Measuring methods for three kinds of polyhydroxyalkanoates from activated sludge by gas chromatography

Gas chromatography determination of polyhydroxyalkanoates has been common;however,the pretreatment steps are often complex,and gas chromatography operation conditions are not given in detail.In this study,gas chromatography is used for analyzing PHB,PHV and PH2MV,three majors of PHAs in activated sludge.The sample was centrifuged at a speed of 4000 r/min for the separation of floc and supernatant,freezen,and dried for 12 h in vacuum freezing drier;and then transferred to the fridge for freezing to ice and drying for 12 h in vacuum freezing drier;then chloroform and a simple composition digestion solution including methanol,sulfuric acid and benzoic acid was added;digested at 105 ℃ for 6 h;cooled to room temperature,the lower solution of the result can be used for analyzing.Samples were analyzed by gas chromatography with FID detector and auto sampler;the standard curve of standard material shows an excellent linear relationship with correlation coefficients larger than 0.99;the relative standard deviation (RSD) of sludge samples is less than 1%.The recovery rates of each sample are between 95%-105%.The GC analysis time of each PHA sample is shorter than 10 minutes.     

杂酚废水对厌氧颗粒污泥微生物影响

为去除生产双酚A工业废水中的苯酚、丙酮、双酚A以及溶解于丙酮中很多难以监测的含酚类成分,通过厌氧颗粒污泥静态培养及驯化,验证其厌氧微生物对此类废水的适应性及处理效果．在颗粒污泥对该杂酚废水的静态适应性实验中,其微生物对该杂酚废水有较好的适应性,6 h的接触时间就可以使原水的COD降低约58％．驯化及连续运行60 d后在水力停留时间为9 h时,可使COD去除率达50％．利用扫描电镜观察反应器内实验前后的颗粒污泥,发现其内部和表面微生物均有很大的差异．     

含油污泥制备高比表面积活性炭

以含油污泥为原料,氢氧化钠为活化剂,在氮气保护下,通过室内静态热解炉制备高比表面积活性炭。研究炭化温度、活化升温方式、活化温度、活化时间和碱碳质量比m(NaOH)／m(C)对高比表面活性炭的影响。采用全自动比表面与孔隙度分析仪、钨灯丝环境扫描电子显微镜等测试设备,分别对产品的比表面积与孔径分布、组成及微观形貌进行定性或定量分析。研究结果表明,含油污泥制备高比表面积活性炭的较佳条件为:炭化温度500℃,活化升温方式(c),活化温度800℃,活化时间1h, m(NaOH)／m(C)=2。采用本方法制备的活性炭比表面积大于2000m2/g,平均孔径小于2nm,总孔容大于2cm3/g,性能优于普通活性炭,可作为能源储存介质、电极材料、高效吸附剂的基础材料,为含油污泥的资源化利用提供了一条新途径。     

快速筛检活性污泥中硫酸盐还原菌的新方法

由于硫酸盐还原菌(SRB)的生物学多样性以及在系统发育学上的分散性,采用传统方法筛选活性污泥中的SRB准确率不高,且耗时、耗力,而直接采用16S rRNA基因(rDNA)序列分析方法既耗资又不适合从大量细菌中检测SRB.本研究开发出一种新方法,采用SRB16S rDNA特异引物SRB385F为正向引物,真细菌通用引物EUB926R为反向引物,通过梯度PCR,选择适当的退火温度来扩增SRB通用培养基分离的细菌,通过扩增条带与阳性和阴性对照比较,判断待检测菌株是否为SRB,整个过程仅需6h即可完成.将测试菌株进行16S rDNA测序表明该技术获得的阳性菌株全部为SRB.     

扫描电镜中纳米材料的原位操纵和动态观察

介绍了配置在扫描电镜(SEM)中的微操纵仪(MMS)的操作原理、性能及应用.MMS在水平转动(X轴),上下转动(Y轴)和线性进退(Z轴)的移动精度分别达到5,3.5,0.25nm.利用具有纳米精度的移动和定位的MMS,对BiVO_4晶体、硅藻土、蛋白石和ZnO纳米线等纳米材料进行了原位操纵和动态观察.该装置可操纵质量为纳克级,尺寸为几百纳米至几微米的样品.SEM-MMS系统为原位分析纳米材料提供了一种崭新的手段.     

