Tapered element oscillating microbalance (TEOM) studies of isobutane,n‐butane and propane sorption in β‐ and Y‐zeolites

A TEOM is used to elucidate the adsorption/desorption characteristics of alkylation reactants on USY‐ and β‐zeolites. Equilibrium adsorption isotherms were obtained on USY‐ and β‐zeolites using n‐butane, isobutane and propane as proxy reactant molecules (T = 303–398 K, adsorbate partial pressure 0–1.2 bar). Analysis of the transient adsorption/desorption profiles of these molecules from either a bed of the zeolite or pelletized particles of the crystals (with mean size < 1 μm) demonstrate that diffusion in the secondary meso‐/macroporous structure formed in the packing or the pellets controls the overall sorption rates. The experimental adsorption/desorption profiles from the pelletized zeolites were regressed with available mathematical models to obtain effective meso‐/macropore diffusivities for reactant molecules, and nearly perfect fits of the experimental and the modeled profiles. Taking into account the dead volume in the system, a criterion for reliable measurements of either micropore or mesopore diffusivities by the TEOM technique is derived. © 2009 American Institute of Chemical Engineers AIChE J, 2010     

Development of a quantitative method for headspace analysis of methylsulfanyl-volatiles from kiwifruit tissue

Minor fruit volatiles are likely to be missed using sampling techniques optimized for the extraction of major compounds. This can be a disadvantage if these minor compounds contribute to characteristic fruit flavors. In this comparative study, headspace solid-phase microextraction (HS-SPME) and dynamic headspace sampling (DHS) parameters were systematically optimized to ensure highest extraction yields of methylsulfanyl-volatiles from kiwifruit tissue samples. A significant “salting-out” effect from the fruit matrix was observed using both sampling techniques after (NH₄)₂SO₄ saturation. HS-SPME at optimized conditions (polydimethylsiloxane-divinylbenzene-coated fiber, (NH₄)₂SO₄ saturation, 5 min equilibration and 20 min sampling at 40 °C) was faster and more convenient to use than DHS for qualitative purposes. Despite this, the qualitative and quantitative methylsulfanyl-volatile profile was improved using optimized DHS ((NH₄)₂SO₄ saturation; sampling time 20 h; flow rate 30 mL min^− 1) compared with HS-SPME, making this the more sensitive and preferred method for quantitative studies. The optimization strategies for increasing headspace extraction yields of trace compounds presented in this study can easily be applied to tissue samples from other fruit.     

响应面优化蒲公英橡胶草菊糖提取工艺及其MALDI-TOF MS分析

以蒲公英橡胶草根为原料,采用超声提取的方式,通过单因素实验和响应面试验探究了超声功率、提取时间、超声温度、液料比对蒲公英橡胶草菊糖提取率的影响,得到蒲公英橡胶草菊糖提取的最佳工艺为:超声功率230 W、超声时间34 min、超声温度61 ℃、液料比30:1（mL:g）,菊糖提取率为20.14%±0.19%。采用氢氧化钙-磷酸法、三氯乙酸法、Sevage法进行脱蛋白纯化,得出氢氧化钙-磷酸法的效果最好,其蛋白清除率达90.78%,菊糖损失率为26.44%。将菊糖粗提液经蛋白纯化、脱色、旋蒸、醇沉及真空冷冻干燥后得到纯度为80.8%的菊糖,为白色固体粉末。经MALDI-TOF MS进行表征分析,确定其单体的分子量为162,端基的分子量和为179,能检测到的聚合度范围为2~30。此研究为蒲公英橡胶草的综合利用研究提供了理论依据。     

Stabilized Magnesium/Perfluoropolyether Nanocomposite Films by Helium Droplet Cluster Assembly

The production of stable, pre‐reactive, nanocomposite mixtures of magnesium and a perfluoropolyether (PFPE) has been achieved through the application of helium droplet cluster assembly. The nanocomposite films presented in this work demonstrated clear thermal desorption features that indicate the formation of an MgF₂ passivation layer between unreacted magnesium cores and PFPE shells upon heating. Additional heating resulted in the later rupture of the MgF₂ layer and release of trapped magnesium. The passivation behavior occurred only after deposition with the input of thermal energy, demonstrating the ability of helium droplets to assemble and deposit clusters in a pre‐reactive state.     

