磷锑钼三元杂多酸光度法测定药品中的抗坏血酸

研究了少量抗坏血酸与磷锑钼三元杂多酸体系的显色特性，建立了借磷锑钼三元杂多蓝测定抗坏血酸的分光光度法。最佳显色条件为［ＰＯ３－４］＝３０×１０－４ｍｏｌ·Ｌ－１，［ＳｂⅢ］＝４５×１０－５ｍｏｌ·Ｌ－１，［ＭｏＯ２－４］＝７５×１０－３ｍｏｌ·Ｌ－１，Ｐ∶Ｓｂ∶Ｍｏ＝１∶０１５∶２５，［Ｈ加入］／［Ｍｏ］＝５７。测定波长为λｍａｘ＝７１０ｎｍ，线性范围为１～５０μｇ·ｍＬ－１，回归方程为Ａ＝３６８０Ｃ－００１４，线性相关系数ｒ＝０９９９８，表现摩尔吸光系数ε７１０＝３６８×１０３Ｌ·ｍｏｌ－１·ｃｍ－１，检出限为０２μｇ·ｍＬ－１，标准回收率为９５％～１００％，变异系数ｃｖ≤０３４％（ｎ＝６）。与二元磷钼杂多酸方法相比，省去了水浴加热的繁琐操作，而且由于锑（Ⅲ）的引入，显色在室温下３５ｍｉｎ便可完成，并可稳定５ｈ。     

四氯邻苯二甲酸二辛酯的合成

以四氯苯酐和辛醇为原料进行催化酯化反应,产物经固体碱和吸附剂后处理合成了新型阻燃增塑剂四氯邻苯二甲酸二辛酯,四氯苯酐的转化率９９６％,产品的酯含量９９９７％、酸值００１５ｍｇＫＯＨ／ｇ、体积电阻１４６×１０１３Ω·ｃｍ、色泽（铂 钴）１０～２０号。最佳工艺条件是,原料摩尔比为ＴＣＰＡ∶辛醇∶催化剂＝１∶３∶１２４×１０－２,反应温度为２１０±２℃,反应时间为３～３５ｈ。     

测定亚硝胺的电位型霉变玉米胚组织传感器研究

利用霉变玉米胚组织研制了对二甲基亚硝胺（ＤＭＮＡ）、二乙基亚硝胺（ＤＥ－ＮＡ）和甲基苄基亚硝胺（ＭＢＮＡ）等选择性响应的新型组织传感器。该传感器灵敏度高,重现性好,选择性好,其线性范围２．０×１０－６～２．０×１０－３ｍｏｌ·Ｌ－１,检测下限１．３×１０－７ｍｏｌ·Ｌ－１,斜率为５９．２（３０°Ｃ,ｐＨ７．５）。     

化学发光法测定微量铁

本文利用Ｆｅ（Ⅱ）对Ｃｒ（Ⅵ）－ＫⅠ反应的催化作用和Ⅰ２－鲁米诺化学发光反应，建立了测定微量铁的新方法。提出了测定的最佳条件，检出限为５．６×１０（－１１）ｇ·ｍｌ（－１）的铁，线性范围１．０×１０（－１０）～１．０×１０（－８）ｇ·ｍｌ（－１）的铁。用于自来水和工业盐酸中铁的测定，结果满意。     

分光光度法测定盐酸环丙沙星

研究了０．１ｍｏｌ·Ｌ－１的硫酸介质中,盐酸环丙沙星与三氯化铁的显色反应。盐酸环丙沙星浓度在３．３×１０－５～７．３×１０－４ｍｏｌ·Ｌ－１（０．０１２～０．２７ｍｇ·Ｌ－１）范围内符合比尔定律,ε＝１．８５×１０３Ｌ·（ｍｏｌ·ｃｍ）－１。测得络合物组成比为１∶１。本方法简便准确,可用于片剂和胶囊中盐酸环丙沙星的测定。     

