加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱测定土壤和沉积物中8种多溴联苯醚

建立了土壤和沉积物中8种多溴联苯醚(PBDEs,BDE-28、BDE-47、BDE-99、BDE-100、BDE-153、BDE-154、BDE-183和BDE-209)加速溶剂同时萃取和净化-气相色谱-三重四极杆串联质谱(ASE-GC-MS-MS)的分析方法。通过优化加速溶剂萃取与弗罗里硅土在线净化和串联质谱多反应监测模式的条件,较好地去除基质干扰,并提高了三重四极杆串联质谱定性的准确性及定量的灵敏性。该方法采用改进的色谱柱能同时分析包括高溴代联苯醚BDE-209在内的8种PBDEs,其浓度范围为1～100 ng/mL(BDE-209为10～1 000 ng/mL),线性良好,线性回归系数均大于0.997。方法检出限为0.004～0.1 ng/g,方法回收率为75%～110%,方法精密度为2.4%～15.6%。适于批量处理土壤和沉积物中含有多组分痕量PBDEs的样品。     

环境空气质量自动监测站的管理与维护

随着工业化、城镇化的深入推进,二氧化硫、氮氧化物、烟粉尘和挥发性有机物等各类污染物排放到环境中,致使中国大气受到严重污染,给人体的健康、动植物的生长、发育和繁殖等带来负面的影响。为实时监测环境空气质量,建立环境空气质量自动监测站逐渐成为大气污染防治的主要手段。文中以环境空气质量自动监测站为研究对象,提出环境空气质量自动监测站管理与维护面临的问题,探讨相应的解决措施,以期为环境空气质量自动监测站的管理与维护提供参考依据。     

瓦斯抽采PC-CAS基封孔材料优化及其膨胀作用分析*

为了研制以硅酸盐/铝酸盐水泥、生石灰、生石膏为主的PC-CAS基封孔材料，采用正交试验优化材料配比、开展膨胀力研究，并用扫描电镜观测料-煤胶结形貌。研究结果表明:材料的最优配比为A2B2C4，其具备优良的流动性、强度及致密性，造浆量达2 100 mL/kg；PC-CAS基材料具有显著的膨胀性，其膨胀力随时间先增大而后趋于稳定，并且该膨胀力随着径向约束的提高而增大；相比于FP材料，PC-CAS基材料产生的膨胀力能够显著降低材料-煤岩界面的空隙并在一定程度上压密煤体内部的裂隙；该材料产生的膨胀力可压密封孔段围岩、提高封孔质量，并为后期“二次注浆”提供保压条件。工业试验结果表明，采用PC-CAS基材料进行封孔可显著改善抽采效果，将原有平均浓度10.11%提升至20.08%。     

气相色谱法测定土壤中37种有机磷农药残留

采用气相色谱法测定土壤中37种有机磷农药,当取样量为10 g时,37种有机磷农药方法检出限为0. 002～0. 015 mg/kg,测定下限为0. 008～0. 060 mg/kg。低含量加标样品中有机磷农药的加标回收率为72. 8%～104%,相对标准偏差为4. 2%～13. 8%;中含量加标样品中有机磷农药的加标回收率为71. 5%～101%,相对标准偏差为4. 3%～13. 5%;高含量加标样品中有机磷农药的加标回收率为74. 6%～109%,相对标准偏差为6. 8%～14. 6%。该方法灵敏度高、分离效果好、重现性好,能够满足土壤中37种有机磷农药残留检测的要求。     

氨气敏电极法和纳氏试剂分光光度法对地表水中氨氮的比对测试

采用不同质量浓度的氨氮标准样品和实际样品,用氨气敏电极法和纳氏试剂分光光度法进行同步测试。结果表明,2种分析方法在水样氨氮质量浓度在0. 159～2. 81 mg/L范围内具有良好的可比性、精密性和准确性。氨气敏电极法的检出限为0. 03 mg/L,平行6次测定样品的相对标准偏差为0. 4%～4. 2%,加标回收率为85. 0%～110%;纳氏试剂分光光度法的检出限为0. 025 mg/L,平行6次测定样品的相对标准偏差为0. 5%～6. 4%,加标回收率为93. 0%～99. 8%。同时氨气敏电极法在样品预处理、试剂配制和分析时间上要优于纳氏试剂分光光度法。氨气敏电极法能够满足地表水自动监测在线比对实际工作的需求,该方法具有良好的适用性。     

