GC-MS有机定性扫描法在环境事件固体废物危险特性鉴定中的应用研究

环境事件中对于具有明显有机物刺激性气味的固体废物进行危险特性鉴别,可通过有机定性手段快速筛选主要/特征污染物,为环境损害司法鉴定提供重要依据。本研究以某环境事件中具有芳香族有机化合物刺激性气味的固体废物为研究对象,通过GC-MS检测方法对待鉴别固体废物进行有机定性扫描,根据结果确定待鉴别固体废物主要有害成分为有机物,确定对待鉴别固体废物进行浸出毒性甲苯指标定量检测。根据浸出毒性甲苯指标检测结果,对照《国家危险废物名录(2021年版)》废物代码编码原则,确定待鉴别固体废物代码为“900-00-06”。本研究不局限于环境事件固体废物鉴定最小样品份样数,通过定性与定量结合的技术方法开展固体废物危险特性鉴定工作,在降低鉴定成本、提高工作效率的基础上,精准得出鉴定结论,可为环境损害司法鉴定、固体废物危险废物鉴别从业技术人员提供参考性建议。

GC-MS有机定性分析法在工业废盐危险特性鉴别中的应用研究

本文以具有明显有机化合物刺激性气味的工业废盐为研究对象,通过GC-MS有机定性分析法对工业废盐代表性样品进行分析,初判废盐中可能含有苯胺物质,确定对采集的5个样品进行浸出液苯胺指标和成分苯胺含量检测。5个样品的浸出液和成分均有苯胺检出,依据《危险废物鉴别标准(征求意见稿)编制说明》确定浸出毒性苯胺指标标准限值参考值为10 mg/L,最终判定待鉴定工业废盐为危险废物。本研究旨在为从事固体废物鉴定、污染物性质鉴定等领域的技术人员提供“定性-定量”相结合、多种途径分析固体废物潜在危险特性的技术逻辑。

反相高效液相色谱法同时测定乙酰磺胺酸钾及糖精钠、苯甲酸、山梨酸

用反相高效液相色谱法（ＲＰ－ＨＰＬＣ），同时快速测定在不同食品中的新型人工甜味剂乙酸磺胺酸钾及糖精钠、苯甲酸、山梨酸。用ＯＤＳ分离短柱（ＸＬ－ＯＤＳ３μｍ４．６ｍｍ×７．０ｃｍ），以ＣＨ３ＯＨ／０．０２ＭＮＨ４ＡＣ（１２：８８Ｖ／Ｖ，ＰＨ５．４）替代乙腈／磷酸盐流动相，根据色谱保留时间ｔｒ结合对组份不停泵紫外光谱扫描进行定性，外标法峰高定量。

对新型材料化学分析方法建立的探讨

本文提出借助XRF定性扫描、ON分析、红外碳硫分析等手段在全面对新型材料金属硅粉及新型硅球进行组成分析的基础上,选择最贴和的方法完成其中Si及P、Ca、Al、Mn方法建立,满足生产检测需求,是新型材料方法建立的很好模式。

两种脂肪酸聚甘油酯(PGE)的性质比较

脂肪酸聚甘油酯(Polyglycerol esters of fattyacids,简写为PGE)在常温下有半固态和固态两种存在状态,本文通过对分别添加这两种PGE的软冰淇淋基料进行粘度、pH、粒径分析和垂直扫描分散稳定性分析(Turbiscan),发现半固态PGE的添加量为0.2%时,乳状液的粘度最低,粒径最小,稳定性最好;固态PGE的添加量为0.4%时,乳状液的粘度最低,粒径最小。通过比较发现,两种PGE对基料的影响有很大差别:半固态PGE能使乳状液的粒子更小,并能有效延长乳状液的稳定性;而固态PGE由于其熔点较高,可以促进脂肪结晶。

Structure and stability of Li-Mn-Ni composite oxides as lithium ion sieve precursors in acidic medium

