SI-traceable certification of Cu, Cr, Cd and Pb in sediment and fly ash candidate reference materials

Many fields in environmental analytical chemistry deal with very low limits and thresholds as set by governmental legislations or transnational regulations. The need for the accuracy, comparability and traceability of analytical measurements in environmental analytical chemistry has significantly increased and total uncertainties are even asked for by accreditation bodies of environmental laboratories. This paper addresses achieving these goals to guarantee accuracy, quality control, quality assurance or validation of a method by means of certified reference materials. The assessment of analytical results in certified reference materials must be as accurate as possible and every single step has to be fully evaluated. This paper presents the SI-traceable certification of Cu, Cr, Cd and Pb contents in geological and environmentally relevant matrices (three sediments and one fly ash sample). Certification was achieved using isotope dilution (ID) ICPMS as a primary method of measurement. In order to reduce significantly the number of analytical steps and intermediate samples a multiple spiking approach was developed. The full methodology is documented and total uncertainty budgets are calculated for all certified values. A non-element specific sample digestion process was optimised. All wet chemical digestion methods examined resulted in a more or less pronounced amount of precipitate. It is demonstrated that these precipitates originate mainly from secondary formation of fluorides (essentially CaF2) and that their formation takes place after isotopic equilibration. The contribution to the total uncertainty of the final values resulting from the formation of such precipitates was in general < 0.1% for all investigated elements. Other sources of uncertainty scrutinised included the moisture content determination, procedural blank determination, cross-contamination from the different spike materials, correction for spectral interferences, instrumental background and deadtime effects, as well as the use of either certified values or IUPAC data in the IDMS equation. The average elemental content in the sediment samples was 30-130 micrograms g-1 for Pb, 0.5-3 micrograms g-1 for Cd and 50-70 micrograms g-1 for Cu. Cr was measured in one sample and was about 60 micrograms g-1. The concentrations in the fly ash sample were up to 2 orders of magnitude higher. Expanded uncertainty for the investigated elements was about 3% (coverae factor k = 2) except for Cr, (measured by high resolution ICPMS), for which the expanded uncertainty was about 7% (k = 2).     

浅谈外墙保温材料对建筑防火的影响

本文通过对几种外墙保温材料及国内外外墙保温技术的介绍,从中分析出引起建筑耐火极限降低的原因,找到在目前条件下,最适合外墙保温的材料及技术,以降低火灾的发生。     

典型南方水源溶解性有机物荧光特性变化与去除

于2014年4-9月,研究我国一典型南方水源溶解性有机物(DOM)的荧光特性变化与去除情况,同时分析了DOM荧光组分与三氯乙醛生成势(CHFP)的相关性。结果表明,该水源DOM主要以芳香性蛋白质类物质组成,溶解性微生物代谢产物类物质、富里酸类物质和腐殖酸类物质含量逐渐增加;5个荧光区域的积分体积(ΦⅠ,n、ΦⅡ,n、ΦⅢ,n、ΦⅣ,n和ΦⅤ,n)所占总体积(ΦT,n)平均比例依次为:13.55%、27.53%、25.00%、16.02%和17.91%;原水DOM的CHFP范围为27.06~81.20μg/L,平均值为46.60μg/L,三氯乙醛(CH)前体物含量与水体中溶解性微生物代谢产物类物质相关性最好;与常规处理工艺相比,O3/BAC深度处理工艺对于溶解性微生物代谢产物类物质的去除率大幅提高,更有利于CH的控制。     

Optimum conditions for Al13 polymer formation in PACl preparation by electrolysis process

This paper introduces a new and effective method for preparation of PACl-electrolysis process. A series of PACl with high content of Al13 polymer was successfully prepared by electrolysis process. The amount of Al13 polymer formed in electrolysis process was found to be highly influenced by current density (di), the distance between the electrodes, electrolysis time and the stirring rate of the electrolyte. For the AlT (total aluminum concentration) of 2.0 M PACl obtained by electrolysis process, the optimal di and distance between the electrodes were 1.1 Adm(-2) and 10 mm respectively. The optimum circulating rate was 5.5 l h(-1). Because of the inhomogeneous pH between the surface of cathode and the bulk solution, the electrolysis process has the advantage to form more Al(OH)4- as precursor of Al13 polymer. At the optimum condition, Al13 polymer accounted for above 70% of AlT (PACl of AlT=2.0 M and B=2.0), which was much higher than that of PACl prepared by other method.     

