Synthesis of methyl,propyl, butyl,isobutyl, hexyl,cyclohexyl, octyl,and 2-ethylhexyl esters of epoxyoleic acid

A series of esters of 12,13-epoxyoleic acid were prepared by means of alcoholysis of triepoxyolein (trivernolin). The procedure for the alcoholysis, and isolation and purification of the esters are described. Analytical characteristics of the esters are reported. E. Util. Res. Devel. Div., ARS, USDA.     

DUO-ICP-AES测定精对苯二甲酸中的钴、铬、铁、锰、钼、镍、钛

采用DUO-ICP-AES同时测定精对苯二甲酸中钴、铬、铁、锰、钼、镍、钛,并对仪器的分析线选择、背景校正、入射功率、雾化器压力、辅助气流量、冷却气流量、蠕动泵转速的影响及共存元素的干扰、硝酸铯灰化助剂等因素进行了详细的研究。方法的检测限:钴0.0097 mg/L;铬0.0021 mg/L;铁0.0078 mg/L;锰0.0012 mg/L;钼0.0027 mg/L;镍0.016 mg/L;钛0.0027 mg/L,回收率和精密度分别为93.0%～99.5%和0.37%～3.2%。该方法快速简便,具有良好的精密度和准确度,适用于进出口精对苯二甲酸的日常检验。     

Continuous solvent extraction of sunflower,seed, groundnuts,palmkernels, rapeseed,and copra

In principle, the oil milling process is straightforward. The wide variety of equipment in use reflects, however, a multiparametric process. The main limiting parameters are kind of seed, oil content, particle strength, particle structure, temperature, moisture, particle size, residence time, mechanical forces, etc. Additionally, the seed specific parameters vary not only between kinds of seed but also for the same seed, due to different conditions in climate, soil, and harvesting. Therefore, equipment design must be widely based on statistical averages of the limiting parameters. In other words, exact precalculation of the single technological steps is impossible. As a consequence, for more than 5,000 years, the oil milling process has been in the stage of being optimized. The acutal technical standard is very satisfying, but there is still a strong need for further research and development. Currently, as in the past, the oil milling process seems to be not so much a science as an art.     

微波消解ICP-AES法测定润滑油中的铁,镍,铜,锌,硼,磷

通过微波消解处理润滑油,ICP法测定润滑油中铁,镍,铜,锌,硼等元素,通过正交实验进行微波消解条件优化,并进行了精密度实验,标准样品的回收率为98%以上,相对标准偏差小于1%。     

Melting of Forsterite, Monticellite, Merwinite, Spinel, and Periclase Assemblages

Experimental data which define melting temperatures and crystalline solution compositions show that the assemblage forsterite+monticellite+spinel+periclase melts near 1425°C and that the assemblage monticellite+merwinite+spinel+ periclase melts between 1406° and 1420°C. The melting of the former assemblage is a double reaction point. The forsterite crystalline solution contains 13 mol% monticellite and the monticellite crystalline solution contains 22 mol% forsterite. A projection system shows that the new data agree with much previous data but highlight inconsistencies in previous data for assemblages containing more CaO, such as merwinite+dicalcium silicate+spinel+periclase. These assemblages are encountered in magnesite refractories with CaO:SiO₂<2.0 during firing and in service.     

水镁石、水菱镁石和斜方云石资源、加工与应用

对水镁石、水菱镁石和斜方云石资源及其加工和应用进行了评述。包括上述资源的发展历史、化学组成和物性参数、资源储量和矿石品位、生产加工以及在不同领域(如镁质阻燃剂、中和剂、重金属离子脱除剂、镁肥、饲料添加剂等)的应用,并对它们的发展前景进行了展望。     

新时代，以创新思维审议磷矿加工方法

地球已进入以人类为中心的“人类纪元”。为使全球可持续发展,应考虑今后几十代人对磷资源的需求。介绍了世界磷资源现况及国内外最新磷矿储量数据,分析了我国磷肥产品结构;提出高品位、易加工磷资源用于磷化工、磷化学品合成,低品位、难选磷矿用于含磷肥料生产的新思路,并认为生产过磷酸钙、钙镁磷肥比生产磷铵类肥料对磷资源利用更合理。提出了磷肥产业结构调整新战略,以使我国磷资源的可采寿命从目前的100—200年延长至500年。     

新型高效肥料创制的意义,现状及发展趋势

系统分析了新型高效肥料创制的意义,阐述了缓／控释肥料、稳定肥料、复合（混）肥料和有机肥料的发展现状和趋势,提出了今后我国新型高效肥料创制的方向。     

Synthesis of Hexabenzo[a,cd,f,j,lm,o]perylene

Hexabenzo[a,cd,f,j,lm,o]perylene (HBP), an undecacyclic condensed polycyclic aromatic hydrocarbon with two severely crowded fjord regions, was synthesized by Clar's method; the starting material 8H-benzo[fg]-naphthacene-8-one was newly prepared by the glycerol condensation of 5,12-dihydro-naphthacene-5,12-dione. ¹H and ¹³C NMR spectra of HBP were measured and the chemical shifts were completely assigned. Absorption and fluorescence spectra of HBP were also measured and the effects of nonplanarity on its spectroscopic properties was discussed.     