A series of spinel Li-Mn-Ni composite oxides with theoretical chemical formula of LiNixMn2-xO4 （0〈_x〈_1.0） were synthesized by liquid phase method. Their structure and morphology were characterized by X-ray diffractometry （XRD） and scanning electron microscopy （SEM）, respectively. The stability of these Ni-substituted spinel oxides prepared at different temperatures was investigated in acidic medium as well. The results show that Ni can be brought into the spinel framework completely to form well-crystallized product when x〈_0.5 and the optimized synthesis temperature is 800℃. LiNi0.4Mn1.6O4 prepared at 800℃ can maintain the spinel structure and morphology with Li extraction ratio of 30.37%, Mn extraction ratio of 8.78% and Ni extraction ratio of 1,82% during acid treatment. The incorporated Ni not only inhibits the dissolution of Mn, but also reduces the extraction of Li due to the lattice contraction

Experimental study on the effects of drying methods on the stabilities of lignite

The drying processes are always applied prior to the transportation or utilization of lignite, and result in notable changes in the stabilities of lignite. In this paper, the study on the effects of nitrogen and MTE drying process on the physico-chemical properties and stabilities of Zhaotung lignite was carried out. The briquettes produced by MTE drying in this study were 150 mm in dimension, and so had a much larger particle size than nitrogen- dried samples. Nitrogen adsorption, mercury intrusion porosimetry and scanning electron microscopy all suggested that drying was accompanied by the transformation of larger pores into smaller ones. Compared to nitrogen drying, the pore structures could be stabilized by the MTE process. The soluble salts were removed during MTE drying which resulted in the decrease in ash and the concentrations of some of the major metals. The removal of water enhanced the hydrophilicity of nitrogen dried samples, but did not affect the hydrophilicity of MTE dried samples. The moisture holding capacity of MTE dried samples reduced faster than nitrogen dried samples with the decrease of residual moisture content. The moisture readsorption processes of MTE dried sam- ples were strongly inhibited due to the much larger particle size of sample produced by MTE drying than nitrogen drying. The susceptibility to spontaneous combustion, indicated by cross point temperature and self-heating tests, of nitrogen and MTE dried samples increased with the decrease of residual moisture content. The MTE dried samples are more liable to spontaneous combustion than nitrogen dried samples with the same residual moisture and particle size. However, the larger particle size of the MTE product made it more stable with respect to spontaneous combustion and also moisture readsorption.

Stabilization of Magnetite Nanoparticles by Encapsulation into the Silica Matrix

Different methods have been investigated for the synthesis of magnetic nanoparticles. Control of the particle size, dispersion, purity and stability have been always regarded an issue. In this study magnetite （Fe304） superparamagnetic nanoparticles with a size range about 20 nm have been successfully synthesized using chemical co-precipitation method from the solution of ferrous/ferric mixed salt-solution in alkaline media in oxygen-free environment. The sol-gel method has been chose to encapsulate magnetic nanoparticles into silica matrix. The phase structures, morphologies, surface area, functional classes and magnetic properties have been characterized by X-ray diffraction, SEM and AFM, BET, FT-IR and VSM. The results showed that the resultant films, consisting of encapsulated magnetite have crack free and smooth surface with a roughness value 1.5 rim.

Thermal stability of nanocrystalline in surface layer of magnesium alloy AZ91D

Isothermal and isochronal annealing was conducted to study the thermal stability of the nanocrystalline in the surface layer of Mg alloy AZ91D induced by high-energy shot peening(HESP) .Field emission scanning electron microscope(FESEM) and X-ray diffractometer were used to characterize the microstructure.Results showed that nanocrystalline produced by HESP on the surface layer of the magnesium alloy AZ91D was 60-70 nm on average.The nanocrystalline could remain stable at about 100℃,and grew up slowly between 100℃ and 200℃.When the annealing temperature reached 300℃,the growth rate of the nanocrystalline increased significantly.The kinetic coefficient n of the nanocrystalline growth was calculated to be 2-3 and the grain growth activation energy Q=39.7 kJ/mol,far less than the self-diffusion activation energy of magnesium atoms in the coarse polycrystalline material.

