characterized using variety of physical chemistry techniques including, high resolution solid state ¹³C and ²⁹Si CP/MAS NMR, X‐ray photoelectron spectroscopy (XPS), thermal analysis (TGA and DTA), elemental analysis, and BET surface analysis as well as infrared spectroscopy (FTIR). New support was used for the selective extraction and concentration of lead ions by silica gel modified with thiosalicylic acid, as a highly selective and stable reagent, from aquatic samples and its determination with FAAS. Lead ions can be desorbed with 4 mol dm^?3 HNO₃. The sorption capacity for lead ions are found in the range of 64.40 to 69.90 µmol g^?1 of chelating matrix. Tolerance limits for electrolytes and some trace metals in the sorption of lead is reported. Preconcentration factor was found as 150 for Pb(II). The lead in drinking water, mineral water, tap water, and fruit juice was quantitatively recovered with a relative standard deviation lower than 1.50%. A detection limit of the method for lead ions was found as 3.7 µg l^?1.     

稀释剂粉末压片-X射线荧光光谱法测定锑矿石中锑及主量组分

利用X射线荧光光谱仪结合稀释剂粉末压片法来测定锑矿石中锑及主量组分。通过稀释剂的加入,减弱了样品的基体效应。人工配制了一系列具有浓度梯度的样品来解决标准样品个数偏少的问题。方法简便、实用,具有较高的精密度和准确度,测定结果满足实际工作需要。方法的相对标准偏差(RSD)为0.19%～2.0%,与常规分析结果基本一致。     

A 7.72% efficient dye sensitized solar cell based on novel necklace-like polymer gel electrolyte containing latent chemically cross-linked gel electrolyte precursors

Novel necklace-like polymer gel electrolytes containing latent chemically cross-linked gel electrolyte precursors were prepared for quasi-solid dye sensitized solar cells with a highest efficiency of 7.72% and an active area of 0.25 cm2 under AM1.5 condition at 100 mW cm(-2) irradiation.     

Quasi-solid dye sensitised solar cells filled with ionic liquid--increase in efficiencies by specific interaction between conductive polymers and gelators

Photo-energy conversions for quasi-solid dye sensitised solar cells increased when gel electrolytes were combined with conductive polymers as counter electrodes and the conversion surpassed that for DSSCs equipped with conventional Pt counter electrodes.     

The accurate determination of gold and silver in ores and concentrates by wet-chemical analysis of the lead assay button

Hydroquinone or formic acid can be used as reductant for the quantitative precipitation of gold in the lead perchlorate solution obtained after the lead assay button has been parted with perchloric acid. Silver chloride can be completely precipitated by dilution and overnight standing of the parting solution, thus both gold and silver can be isolated by filtration for the final measurement. The proposed lead-wet chemical method was successfully applied to ores, concentrates, dusts, etc.     

Old Masters' lead white pigments: investigations of paintings from the 16th to the 17th century using high precision lead isotope abundance ratios

White lead (2PbCO(3).Pb(OH)(2)), a common component in 17c. artists' painting materials, was singled out to investigate the potential of lead isotope abundance ratios in the field of authentication and origin assignment. Paintings by Peter Paul Rubens, Anthony van Dyck and other Old Masters of the Northern and Southern schools were chosen for this study. An interdisciplinary approach was chosen using both analytical instrumental methods, art technological and art historical knowledge. Minute samples taken from paintings from selected art collections worldwide were investigated using mass spectrometry, scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDX). The high precision lead isotope abundance ratios were measured by multiple collector inductively coupled plasma mass spectrometry (MC-ICP-MS). The determination of the calcium matrix influence with respect to possible bias effects to the isotope ratios gave clear decision support, to whether a result lies within the stated combined measurement uncertainty of the result, to eliminate time-consuming matrix separations. The scatter plots of the measured isotope abundance ratios for the painting pigments from P. P. Rubens, A. van Dyck and other Flemish painters exhibit a very narrow distribution forming a cluster. The range of the measured ratio (206)Pb/(204)Pb amounts to 0.55% and for the ratio (207)Pb/(204)Pb to 0.2%. The comparison of the data to cis-alpine (Italian) sample pigments from paintings from the same time period reveals a clear distinction between the two fields. With respect to the lead isotope data originating from the ores it is assumed that the pigment isotope ratio distribution can be explained by very distinct origin of raw materials. Presumably, no mixing of different lead ores from Europe took place. The comparison of the measured white lead isotope ratio values (Flemish paintings) and the data from ore samples led to the unexpected conclusion that local ores were not used for the pigment production but British or German sources.     