Cleaning,cracking, dehulling,decorticating, and flaking of oil-bearing materials

Techniques and equipment for cleaning, cracking, dehulling, decorticating, and flaking of oil-bearing materials are described. Particular methods and cautions for unusual materials are discussed.     

Morphological,structural, surface,thermal, chemical,and magnetic properties of Al-doped nanostructured copper ferrites

Aluminum-doped copper ferrite nanoparticles synthesized via thermal decomposition were analyzed for Al³⁺ substitution effects. Nanocrystalline doped copper ferrite with a crystallite size <9 nm was characterized using several advanced techniques, including X-ray diffractometry (XRD), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), scanning electron microscopy (SEM), energy-dispersive X-ray spectroscopy (EDX), and X-ray photoelectron spectroscopy (XPS). The degree of thermal decomposition used for doping copper ferrite at the nanoparticle level correlates well with the quantitative, dimensional, and structural characterizations. The Scherrer equation and Williamson–Hall method were employed to determine the general lattice strain and constants. Structural properties, such as the oxygen positional parameters, radii of the octahedral and tetrahedral sites, hopping lengths, bond lengths and angles, site bonds, and edge lengths, were determined using XRD patterns. The improved A–B super-exchange interaction was demonstrated by the discrepancy in the theoretically anticipated bond angles. The analysis of magnetic hysteresis (M − H) using a vibrating sample magnetometer (VSM) and XPS confirmed the improvement in the super-exchange interaction. XPS results suggest that Fe and Cu in the crystal lattice are in the form of Fe^III and Cu^II, respectively. The investigation of the degree of inversion, state, and composition using XPS aids to understand the properties of the nanostructured copper ferrites. The saturation and remnant magnetization were determined from hysteresis loops at 1.8 T obtained using the VSM at room temperature. The noncollinear spin and efficient sublattice interactions are responsible for the decrease in M_s and M_r.     

ICP-AES分析低合金钢中的Mn、Mo、V、Ni、Al、Cu、Cr元素

用等离子发射光谱法测定低合金钢中的Mn、Mo、V、Ni、Al、Cu、Cr元素,试样用HNO3和HCl在加热条件下分解,经过系列试验,选择仪器的工作条件,进行测定,建立了一套分析方法,经对照分析,分析结果令人满意。本方法快速准确,精密度良好,完全可以满足生产需要。     

汉中绿茶中铜、铁、锰、锌、氟含量的测定

为了解汉中地区绿茶中铜、铁、锰、锌、氟的含量,采用微波消解-原子吸收分光光度法及氟离子选择电极法对汉中绿茶中的铜、铁、锰、锌、氟含量进行了测定。结果显示,汉中绿茶中铜、铁、锰、锌、氟的含量范围分别为66.96μg.g-1,482.30μg.g-1,854.57μg.g-1,89.75μg.g-1,48.6μg.g-1。与文献相比,汉中绿茶中铁、锌含量远高于平均值,锰和铜的含量与平均值相当;氟含量略低于绿茶平均氟含量。     

ICP-OES测定大量元素水溶肥料中锌、镁、铜、铁、锰、钼、硼含量

采用ICP-OES对大量元素水溶肥料中微量元素锌、镁、铜、铁、锰、钼、硼进行分析,研究确定了最佳分析条件。加标回收率为96.94%～106.2%,RSD为0.50%～1.40%,检出限为0.001 8～0.218 0 mg/L,方法简便、快速、准确。     

Characterization of crystalline cellulose in biomass: Basic principles, applications, and limitations of XRD, NMR, IR, Raman, and SFG

Cellulose is among the most important and abundant biopolymers in biosphere. It is the main structural component of a vast number of plants that carries vital functions for plant growth. Cellulose-based materials have been used in a variety of human activities ranging from papers and fabrics to engineering applications including production of biofuels. However, our understanding of the cellulose structure in its native form is quite limited because the current experimental methods often require separation or purification processes and provide only partial information of the cellulose structure. This paper aims at providing a brief background of the cellulose structure and reviewing the basic principles, capabilities and limitations of the cellulose characterization methods that are widely used by engineers dealing with biomass. The analytical techniques covered in this paper include x-ray diffraction, nuclear magnetic resonance, and vibrational spectroscopy (infrared, Raman, and sum-frequency-generation). The scope of the paper is restricted to the application of these techniques to the structural analysis of cellulose.     

