HJ505-2009法测定生化需氧量[BOD_5]不确定度评定

测量不确定度（uncertainty of measurement）是表征合理地赋予被测量之值的分散性,与测量结果相联系的参数。不确定度一词指可疑程度,广义而言,测量不确定度是对测量结果正确性的可疑程度。如何对测量结果的不确定度进行合理评定,一直是困扰检测实验室的一个难题。依据HJ505—2009标准的方法,测定了水样的生化需氧量BOD5,估算了测试过程中的随机效应和系统效应所产生的不确定度分量,最终评定了生化需氧量浓度的测量不确定度。     

臭氧氧化浮选药剂丁基黄原酸钾反应动力学研究

烃基黄原酸盐是有色金属硫化矿浮选中经常使用的有机浮选药剂,本文研究臭氧氧化浮选药剂丁基黄原酸钾(potassium n-butyl xanthate,简称KBX)的反应速率常数.采用两种不同动力学模型对臭氧分子与KBX直接反应速率进行测定:①直接测定臭氧消耗对数模型,②竞争动力学模型.当[KBX]0≥10[O3]0,加...     

Impact of fertilization on chestnut growth, N and P concentrations in runo water on degraded slope land in South China

Growing fruit trees on the slopes of rolling hills in South China was causing serious environmental problems because of heavy application of chemical fertilizers and soil erosion. Suitable sources of fertilizers and proper rates of applications were of key importance to both crop yields and environmental protection. In this article, the impact of four fertilizers, i.e., inorganic compound fertilizer, organic compound fertilizer, pig manure compost, and peanut cake （peanut oil pressing residue）, on chestnut （Castanea mollissima Blume） growth on a slope in South China, and on the total N and total P concentrations in runoff waters have been investigated during two years of study, with an orthogonal experimental design. Results show that the organic compound fertilizer and peanut cake promote the heights of young chestnut trees compared to the control. In addition, peanut cake increases single-fruit weights and organic compound fertilizer raises single-seed weights. All the fertilizers increased the concentrations of total N and total P in runoff waters, except for organic compound fertilizer, in the first year experiment. The observed mean concentrations of total N varied from 1.6 mg/L to 3.2 mg/L and P from 0.12 mg/L to 0.22 mg/L, which were increased with the amount of fertilizer applications, with no pattern of direct proportion. On the basis of these experiment results, organic compound fertilizer at 2 kg/tree and peanut cake at 1 kg/tree are recommended to maximize chestnut growth and minimize water pollution.     

关于水中硫化物测定几个影响因素的探讨

本文通过改变实验室温度、显色时间、是否加入乙酸锌-乙酸钠、稀释水的酸碱性等试验条件,探讨硫化物的最佳测定条件。试验结果表明,在温度为18~22℃、稀释水p H在8~10、使用液中加入乙酸锌-乙酸钠时,采用亚甲基蓝分光光度法测定硫化物标准样品,可以得到较准确的测定结果。     

Photolysis of chlortetracycline in aqueous solution: Kinetics, toxicity and products

The aqueous photodegradation of the widely used antibiotic chlortetracycline (CTC) was investigated under simulated sunlight. The quantum yield of photodegradation increased from 3.3 × 10^-4 to 8.5 × 10^-3 within the pH range of 6.0 to 9.0. The presence of Ca²⁺, Fe³⁺, and NO₃^- enhanced the photodegradation of CTC, whereas Mg²⁺, Mn²⁺, and Zn²⁺ inhibited the degradation with the order Mn²⁺ > Zn²⁺ > Mg²⁺ at pH 7.3. The monovalent cations (Na⁺ and K⁺) had negligible effect on the photolysis of CTC. Fulvic acid (FA) decreased the photodegradation of CTC due to light screening effect. Hydrogen peroxide (H₂O₂) was formed concurrently with direct photodegradation of CTC. The generation rate of H₂O₂ increased from 0.027 to 0.086 μupmol/(L.min) when the pH ranged from 6.0 to 9.0. The CTC solution was about three-fold more toxic to the Photobacterium phosphoreum bacteria after irradiation, suggesting that the photoproducts and H₂O₂ formed in the CTC solution exhibited high risk on the bacteria. By LC-ESI(+)-MS, the photoproducts of CTC were identified. The direct photodegradation of CTC was involved in hydroxylation and N-demethyl/dedismethyl processes. The main photoproducts included the iso-CTC analog containing hydroxyl groups (m/z 511.4 and 495.4), and the N-demethyl/dedismethyl products of the photoproduct m/z 495.4 (m/z 481.3 and 467.4). In addition, the photochemical dechlorination of CTC led to tetracycline (m/z 445.5).     