聚合物/TiO2杂化纳米纤维微孔膜的制备及其在染料敏化太阳能电池中的应用

利用静电纺丝技术,制备了不同的聚合物/TiO2杂化纳米纤维微孔膜,吸附液体电解质后形成聚合物/TiO2杂化纳米纤维微孔膜准固态电解质,应用于制备准固态染料敏化太阳能电池(DSSCs).测试了电纺聚合物纳米纤维微孔膜电解质的吸液率、孔隙率、离子电导率等参数,研究了纳米纤维微孔膜准固态电解质DSSCs的光伏性能.结果显示,TiO2的掺入可提高聚合物/TiO2杂化纳米纤维微孔膜对液态电解质的浸润扩散性能,从而提高纳米纤维微孔膜对液态电解质的吸附能力.组装的DSSCs的光电转换效率可达液态电解质的90%以上,并具有较好的长期工作稳定性.     

The solvent extraction is a potential choice to recover asphalt from unconventional oil ores

The abundant unconventional oil ores (about 70% of total world oil) are playing an increasingly important role in global energy supply. To obtain asphalt in unconventional oil ores, different methods, including hot water-based extraction, pyrolysis and solvent extraction, were used to recover asphalt from oil ores (i.e., Canadian, Indonesian, and Iranian oil ores). It is found that asphalt recovery obtained by solvent extraction is the highest. Multi-staged single solvent extraction was used to recover asphalt from oil ores (i.e., toluene, tetrahydrofuran: THF, xylene, petroleum: PE, ethanol), resulting in a cumulative asphalt recovery over 98% at ambient conditions by using toluene. Take Iranian oil ores with the highest oil content (83.79 wt%) as an example, great asphalt recovery was obtained by using multi-staged composite solvents extraction (i.e., toluene@xylene, toluene@THF, toluene@PE, toluene@ethanol). It is also found that introduction of toluene in the composite solvents can significantly increase the ability of single solvent’s (xylene, THF, PE and ethanol) asphalt recovery. After solvent extraction, the solvent recovery was more than 95%. This finds suggest that solvent extraction method would be potential choice to recover asphalt from unconventional oil ores, and it possesses great prospect of industrial application in the future.     

Dependence of solar cell performance on the nature of alkaline counterion in gel polymer electrolytes containing binary iodides

Performance of dye-sensitized nano-crystalline TiO₂ thin film-based photo-electrochemical solar cells (PECSCs) containing gel polymer electrolytes is largely governed by the nature of the cation in the electrolyte. Dependence of the photovoltaic performance in these quasi-solid state PECSCs on the alkaline cation size has already been investigated for single cation iodide salt-based electrolytes. The present study reports the ionic conductivity dependence on the nature of alkaline cations (counterion) in a gel polymer electrolyte based on binary iodides. Polyacrylonitrile-based gel polymer electrolyte series containing binary iodide salts is prepared using one of the alkaline iodides (LiI, NaI, KI, RbI, and CsI) and tetrapropylammonium iodide (Pr₄NI). All the electrolytes based on binary salts have shown conductivity enhancement compared to their single cation counterparts. When combined with Pr₄NI, each of the Li⁺, Na⁺, K⁺, Rb⁺, and Cs⁺ cation containing iodide salts incorporated in the gel electrolytes has shown a room temperature conductivity enhancement of 85.59, 12.03, 12.71, 20.77, and 15.36%, respectively. The conductivities of gel electrolytes containing binary iodide systems with Pr₄NI and KI/RbI/CsI are higher and have shown values of 3.28, 3.43, and 3.23 mS cm⁻¹, respectively at room temperature. The influence of the nature of counterions on the performance of quasi-solid state dye-sensitized solar cells is investigated by assembling two series of cells. All the binary cationic solar cells have shown more or less enhancements of open circuit voltage, short circuit current density, fill factor, and efficiency compared to their single cation counterparts. This work highlights the importance of employing binary cations (a large and a small) in electrolytes intended for quasi-solid state solar cells. The percentage of energy conversion efficiency enhancement shown for the PECSCs made with electrolytes containing Pr₄NI along with Li⁺, Na⁺, K⁺, Rb⁺, and Cs⁺ iodides is 260.27, 133.65, 65.27, 25.32, and 8.36%, respectively. The highest efficiency of 4.93% is shown by the solar cell containing KI and Pr₄NI. However, the highest enhancements of ionic conductivity as well as the energy conversion efficiency were exhibited by the PECSC made with Li⁺-containing binary cationic electrolyte.

