U(VI) biosorption by Azolla imbircata dry power from solution

Journal of Radioanalytical and Nuclear Chemistry - Azolla imbircata dry powder (Ai-dp) was prepared by collecting wild Azolla imbircata, drying and grinding. SEM, FTIR and XPS have been used to...     

Off-line system for measurement of nitrous oxide concentration in gases leaving the irradiation chamber

The N₂O concentration in the gas leaving the irradiation chamber was determined by off-line gas chromatographic analysis. The grab sample system involved the scrubber with a 1.0 N NaOH solution and the drying columns. The paper presents preliminary results of N₂O concentration measurement for two different gas irradiation doses with other technological parameters of the pilot installation being constant.     

Bovine liver sample preparation and micro-homogeneity study for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry

This work describes a systematic study for the bovine liver sample preparation for Cu and Zn determination by solid sampling electrothermal atomic absorption spectrometry. The main parameters investigated were sample drying, grinding process, particle size, sample size, microsample homogeneity, and their relationship with the precision and accuracy of the method. A bovine liver sample was prepared using different drying procedures: (1) freeze drying, and (2) drying in a household microwave oven followed by drying in a stove at 60 °C until constant mass. Ball and cryogenic mills were used for grinding. Less sensitive wavelengths for Cu (216.5 nm) and Zn (307.6 nm), and Zeeman-based three-field background correction for Cu were used to diminish the sensitivities. The pyrolysis and atomization temperatures adopted were 1000 °C and 2300 °C for Cu, and 700 °C and 1700 °C for Zn, respectively. For both elements, it was possible to calibrate the spectrometer with aqueous solutions. The use of 250 μg of W + 200 μg of Rh as permanent chemical modifier was imperative for Zn. Under these conditions, the characteristic mass and detection limit were 1.4 ng and 1.6 ng for Cu, and 2.8 ng and 1.3 ng for Zn, respectively. The results showed good agreement (95% confidence level) for homogeneity of the entire material (> 200 mg) when the sample was dried in microwave/stove and ground in a cryogenic mill. The microsample homogeneity study showed that Zn is more dependent on the sample pretreatment than Cu. The bovine liver sample prepared in microwave/stove and ground in a cryogenic mill presented results with the lowest relative standard deviation for Cu than Zn. Good accuracy and precision were observed for bovine liver masses higher than 40 μg for Cu and 30 μg for Zn. The concentrations of Cu and Zn in the prepared bovine liver sample were 223 mg kg^− 1 and 128 mg kg^− 1, respectively. The relative standard deviations were lower than 6% (n = 5). The accuracy of the entire procedure was checked with bovine liver from NIST (1577b) and determination of Cu and Zn using flame atomic absorption spectrometry after microwave-assisted sample digestion.     

Chemical characterization and screening of hydrocarbon pollution in industrial soils by headspace solid-phase microextraction.

A headspace solid-phase microextraction method, followed by a gas chromatographic-mass spectrometric analysis, has been developed for the screening of soil samples polluted by coal tar or refined petroleum products. Vapor pressures of target analytes were determined using a capillary GC method to identify environmentally important components with a sufficiently high vapor pressure to be analyzed in the headspace mode. The method was optimized under non-equilibrium conditions with simplicity and automation in mind and does not require any extraction procedure or sample preparation, other than grinding, drying and homogenizing. The analytical performance and the significance of the results for the purpose of chemical characterization, source discrimination, determination of individual isomer distributions and to calculate source or weathering ratios, is discussed.     

Dependence of Electrochemical Characteristics of Carbon Monofluoride Electrodes on the Production Method

The polarization and discharge parameters and ohmic, electrochemical, and diffusion losses are measured for two types of cathodes of Li–CF _x power sources. One type is produced with a standard procedure by mixing starting components of the active mass in a liquid form, and then drying and grinding them. The other is prepared from an active mass of starting components subjected to joint action of high pressure and shear deformations at a high-pressure apparatus similar to Bridgman's anvil. The high-pressure processing of a mixture of starting components decreased all the components of polarization losses. This is indicated by a higher potential of the second-type electrodes at the same discharge current.     