The introduction of alkyl,ester, carboxylate,amino, hydroxyl,and phosphate functional groups to the surface of polyethylene

The surface of polyethylene was derivatized with ester, carboxylate, amino, hydroxyl, and phosphate functional groups. α, ω bifunctional alkanes, containing on one end a primary amine, were coupled to oxidized polyethylene through an amide linkage. Polyethylene was first oxidized with chromic acid, the carboxylate groups were converted to the acyl chloride with phosphorus pentachloride, and then reacted with a primary amine to give the covalently bound amide. The copposing ends of the bifunctional alkanes were the methyl, tertiary amine, ester, and hydroxyl groups. The ester was converted to the carboxylate by acid cleavage and the hydroxyl group converted to the phosphate by treatment first with phosphorus oxychloride and then aqueous base. Attenuated total reflection FTIR, XPS, and pH-dependent contact angle wetting were used to characterize the surfaces. The FTIR data were used to confirm the formation of the amide and to detect an undesired carboxylate/ammonium ion complex formed in the presence of trace amounts of water. XPS data were used to confirm expected changes in elemental composition and to provide quantitative estimates of the yields. Oxidation of the polyethylene introduced 5 × 10¹⁴ carboxylate groups/cm² in the 25 Å XPS sampling depth. Of these, up to 98% could be converted to the amide. The advancing contact angle data confirmed the acid/base behavior of the functional groups.     

Preparations,optical, structural,conductive and magnetic evaluations of RE's (Pr,Y, Gd,Ho, Yb) doped spinel nanoferrites

Rare earths RE's (Pr, Y, Gd, Ho, Yb) substituted MnZn spinel ferrites with composition of Mn_0.5Zn_0.5M_0.02Fe_1.98O₄ (M = Pr, Y, Gd, Ho, Yb) are prepared by sol gel combustion approach. Low sintering temperature (500 °C) is used to sinter the RE's doped MnZn samples. MnZn samples are further characterized by X-ray diffraction (XRD) and field emission scanning electron microscopy (FESEM) to measure the cubic crystalline structure, particle size, morphology, porosity and grain size. Cubic crystalline phase of prepared RE's doped MnZn ferrites is confirmed by x-ray diffraction (XRD). The morphology, porosity and grain size are observed using FESEM. The magnetic properties of RE's doped MnZn nanoferrites are analyzed by vibrating sample magnetometer (VSM). Coercivity (H_c), remanence (M_r) and saturation magnetization (M_s) are calculated from the magnetic loops. The saturation and remanence of the nanoferrites are increased by the substitution of RE's metal ions and varies from 14.76 to 26.36 emu/g and 9.98–22.48 emu/g respectively. Bohr magneton and anisotropy constant are calculated from the recorded magnetic data. The conductive analysis of the prepared samples is studied at 40 °C −300 °C temperature, leading to the conductivity measurements from 1.12 × 10^-2 Ω^-1-cm^-1 to 9.52 × 10^-2 Ω^-1-cm^-1. UV–Vis spectroscopy is used to determine the semi conducting nature of RE's doped MnZn spinel ferrite samples. The magnetic, conductive and optical study of the RE's doped MnZn nanoferrites sintered at low temperature suggests the use of these materials for microwave absorption, supercapacitor, lithium ion batteries and nanoelectronics industrial applications.     

电感耦合等离子体原子发射光谱法同时测定金属饰品中铅、镉、铬、汞、锑、砷、硒、钡、镍含量

采用电感耦合等离子体原子发射光谱法同时测定金属饰品中铅、镉、铬、汞、锑、砷、硒、钡、镍的含量.用体积比为3∶1的浓硝酸和浓盐酸微波溶解样品,研究了样品的消解方法、消解介质、分析谱线及工作参数等对检测结果的影响.方法的检测限(mg/L):铅0.06、镉0.009、铬0.002、汞0.04、砷0.02、硒0.01、钡0.0...     

ICP—AES法测定镍铁中Si、Co、Cu、P、Mn、Cr

研究了用ICP—AES法测定镍铁中Si、Co、Cu、P、Mn、Cr元素含量的分析方法。分析了镍基和铁基效应对某些元素强度影响情况,采用基体匹配法消除镍基和铁基的干扰效应。采用信倍比和净强度为仪器测量的选择条件,用多元素混合标准溶液绘制工作曲线。测出镍铁中的Si、Co、Cu、P、Mn、Cr元素分析方法检出限。此方法有较高准确度和精密度。