饱和烃经5à分子筛络合前后单体烃碳同位素分析对比研究

通过对自配标准样品(正构烷烃)进行5à分子筛吸附试验,测定了用5分子筛吸附法分离前后正构烷烃、异构烷烃和环烷烃碳同位素值,探讨试验前后碳同位素值的变化。尽管实验过程中样品经过85℃长时间加热回流及吸附样品的5à分子筛用氢氟酸酸化处理,但实验结果经仪器检测,证明该方法对正构烷烃碳同位素值影响因素不大。本文还介绍了原油和煤可溶有机质中饱和烃络合前后的单体烃碳同位素分析方法。并在前人工作的基础上,改进采用微型索氏抽提加热回流实验装置,既提高了样品的回收率,也减少了样品中轻组分的损失。     

Environmental Properties of Minerals and Contaminants Purified by the Mineralogical Method

The investigation of the environmental properties of minerals, i.e., environmental mineralogy, is a branch of science dealing with interactions between natural minerals and spheres of the Earth surface as well as a reflection of global change, prevention of ecological destruction, participation in biomineralogy, and remediation of environmental pollution. Pollutant treatment by natural minerals is based on the natural law and reflects natural self-purification functions in the inorganic world, similar to that of the organic world - a biological treatment. A series of case studies related to natural self-purification, which were mostly completed by our group, are discussed in this paper. In natural cryptomelane there is a larger pseudotetragonal tunnel than that formed by [MnO6] octahedral double chains, with an aperture of 0.462-0.466 nm2, filled with K cations. Cryptomelane might be a real naturally-occurring mineral of the active octahedral molecular sieve (OMS-2). CrⅥ-bearing wastewater can be treate     

Curve-Fitting Schemes for Fragmentation Data

Fragmentation measurements in the form of sieve passing and mass fraction data were used to test the capability of three different distributions to fit the observed data over a wide range in fragment size and mass. These distributions were based on Rosin-Rammler, lognormal and simple sigmoidal (S-shaped) functions, having 2 input parameters for the single-component versions and 5 input parameters for the two-component versions. Provided convergence was achieved in the non-linear curve-fitting technique, the two-component versions always provided superior fits to the observed data. However, these versions were very sensitive to variations in the values chosen for the input parameters. In this particular regard, the two-component sigmoidal function was the most robust. The present results also show that the two-component lognormal function provided the best fit to the fragmentation data in a general sense, and the two-component Rosin-Rammler function provided the worst fit. However, there was not a significant difference between any of the three methods.     

分子筛/石墨烯复合电极材料电化学性能的对比研究

利用溶液共混法制备得到分子筛/石墨烯(RGO)复合电极材料。比较了分子筛(4A、13X、SBA-15)种类、煅烧温度以及分子筛与氧化石墨烯(GO)质量比等因素,对分子筛/RGO复合电极材料电化学性能的影响。采用X射线衍射(XRD)、孔径分析、扫描电镜(SEM)和电化学测试等分析方法考察了3种复合电极材料的结构、形貌及电化学性能。结果表明,RGO可以将4A很好地包覆,且4A均匀镶嵌在RGO层间并阻止RGO团聚,形成了三维空间导电网络结构,13X、SBA-15并不能完全被RGO包裹,RGO层间团聚现象仍较严重,不能形成三维导电网络结构。当分子筛与RGO质量比为6∶1,煅烧温度为320°C时,在4 A/g电流密度下,4A/RGO复合电极材料的比电容为450 F/g,而相应的13X/RGO、SBA-15/RGO复合电极材料的比电容分别为195、43 F/g。4A/RGO复合电极材料优异的超级电容性能可归于4A与RGO之间较强的协同效应。     

Assessment of micro‐aggregation using laser diffractometry

In order to evaluate the influence of the measuring technique on the determination of (micro‐)aggregation in soil and sediment samples, results of grain size distributions of undispersed silty soil samples obtained by the sieve‐pipette method are compared with those obtained using a laser diffraction grain size analyser, the Coulter LS‐100. Reduced major axis relationships are calculated which may be used to convert Coulter LS‐100 results to those obtained by the sieve‐pipette method. The relationships obtained are very similar to the reduced major axis relationships established for dispersed silty soil samples. The results also show that the Coulter LS measurements have a systematic bias compared to the sieve‐pipette data. This implies that, if the percentage of (micro‐)aggregation is determined, the (interpretation of the) results will be strongly dependent on the measurement technique used. Using the calibration relationships that were established, nomographs can be developed to predict the level of sieve‐pipette (micro‐) aggregation from Coulter LS‐100 data. Copyright © 1999 John Wiley & Sons, Ltd.     

