浅析铝土矿烧失量的差异在X-射线荧光光谱分析中造成的影响刘静,马慧侠,彭展,白万里

本文探讨了一水铝土矿与三水铝土矿烧失量的差异在X-射线荧光光谱分析中造成的影响。采用试验的方式考察了硼酸锂熔融制样过程中铝土矿的烧失量损失情况;运用理论计算分析了烧失量的损失对测量结果的影响。试验与理论分析结果表明：当采用一水铝土矿绘制工作曲线来测量三水铝土矿样品时,将导致三水铝土矿中各组分测量结果偏高;烧失量的差异对主量元素测量结果影响较大,而对微量元素测量结果影响较小;待测物质的烧失量与基准物质烧失量差异越大,测量结果的偏差也就越大。     

浅析铝土矿烧失量的差异在X-射线荧光光谱(XRF)分析中造成的影响

探讨了一水铝土矿与三水铝土矿烧失量的差异在X-射线荧光光谱(XRF)分析中造成的影响。采用实验的方式考察了硼酸锂熔融制样过程中铝土矿的烧失量损失情况,实验表明,在熔融过程中,烧失量越大的样品质量损失也越多。运用理论计算分析了烧失量损失对测定结果的影响,结果表明:当采用一水铝土矿绘制工作曲线测定三水铝土矿样品时,将导致三水铝土矿中各组分测定结果偏高;烧失量的差异对主量元素测定结果影响较大,而对微量元素测定结果影响较小;待测物质的烧失量与基准物质烧失量差异越大,测定结果的偏差也就越大。     

粉煤灰烧失量测定方法探讨

按照标准GB/T 1596–2005中方法检测粉煤灰烧失量,发现存在检测结果为负值的现象,为了解释该现象,完善针对该类粉煤灰烧失量的检测方法,以及给出该检测方法的适用条件,分别按照标准GB/T 176-2008和GB6730.8–1986对灼烧[(950±25)℃]前后粉煤灰中硫化物和亚铁含量进行测定,同时对灼烧后粉煤灰的颜色不同进行分析。结果表明,粉煤灰中亚铁是引起粉煤灰烧失量为负值的主要原因,亚铁含量与灼烧后粉煤灰颜色有一定相关性,对于灼烧后为红棕色的粉煤灰,应对灼烧前粉煤灰中亚铁含量进行测定,视其对烧失量的影响程度,决定是否对烧失量进行校正。     

显微镜鉴别有色金属矿产品的固体废物属性

为探索有色金属矿产品与冶炼渣的微观形貌特征差异,本文采用超景深显微镜结合扫描电镜,分析有色金属矿产品微观形貌和成分组成,观察有色金属矿产品在超景深显微镜下的矿物特有的金属光泽、晶体外观,结合扫描电子显微镜手段,表征有色矿产品共生矿物情况,比对冶炼渣的无金属光泽的微观特征及非天然矿物的组成成分,实现有色金属矿产品与冶炼渣的区分,为有色金属矿产品的固体废物属性鉴别提供参考。     

微波加热测定硅酸盐矿石样品的烧失量

分别以微波加热和传统加热两种方法测定某些标准样品和管理样品的烧失量。通过试验表明，微波加热法取代传统加热法测定样品的烧失量，不仅有较高的准确度和精密度，还可以大大缩短测定时间，提高测定效率，节能效果也十分显著。     

矿产品水分含量代表值Bootstrap模拟取样估计

在对矿产品水分含量基础统计学特征描述的基础上,采用内核密度估计对水分含量数据多态性进行了分析,根据双态分布的特点,使用Bootstrap模拟取样方法对试验样本值模拟重复取样,以多次Bootstrap模拟取样的均值与标准偏差作为矿产品水分含量有限样本代表值及标准偏差的稳健估计,实践证明Bootstrap模拟取样估计对矿产品水分含量代表值的估计是有效的,该项研究为矿产品水分含量代表值的准确评估提供了一种新方法.     