2-萘酚生产废水综合治理与资源化利用工程实例

针对2-萘酚生产废水p H值低、色泽深,亚硫酸盐和萘磺酸盐高、COD浓度高的特点,采用酸化脱硫-两级络合萃取-氧化絮凝工艺处理,介绍了专利工艺的流程设计,给出了主要工艺设计参数及投资运行成本。工程运行结果表明,该工艺设计合理、技术成熟、处理效果稳定,2-萘酚生产废水经处理后达到GB 8978—1996《污水综合排放标准》一级排放标准要求;回收的萘磺酸钠固体可返回2-萘酚生产系统套用;反萃取黑液经蒸发浓缩,合成的减水剂产品各项指标达到或超过GB 8076—2008《混凝土外加剂》高效减水剂指标要求。     

柠檬酸对砷污染土壤的萃取优化条件实验研究

论文以新邱矿矸石山排土场土壤为研究对象,以去离子水做空白试验,选取尿素、十二烷基磺酸钠、碳酸氢钠、醋酸、柠檬酸等12种化学试剂做了萃取剂初选试验;并以柠檬酸为萃取剂进行了三因素三水平L9(33)正交实验。实验结果表明:柠檬酸和氢氧化钠可作为砷污染土壤的萃取剂,具有良好的萃取效果。柠檬酸作为砷污染土壤萃取剂的最优化条件是液土比为10mL/g,萃取时间为12h,萃取剂浓度为0.1mol/L。实验结果可为砷污染土壤的治理提供参考。     

固相萃取-高效液相色谱法测定水中丙烯酰胺研究

采用固相萃取-高效液相色谱法对水中的丙烯酰胺定性、定量分析。结果显示:丙烯酰胺含量在20μg/L~400μg/L之间呈良好线性关系,回归方程Y=0.476 8X+0.845 4,相关系数R为0.997 72,检出限0.1μg/L,样品回收率在71.85%~92.28%之间,相对标准偏差为3.4%~10.9%。该方法减少了有机溶剂用量,缩短了有机溶剂暴露时间,降低污染,且能满足地表水环境质量标准(GB 3838-2002)限值要求,是水中丙烯酰胺含量准确稳定的检测方法。用该方法测定了呼和浩特市引黄入呼左岸、右岸、中浅和中深4个断面水样,均未检出丙烯酰胺。     

Antimony smelting process generating solid wastes and dust：Characterization and leaching behaviors

A large amount of solid waste has been produced by the antimony smelting process in the＂World Capital of Antimony＂, Xikuangshan area in China. This study comprehensively investigated the physical and chemical characteristics of the various solid wastes, as well as the leaching behavior of the solid wastes, which included water-quenched slag,arsenic-alkali residue, desulfurized slag and blast furnace dust. These four types of waste were enriched in a variety of heavy metals and metalloids and more specifically with As and Sb levels up to 8.6 × 104 and 3.16 × 105mg/kg, respectively, in arsenic-alkali residue. For desulfurized slag and water-quenched slag, the leaching concentration of Sb significantly exceeded the acceptable limits during the leaching tests using the toxicity characteristic leaching procedure and the synthetic precipitation leaching procedure. In addition, As leaching in arsenic-alkali residue was extraordinarily hazardous, being three orders of magnitude higher than the regulatory level of As. According to the results of the extraction tests, all the tested wastes were classified as hazardous waste.     

Evaluation of soil washing process with carboxymethyl-β-cyclodextrin and carboxymethyl chitosan for recovery of PAHs/heavy metals/fluorine from metallurgic plant site

Polycyclic aromatic hydrocarbons(PAHs)/heavy metals/fluorine(F) mixed-contaminated sites caused by abandoned metallurgic plants are receiving wide attention. To address the associated environmental problems,this study was initiated to investigate the feasibility of using carboxymethyl-β-cyclodextrin(CMCD) and carboxymethyl chitosan(CMC) solution to enhance ex situ soil washing for extracting mixed contaminants. Further,Tenax extraction method was combined with a first-three-compartment model to evaluate the environmental risk of residual PAHs in washed soil. In addition,the redistribution of heavy metals/F after decontamination was also estimated using a sequential extraction procedure. Three successive washing cycles using50 g/L CMCD and 5 g/L CMC solution were effective to remove 94.3% of total PAHs,93.2% of Pb,85.8% of Cd,93.4% of Cr,83.2% of Ni and 97.3% of F simultaneously. After the 3rd washing,the residual PAHs mainly existed as very slowly desorbing fractions,which were in the form of well-aged,well-sequestered compounds; while the remaining Pb,Cd,Cr,Ni and F mainly existed as Fe–Mn oxide and residual fractions,which were always present in stable mineral forms or bound to non-labile soil fractions. Therefore,this combined cleanup strategy proved to be effective and environmentally friendly.