Preparation of disk-like cellulose particles

Disk-like cellulose particles were facilely prepared by stirring a dispersion of spongy cellulose particles that were prepared with a solvent-releasing method (SRM) with a magnetic stir bar. The obtained particles were thick and disk-like and retained their spongy structure in the wet state. The thick, disk-like particles became thinner in a specific direction upon drying because of capillary force. In contrast, when the same procedure was conducted using cellulose particles with dense structures, the particle shapes were not deformed, and disk-like shapes did not appear. Moreover, when the stirring was carried out using a shaking bath or a touch mixer, the shape transformation was not observed. These results suggest that the spongy structure of the cellulose particles would be a pseudo-plasticization state, which can cause the cellulose particles to deform. The disk-like particles formed as a result of the grinding of spongy cellulose particles between the stir bar and the vial. The number of disk-like particles and the degree of deformation increased with increasing of the stirring time, the speed and the contact area.     

低温固态反应制备纳米Ba_(1-y)Sr_yTi_(1-x)Zr_xO_3介电材料及性能研究

将TiCl4的水解产物与固体Ba(OH)2按摩尔比1∶1混合,混合物经室温研磨、100℃烘干,得到钛酸钡纳米晶;按相同工艺掺杂,合成了一系列Ba1-ySryTi1-xZrxO3(0x≤0.3,0y≤0.4)固溶体;采用X射线衍射分析了产物的晶体结构,采用透射电镜观察了其形貌;并测定了系列固溶体的室温介电常数、介电损失.结果表明,所制备的Ba1-ySryTi1-xZrxO3为完全互溶取代固溶体,由平均粒径70 nm的球形微粒组成.经低温固态反应掺入适量锆、锶后,BaTi O3的室温介电常数由3 000提高到20 000左右.     

Effects of Poly(Ethylene Glycol) on the Physical Properties of Blended Molecules of Starch and Poly(Ethylene-co-Acrylate,Ammonium Salt)

Abstract

A mixture of starch (36%) poly(ethylene-co-acrylate, ammonium salt) (41%), water (12.5%), urea (8.4%), and poly(ethylene glycol) (M _n 4600) (2.1%) were converted to plastic test pieces by extruding (130°C), drying and grinding (25°C), and hot pressing (175°C). After equilibration at ?50% relative humidity and 25°C, the test pieces contained 3.5–4.6% moisture and 2.3% poly(ethylene glycol) (PEG). Among wheat, corn, potato, and rice starches, the wheat starch (WS) blend showed the highest Young's modulus (181.3 MPa), whereas the corn starch (CS) blend had a modulus and elongation that almost matched those of lowdensity polyethylene. When PEG was eliminated from the WS formulation, tensile strength remained constant, but Young's modulus doubled. The modulus decreased continually as test pieces absorbed water up to 27% moisture, but elongation and argon laser light transmittance were optimum at ?12% moisture. Differential scanning calorimetry indicated that PEG formed a solid inclusion complex with amylose upon drying at 60°C, but no complex was detected in dilute alkali by optical rotation.     

关于澳洲GoLden Grove金精矿磨样方法的研究

金精矿样品的粒度,直接影响金精矿中金含量测定的精密度和稳定性,本文通过对Golden Grove金精矿采用不同的磨样工具和磨样时间,得到不同粒度的样品,对不同样品进行了金含量的测定,并对测定结果的精密度进行了分析。其中磨样方式：滚筒磨样机、磨样时间为5h、磨样粒度为0.040mm(360目)95%以上的B样品,测定精密度最好。C样品测定精密度相对较差,反映出振动粉碎机磨样均匀度相对较差。     

Study of contamination sources in the process of cryogenic grinding

The study of contamination effect during cryogenic grinding of pure cellulose was carried out. The optimisation of important parameters of the grinding process (pre-cooling time, grinding time, cooling time and number of cycles) was performed and the different sources of a possible contamination of samples (earlier processed sample, metal parts of grinding tool) were evaluated. The results of ICP-oa-TOF MS analysis after microwave digestion of cellulose samples were used in this study. Significant contamination of cellulose samples by Fe at the level 130 microg kg(-1) caused by wearing of steel stoppers and an impact bar was detected. Cross-contamination by Fe, Cr, Mn and Cu at the level 400, 200, 200 and 2100 microg kg(-1), respectively was caused by previous grinding of electro-waste sample. This cross-contamination was possible to be avoided by changing of a polycarbonate part of a grinding vessel.     

