ICP-AES法同时测定水中多种元素

建立了电感耦合等离子体发射光谱(ICP-AES)法同时测定水和废水中的铜、铅、铁等方法，对ICP工作参数选择、酸度对测定的影响、元素分析线选择以及背景和扣除方式等进行了研究。     

茶叶中多种元素测定与茶叶污染剖析

本文用等离子发射光谱法(ICP-AES)测定了若干种茶叶中Ca、Mg、Al、Fe、Mn、Cu、Zn、Pb、Cd、Ni、B、V等12种元素的含量,并就其在茶汤中的浸出状况进行了分析;从环境污染的角度探讨了茶叶中有害元素的来源及对人体健康的影响。     

镁渣固化/稳定污酸渣中重金属Pb

研究利用镁渣固化/稳定污酸渣中重金属Pb。将质量为0%、10%、20%、60%和80%镁渣与污酸渣混合,并添加不同浓度的含铅化合物,采用HJ/T299-2007硫酸硝酸法做毒性浸出实验,用ICP-AES检测原渣及浸取液中Pb含量,用SEM及EDX观察样品的微观形貌,用XRD研究样品的物相变化。研究表明:镁渣对污酸渣中Pb有良好的固化/稳定效果,且随着镁渣掺杂量的增加固化/稳定化效果越好;掺杂60%镁渣的污酸渣中Pb主要以PbSO_4、PbO和CdO·PbO_2形式存在;掺杂60%镁渣的污酸渣经过1150℃,6h高温处理,产生了CaO·Al_2O_3·SiO_2的胶凝体系及C_3A相,优化了固化/稳定重金属Pb的效果。     

固体废物中挥发性有机物现场快速测定方法及有效性研究

采用便携式顶空/气相色谱—质谱(GC—MS)法与吹扫捕集/GC—MS法对实验室加标固体样品和实际固体废物(以下简称固废)中的挥发性有机物(VOCs)含量进行比对测定,探讨了便携式顶空/GC—MS法现场快速测定固废中VOCs的标准曲线时间有效性。结果表明:采用便携式顶空/GC—MS法测定固体样品中54种VOCs的准确度(以加标回收率计)和精密度分别为70%~123%、4.8%~17.6%,均能满足应急监测分析的要求,其检出限略高于吹扫捕集/GC—MS;其标准曲线在3d内有效性很好,7d后有效性明显下降,14d后需重新做标准曲线进行定量分析。便携式顶空/GC—MS测定固废中的VOCs基体加标回收率为69%~145%,测定结果与吹扫捕集/GC—MS相比,相对偏差小于10%,现场出具的监测数据有效,可为后续固废属性的鉴别和固废的处置提供依据。     

Fe负载量对xFe/ZSM-5催化剂氨选择性催化还原NO的影响

采用旋转蒸发法,将过渡金属Fe负载到ZSM-5分子筛上,控制Fe负载量的变化,制备一系列xFe/ZSM-5(x为Fe负载量,x=0.1%(质量分数,下同)、0.7%、1.4%、2.1%,省略%)分子筛催化剂。对所制备xFe/ZSM-5的氨选择性催化还原(NH_3-SCR)NO活性进行评价,并通过不同表征技术对催化剂的结构和理化性质进行了测定。结果表明,Fe负载量对xFe/ZSM-5的NH_3-SCR活性影响较大。其中1.4Fe/ZSM-5取得最宽的活性温度窗口,在250～530℃的NH_3-SCR活性达到80%以上(以NO转化率计)。孤立Fe~(3+)物种为xFe/ZSM-5催化剂低温段的主要活性物种,而低聚态Fe_2O_3物种会促进高温段NH_3的非选择性氧化,造成高温段NH_3-SCR活性下降;负载Fe物种后催化剂的强酸位数量减少,中酸位数量增加,中酸位有利于提高催化剂NH_3-SCR性能。     