预处理低有机质剩余污泥两相厌氧消化

为提高低有机质剩余污泥的厌氧消化效率,采用超声波(40kHz,50W)与生石灰(投量为560mg/L)联合预处理剩余污泥,然后将预处理的剩余污泥进行中温两相厌氧消化.试验污泥取自长春市某污水处理厂,试验中主要考察剩余污泥的消化性能、产气情况及脱水性能变化.结果表明,当剩余污泥的VS/TS比值为0.56、水力停留时间(HRT)为20d时,预处理污泥厌氧消化后VS去除率达到40.8%.在消化过程中系统稳定,产酸相内挥发酸成分以乙酸和丁酸为主,而产甲烷相内以少量乙酸为主.产甲烷相的甲烷产率为0.33L/gVS去除,产气中甲烷平均含量可达到59.2%,但消化后污泥的脱水性能变差.污泥的联合预处理增加了液相中溶解性有机物的含量,提高了进料污泥的pH与碱度,有助于低有机质剩余污泥的后续厌氧消化处理.     

低温SBR系统活性污泥硝化效能的pH调控

为进一步提高低温(15 ℃)SBR系统的硝化效能,通过间歇培养实验探讨pH对系统活性污泥硝化效能的调控与影响．结果表明,将初始pH控制为8.0～9.0,低温SBR系统的活性污泥(以MLSS计)具有最佳的氨氮氧化能力,在NO₂--N积累阶段对NH₄+-N的比去除速率可达25.49 g·kg-1·d-1,NO₂--N的比生成速率达22 g·kg-1·d-1;初始pH为7.5～8.0时,NO₂--N氧化效果最佳,NO₃--N的比生成速率可达35.6 g·kg-1·d-1;将反应系统的pH维持在8.0,可使亚硝酸菌和硝酸菌代谢活性均保持在较高水平,达到良好的硝化效果．     

煤中黄铁矿表面细菌氧化的XRD及SEM/TEM研究

借助于XRD和SEM/TEM 等表面分析测试技术,对煤中黄铁矿表面经氧化亚铁硫杆菌作用前后的表面微观结构的变化进行了研究.作为对比,同时采用了氧化剂（H2O2）对黄铁矿表面进行氧化试验.结果表明,氧化亚铁硫杆菌在黄铁矿表面的氧化形式与氧化剂（H2O2）在黄铁矿表面的氧化形式不同.从黄铁矿表面微观结构的变化来看,氧化剂氧化的结果多出现钮扣状的片起,表现为较为剧烈的直接强氧化作用,而氧化亚铁硫杆菌氧化则呈现坑蚀,表现为相对缓和的吸附氧化作用.这为研究细菌对煤中黄铁矿表面的作用机理提供了一定的参考.     

废轮胎回转窑中试热解炭孔隙及表面化学特性

为了设计和优化废轮胎热解炭利用工艺,利用氮气吸附法、傅里叶变化红外光谱（FTIR）和X射线光电子能谱（XPS）对废轮胎回转窑中试热解炭的孔隙结构及表面化学特性进行研究,分析热解温度和热解炭粒径的影响因素,并与商用炭黑进行比较.结果发现,热解炭中有很多大孔而微孔很少,Brumauer-Emmett-Teller (BET)比表面积随热解温度的升高而增大;热解炭BET比表面积与N660相当,分型维数与N330相当,热解炭粒径越大,BET比表面积越大;热解炭中C和O的含量高,含氧官能团主要为醇、酚、酯、内酯、酸酐和醚,有大量芳香稠环的存在,热解温度越高,芳构化越高;商用炭黑芳构化高于热解炭;热解炭中S元素主要以硫化物存在,N元素多以胺形态存在,而商用炭黑中S元素主要以“S-C/R-S-S-R”的形态存在.     

静电纺丝技术制备EVOH-g-SO3H无纺布膜的研究

采用高压静电纺丝法制备了EVOH-g-SO3H离子聚合物无纺布膜,并采用扫描电子显微镜(SEM)及X射线衍射仪(XRD)对该无纺布膜的微观形貌及结晶行为进行了表征.结果表明:EVOH-g-SO3H离子聚合物无纺布膜中存在无规的纤维和珠状物;当纺丝电压和板间距增大,或者采用快挥发性溶剂时,无纺布膜中纤维和珠状物的平均直径将减小;当纺丝液浓度从12%变化到20%时,无纺布膜的微观形貌由球滴状物变化为珠丝状物,可以明显地观察到从电喷到电纺的变化过程;XRD分析表明通过静电纺丝有新晶形的形成.     

