Simple Method for Determination of Lead in Hair Dyes Using Slurry Sampling Graphite Furnace Atomic Absorption Spectrometry

A fast, simple and sensitive method for determining of lead in hair dyes using graphite furnace atomic absorption spectrometry with slurry sampling was developed. Multivariate optimization was used to establish optimal analytical parameters through a fractional factorial and a central composite design. The samples were submitted for direct analysis without prior digestion and were diluted in 2.5% v/v HNO₃ and 1.5% v/v H₂O₂. Palladium (chemical modifier) and rhodium (permanent modifier) were selected from several potential modifiers. The optimal conditions were a pyrolysis time of 10 s (liquid and dust dyes) 20 s (cream dyes), a pyrolysis temperature of 789°C (liquid dyes) or 750°C (cream and dust dyes) and an atomization temperature of 1800°C for all dyes. Under optimum conditions, the calibration graph is linear in the 1.50–50.0 µg L^?1 concentration range, with a detection limit of 0.33, 0.44, and 0.39 µg L^?1 for liquid, dust, and cream hair dyes, respectively. The relative standard deviation ranged from 1.63 to 4.56%. The recovery rate ranged from 85 to 108%, and no significant differences were found between the results obtained with the proposed method and the microwave decomposition analysis method of real samples. The concentration ranges obtained for lead in the hair dyes samples were 1.00–11.3 µg L^?1 for liquid dyes, 14.0–100 µg kg^?1 for dust dyes, and 19.9–187 µg kg^?1 for cream dyes.     

锆对低温液相合成甲醇Cu-Cr催化剂性能的影响

Cu-Cr and Cu-Cr-Zr catalysts for the low temperature methanol synthesis slurry phase, with the surface area of 77.9 and 113.2 m2/g respectively, were prepared by the co precipitation approach. The activity and selectivity of these catalysts were evaluated in a stainless steel autoclave at 5.5 MPa and at different temperatures of 383 and 423 K separately. It was found that the activity of Cu-Cr-Zr catalyst was obviously higher than that of Cu-Cr catalyst, whereas the methanol selectivity of Cu-Cr-Zr catalyst was a little lower. The concentration of sodium compounds in the solution after reaction was also measured. The results showed that the concentration of sodium formate after reaction is much lower than that before reaction, which is quite different from the observations from the Cu-Cr catalyst previously. This implies that the conversion of sodium methoxide to sodium formate has been completely suppressed in the presence of zirconia in Cu-Cr-Zr catalyst. This finding is more beneficial to improve the performance of Cu-Cr catalyst and to increase the life of catalyst system as well.     

稀土储氢合金浆液的吸氢性能

研究了富镧混合稀土－镍储氢合金与有机溶剂组成的悬浮浆液的吸氢行为。测定了温度,搅拌速度及浆液中合金含量对吸氢速率的影响,并以膜模型进行分析,计算。在温度４０℃和４２ｒ．ｓ＾－１的搅拌速度下,合金含量为０．０８ｋｇ．ｋｇ＾－１的浆液中,金属氢化物的转化率可达９５％。     

Experiment and simulation of slurry flow in irregular channels to understand proppant transport in complex fractures

Slurry flow and proppant placement in irregular fractures are crucial to evaluate hydraulic fracturing stimulation but need to be better understood. This study aims to investigate how irregular fracture affects proppant transport and distribution using laboratory experiments and micro-scale numerical models. The unresolved method of the computational fluid dynamics (CFD) and the discrete element method (DEM) considers Saffman lift force, Magnus force, and virtual mass force to accurately capture the frequent interaction between proppant and slickwater. Experimental results validated the reliability of the optimized CFD-DEM model and calibrated primary parameters. The effects of crack height and width, bending angle, and distance between the crack and inlet on particle distribution were studied. The results indicated that the improved numerical method could rationally simulate proppant transport in fractures at a scale factor. The small crack height causes downward and upward flows, which wash proppant to the fracture rear and form isolated proppant dunes. A wider region in the fracture is beneficial to build up a large dune, and the high dune can hinder particle transport into the fracture rear. When the crack is close to the inlet, the primary fracture without proppants will close to hinder gas production. The smaller the bending angle, the smaller the proppant dune. A regression model can precisely predict the dune coverage ratio. The results fundamentally understand how complex fractures and natural cracks affect slurry flow and proppant distribution.     

电热原子吸收悬浊液进样法测定煤飞灰中的铅

本文利用生物胶作为稳定剂和基体改进剂，把难溶剂环境固体样品制备成悬浊液，直接进行测定煤飞灰中的铅，得到了准确的结果。找出了日立１８０－８０石墨炉子原子吸收光谱仪的最佳线性范围７．０～６６．７ｎｇ／ｍＬ，原子化适宜温度２０００℃，生物胶量最佳用量范围０．２～１．２‰，并分析了酸度，搅拌，粒度对测定结果的影响。     

Laser processed micro-supercapacitors based on carbon nanotubes/manganese dioxide nanosheets composite with excellent electrochemical performance and aesthetic property

A laser processed micro-supercapacitor (LPMS) based on carbon nanotubes/manganese dioxide composite is fabricated through slurry dispensing and laser scribing techniques. This device presents superior electrochemical performance and aesthetic property.     