危险废物焚烧灰渣熔融过程中重金属元素热力学平衡计算

熔融固化是目前危废焚烧灰渣处置的有效方法之一。为了能够有效地控制熔融过程中重金属元素的迁移,采用HSC Chemistry软件模拟研究了重金属元素As、Pb、Zn、Cu、Ni、Cr等在熔融过程中的物质变化历程,考察了不同气氛、温度、氯化物种类的影响。结果表明:在还原性气氛下,As、Pb几乎100%以As S(g)和Pb S(g)的形式挥发进入气相;Zn主要以气态金属挥发,1 500℃时90.8%的Zn进入气相;Cu、Ni、Cr与灰渣中的Fe2O3、Al2O3等形成不易挥发的化合物,几乎完全被熔渣固化。氧化性气氛有利于各重金属元素的固化,除46.47%的Pb以Pb Cl2(g)、Pb Cl(g)、Pb O(g)的形式挥发外,其余重金属元素均能被固溶在渣中。与灰渣中Na Cl相比,Ca Cl2不影响As、Cr的平衡形态分布,但能促进Pb、Zn、Cu、Ni以气态氯化物的形式挥发进入气相,不利于重金属元素的固化。     

生物沥浸含锰烟粉尘中的锰及其浸出机理研究

含锰烟粉尘是钢铁行业产生的一类含有锰、锌、铅和硅等元素的工业固废，既存在一定的环境风险，又具有潜在的资源回收价值。对含锰烟粉尘分别用生物酸和无机酸进行沥浸，分析锰的浸出机理，进一步通过响应面法确定生物酸沥浸锰的最佳工艺条件。结果表明，锰的浸出机理为酸溶和生物酸还原的复合机理，生物酸中的还原性物质和沥浸过程中产生的Fe²⁺能够将高价锰还原为Mn²⁺,使生物酸体系锰的浸出率比无机酸体系高。生物酸浸出锰的最佳工艺条件：固液比为1.22 g∶100 mL,初始pH为0.81,温度为29.14℃,转速为152.29 r/min,此条件下实际锰浸出率为76.51%。     

元素硫颗粒粒径对污泥重金属生物沥滤的影响

以城市污水处理厂剩余污泥作为处理介质,土著嗜酸氧化硫硫杆菌(Acidithiobacillus thiooxidans,A.thiooxi-dans)为主要沥滤微生物,采用序批式生物沥滤装置,就投加150~725μm的不同粒径元素硫对沥滤的酸化效果、硫酸根产率和重金属去除效果的影响进行了研究。结果表明,在元素硫投配量为3 g/L,曝气强度为1.0 L/(min.L)的条件下,元素硫粒径在165~215μm范围减小时能显著改善污泥酸化速度、提高酸化程度和硫酸根产率。底物元素硫的最佳粒径为165μm,此时沥滤体系pH下降速率为0.85个pH单位/d,硫酸根的产率为454.9 mg/(L.d),沥滤6 d后污泥中高浓度重金属Cu、Zn、Cd的去除率达到70.3%、81.2%、87.8%.     

微生物酶促高效提制废次烟草中烟碱的研究

采用酶促反应利用微生物发酵处理废次烟叶提取烟碱,对比发酵及微波协助等不同方式,利用分光光度法测定发酵体系中烟碱溶出含量,优选出发酵菌种,并探讨接种量和培养基质及不同工艺参数等对烟碱含量的影响。实验结果表明:选用白腐真菌和管囊酵母(1∶1)在微波协助处理下,当烟叶与水的重量比为3∶20,豆粕与烟叶重量百分比为15%,接种量40%,pH=6,30℃发酵48 h,能得到烟草中烟碱溶出浓度为3.291 g/L,为有效实现废次烟草减量化排放与资源化利用结合奠定基础。     

废晶硅太阳能电池资源化分类回收技术研究

晶硅太阳能电池报废后将会产生大量固体废弃物。采用不同浓度盐酸、硝酸和硝酸-氢氟酸混酸分步回收废晶硅太阳能电池中的铝、银和硅,得到了室温下废晶硅太阳能电池资源化回收技术的最佳参数:经20%(体积分数,下同)盐酸反应40min,铝浸出率为99.77%;经35%硝酸反应30 min,银浸出率为99.60%;经40%硝酸-6%氢氟酸混酸反应75 min,硅回收率为85.51%。     

