低压离子分离-化学发光在线检测过渡金属离子

 研究了低压离子 (LPIC)分离 柱后鲁米诺化学发光 (CL)检测方法 ,并分离测定了Cu2 + ,Co2 + ,Cr3 + ,Fe2 + ,Mn2 + 等 5种过渡金属离子。以草酸 柠檬酸混合溶液作为洗脱液 ,Luminol H2 O2 Mn + 作为化学发光检测体系 ,对过渡金属离子进行在线检测。测定的线性范围分别为 (mg·L-1) :Co2 + ,0 0 0 1～ 0 .1;Cu2 + ,0 1～ 6 ;Mn2 + ,0 0 6～ 4 ;Fe2 + ,0 0 3～ 5 ;Cr3 + ,0 0 2 5～ 1。检测限分别为 (μg·L-1) :Co2 + ,0 85 ;Cu2 + ,85 ;Mn2 + ,4 2 ;Fe2 + ,2 1;Cr3 + ,2 0。     

真空紫外光电离质谱技术进展及其在快速分析中的应用

真空紫外光电离源(VUV-PI)是一种普适性的质谱软电离源,真空紫外光电离质谱谱图无碎片、易解析、灵敏度高,适合于在线快速分析.真空紫外光电离质谱根据分析对象不同可以直接采用单光子电离或添加掺杂剂实现化学电离,能实现气、液、固体分析,也可实现成像分析.该文介绍了真空紫外光电离源的电离原理、光源类型,分析了光电离质谱灵敏...     

在线阴离子富集-石墨炉原子吸收光谱法的研究

将流动注射在线预富集系统与石墨炉原子吸收光谱法联用,以强碱型阴离子交换纤维为柱填充材料,以浓盐酸为络合剂,以稀盐酸为洗脱液,用固定洗脱液体积方式测定了Cd,Pb和Zn,富集倍数分别为19,17和15(与直接引入40μL进样量相比),检出限(3σ,ng/L)分别为1.1,8.2和2.6.     

Comparison of two laser-induced breakdown spectroscopy techniques for total carbon measurement in soils

The potentials of two advanced laser-induced breakdown spectroscopy (LIBS) techniques which are used to determine the total carbon content in soils have been examined. The first one is the combination of a single-pulse laser ablation with spark excitation of plasma plume triggering the gap between electrodes close to the target surface. The second one is a more conventional double-pulse LIBS. In both modes the calibration graphs have a nonlinear trend in the actual range of carbon contents and present a good R² value (0.97). In the combined laser-spark approach, using low-cost and portable laser instrumentation is possible, as well as inducing a micro-damage on the target surface. Certain regularities in the spectral line intensities of soil nutritious elements have been detected and appear to be connected to the total carbon content and to the soil origin.     

Continuous Spectroscopy Characterization of Emulsions

In emulsion polymerization, the formation of particles has an important effect on the rate of reaction and on the final properties of the latex. To investigate particle nucleation mechanisms in emulsion polymerization it is necessary to establish the initial conditions of the emulsified system before the reaction takes place. This research reports on a technique to continuously monitor the droplet size distribution of liquid-liquid emulsions using spectroscopy. The on-line particle characterization methodology is based on an integrated sampling and dilution strategy combined with spectroscopy methods. It is shown that the sampling system integrated with a multiwavelength turbidity detector provides reliable estimates of droplet populations as function of the dispersed phase concentration in emulsions of saturated hydrocarbons. The results provide not only the groundwork necessary for the elucidation of particle nucleation during emulsion polymerization process but also suggests the potential of this combined technology to further our understanding of liquid-liquid emulsions.     

糖类相关基因芯片的设计与制备

随着糖组学的发展,研究表明某些疾病如肿瘤等的发生伴随着体内糖蛋白表面糖链结构的变化,而糖链结构的形成与修饰经过糖基转移酶、糖苷酶和磺基转移酶的参与.本研究从Genebank等数据库中选取人类糖基转移酶基因127条、糖苷酶基因34条和磺基转移酶34条以及管家基因10条.通过对每个基因的mRNA序列进行探针设计,制备出一款糖类相关基因芯片,用于研究糖类相关基因的表达谱,旨在揭示疾病发生与糖类相关基因表达变化的关联性.制备的芯片应用于人肝癌细胞系SMMC-7721与正常肝细胞系Chang’s liver的研究,筛选出差异表达的基因34个,其中上调基因19个、下调基因15个.通过对2个上调基因和2个下调基因进行Realtime-PCR验证,得到了一致的实验结果.     