ZrO2/PMMA Nanocomposites： Preparation and Its Dispersion in Polymer Matrix

ZrO2/PMMA nanocomposite particles are synthesized through an in-situ free radical emulsion polymerization based on the silane coupling agent （Z-6030） modified ZrO2 nanoparticles, and the morphology, size and its distribution of nanocomposite particles are investigated. Scanning electron microscopy （SEM） images demonstrate that the methyl methacrylate （MMA） feeding rate has a significant effect on the particle size and morphology. When the MMA feeding rate decreases from 0.42 ml-min-1 to 0.08 ml. min-1, large particles （about 200-550.nm） will not form, and the size distribution become narrow （36-54 nm）. The average nanocomposite particles size increases from 34 nm to 55 nm, as the MMA/ZrO2 nanoparticles mass ratio increased from 4 ： 1 to 16 ： 1. Regular spherical ZrO2/PMMA nanocomposite particles are synthesized when the emulsifier OP-10 concentration is 2 mg.m1-1. The nanocomposite particles could be mixed with VAc-VeoVa10 polymer matrix just by magnetic stirring to prepare the ZrOE/PMMA/VAc-VeoVal0 hybrid coatings. SEM and atomic force microscopy （AFM） photos reveal that the distribution of the ZrO2/PMMA nanocomposite particles in the VAc-VeoVal0 polymer matrix is homogenous and stable. Here, the grafted-PMMA polymer on ZrO2 nanoparticles plays as a bridge which effectively connects the ZrO2 nanoparticles and the VAc-VeoVal0 polymer matrix with improved comparability. In consequence, the hybrid coating with good dispersion stability is obtained.

Acidic Montmorillonite/Cordierite Monolithic Catalysts for Cleavage of Cumene Hydroperoxide

In this work,a series of acidic montmorillonite/cordierite monolithic catalysts were prepared by a coating method using silica sol as the binder.The morphology and structure of the acidic montmorillonite/cordierite samples were characterized by means of X-ray diffraction(XRD),N_2 adsorption/desorption isotherms,and scanning electron microscope(SEM).The cleavage of cumene hydroperoxide(CHP) in a conventional fixed-bed reactor was chosen as a model reaction to evaluate the catalytic activity of the monolithic catalysts.The influences of acidic montmorillonite loading,reaction temperature.CHP concentration,and weight hourly space velocity(WHSV) on the catalytic activity and selectivity of phenol were studied.The results indicated that the obtained acidic montmorillonite/cordierite monolithic catalysts were firm and compact,and the loading of acidic montmorillonite was found to reach 40%(by mass) after three coating operations.The surface area of acidic montmorillonite/cordierite catalysts increases greatly as acidic montmorillonite loading increases due to higher surface area of acidic montmorillonite.Under the optimal reaction conditions(acidic montmorillonite loading of 32.5%(by mass),temperature of 80 ℃,a mass ratio of CHP to acetone of 1:3,and WHSV of CHP of 90 h^(-1)),the conversion of CHP can reach 100%,and the selectivity of phenol is up to 99.8%.

Influence of the characteristics of fault gouge on the stability of a borehole wall

How to find more effective way to stabilize the borehole wall in the fault gouge section is the key technical challenge to control the stability of the borehole wall in the Wenchuan fault gouge section during the process of core drilling. Here we try to describe the characters of deep fault gouge in fracture zones from the undisturbed fault gouge samples which are obtained during the core drilling. The X- Ray Diffraction （XRD）, X-Ray Fluorescence （XRF） and Scanning Electron Microscope （SEM） provided the detailed information of the fault gouge＇s microscopic characteristics on the density, moisture content, expansibility, dispersity, permeability, tensile strength and other main physical-mechanical properties. Based on these systematic experimental studies above and analysis of the fault gouge instability mechanism, a new technical procedure to stabilize the borehole wall is proposed -- a low water and a low loss low permeability drilling fluid system that consists of 4% day ＋ 0.5% CMC-HV ＋ 2% S-1 ＋ 3%sulfonated asphalt ＋ 1% SMC ＋ 0.5% X-1 ＋ 0-5% T type lubricant ＋ barite for core drilling in fault gouge sections.