M(o)ssbauer and electron microscopy study of martensitic transformations in an Fe-Mn-Mo alloy

The kinetic,morphological,crystallographic,and magnetic characteristics of thermally induced martensites in Fe-13.4wt%Mn-5.2wt% Mo alloy were investigated by scanning electron microscopy(SEM),transmission electron microscopy(TEM),and M(o)ssbauer spectroscopy.The experimental results reveal that two types of thermal-induced martensites,ε(hcp)and αˊ(bcc)martensites,are formed in the as-quenched condition,and these transformations have athermal characters.Mo addition to the Fe-Mn alloy does not change the coexistence of ε and αˊ martensites with the Mn content between 10wt% and 15wt%.Besides,M(o)ssbauer spectra reveal a paramagnetic character with a singlet for the γ(fcc)austenite and ε martensite phases and a ferromagnetic character with a broad sextet for the αˊ martensite phase.The volume fraction of αˊmartensite forming in the quenched alloy is much more than that of the ε martensite.     

污泥基催化剂强化臭氧深度处理煤制气废水中试性能

为解决煤制气废水生化处理后出水仍含有大量有毒和难降解污染物,对环境产生严重污染的问题,以污水污泥为原料制备污泥基活性炭,采用浸渍法将其负载过渡金属锰和铁的氧化物(主要为Mn_3O_4和Fe_3O_4,负载量分别为15.52%和7.45%),制备比表面积分别为327.5和339.1 m~2/g的臭氧催化剂.中试实验结果表明,催化剂的使用显著提高臭氧氧化废水污染物的效能,处理后出水COD、TOC、总酚和氨氮质量浓度分别为41~43,19~20,0.6~0.9和4.3~4.5 mg/L,均达到城镇污水处理厂污染物排放一级A标准;在最佳的臭氧投加量18 g/h条件下,催化剂的使用将臭氧利用率提高40%,达1.24 mg/mg(以COD计),显著降低工艺运行成本;相比新鲜的催化剂,连续50次的催化臭氧氧化运行,COD去除率仅下降5.2%.催化剂具有良好的稳定性,制备成本仅为5 000元/t.制备的臭氧催化剂具有性能高效稳定、经济节约和可持续发展的技术优势,适用于强化臭氧深度处理煤制气废水.     

X射线透射成像技术原位追踪混凝土吸水过程

为了表征二维混凝土的传输过程,制备厚度为1 mm的混凝土薄片. 采用X射线透射成像（TXR）技术,联合扫描电镜、背散射和能谱分析技术（SEM/BSE/EDS）原位追踪水在2维混凝土薄片中的毛细自吸过程. 测试不同质量分数CsCl溶液对X射线透射图像的增强效果. 结果表明,CsCl能够提高吸水过程中混凝土薄片的TXR图像对比度,使得水在混凝土中的渗流路径更清晰、可辨. 水泥浆体在吸收CsCl后,扫描电子背散射图像的对比度显著增强. 不同位置铯原子的EDS能谱结果验证了TXR技术确定吸水前锋位置的准确性.     

Understanding the influence of petrographic parameters on strength of differently sized shale specimens using XRD and SEM

Ground failure is a major contributor to fatalities in underground mines in the US. Underground coal mines in the Northern Appalachian have weak roof rock composed of shale, which is prone to failure under high horizontal stress. Understanding the relationship among strength, specimen size and rock petrographic parameters is essential for developing an effective ground control plan. Size effect studies have found that rock strength varies with specimen size. This paper attempts to understand this strength variation using three specimen sizes(254-mm, 508-mm, and 762-mm). The specimen strength was measured and the major petrographic parameters affecting the strength, namely grain size, grain shape,quartz content, clay content, etc. were analyzed using X-ray diffraction(XRD) and scanning electron microscopy(SEM). The petrographic parameters were then correlated with the strength of the three differently sized specimens. The results showed that 508-mm specimen had the lowest strength. Quartz content of the 508-mm specimen was lower than that of 254-mm and 762-mm specimens. Clay content and average grain size of the 508-mm specimen were higher than those of 254-mm and 762-mm specimens. These results clearly show that grain size, quartz content and clay content contribute to strength variation observed in differently sized shale specimens.     

实时控制实现短程硝化过程中种群结构的演变

为了考察实时控制下实现短程硝化过程中硝化污泥种群结构的演变,采用荧光原位杂交技术(FISH)和扫描电镜(SEM)对处理生活污水的序批式反应器内污泥进行了跟踪观测.结果表明:通过检测pH曲线上的"氨谷"特征点快速启动了短程硝化,短程硝化维持期间亚硝化积累率平均在93%左右.接种污泥形态多样,含长杆、短杆及球状菌,而随着运行的延续,污泥形态呈现了向短杆状、球状转变的态势.实时控制下反应器内亚硝酸氧化菌(NOB)逐渐被淘洗,而氨氧化菌(AOB)得到了富集.从短程硝化启动初期到短程硝化稳定运行102d,AOB的相对数量从3.5%逐渐上升到8.5%,而对应的NOB相对数量从3.1%下降至0.5%以下.利用好氧曝气时间实时控制实现短程硝化是一种面向种群优化的控制方法,有利于短程硝化系统长期稳定的运行.     