表面解吸常压化学电离质谱法快速鉴别羊肉真伪

采用自行研制的表面解吸常压化学电离源（DAPCI）,在无需样品预处理的条件下,通过DAPCI-MS方法直接获取不同肉类样品（鸭肉、牛肉、猪肉、羊肉、自制假羊肉）的指纹谱图。采用主成分分析（PCA）方法对指纹谱图信息进行数据分析,以区分不同肉类样品。结果表明：鸭肉、牛肉、猪肉、羊肉和自制假羊肉的指纹谱图之间存在差异,采用PCA方法能较好地区分这些肉类样品。本方法无需样品预处理,分析速度快,可实现高通量肉类的快速鉴别,为食品安全中辨别肉类样品提供了一种快速、高效的分析方法。     

用酸性吸附-碱性淋洗工艺从硫酸浸出液中提铀

研究了用弱碱性阴离子交换树脂从硫酸浸出液中吸附铀,NaOH预处理负载树脂,碳酸钠和碳酸氢钠解析负载树脂的酸性吸附-碱性淋洗工艺。研究结果表明:该工艺能有效吸附溶液中的铀酰离子,选择性高;NaOH预处理工艺在中和树脂中氢离子的同时,能有效去除硫酸根离子,并降低钼、硅、铁等杂项元素含量;通过控制碳酸钠和碳酸氢钠溶液的流速,可成功将树脂上的铀淋洗到溶液中,实现铀的净化提取。     

反循环原位快速取样技术在煤层瓦斯含量准确测定中的应用研究

瓦斯含量测值的准确度是影响矿井瓦斯防治措施制定与实施的关键因素,而实现原位快速取样则是准确测定瓦斯含量的前提条件,为研究不同取样方式对瓦斯含量测值的影响,以仲恒煤矿1320_-11工作面的20_-1^#煤层为例,利用基于反循环钻进原理研发的原位快速取样技术及装置,对相同深度下反循环原位快速取样与孔口接粉取样方式所采取煤样粒度分布情况进行对比分析,对不同取样方式所采取的煤样利用直接法进行可解吸瓦斯含量测定对比分析,并对不同暴露时间、不同煤样粒度对瓦斯损失量的影响进行了实验室分析。结果表明:原位快速取样技术所取样品不受孔壁残粉影响,取样时间短、暴露时间少,煤样粒度大、瓦斯含量测定结果准确性更高。     

Mn含量对(V60Ti22.4Cr5.6Fe12)100-xMnx(0≤x≤3)合金吸放氢性能的影响

系统研究了采用FeV80中间合金制备的低成本(V60Ti22.4Cr5.6Fe12)100-x Mnx(0≤x≤3)合金的吸放氢性能及微观组织结构。XRD及PCT测试结果表明,随着Mn含量的增加,合金的晶格常数减小,放氢平台压先升高后降低;吸氢量随Mn含量的增加不断降低,而Mn含量的增加对放氢量没有显著影响。当Mn含量为2.5 at%时,合金室温下的放氢平台压达到最大值0.14 MPa,吸氢量为3.64%(质量分数,下同),放氢量为2.00%。SEM及EDS分析表明,不同Mn含量的合金均由bcc主相、富钛二相及稀土氧化物相组成,且Mn主要存在于合金的bcc主相中,而在富钛二相中分布相对较少。     

Mg(NH2)2的合成以及Mg(NH2)2-LiH的储氢性能研究

通过机械球磨的方法,将MgH2粉末与高纯NH3球磨反应后在300℃下热处理晶化,制备出了高纯度的Mg(NH2)2。在150~240℃的温度范围内,对Mg(NH2)2+2.2LiH(摩尔比)储氢体系的储氢性能进行了研究,结果发现,在系统脱氢后的产物为Li2Mg(NH)2。放氢动力学揭示了该系统在200~240℃时可逆储氢量可达4.5%(质量分数)左右。该系统在150℃开始脱氢,在动力学数据的基础上可以计算出其活化能为51.7 kJ/mol。此外,脱氢反应的焓变和熵变可由P-C-T曲线得到,其值分别为42.8 kJ/mol H2和149.2 J·K-1/mol H2。     

潘庄煤层气井分压合采技术及其应用分析

为了查明潘庄煤层气分压合采井的主控因素和适用条件,选用了潘庄区块生产达五年以上的分压合采井为研究对象,通过对储层地质特征、水力压裂施工参数和排采数据的整理分析,探讨了分压合采井成功实施的地质和工程因素。研究结果表明,煤层气合采井成功的关键是压裂裂缝在煤层中充分扩展,控制裂缝的缝高,避免煤层与顶底板含水层在近井地带发生水力联系;各煤层的原始储层压力、临界解吸压力相匹配时或相差不大时,通过坚持"连续、缓慢、稳定"的排采方针,合层排采会取得成功。