     

Contribution au dosage chimique des matières plombifères

This paper describes a method for the quantitative determination of various lead compounds present in ores and metallurgical products. The method consists, in principle, of dissolving selectively and successively the different lead compounds and determining the lead in each of the filtrates thus obtained.The method guarantees the automatic control of the results.     

Latent gel electrolyte precursors for quasi-solid dye sensitized solar cells

New latent chemically-cross-linked gel electrolyte precursors for quasi-solid dye sensitized solar cells (QDSC) are reported. The gel electrolyte precursors consist of nano-particles and dicarboxylic acids as the latent gelators. The viscosity of the precursor is low at first and does not increase during storage at room temperature. However, when the precursor is baked at 80 degrees C, it solidifies immediately. Photo-voltaic performance is maintained after solidification.     

Wavelength dispersive X-ray fluorescence imaging using a high-sensitivity imaging sensor

A new wavelength-dispersive X-ray fluorescence (WD-XRF) imaging spectrometer equipped with a high-sensitivity imaging sensor was developed in our laboratory. In this instrument, a straight polycapillary optic was applied instead of a Soller slit as well as a 2D imaging X-ray detector instead of X-ray counters, which are used in conventional WD-XRF spectrometers. Therefore, images of elemental distribution were available after a short exposure time. Ni Kα images and Cu Kα images were clearly obtained at corresponding diffraction angles for a short exposure time of 10 s. By optimizing the spectrometer, the time required for imaging is reduced, leading to XRF image movies. It is difficult to distinguish two peaks (Ti Kα (4.508 keV) and Ba Lα (4.465 keV)) due to the poor energy resolution of EDXRS. However, Ti and Ba images could be successfully observed by the WD-XRF imaging spectrometer. The energy resolution of the developed spectrometer was 25 eV at the Ti Kα peak.     

Interaction of <Emphasis Type="Italic">Moringa oleifera</Emphasis> seed lectin with humic acid

The aim of this work was to characterise the affinity of protein preparations from Moringa oleifera seeds, specifically extract (seeds homogenised with 0.15 M NaCl), fraction (extract precipitated with 390 mg mL⁻¹ of ammonium sulphate) and cMoL (coagulant M. oleifera lectin) to bind humic acids using a haemagglutinating activity assay with rabbit erythrocytes and a radial diffusion assay in agarose gel. Specific haemagglutinating activity (SHA) decreased by 94 % for the extract and cMoL and by 50 % for the fraction in the presence of humic acid. Precipitation bands were observed in the diffusion gel. Both results suggested humic acid-cMoL binding. Carbohydrates, potassium, and calcium ions and pH affected the SHA of cMoL. As an example of application, cMoL was immobilised on a column packed with sepharose receiving 20 mg mL⁻¹ of carbon humic acid solution, 30 mg of humic acid per gram of support was removed. This result suggested that protein preparations might be used in water treatment to remove humic acids.