玉米须多糖微波提取工艺及其红外光谱结构分析

采用Plackett-Burman设计方法筛选出了影响微波提取玉米须多糖的显著性因素:微波提取温度、提取功率和液固比。在考察影响多糖得率主效应因素变化趋势的基础上,结合最陡爬坡试验进一步逼近最优提取条件,通过中心组合试验及响应面分析优化微波法提取玉米须多糖的工艺条件,得到回归模型。通过数学统计分析可知,所得模型与实际值拟合较好。最后求极大值得到微波法提取玉米须多糖中心组合设计的最优工艺参数为:温度为85℃,功率为400W,液固比为80∶1,此条件下多糖含量实际值为9.36%。另外,红外光谱分析发现多糖类物质具有明显的多糖物质特征吸收峰。     

真实水压作用下裂隙大理岩蠕变特性试验研究

软弱层间带裂隙岩石的水压弱化效应是水利工程长期稳定研究的重要方向。针对锦屏一级坝肩软弱层间带裂隙大理岩在高水压力作用下的长期变形特性,采用特定的岩石流变试验系统,开展不同水压作用下预制裂隙大理岩的蠕变试验,结合典型蠕变过程曲线分析水压对裂隙岩石蠕变变形、蠕变速率、蠕变破坏荷载及长期强度的影响,并基于蠕变破坏断口的电镜扫描成果,从细观角度分析岩石蠕变破坏机制。结果表明：裂隙岩石宏观破裂现象与断口微观特征相吻合,随着水压的增加,岩石破裂形式逐渐由张拉破裂向剪切破裂过渡,破裂断口由凹凸锯齿状逐渐趋于平滑。压力水沿岩石裂隙的“楔入”可加速原始裂纹的发育,促进岩石的蠕变发展,水压越大,“楔入”效应越明显,加速蠕变速率越大,加速阶段持续时间越短,蠕变破坏的分级荷载越小;相较于稳定蠕变阶段,水压对加速蠕变阶段的影响效应更大。裂隙岩石长期强度约占完整岩石峰值强度的50%~70%,水压的增大会降低岩石的长期力学性能,并加速岩石的蠕变破坏,工程中建议取稳定蠕变阶段最大一级强度作为裂隙岩石的长期强度。研究成果的应用可提高锦屏一级水电站长期稳定运行评估的准确性,并为裂隙岩石蠕变本构模型研究提供重要支撑,具备显著的工程应用与理论研究价值。     

Al靶中稀土Y含量对薄膜CrAlTiN的影响

研究了Al靶中加入不同含量的稀土Y对CrAlTiN薄膜的影响。应用SEM、EDS、XPS、显微硬度计对薄膜样品进行分析。结果表明,在Al靶材中加入稀土Y后,不但提高了薄膜的厚度,而且随着稀土Y含量的增加,薄膜的表面相逐渐由CrN、Cr2N向Cr变化,Al的含量也是随着Y含量的增加而增加。CrAlTiN薄膜的硬度随着稀土Y含量的升高而降低,并且随着Y含量的升高而逐渐趋于1500 HV。     

Thermal aging behavior of high performance poly(vinyl alcohol) hydrogel

The thermal aging behavior of poly(vinyl alcohol) (PVA) hydrogel was studied at four different temperatures of 40 ℃, 50 ℃, 60 ℃ and 70 ℃ in one year. The samples of PVA hydrogel were closely covered by plastic film. The changes of their chemical structures and physical properties during aging were measured through different measurable techniques including tensile testing, gel permeation chromatography (GPC), viscosity analysis, and Fourier transform infrared (FTIR) spectrum. The results showed that the molecular weight of PVA in hydrogel changed little with time and temperature. FTIR spectra of PVA in all the samples were similar to those of the original samples. The tensile strength of PVA hydrogel didn’t change until the 330th days.     

Mierostructral Evolution of Well-aligned ZnO Nanorods Array Films in Aqueous Solution

By means of scanning electron microscopope and X-ray diffraction,microstructural evolution of well-aligned ZnO nanorod array films was studied.The films were prepared on a glass using direct deposition method in an aqueous solution.The experimental results show that the highly oriented rods grew from the randomly oriented crystals.Those rod-like randomly oriented crystals began to impinge on other neighboring crystals and their growth became physically limited;only the rods perpendicular to the substrate were allowed to grow freely.This kinetically controlled nucleation and growth would be responsible for producing the uniformly oriented nanorods.During the ZnO rods' growth,the topology of their top faces changed from flat,prismatic to finally flat.