几种含有酰胺基团超滤膜吸水情况的FTIR,TGA和DSC研究

对几种超滤膜的TGA、DSC及FTIR研究表明,室温下含酰胺基的干燥膜体仍以氢键的形式结合一定数量的单分子水,同时也含有微量的二聚水和多聚水。当温度上升到40℃左右,水与膜体形成的氢键几乎完全断裂。每个酰胺基吸附水量的顺序为:聚砜酰胺>聚苯并咪唑酮>芳香聚酰胺;每种膜吸附水的绝对量顺序为芳香聚酰胺>聚砜酰胺>聚苯并咪唑酮。     

铁矿和氧化铁皮的热力学特性

采用热重分析-差示扫描量热法(TGA-DSC)同步热分析技术对铁矿和氧化铁皮的热力学特性进行了研究。利用STAR~e软件方法分别比较了铁矿和氧化铁皮在氧气气氛和氮气气氛中不同升温速率条件下的TGA和DSC曲线。结果表明:在氧气气氛中,20K·min~(-1)的升温速率下得到较为理想的铁矿和氧化铁皮特征曲线。还重点分析了铁矿和氧化铁皮的TGA及DSC曲线的差异,为两者的鉴别提供了一种新的方法。     

锌电解新液中微量碲的测定—MIBK萃取火焰原子吸收光谱法

湿法炼锌厂家偶尔会发生不明原因的“烧板”现象 ,除了常见的能引起“烧板”的杂质元素砷、锑、锗、镍及钴外 ,碲有时也需要了解和掌握。锌电解新液中微量碲的测定国内尚无详细文献报道 ,文献 [1 ]介绍了工业硫酸中微量碲的测定方法 ,但方法流程较长 ,对及时指导生产存在一定的局限性。本文在文献[2 ]的基础上采用 5mol· L-1的盐酸介质中 ,用MIBK萃取微量碲 ,有机相于 2 1 4.3nm波长处以火焰原子吸收光谱法测量 ,方法的灵敏度和测定结果均符合分析要求。1　试验部分1 .1　仪器、工作条件及试剂WFX- 1 E型原子吸收光谱仪 (北京第二光学…     

熔融制样-X射线荧光光谱法同时测定石煤钒矿中12种主次成分

建立熔融制样–X射线荧光光谱法同时测定石煤钒矿中V,Ba,SiO_2等12种主次成分。采用样品与混合熔剂的质量比为1∶10熔融制样,高温煅烧除去石煤钒矿中的还原性物质,以人工混合标准样品和历年比对的石煤钒矿样品绘制标准工作曲线,采用烧失量–理论系数法校正样品的基体效应,扣除谱线重叠干扰。样品中主次成分的相对标准偏差均小于5.0%(n=10),用该方法对4种石煤钒矿管理样品进行测定,相对误差为–4.55%～4.35%,测定值和标准值基本一致。该方法应用于生产实践中,取得良好的测量效果。     

C60的氧化反应研究

在C60的甲苯或二氯苯溶液中通入O3,通过改变O3的吸收量及反应时间可得到两种氧化产物,一种产物在有机溶剂及水中均不溶,但经性水解后得到水溶性产物,其红外光谱与C60羟基化合物相似,在长时间通O3条件下,得到水溶性的C60氧化产物,用变温红外光谱、XPS、元素分析、热谱和质谱研究了氧化产物的可能结构,发现生成的C60氧化产物对热不稳定,随着温度升高,有CO2,CO和H2O放出。     

X射线荧光光谱法测定黑龙江省有机碳含量较高样品中的硅、铝、铁等元素

通过事先对有机碳含量较高的样品进行高温灼烧,计算其烧失量,再将灼烧后的样品经专用熔剂熔融制样后,经X射线荧光光谱仪测定,能够有效地去除因有机质含量高导致的分析结果的偏差,而且较湿法化学分析节省时间。实验结果表明,该方法的分析结果与湿法化学分析结果偏差很小,准确度较直接压片分析有了大幅提高。     