4A沸石分子筛对KNO3和NH4NO3的吸持作用

实验研究了4A沸石分子筛经熔融盐处理后对KNO₃和NH₄NO₃的吸持作用。结果表明：在实验条件下,KNO₃处理后的4A沸石中含钾(以K₂O计)15.01%,含NO^-₃ 9.23%;NH₄NO₃处理后的4A沸石中含NO^-₃ 10.78%,含NH⁺₄ 0.94%。熔融盐处理后的样品X射线衍射峰相对强度发生了变化,红外光谱中1 640 cm^-1附近水的吸收带强度减弱,1 390 cm^-1附近出现的NO^-₃离子的强吸收带及825 cm^-1附近出现的NO^-₃离子的弱吸收带,以及热重-差热曲线中KNO₃和NH₄NO₃的热失重和分解热效应均证明沸石中吸持盐的存在。处理后4A沸石分子筛的基本骨架结构没有被破坏,吸持盐的4A沸石对营养盐的储备大大提高,是潜在的缓释肥料。     

柱色谱分离-分子筛络合洗脱过程中正构烷烃单体碳同位素分馏研究

应用气相色谱-气体同位素质谱(GC-C-IRMS)分析正构烷烃单体碳同位素之前,需要对饱和烃样品中正构烷烃和异构烷烃进行预分离、富集,在预分离和富集过程中正构烷烃单体碳同位素是否发生分馏是高精度分析正构烷烃单体碳同位素比值(δ~(13)C)的关键。本文以正构烷烃混合溶液为对象,利用柱色谱、5■分子筛络合、环己烷-正戊烷混合溶剂两次洗脱,GC-C-IRMS分析正构烷烃单体碳同位素,研究前处理过程中正构烷烃单体碳同位素是否发生分馏。结果表明:使用柱色谱分离前后,多数正构烷烃单体碳同位素比值相差-0.2‰～0.2‰;当5■分子筛不完全络合时,未络合的正构烷烃单体碳同位素比值偏重约0.7‰,可能发生了微弱的碳同位素分馏,但并未影响洗脱后的正构烷烃单体碳同位素比值;使用环己烷-正戊烷混合溶剂洗脱前后,碳同位素比值相差-0.2‰～0.5‰,以同样方式洗脱第二次,获得的正构烷烃单体碳同位素比值与模拟样品相差-0.3‰～0.2‰。分析不同回收率(20%)正构烷烃的单体碳同位素比值,处理前后的差值基本在0.3‰以内,可见当正构烷烃回收率低至20%左右时,其单体碳同位素仍未发生明显分馏。柱色谱分离-5■分子筛络合-混合溶剂洗脱方法适用于回收率大于20%的正构烷烃单体碳同位素分析。     

Estimating the settling velocity of bioclastic sediment using common grain‐size analysis techniques

Most techniques for estimating settling velocities of natural particles have been developed for siliciclastic sediments. Therefore, to understand how these techniques apply to bioclastic environments, measured settling velocities of bioclastic sedimentary deposits sampled from a nearshore fringing reef in Western Australia were compared with settling velocities calculated using results from several common grain‐size analysis techniques (sieve, laser diffraction and image analysis) and established models. The effects of sediment density and shape were also examined using a range of density values and three different models of settling velocity. Sediment density was found to have a significant effect on calculated settling velocity, causing a range in normalized root‐mean‐square error of up to 28%, depending upon settling velocity model and grain‐size method. Accounting for particle shape reduced errors in predicted settling velocity by 3% to 6% and removed any velocity‐dependent bias, which is particularly important for the fastest settling fractions. When shape was accounted for and measured density was used, normalized root‐mean‐square errors were 4%, 10% and 18% for laser diffraction, sieve and image analysis, respectively. The results of this study show that established models of settling velocity that account for particle shape can be used to estimate settling velocity of irregularly shaped, sand‐sized bioclastic sediments from sieve, laser diffraction, or image analysis‐derived measures of grain size with a limited amount of error. Collectively, these findings will allow for grain‐size data measured with different methods to be accurately converted to settling velocity for comparison. This will facilitate greater understanding of the hydraulic properties of bioclastic sediment which can help to increase our general knowledge of sediment dynamics in these environments.     

利用钾长石粉水热合成13X沸石分子筛的实验研究

对综合利用钾长石提钾工艺中的重要高附加值副产品13X沸石分子筛的合成进行了实验研究。对福建沙县的钾长石粉加入配料NaCO3进行焙烧实验，确定培烧的最佳工艺参数为：钾长石粉：NaCO3=1：1．30(摩尔比)，焙烧温度为845℃，焙烧时间为150min；优化的水热合成条件为M2O／SiO2(mo1)=1．50，H2O／M2O(mo1)=40．0，合成时间为8h，晶种加入量为9．0％。对合成样品化学成分分析、X射线物相分析、红外光谱分析、扫描电镜分析表明，合成13X沸石分子筛结晶完好，性能优良．水热反应经由溶解水合反应和聚合浓缩反应两大阶段。     

13X沸石分子筛的比表面积和孔分布

对利用钾长石粉水热合成的13X沸石分子筛分别进行了比表面积和孔分布测定。结果表明:13X沸石分子筛比表面积约为621.50~747.40 m²/g,总孔体积约为0.344 70~0.393 70 cm³/g;具有高比例且孔径小于2.50 nm的微孔,中-小型实验样品(SXZ-10g和SXZ-1kg)的微孔体积比例相近,为81.33%~84.70%,而扩大实验样品(SXZ-10kg)的微孔体积比例为67.90%~67.98%。13X沸石分子筛微孔的含量是决定13X沸石分子筛具有高比表面积和高效吸附性能的前提。