Improvement of receptor model use in analytical aspect

In this study, four certified particle standards including NIST SRM 1648 urban particulate matter, BCR Reference Material No. 176 city waste incineration ash, NIST SRM 2709 San Joaquin soil, and NIST SRM 1633b coal fly ash were used to simulate ambient particulate matter. Twenty-five samples were prepared with the four certified particulate standards. A total of 23 elements were analyzed per sample, 19 by ICP-AES and ICP-MS, three by IC, and one element, Si, by spectrophotometer. Results showed that combining the three IC-analyzed ionic species with the 19 ICP-AES/MS analyzed elements into the CMB model did not improve the source identification significantly. In addition, when all 23 analyzed chemical species per sample were used in the CMB model, they were still not good enough to effectively make the parameters of the CMB model fit the statistical criteria. Some of high variation and low recovery chemical species, i.e. Cd, V, Sb, etc., may have caused poor CMB model simulation. Omitting some poor quality analyzed species (such as relative analysis error >20%) could improve the CMB model simulation. Therefore, high quality chemical species data are important for the CMB model. In addition, co-linearity of source profiles also affects the CMB model; combining the co-linear sources could enhance the solubility of the CMB model. In this study, a two-step procedure was developed for CMB model simulation to improve source identification.     

Environmental impact of a coal combustion-desulphurisation plant: abatement capacity of desulphurisation process and environmental characterisation of combustion by-products

The fate of trace elements in a combustion power plant equipped with a wet limestone flue gas desulphurisation (FGD) installation was studied in order to evaluate its emission abatement capacity. With this aim representative samples of feed coal, boiler slag, fly ash, limestone, FGD gypsum and FGD process water and wastewater were analysed for major and trace elements using the following techniques: inductively coupled plasma-mass spectrometry (ICP-MS), inductively coupled plasma-atomic emission spectrometry (ICP-AES), ion chromatography (IC), ion selective electrode (ISE) and atomic absorption spectroscopy (AAS). Mass balances were established allowing to determine the element partitioning behaviour. It was found that, together with S, Hg, Cl, F, Se and As were those elements entering in the FGD plant primarily as gaseous species. The abatement capacity of the FGD plant for such elements offered values ranged from 96% to 100% for As, Cl, F, S and Se, and about 60% for Hg. The environmental characterisation of combustion by-products (boiler slag, fly ash and FGD gypsum) were also established according to the Council Decision 2003/33/EC on waste disposal. To this end, water leaching tests (EN-12457-4) were performed, analysing the elements with environmental concern by means of the aforementioned techniques. According to the leaching behaviour of combustion by-products studied, these could be disposed of in landfills for non-hazardous wastes.     

Sources and fates of lead and cadmium in municipal solid waste

Lead and cadmium enter the municipal solid waste stream as components of a variety of consumer products. Average empirical data from several resource recovery plants were analyzed to obtain an estimate of the source and fate of the subject elements. The total amounts of lead and cadmium found in municipal solid waste, determined from empirical data sources, were found to agree closely with those based on materials flow data. It was determined that most of the cadmium enters the waste stream in the combustible fraction and can account for a major share of the cadmium observed in fly ash and in atmospheric particulates. The most likely sources of cadmium are plastics and pigments. The lead emissions appeared to be derived from both combustible and noncombustible discards of batteries, plastics, and pigments. The data suggests that it would be useful to perform mass balance studies to provide primary data for the determination of the most effective methods for managing discards containing lead and cadmium. The purpose of the suggested research is the reduction of lead and cadmium emissions into the environment from resource recovery plants.     