Effect of cyclic drying and wetting on engineering properties of heavy metal contaminated soils solidified/stabilized with fly ash

Solidification/stabilization （S/S） is one of the most effective methods of dealing with heavy metal contaminated soils. The effects of cyclic wetting and drying on solidified/stabilized contaminated soils were investigated. A series of test program, unconfined compressive strength （UCS） test, TCLP leaching test and scanning electron microscopy （SEM） test, were performed on lead and zinc contaminated soils solidified/stabilized by fly ash. Test results show that UCS and the leaching characteristics of heavy metal ions of S/S contaminated soils are significantly improved with the increase of fly ash content. UCS of S/S soils firstly increases with the increase of the times of drying and wetting cycles, after reaching the peak, it decreases with it. When the pollutant content is lower （1 000 mg/kg）, the TCLP concentration first slightly decreases under cyclic drying and wetting, then increases, but the change is minor. The TCLP concentration is higher under a high pollutant content of 5 000 mg/kg, and increases with the increase of the times of drying and wetting cycles. The results of scanning electron microscopy （SEM） test are consistent with UCS tests and TCLP leaching tests, which reveals the micro-mechanism of the variations of engineering properties of stabilized contaminated soils after drying and wetting cycles.

A rapid method for determination of acid value in transformer oil by PPy modified electrode

A polypyrrole-modified glassy carbon electrode （PPy/GC electrode） was prepared and its electrocatalytic behavior towards naphthoquinone in the presence of acid was characterized by linear sweep voltammetry （LSV）. A well-defined new reduction peak appeared at a more positive potential than the original reduction peak. The new reduction peak current was linearly related to the acid value （AV） of oil. Based on it, a rapid electrochemical method for determining AV of transformer oil was developed using PPy/GC electrode. A working curve was obtained in the AV range of 0.01 to 0.40 mg（KOH）.g^-1, with a sensitivity of 39.42 μA0.5/（mg（KOH）.g-l） and the detection limit of 0.0014 mg（KOH）.g^-1 （signal-to-noise ratio is 3, standard deviation is 2.247%）. Moreover, the proposed method has been successfully applied to AV determination of several transformer oil samples with advantages of rapidness, high sensitivity and accuracy compared to the conventional method.

Characterization and Stability of Na-doped p-type ZnO Thin Films Preparation by Reactive DC Magnetron Sputtering

Na-doped p-type ZnO thin films have been realized by DC reactive magnetron sputtering with a set of metal-Zn targets doped with various Na contents and under different substrate temperatures, respectively. Hall effect measurement, field-emission SEM, X-ray diffraction and optical transmission were carried out to investigate the effects of Na content and substrate temperature on the properties of p-type films. Results indicate that all the Na-doped ZnO films are strongly （002） oriented, and have an average transmittance -85 % in the visible region. Na-doped p-type ZnO films with good structural, electrical, and optical properties can only be obtained at an intermediate amount of Na content and under appropriate substrate temperature. At the optimal condition, the Na-doped p-type ZnO has the lowest resistivity of 13. 8 Ω· cm with the carrier concentration as high as 1.07 × 10^18 em^-3. The stability of the Na-doped p-type ZnO is also studied in this paper and it is found that the electrical properties keep stable in a period of one month.

Al_2O_3 coating for improving thermal stability performance of manganese spinel battery

The synthesis of Al2O3-coated and uncoated LiMn2O4 by solid-state method and fabrication of LiMn2O4/graphite battery were described. The structure and morphology of the powders were characterized by X-ray diffraction (XRD) and scanning electron microscopy (SEM), respectively. The electrochemical and overcharge performances of Al2O3-coated and uncoated LiMn2O4 batteries were investigated and compared. The uncoated LiMn2O4 battery shows capacity loss of 16.5% after 200 cycles, and the coated LiMn2O4 battery only shows 12.5% after 200 cycles. The uncoated LiMn2O4 battery explodes and creates carbon, MnO, and Li2CO3 after 3C/10 V overcharged test, while the coated LiMn2O4 battery passes the test. The steadier structure, polarization of electrode and modified layer are responsible for the safety performance.