Flame retardant polypropylene through the joint action of sepiolite and polyamide 6

The influence of the incorporation of polyamide-6 (PA) and natural sepiolite nanoparticles on both the thermal degradation and fire behaviour of polypropylene (PP) matrix has been investigated by thermogravimetric analysis (TGA) and mass loss calorimetry. For that purpose, PP/PA blends and nanocomposites thereof were prepared by melt processing. TGA results evidenced that the use of maleic anhydride grafted-polypropylene (MA-g-PP) as compatibilizer led to a significant improvement in thermal stability under air. Such improvement was linked to the formation of a char layer preventing the thermo-oxidative degradation of PP. Interestingly, the thermal resistance of this char layer was further improved by adding 5 wt% of natural sepiolite leading to important increase of time to ignition and reduction of peak of heat release rate (pHRR) during mass loss calorimeter test.     

Thermal degradation behaviour of radiation grafted FEP-g-polystyrene sulfonic acid membranes

The thermal degradation behaviour and the gaseous products of FEP-g-polystyrene sulfonic acid membranes prepared by radiation-induced grafting of styrene onto poly(tetrafluoroethylene-co-hexafluoropropylene) (FEP) films and the subsequent sulfonation were studied using thermal gravimetric analysis coupled with Fourier transform infrared spectrometry (TGA/FTIR). The membranes were found to have a three-step degradation behaviour due to water removal, elimination of sulfonic acid groups and decomposition of the FEP matrix. The evolving gaseous products were identified using FTIR analysis. The degree of grafting was found to have a strong effect on the weight loss in the membranes, whilst the degradation temperatures of the individual membrane components were shown to be independent of the degree of grafting.     

Synthesis and characterization of konjac glucomannan-graft-polyacrylamide via gamma-irradiation

The synthesis of konjac glucomannan-graft-polyacrylamide (KGM-g-PAM) was carried out at 25 degrees C by gamma-irradiation under a N2 atmosphere. The effects of absorbed radiation dosage and monomer concentration on grafting yield and water absorbency were studied. The grafted copolymers were characterized using Fourier Transform Infrared(FTIR) spectroscopy, nuclear magnetic resonance (NMR), x-ray diffraction (XRD),thermogravimetric analysis (TGA) and gel permeation chromatography (GPC). The grafting yield was observed to increase with increasing absorbed dosage and monomer concentration. Compared with the original KGM, the grafted copolymers exhibited better thermal stability and water absorbency. The results suggest that gamma-irradiation is convenient and efficient for inducing graft copolymerization of KGM and acrylamide (AM).     

High‐throughput method for estimating the time to sustained ignition of polystyrene–clay nanocomposites based on thermogravimetric analysis

Polymer‐modified clay nanocomposites were prepared by melt blending and the time to ignition was measured by cone calorimetry at various heat fluxes. Based on these experimental results, a critical mass flux and critical percentage mass loss (pml_crit) for piloted ignition were identified and validated for both virgin polystyrene and its composites, across a wide range of heating fluxes. Based on the assumption that the polymer degradation kinetics in the heating segment of the cone calorimetry (up to the moment of ignition) and thermogravimetry experiments are similar, and using the pml_crit, we hypothesized that the onset degradation temperature of the TGA samples (defined here as the temperature at pml_crit) could be used to estimate the time to sustained ignition in cone calorimetry experiments. The onset degradation temperature and the time to sustained ignition showed a good correlation, regardless of the heating flux used in cone calorimetry experiments. Copyright © 2009 John Wiley & Sons, Ltd.     