环评中锅炉房大气污染源强的确定

在环境评价中,污染源强的确定对环境影响因素评价的分析结果有重要作用。对锅炉房污染物排放的分析表明,影响锅炉房大气污染物的主要因素有燃料的构成、发热量和燃烧方式等。确定锅炉房大气污染物的方法主要有物料衡算法、实测法和经验系数法。在这三种方法中,物料衡算法被普遍采用。在确定锅炉房大气污染物的排放量时,也可以采用物料衡算法和实测法相结合的方法。     

含油污泥固化处理后油的迁移研究

利用紫外分光光度计和索氏抽提器,研究了温度、土壤含水率以及水泥与污泥的不同比例等因素在不同时间对含油污泥固化后油迁移的影响。试验结果表明:对于强度为3.84MPa的污泥固化块,油的迁移量从240h迁移6.8mg变为480h迁移178mg,之后变化较小。在20℃～30℃时,随着温度的增加,迁移量从6.8mg增加到20.6mg,超过30℃以后迁移量的增幅变小。水泥与污泥的比例从1∶0.8增加到1∶1.4,油的迁移量从256mg降到27.2mg,之后未检测到。960h后,迁移量达到348mg,此时土壤中油含量为1.16%,在环境的自净作用下,土壤能完全容纳;强度大于9.56MPa时未检测到油。这表明用固化法处理油田含油污泥是安全可靠的。     

青霉素废菌丝体制备石膏缓凝剂联产活性炭

青霉素废菌丝体是一种制药行业的危险固体废弃物。利用其富含蛋白质的特点,采用微波加热水解法制备一种新型建筑石膏缓凝剂（WPM缓凝剂）,同时将制备缓凝剂后的滤渣用于制备活性炭。经过实验研究,确定的缓凝剂制备适宜工艺条件为：温度80 ℃,pH值11,时间10 min。得到滤渣制备活性炭的最佳工艺条件为：炭化时间为1 h,炭化温度为300 ℃,活化剂ZnCl2浓度为20%,液固比为3.0。 本工艺较好地解决了焚烧处置、堆放填埋或直接生产活性炭等处理方法造成的环境二次污染问题以及用作动物饲料可能导致的抗生素滥用问题,实现了青霉素废菌丝体的安全、清洁利用。     

铁盐与铝盐对腈纶废水生化出水混凝特性的对比

针对腈纶废水生化单元出水,对比研究了Al2(SO4)3和Fe2(SO4)3在不同絮凝剂投量和pH时的混凝处理效果,并利用紫外-可见分光光度法(UV-Vis)、三维荧光光谱(EEM)、凝胶渗透色谱(HPSEC)等对混凝特性进行了初步探讨。研究显示,2种混凝剂在投量为63.5 mg/L时可获得30%以上的COD去除率,且最佳pH为中性附近。当投量小于32 mg/L时,Al2(SO4)3较Fe2(SO4)3具有更高的COD去除率,进一步增大混凝剂的投量很难提高Al2(SO4)3对COD的去除率,而Fe2(SO4)3则在有限范围内能持续提高COD去除率。EEM光谱分析显示,与Al2(SO4)3相比,Fe2(SO4)3对有机物具有更广的处理范围和更好的去除效果。HPSEC分析表明,Fe2(SO4)3相对于Al2(SO4)3在去除重均分子量为2 776、1 856和1 325 Da的有机物组分方面具有优势。铁盐或铝盐混凝是深度净化腈纶废水生化单元出水的可行方案之一。     

天然浑浊水中共存无机阳离子的电动化学特征

引入流动电流这一重要电动化学参量，研究了在天然浑浊水中ＳＣ的基本模式，撮了ＳＣ与水中悬浮胶体颗凿表面电荷量及无机阳离子之间的理论关系，探讨了离子的浓度，性质，存在环境等对体系电动特性的影响，并对水中常见８种阳离子共存条件下的电动化学特性进行了实验分析，从而建立了无机阳离子对胶体的聚沉能力与电动响应特性之间的实际联系。