水和土壤中磺胺和激素类药物的同时分析方法

建立了一种水和土壤中磺胺嘧啶、磺胺甲嘧啶、磺胺噻唑、磺胺二甲嘧啶、磺胺二甲氧嘧啶、磺胺甲(噁)唑6种磺胺类药物和17α-雌二醇、17β-雌二醇、雌酮、雌三醇、炔雌醇、乙烷雌酚6种激素类药物同时分析的方法.具体步骤:水样过滤后使用Oasis HLB固相萃取小柱进行净化富集;土壤样品经加速溶剂提取(ASE)之后过Oasis HLB小柱净化富集;采用超高效液相色谱-串联质谱(UPLC-MS/MS)进行检测,分别以乙腈和1mL·L-1甲酸溶液、乙腈和1 mL· L-1氨水溶液作为流动相.磺胺在水和土壤中的回收率分别为87.4％～ 103.6％和58.2％～80.0％,激素在水和土壤中的回收率分别为84.8％～ 101.8％和62.8％～79.3％,相对标准偏差均小于10.3％.水和土壤中磺胺的检测限分别为0.11～0.24ng·L-1和0.01～0.02ng·g-1,激素的检测限分别为0.31 ～2.14 ng·L-1和0.03～0.21ng·g-1.用上述方法检测宿迁某典型养殖场周边的地表水和土壤,结果表明采用该方法检测环境样品中的磺胺和激素类药物是可行的.     

恒压氮气隔断连续流动分析法测定水中化学需氧量

为建立恒压氮气隔断连续流动分析法测定水样化学需氧量的分析方法,将连续流动分析法恒流空气隔断改为恒压氮气隔断,优化试剂配方和反应模块,结果表明：恒压氮气隔断法注入氮气的压力是0.06 MPa,仪器稳定时间是20～35 min,持续分析样品时间大于4 h,指标均优于恒流空气隔断法;标准曲线在2.5～40.0 mg/L范围内,相关系数大于0.999,方法检出限为0.44 mg/L,相对标准偏差为0.2%～2.6%,加标回收率在93.8%～103.8%之间,检出限优于恒流空气隔断法,精密度和正确度满足质量控制要求;实样和标样方法比对测定结果相对标准偏差小于5%,结果精密度优于标准的手工法。恒压氮气隔断连续流动分析法适用于大批量低浓度水样化学需氧量的快速检测,对于密度大、黏度大液流恒压氮气隔断具有更好的稳定性、灵敏度和正确度。     

偶氮染料的光汗协同降解及其生成芳香胺的测定

以活性艳红X-3B为目标染料,选择AATCC标准人工汗液在光照条件下进行偶氮染料的降解反应.通过测定降解过程中紫外-可见吸收光谱的变化,表征了光汗协同对偶氮染料降解过程的影响.结果表明,光照与汗液对偶氮染料的降解脱色具有明显的协同作用.汗液中有机组分对偶氮染料的光汗协同降解起主要作用,但汗液中的无机盐组分对偶氮染料的降解脱色有一定的抑制作用.在相同辐照时间下,染料的降解脱色率随辐照强度的增加而增加,光强为2.68 mW/cm~2辐照240 min时,模拟水样中活性艳红X-3B的降解脱色率达35%以上.光汗协同降解反应过程中-lnA_t/A_0与t的关系符合一级动力学方程;反应的速率常数随光强的增加而增大.通过采用纤维膜保护液相微萃取和毛细管电泳联用的方法,实现了活性艳红X-3B光汗协同降解过程中生成苯胺的测定.     

直接进水样气相色谱法测定水和工业废水中乙腈、丙烯腈、苯胺及硝基苯

直接进水样气相色谱法测定水和工业废水中微量含氮有机污染物具有快速、简便、精确的特点。本法用５３０μｍ熔融石英毛细管柱分离,高灵敏度的氮磷检测器,进样１μｌ时检测限分别为０．４μｇ／Ｌ、０．４５μｇ／Ｌ、４μｇ／Ｌ、１０μｇ／Ｌ。这一灵敏度可满足排污监测及环境评价的要求。     

北京市用水结构现状分析与对策研究

北京是严重缺水的特大城市,但同时由于行业用水结构不甚合理,造成水资源浪费严重。本文以１９９１年为报告期,采用直接用水系数、完全用水系数、用水乘数、重复用水率等指标对本市行业用水结构的现状和变化进行了全面的分析和讨论,提出了相应的对策与建议。为协调本水环境与经济发展的关系,制定合理的水资源利用体系,促进持续发展战略的实施提供依据。