用于制备聚氨酯纳米复合物的高岭石粒子的表征

Clay such as kaolinite， is commonly used as an additive to modify the thermal properties of polymer. In this paper， the morphology， composition， shape and structure of kaolinite was characterized by various advanced techniques. The TEM/ EDX data showed that the kaolinite had a larger particle size and a Si/Al ratio of 1.8. The individual particle of kaolinite was a single crystalline. TEM also showed that these particles were always stacked together due to the presence of electrostatic cohesive energy and hydrogen bond between plaletes. The PAS-FTIR spectra showed that no absorbance of hydroxyl group for hydration water in hydrogen bond region or at 1650cm^-1 was observed at room temperature. It meant a little ability to adsorb water for kaolinite particle. Kaolinite clay also showed no change for its PAS-FTIR spectra with increasing temperature. The TGA results revealed that kaolinite almost doesn′t lose weight at 60℃ due to loss of dehydration of absorbed water， however， it will decomposed around 510℃ and lose its hydroxyl functional group in the form of water (dehydroxylation). The result is consistent with that of PAS-FTIR analysis. This suggests that the structural hydroxyl group on the surface of individual kaolinite clay particle is very stable below 500℃， and the kaolinite composed polymer could be got by the reaction of its stable structural hydroxyl group with isocynate group of polyurethane prepolymer.     

X射线荧光光谱法测定高含量有机碳样品中的钾、钠、钙、镁、硅、铝、铁、钛、锰、磷

通过事先对有机碳含量较高的样品于1000℃ 下灼烧2 h,计算其烧失量,再将灼烧后的样品经Li2 B4 O7(67％)和LiBO2(33％)的混合熔剂熔融制样后,经X射线荧光光谱仪测定,能够有效地去除因有机质含量高导致的分析结果的偏差,总体的平均相对误差从11.1％ 减少到了4.5％,而且较湿法化学分析节省时间.分析结...     

Degradation of sisal fibre/Mater Bi-Y biocomposites buried in soil

Degradation of short sisal fibres/Mater Bi-Y™ biocomposites during indoor burial experiments was analysed. Within the first month, water sorption was the main event followed by weight loss. Water sorption results demonstrated that composites absorbed less water than the matrix. The lower sorption capacity of composites was related to the presence of fibre-fibre and fibre-matrix (both of carbohydrate nature) interactions which delay the water intake and enhances the material stability. In soil burial, all materials followed the same degradation pattern. The amorphous nature of the matrix favoured the preferential removal of starch, which was the most bio-susceptible material, as observed by thermogravimetric analysis (TGA) and scanning electron microscopy (SEM). Fibres seemed to play a secondary role in this process, as confirmed by the slight difference in weight loss between the matrix and composites (40 and 33 wt.%, respectively). The drop in mechanical properties as a function of the exposure time was associated with the preferential loss of matrix and fibre components and the detriment of the fibre/matrix interface.     

Effect of radiation absorption modes on ignition time of translucent polymers subjected to time-dependent heat flux

Majority of previous solid ignition models, including numerical and analytical ones, considered only surface absorption of incident heat flux for simplification. However, the influence of in-depth absorption on pyrolysis and subsequent ignition cannot be ignored for infrared translucent polymers. This work addresses this problem and focuses on time-dependent heat flux to establish an analytical model for ignition behaviors prediction by means of theoretical analysis. Ignition temperature was utilized as the ignition criterion, and both surface and in-depth absorption scenarios were considered. Thermally thick polymethyl methacrylate and polyamide 6 were selected as reference materials to verify the reliability and applicability of the proposed model by comparing the analysis results with experimental data as well as numerical simulations. A method for determining the approximation parameters of the theoretical analysis was presented to derive the relationship between ignition time and the coefficients in heat flux expressions. The results show that the higher surface temperature owing to surface absorption accelerates the pyrolysis rate and results in a shorter ignition time, while in-depth absorption affects the ignition time inversely. The effect of surface heat loss was also evaluated quantitatively through both analytical and numerical models. The uncertainty of the proposed model is mainly caused by the selection of the approximation parameters. Nevertheless, it provides an alternative approach to estimate the ignition time of translucent polymers besides numerical simulation.