黄瓜瓜蒂组织液化学传感器研究

研制了以四（十二烷基）铵（ＴＤＡＣ）－十六烷基苄基二甲基铵（ＣＢＤＭＡＣ）－黄瓜瓜蒂组织液－丙戊酸钠为电活性物,以石墨粉为内导材料的ＰＶＣ膜电位型丙戊酸钠化学传感器。此传感器选择性、稳定性、重现性都较好。其线性范围为３．０×１０－６～１．０×１０－２ｍｏｌ·ｌ－１,检测下限为１．０×１０－６ｍｏｌ·ｌ－１,斜率为５９ｍＶ／ｐＣ（２５℃,ｐＨ＝９～１１）。     

Fe_2O_3－SrO－TeO_2系半导体玻璃电导的研究

用准急压冷法制成Ｆｅ_２Ｏ_３－ＳｒＯ－ＴｅＯ_２系半导体玻璃并对其直流电导率进行了测定。玻璃形成范围为（以摩尔计）；０≤Ｆｅ_２Ｏ_３≤２３％；０≤ＳｒＯ≤１８％；７５％≤ＴｅＯ_２＜１００％。通过Ｓｅｅｂｅｃｋ系数的测定确认Ｆｅ_２Ｏ_３－ＳｒＯ－ＴｅＯ_２系玻璃为ｎ型半导体玻璃。２００℃的直流电导率为３．７２×１０￣（－５）～１．８２×１０￣（－６）Ｓ·ｃｍ￣（－１）。直流电导率随着Ｆｅ_２Ｏ_３含量的增加而增加，１６５℃时的载流子迁移率和浓度分别为１．１２×１０￣（－９）～３．６７×１０￣－７ｃｍ￣２·Ｖ￣（－１）·Ｓ￣（－１）和２．１７×１０￣（２１）～８．３３×１０￣１９ｃｍ￣（－３）．讨论的结果表明Ｆｅ_２Ｏ_３－ＳｒＯ－ＴｅＯ_２系玻璃的电导机理符合小极化子跳越理论。     

Cu(Ⅱ)对DApEM-V(Ⅴ)-H_3PO_4-Mn(Ⅱ)-OP阻抑作用的研究

在酸性介质中Ｃｕ（Ⅱ）能阻抑试剂ＤＡｐＥＭ与Ｖ（Ⅴ）的显色反应。研究了该反应的动力学参数,表观速度常数２．９１×１０－３ｓ－１,表观活化能为５２．８４ｋＪ·ｍｏｌ－１。从而建立了一种测微量Ｃｕ（Ⅱ）的动力学光度法。Ｃｕ（Ⅱ）含量在１．０～８．０μｇ·２５ｍＬ－１范围内,与ｌｇＡ０Ａ呈良好线性,表观摩尔吸光系数为１．１７×１０５Ｌ·ｍｏｌ－１·ｃｍ－１,检出限１．３４×１０－１０ｇ·Ｌ－１,该方法用于人发样品中Ｃｕ的测定,ＲＳＤ％为０．４３％～０．４５％,回收率为９６％～９９％。     

微量铋的示波极谱测定法

在ｐＨ１０．５的Ｋｏｌｔｈｏｆｆ缓冲溶液中，铋－溴邻苯三酚红配合物在单扫描示波极谱仪上产生一灵敏的极谱波，峰电位为－０．６５Ｖ（ｖｓ，ＳＣＥ），峰电流与铋浓度在６．０×１０~（－８）～６．０×１０~（－６）ｍｏｌ·Ｌ~（－１）范围内成线性关系，检测下限为２．０×１０~（－８）ｍｏｌ·Ｌ~（－１）。应用本法测定了化探矿样中的微量铋，获得满意结果。     

5，10，15，20－四（4－羟基－3－磺酸苯基）卟啉光度法测定水中痕量铜的研究

在ｐＨ４．０时，铜与标题试判形成１：１的配合物．作工曲线回归方程为Ｙ＝３．０５×１０（－３）＋０．２３１Ｘ，相关系数ｒ＝０．９９９１，其最大吸收波长在４１２ｕｍ处，摩尔吸光系数ε＝２．０３×１０５Ｌ·ｍｏｌ（－１）·ｃｍ（－１）．用含量在０～２．０μｇ／２５ｍｌ范围内符合朗伯比耳定律．     

镁合金基体上镍磷镀层的阳极退除

采用阳极退除方法退除镁合金上化学镀镍磷镀层,研究了退除液成分对镀层退除的作用,对常用的镁合金化学镀镍层的退除工艺（HF＋NaNO3）进行了改进。退镀液中含有一定浓度的F^-,可保护基体不受腐蚀;溶液中的NaNO3对保护膜起破坏作用;生成的保护膜主要为MgF2。     