Contamination of Rock Samples by Laboratory Grinding Mills

We have measured the contamination of samples of granite, quartz porphyry, greenstone and dolerite after grinding them in steel and cemented carbide grinding mills. The steel mill contaminated the granite with Fe. The cemented carbide mill contaminated all samples with W and Co, and the granite and quartz porphyry with Ta. Contamination during grinding is proportional to the free quartz content of the rock and to the grinding time.     

Influence of different techniques on formulation and comparative characterization of inclusion complexes of ASA with β-cyclodextrin and inclusion complexes of ASA with PMDA cross-linked β-cyclodextrin nanosponges

Acetyl salicylic acid (ASA), a non-steroidal anti-inflammatory drug, was formulated into inclusion complexes by grinding and precipitation with β-cyclodextrin and freeze drying with pyromellitic dianhydride (PMDA) cross-linked β-cyclodextrin nanosponges. Particle size, zeta potential, encapsulation efficiency, accelerated stability study, in vitro and in vivo release studies were used as characterization parameters. TEM studies showed that the particle sizes of different inclusion complexes of ASA have diameters ranging from 40.12?±?8.79 to 59.53?±?15.55?nm. It also revealed the regular spherical shape and sizes of complexes that are even unaffected after drug encapsulation. Zeta potential was sufficiently high to obtain a stable colloidal formulation. The in vitro and in vivo studies indicated a slow and prolonged ASA release from PMDA cross-linked β-cyclodextrin nanosponges over a long period. XRPD, DSC and FTIR studies confirmed the interactions of ASA with nanosponges. XRPD showed the crystalline nature of ASA decreased after encapsulation. These results indicate that ASA nanosponges formulation can be used for oral delivery.     

机械研磨时间对铜基甲醇合成催化剂性能的影响

采用机械研磨燃烧法在不同研磨时间下制备了系列Cu/ZnO/Al2O3催化剂,并评价了其在一氧化碳加氢制备甲醇反应中的活性。催化剂前驱体的焙烧过程通过热重-差热分析仪(TG-DSC)监测。采用X射线衍射(XRD)、扫描电镜(SEM)、N2吸附、程序升温还原(TPR)和N2O氧化后氢气滴定等方法对催化剂进行了表征。结果表明,催化剂的结构性质与研磨时间密切相关,催化剂的比表面积和铜原子的分散度随研磨时间延长先增大后减小,研磨2 h制得的催化剂显示了最高的催化活性。     

The Physical Preparation of Geologic Samples For Chemical Analysis Using Laboratory Robotics

Abstract

An automated system to grind geologic samples has been successfully tested. A Zymate II robotic system, along with specially designed or modified hardware, was used to process partially pulverized geologic samples. the system is capable of processing samples on a 24-hour basis with an average per-samples grinding time of 12.4 minutes. A sample grinding period is followed by a cleanout sequence of air purges, vacuuming and grinding for surface cleaning with quartz sand. Routine operator involvement is limited to adjusting the grinding plates on the Bico vertical grinder at the beginning of each preparation interval. Studies conducted using variable amounts of cleaning sand between grinding of samples indicate that the adjustment interval can be extended to 50 samples (25g cleaning sand) using an acceptance criteria of 80% of sample passing 80 mesh. the processed samples are suitable for direct geochemical analysis using a variety of standard chemical digestions. Cross contamination studies using soil, chromite, and galena/sphalerite samples have revealed that the grinding system is capable of clean-out efficiencies exceeding 99% using as little as 25g of cleaning sand.     