Effects of sludge recirculation rate and mixing time on performance of a prototype single-stage anaerobic digester for conversion of food wastes to biogas and energy recovery

Food wastes have been recognized as the largest waste stream and accounts for 39.25 % of total municipal solid waste in Thailand. Chulalongkorn University has participated in the program of in situ energy recovery from food wastes under the Ministry of Energy (MOE), Thailand. This research aims to develop a prototype single-stage anaerobic digestion system for biogas production and energy recovery from food wastes inside Chulalongkorn University. Here, the effects of sludge recirculation rate and mixing time were investigated as the main key parameters for the system design and operation. From the results obtained in this study, it was found that the sludge recirculation rate of 100 % and the mixing time of 60 min per day were the most suitable design parameters to achieve high efficiencies in terms of chemical oxygen demand (COD), total solids (TS), and total volatile solid (TVS) removal and also biogas production by this prototype anaerobic digester. The obtained biogas production was found to be 0.71 m³/kg COD and the composition of methane was 61.6 %. Moreover, the efficiencies of COD removal were as high as 82.9 % and TVS removal could reach 83.9 % at the optimal condition. Therefore, the developed prototype single-stage anaerobic digester can be highly promising for university canteen application to recover energy from food wastes via biogas production.     

潞城市大气PM_（10）中化学元素分布特征

利用ICP-AES分析了潞城市采暖期和非采暖期4个不同功能区PM10样品中16种化学元素,对不同元素的时空分布特征进行了研究,并采用富集因子和主成分分析初步研究了潞城市PM10中元素的主要来源。结果表明,潞城市PM10中重金属污染较为严重,且各元素在采暖期的平均浓度均明显高于非采暖期。PM10中Ca、V、Cr、As、Ni、Mn、Cu、Zn、Al和Pb的富集因子EF〉10,主要来源于人为污染;而Na、Mg、Si、Fe和K的EF〈10,除部分来自人为活动外,主要来自土壤风沙等自然来源。主成分分析结果显示,潞城市PM10中元素的主要来源按贡献率大小依次为：煤烟尘和工业粉尘50.39%,自然源34.37%和机动车尾气15.24%。     

Characterization of soluble and insoluble components in PM2.5 and PM10 fractions of airborne particulate matter in Kofu city,Japan

A systematic method combining water and diluted-acid extractions has been developed for the manifold evaluation of soluble and insoluble fractions in ambient aerosol. The pre-washed regenerated cellulose membrane filter was used as a collection medium of a low-volume air sampler. The collection time of 7–14 days was required to obtain the sample amounts enough for the systematic analysis. Simple and efficient extraction procedures using the filtration of water and 0.1 M hydrochloric acid were recommended in order to obtain the information about the dissolution behaviors of various elements in the aerosol. Soluble components in both the extracts were determined by inductively coupled plasma atomic emission spectrometry (ICP-AES) and ion chromatography (IC). These extraction procedures were also preferred to prepare thin-layer specimens suitable to the succeeding X-ray fluorescence spectrometry (XRF) for insoluble components. Elemental compositions of the extraction residues were conveniently determined by the XRF calibrated with thin-layer standard specimens prepared with activated carbon. The determination of the 17 representative elements (Na, Mg, Al, Si, S, Cl, K, Ca, Ti, V, Cr, Mn, Fe, Cu, Zn, Br, Pb) in these three fractions from an aerosol sample was performed rapidly within 4 h. The proposed systematic method was applied to PM_2.5 and PM₁₀ aerosol samples collected in Kofu City, Central Japan, and the enrichment behaviors of various elements and their source apportionment such as soil, anthropogenic substances and vehicle exhaust particulates could be demonstrated by the present method.     

Preliminaries on pollution risk factors related to mining and ore processing in the Cu-rich pollymetallic belt of Eastern Carpathians, Romania

The present study focuses on the mineralogical and geochemical patterns of mining and ore-processing wastes from some occurrences in the Eastern Carpathians; its aim is to identify the main factors and processes that could lead to the pollution of the environment. In this respect, the following types of solid waste were investigated: efflorescent salts developed on the surface of rock blocks from a quarry, ore-processing waste from two tailings ponds, and salt crusts developed at the surface of a tailings pond. The potential risks emphasized by these preliminary investigations are the following: (1) the risk of wind-driven removal and transport of the waste from the surface of tailings ponds, given that fine grains prevail (up to 80 %); (2) the risk of tailings removal through mechanical transport by water, during heavy rainfall; (3) the appearance of hydrated sulfates on the rock fragments from the mining waste, sulfates which are highly susceptible to the generation of acid mine drainage (pH?<?4); (4) the high amount of toxic elements (Pb, Cd, Cu, Zn, As, etc.) that acid mine drainage leachates contain; and (5) the development of a salt crust on the flat, horizontal surfaces of the waste deposit, due to this very shape. Statistical data regarding the amount of both major and minor elements in the tailings have revealed two statistical populations for nearly all the toxic metals. This suggests that, beyond the effect that the tailings have upon the environment through their mere presence in a given area, there are alleged additional factors and processes which intensify the pollution: the location of the waste deposit relative to the topography of the area; the shape of the waste deposit; the development of low areas on the surface of the deposit, areas which favor the appearance of salt crusts; and the mineralogy of efflorescent aggregates.     