Elevated-temperature mechanical properties and thermal stability of Al-Cu-Mg-Ag heat-resistant alloy

The elevated-temperature mechanical properties and thermal stability of Al-Cu-Mg-Ag heat-resistant alloy were studied by tensile test, transmission electron microscopy(TEM) and scanning electron microscopy(SEM), respectively. The results show that with the increase of Ag content, the tensile strength and yield strength increase, which is attributed to the increase of the precipitations number and the decrease of the size. The same conclusions are drawn in the study of increasing Mg content. The alloy possesses excellent thermal stability. At 100-150 °C, the strength of the under-aged alloy increases at the initial stage, and after reaching the peak strength, it remains the same. The secondary precipitation of the under-aged alloy occurs in the process of exposure at 150℃, and it distributes diffusely after thermal exposed for 20 h. Then, the tensile strength decreases gradually with increasing the thermal exposure time at 200-250 °C. The strength of the peak-aged alloy decreases gradually, and the precipitation grows up, but the number decreases gradually with prolonging the exposure time at 100-250 °C. The strength of two kinds of alloys decreases with elevating of exposure temperature.

Effect of phosphite and epoxy soybean oil on heat stability of poly （vinylchloride） composite stabilizers

The influences ofphosphite and epoxy soybean oil in combination with liquid calcium/zinc isocaprylates on the thermal stability of flexible poly （vinyl chloride） were studied. The stabilizing effect of poly （vinyl chloride） was evaluated by Congo red method, thermoaging test and Thermogravimetric-differential Scanning Calorimetry （TG-DSC）. The results showed that the addition of the phosphite or epoxy soybean oil improved the thermal stability of PVC with the calcium/zinc isocaprylates stabilizing system, especially epoxidied soybean oil exhibited a remarkable effect, and the synergism on PVC thermal stability for 3：2 phenyl dioctyl phosphite to epoxidized soybean oil weight ratio was acquired. Accordingly, the rapid mass loss in TG curve occured between 258.9 ℃ and 334.4 ℃, which corresponded to the enthalpy of the pyrogenation of 609.2 J/g. It was also found that the stabilized PVC of the best ratio gave better mechanical and processing properties.

Investigation of the Drug Stability at the Amorphous State Using Thermal Analysis

Formulation of poorly water-soluble crystalline drugs in their amorphous counterpart is a common approach to enhance their biodisponibility. In this study, the amorphous forms of ketoprofen and flurbiprofen were obtained by supercooling of the melt in a DSC （differential scanning calorimetry） apparatus and then investigated, especially under the stability point of view. The average rate of molecular motions at any given temperature is probably the most important parameter to know for amorphous pharmaceutical materials, and it was used to explain and predict the stability of ketoprofen and flurbiprofen. A quantitative estimate of the product＇s behaviour upon storage is obtained with additional data, such as the heat capacity of crystalline and amorphous samples and the distribution of molecular relaxation times. Amorphous flurbiprofen demonstrated greater physical stability at any aging temperature tested, when compared to ketoprofen and a different dependence from aging temperature. Both amorphous drugs could he classified as ＂fragile＂ ones.

Assessing the Oxidative Stability of Commercial Chia Oil

The fatty acid composition as well as the antioxidant composition and content of two commercially available chia oils of different origins were studied. The purpose of this work was the study of the oxidative stability from different methods and the antioxidant content of the chia oils compared with other commercial oils. The oxidative stability of the oils was determined based on the oxidative stability index test （OSI test） conducted at 110 ~C and isothermal as well as non-isothermal differential scanning calorimeter （non-isothermal DSC） for the chia oil and the linseed oil. The OSI induction time of chia oil was compared with that of commercially available linseed, canola, sunflower and high-oleic sunflower oils, chia oil being the least stable oil among those studied. The inherent stability value and oxidazibility for linseed oil was lower than the chia oil A may be ascribed to a lower linolenic acid content of the former. The induction time （It） quotient at 110 ~C calculated for chia oil A and linseed oil were similar, suggesting a high degree of consistency between the results obtained by the two methods. The activation energy and specific reaction rate constant of chia and linseed oils were compared based on the results of isothermal and non-isothermal DSC. An apparent inconsistency in the experimental data results from the temperature-dependence of the activation energy of each fatty acid which can explain because the methods conditions were different.