Microwave-assisted steam distillation with simultaneous liquid/liquid extraction of pentachlorophenol from organic wastes and soils

An efficient method for extracting pentachlorophenol (PCP) from organic solid matrices and soils using direct excitation of the fresh samples by microwave energy is presented. Steam-volatile PCP partitioned into the organic solvent n-hexane within the closed extraction vessel, resulting in recovery rates of 85-92% from aged samples. Condensed water provided a boundary layer between extract and sample thus preventing any contact of PCP with and re-partitioning into the sample. Duration of the microwave-assisted process was 35 min. Crude extracts were derivatized by heptafluorobutyric anhydride (HFBA) to improve selectivity and sensitivity resulting in detection limits of 1-2 micro g kg(-1). GC-MS/MS analyses proved that suitable extracts with only minor impurities were obtained. Common sample treatment steps like drying, thorough grinding, frequent transferring, and tedious clean-up, and concentration procedures which all can cause certain losses of analyte were minimized. The efficiency of the method was verified by comparison with an established ultrasonic extraction procedure. This microwave-assisted pressurized steam distillation with simultaneous partition into an organic phase thus provides a streamlined and efficient strategy which requires no additional investment in standard equipment for microwave-assisted extractions (MAE). Degradation of analytes at longer extraction times must be taken into account.     

K417材料缓进深磨烧伤色与氧化膜结构的研究

本实验应用X射线光电子谱仪,在获取磨削弧区温度的基础上研究了K 417镍基铸造高温合金表面氧化膜的成分和结构,其中包括正常缓磨后及出现不同层次烧伤色后的氧化膜,结果表明,氧化膜不是出现烧伤色的试样所特有,对正常缓磨试样也存在,只是氧化膜厚度不同而已。磨削弧区温度越高,烧伤色层次越深,对应的氧化膜厚度亦越大。氧化膜是Ni、Cr、Ti、Al等元素的氧化物及晶体态Ni等以掺合结构所组成。     

无溶剂固相研磨法合成乙酰丙酮铝

以无机铝盐、乙酰丙酮(Hacac)为原料,固体碱为反应促进剂,室温下固相研磨合成了乙酰丙酮铝.考察了碱的用量及种类、物料摩尔比、研磨时间对产率的影响,并和经典方法作了对比,固相研磨法产率较高(90%以上).目标产物用红外、热重进行了表征,结果与标准谱图一致.最佳工艺条件为n(A l3+)∶n(Hacac)=10∶40,固体碱适量,室温研磨1 h.     

研磨破乳的规律及其机理

报道了研磨破乳的实验规律，讨论了研磨破乳的基本步骤：（１）过滤过程中乳状液内相液滴在研磨剂表面铺展成膜并进一步聚结──过滤破乳；（２）研磨剂的相互碰撞使乳状液的分散液滴受到摩擦力和剪切力，导致液滴聚结──研磨破乳。     

Influence of two grinding methods on the uncertainty of determinations of heavy metals in atomic absorption spectrometry/electrothermal atomisation of plant samples

 Chemical analyses of trace elements are affected by relatively high analytical errors due to the different steps of the laboratory procedures: samples grinding, mineralisation and instrumental measurements. In the present communication, the influence of the grinding phase on the global uncertainty of Pb, Cd, Ni and Cr determinations in plant samples by the classical method of atomic absorption spectrometry/electrothermal atomisation (AAS-ETA) after dry ashing is quantified. Two grinding machines, a planetary mill with balls and jars of agate versus a stainless steel grinder were compared by analysing leaf samples of cucumber, strawberry, kiwivines, apple trees and grapevines from agricultural experimental plots under controlled conditions. Variance components due to the difference between grinding methods and experimental plots were estimated. Further, the simultaneous effects of the grinding methods on all considered metals have been evaluated by analysis of variance. With the stainless steel grinder, on average, higher levels of the considered heavy metals were obtained (up to 67% of the mean values). On average, the increments were similar for metals contained in steel (Ni and Cr) and those not contained (Pb and Cd). The true causes of these differences need further investigation to determine whether the higher metal detection is due to possible contamination, to a different grinding quality or to other reasons. Finally, the grinding methods did not seem to affect the combined uncertainty of the analyses. Received: 3 November 1997 · Accepted: 29 November 1997