Effects of GC temperature and carrier gas flow rate on on‐line oxygen isotope measurement as studied by on‐column CO injection

Although deemed important to δ¹⁸O measurement by on‐line high‐temperature conversion techniques, how the GC conditions affect δ¹⁸O measurement is rarely examined adequately. We therefore directly injected different volumes of CO or CO–N₂ mix onto the GC column by a six‐port valve and examined the CO yield, CO peak shape, CO–N₂ separation, and δ¹⁸O value under different GC temperatures and carrier gas flow rates. The results show the CO peak area decreases when the carrier gas flow rate increases. The GC temperature has no effect on peak area. The peak width increases with the increase of CO injection volume but decreases with the increase of GC temperature and carrier gas flow rate. The peak intensity increases with the increase of GC temperature and CO injection volume but decreases with the increase of carrier gas flow rate. The peak separation time between N₂ and CO decreases with an increase of GC temperature and carrier gas flow rate. δ¹⁸O value decreases with the increase of CO injection volume (when half m/z 28 intensity is <3 V) and GC temperature but is insensitive to carrier gas flow rate. On average, the δ¹⁸O value of the injected CO is about 1‰ higher than that of identical reference CO. The δ¹⁸O distribution pattern of the injected CO is probably a combined result of ion source nonlinearity and preferential loss of C¹⁶O or oxygen isotopic exchange between zeolite and CO. For practical application, a lower carrier gas flow rate is therefore recommended as it has the combined advantages of higher CO yield, better N₂–CO separation, lower He consumption, and insignificant effect on δ¹⁸O value, while a higher‐than‐60 °C GC temperature and a larger‐than‐100 µl CO volume is also recommended. When no N₂ peak is expected, a higher GC temperature is recommended, and vice versa. Copyright © 2015 John Wiley & Sons, Ltd.     

Interfacial bonding mechanism and bonding strength of AlTiCrN coating by cathodic arc ion plating

AlTiCrN coating was prepared on the surface of YT14 tungsten carbide cutting tools by cathodic arc ion plating with Ti, Al and Cr as targets. The surface morphologies, interface energy spectrum, phase and elements' binding energy of the coatings were observed with SEM, EDS, XRD and XPS, respectively, and bonding strength of the coating interface was measured with scratch tester. The results show that the phases of AlTiCrN coating are mainly composed of AlN, CrN and TiN, the crystal plane of (111) has a strong preferred orientation. The concentrations of Al, Ti, Cr, N in the coating are higher than those in the substrate, showing the gradient diffusion distribution at the bonding interface, while C atoms of the substrate have diffused into the lattices of TiN, AlN and CrN to form an obvious interdiffusion layer, and the average bonding strength of coating interface is 57.65 N. Copyright © 2014 John Wiley & Sons, Ltd.     

On‐line flow‐through extraction–preconcentration‐large volume injection‐RP LC for trace determination of pyrethroids in Slovak soil

A rapid micro‐analytical multiresidue method was developed for analysis of pyrethroids (kadethrin K, cypermethrin C and permethrin P) in soil micro‐sample (200 mg). It uses on‐line flow‐through extraction of soil micro‐samples (packed into a short glass column) with a methanol‐aqueous citric acid buffer mixture, successive on‐line SPE preconcentration of analytes from the extract and on‐line RP‐HPLC analysis with UV photometric detection. The separation of pyrethroids is performed on a Purospher RP‐18e column with methanol/water as mobile phase. Effects of sorbent placed at the bottom of a short column holding the soil sample and different kinds of on‐line SPE columns were tested. Besides, the influence of volume of the effluent on the pyrethroids recovery was also studied. Calibration curves were linear over the range assayed from 0.01 to 0.2 μg/mL with correlation coefficients of linear regression (least‐squares method) in the range 0.998–0.999. Recovery studies were carried out at 0.25–1.00 μg/g dry soil fortification level and obtained recoveries were for K 81–84%, C 56–59% and for P 58–63%. Achieved LOD (confidence band) of studied pyrethroids were for large‐volume injection (1 mL) 4.5 ng K, 3.7 ng C, 3.6 ng P or 27 ng/g K, 32 ng/g C and 29 ng/g P in dry soil “solid sampling HPLC”.