Abrasive properties of nano silica particles prepared by a sol–gel method for polishing silicon wafers

Abrasive properties of cocoon shaped silica particles fabricated by a sol–gel method have been studied. Since silicon wafers are polished with slurry by the mechanism of Chemical Mechanical Polishing, polishing rates may depend on various chemical and mechanical factors, such as particle concentration in slurry, slurry pH and kinds of basic compounds for controlling the slurry pH. The silicon wafer was polished by slurry continuously fed on a pad, and the polishing rate was estimated as a weight loss of the wafer. For studying the effects of the various factors on the rate, the slurries were prepared by adding the silica particles, basic compounds or salts, and the polishing rates of the slurry were measured. The effects of the various factors were made clear as follows: For the effect of particle concentration, the rates increased with increasing of the concentrations up to 1.0 wt.%. And for the effect of the slurry pH, slurries added basic compounds, such as KOH, NaOH, ammonia, were tested, and it was found that increasing of the slurry pH brought increases of the polishing rates. KOH-containing slurry of pH 13.2 had the fastest rate, 3.6 times as fast as the standard slurry with pH 9.4. For the effect of the adding of salts, it was indicated that the salts, such as KCl, NaCl, NH₄Cl, NaNO₃ and K₂SO₄ increased the polishing rates, and that KCl-containing slurry of 0.36 mol/l had the highest polishing rate, 3.4 times as fast as that of the standard slurry containing no salts.     

Electrochromatography in packed tubes using 1.5 to 50 μm silica gels and ODS bonded silica gels

Summary Electrochromatography (that is HPLC where the eluent is driven along the column by electro-osmosis using fields of up to 100 kV m⁻¹) promises plate efficiencies for HPLC which are comparable to those attained in capillary gas chromatography, but this requires that narrow-bore columns can be successfully packed with submicron particles. This paper demonstrates that we have now moved a considerable distance towards this goal. We show (1) that, following theory, there is no evidence of any reduction in electroosmotic velocity in columns packed with particles down to 1.5 μm diameter, (2) that reduced plate heights as low as unity are attainable for unretained solutes using both slurrypacked and drawn-packed columns 30 to 200 μm bore and up to 1 m long when packed with conventional 3 and 5 μm silica gels or with 1.5 μm impermeable silica spheres, (3) that columns driven electrically show higher plate efficiencies than identical columns driven by pressure, and (4) that 100,000 plate HPLC separations can be achieved in relatively short times of 30 minutes using in situ derivatised drawn packed capillaries containing 3 and 5 μm ODS-silica gels.     

Determination of As, Ge, Hg, Pb, Sb, Se and Sn in coal slurries by CVG-ETV-ICP-MS using external or isotopic dilution calibration

A method for the multi-elemental determination of As, Ge, Hg, Pb, Sb, Se and Sn in coal reference materials by slurry sampling chemical vapor generation (CVG) using external calibration and isotopic dilution (ID) calibration and detection by electrothermal vaporization inductively coupled plasma mass spectrometry (ETV-ICP-MS) is proposed. As, Ge, Sb, Se and Sn were determined using the external calibration, while, Hg, Pb, Se and Sn were determined by isotopic dilution. About 50–250 mg of sample was mixed with an acid solution, containing aqua regia and HCl, in an ultrasonic bath. For the isotopic dilution calibration, the enriched isotopes ²⁰¹Hg, ²⁰⁶Pb, ⁷⁷Se and ¹¹⁹Sn were added to the slurry in an adequate amount in order to produce an altered isotopic ratio close to 1. The vapor produced by the reaction of the sample slurry with the reducing agent was transported to the vaporizer and trapped in a Ir-treated graphite tube at 200 °C, before vaporization at 2100 °C and transportation of the vapor to the plasma. The accuracy of the method was assured by the analysis of four certified reference coal samples, using external calibration with aqueous solutions, prepared in the same medium and subjected to the same CVG and trapping procedure as the slurries and also by isotopic dilution calibration. The obtained concentrations were in agreement with the certified values, using the t-Student test for a confidence level of 95%. The detection limits (3 s; n = 5) of isotopic dilution, in ng g^− 1, were: 0.4 for Hg, 900 for Pb, 0.3 for Se and 0.2 for Sn. For external calibration, the detection limits, in ng g^− 1, were: 1.6 for As, 0.1 for Ge, 0.3 for Sb, 0.9 for Se and 7.5 for Sn. The relative standard deviations generally were lower than 14%, adequate for slurry analysis.     

悬浮液进样原子吸收光谱分析中样品的粒径效应

研究了悬浮液进样 FAAS和悬浮液进样 GFAAS中样品粒径效应。实验表明 ,悬浮液颗粒粒径 <30 μm能满足石墨炉原子化测定需要 ,而火焰原子化要求在粒径≤ 5 μm的前提下 ,再根据待测元素的性质选择合适的火焰类型 ,方能达到较满意的测定效果。