Biogeometallurgical pre-mining characterization of ore deposits: an approach to increase sustainability in the mining process

Based on the knowledge obtained from acid mine drainage formation in mine waste environments (tailings impoundments and waste rock dumps), a new methodology is applied to characterize new ore deposits before exploitation starts. This gives the opportunity to design optimized processes for metal recovery of the different mineral assemblages in an ore deposit and at the same time to minimize the environmental impact and costs downstream for mine waste management. Additionally, the whole economic potential is evaluated including strategic elements. The methodology integrates high-resolution geochemistry by sequential extractions and quantitative mineralogy in combination with kinetic bioleach tests. The produced data set allows to define biogeometallurgical units in the ore deposit and to predict the behavior of each element, economically or environmentally relevant, along the mining process.     

Recovery of high purity sulfuric acid from the waste acid in toluene nitration process by rectification

Waste sulfuric acid is a byproduct generated from numerous industrial chemical processes. It is essential to remove the impurities and recover the sulfuric acid from the waste acid. In this study the rectification method was introduced to recover high purity sulfuric acid from the waste acid generated in toluene nitration process by using rectification column. The waste acid quality before and after rectification were evaluated using UV–Vis spectroscopy, GC/MS, HPLC and other physical and chemical analysis. It was shown that five nitro aromatic compounds in the waste acid were substantially removed and high purity sulfuric acid was also recovered in the rectification process at the same time. The COD was removed by 94% and the chrominance was reduced from 1000° to 1°. The recovered sulfuric acid with the concentration reaching 98.2 wt% had a comparable quality with commercial sulfuric acid and could be recycled back into the toluene nitration process, which could avoid waste of resources and reduce the environmental impact and pollution.     

利用白云石回收污泥厌氧消化液中的磷

为经济有效地从污泥厌氧消化液中回收磷,构建了以白云石提供钙镁源的磷回收方法,探讨了磷回收的工艺条件与效果。通过盐酸酸化厌氧消化液以降低其碳酸盐含量,同时利用白云石溶于冷稀盐酸的特性使其钙镁缓慢释放到酸化的厌氧消化液中形成第一步磷回收体系,考察体系酸化pH、白云石与厌氧消化液的固液比以及反应pH对白云石的钙镁释放和磷回收效果的影响;第一步磷回收后的上清液为第二步厌氧消化液磷回收提供钙镁源,研究投加钙磷摩尔比对磷回收效果的影响。实验结果表明,当固液比为5.0时,在酸化pH为4.0～4.5且酸化溶出时间为10 h以及反应pH为9.0的条件下,第一步磷回收产物以磷酸钙盐沉淀为主,厌氧消化液磷回收率及回收产物含磷率（以P2O5计）分别达到99.43%和38.49%;第一步磷回收后的上清液按一定的钙磷摩尔比投加到酸化后的厌氧消化液中进行第二步磷回收,当投加钙磷摩尔比为0.20时,在反应pH为9.0的条件下,回收产物同时含有磷酸钙盐和磷酸铵镁,厌氧消化液中氮、磷回收率分别达到13.19%和90.90%,回收产物氮、磷含量（以P2O5计）分别为0.26%和39.58%;经XRD、XRF、ICP及SEM等分析表征,2步磷回收的产物以磷酸钙盐和磷酸铵镁为主要成分,杂质少。研究表明,利用白云石为钙镁源,通过分别构建不同的磷回收体系可以分步从污泥厌氧消化液中经济有效地回收磷,且磷回收率和回收产物含磷率高。