Experimental model validation of an integrated process for the removal of carbon dioxide from aqueous ammonia solutions

In this work modelling and experimental validation of an integrated process for the removal of carbon dioxide from ammonia solutions - the so called decarbonisation - is presented. In this process, carbon dioxide and small amount of ammonia is stripped out from the solution at ambient pressure in a packed column. Recovery of the stripped ammonia can be reached by combining absorption of ammonia and condensation of stripping steam. The integration of stripping, absorption and direct-contact condensation (DCC) can be achieved in one compact unit in which stripping takes place in the lower part of the packed column, and the DCC and ammonia absorption in its upper part. This unit has been modelled in a rigorous way considering heat and mass transfer as well as reaction rates in multicomponent reactive stripping, absorption and direct-contact condensation in packed columns (Ma?kowiak et al., 2009). Extensive experimental investigations in a pilot scale packed column with diameters of 0.15 and 0.32 m have been performed for both, the stripping and for DCC. Relevant operation parameters as well as column dimensions were varied during the experiments in order to investigate their influence on the selectivity of the decarbonisation and to achieve a broad data base for the validation. Experimental validation of the two sub-processes and the entire decarbonisation shows good agreement between calculated and experimental values. Based on the validated model a successful optimisation of the decarbonisation process in industrial scale has been performed, leading to increased carbon dioxide removal and reduction of ammonia losses.     

单塔加压汽提装置在鲁奇炉污水处理中的应用

采用新的工艺方法即单塔加压汽提装置处理鲁奇炉煤制气过程中洗涤粗煤气所产生的含高浓度酚及氨等生产污水。该装置工作原理是在较高的温度下H2S、NH3都以游离的分子状态存在于液相中,在热料减压闪蒸和塔底蒸汽的汽提作用下,液相中的H2S、NH3分子由液相转入汽相实现汽提,将污水中的CO2、H2S等酸性气体和氨在同一个加压塔内脱除。处理后的污水进入后续的萃取装置,萃取剂是甲基异丁基酮(MIBK),MIBK对单元酚和多元酚分配系数都较高,萃取效果好,且萃取剂用汽提的方式回收后可再利用。处理后的污水酚、氨、硫化氢及pH值都有显著降低,不仅显著降低了生产成本而且给污水的后续生化处理提供了方便。该方法实践证明对处理鲁奇炉生产污水非常有效。     

印刷线路板退焊锡废水再生利用研究

以铁粉还原调节溶液氧化还原性,再用硫基沉淀剂（P）和聚丙烯酰胺（PAM）使金属离子（Cu,Fe,Pb,Sn)絮凝沉淀,过滤工后母液补加硝酸,可使印刷线路析退铅锡废水实现再生利用,适宜的沉淀条件为,按每升废液加入30g还原铁粉,按理论量加入P,同时加入2－3mL1%PAM(M=600000),沉淀过滤后母液的铁深度和游离酸度可分别恢复到17.0g/L和181.3g/L,经补加硝酸后其退锡速度和退锡容量等性能与原退锡液无异。     

Recovery of copper from ammoniacal/ammonium sulfate medium by LIX 54

The extraction‐stripping reaction of Cu(II) by LIX 54 in Iberfluid from aqueous ammonium sulfate medium at pH 8.5 has been investigated. The effects of pH, metal ion, extractant concentration as well as the loading capacity of the reagent were studied. The extraction equilibrium constant for copper was determined numerically to be 7 × 10⁻⁷. Experimental data can be explained assuming the formation of CuR₂ species in the organic phase (R represents the extractant). Copper stripping was studied using typical spent copper electrowinning solutions as stripping medium. The number of stages required for the extraction and stripping of copper was also evaluated. The results were used to asses the conditions for purification of industrial waste solutions (eg spent etchants) containing copper through counter‐current extraction‐stripping. © 1999 Society of Chemical Industry     

Hollow fiber supported liquid membrane process for the separation of NH3 from aqueous media containing NH3 and CO2

A hollow fiber supported liquid membrane (SLM) process was investigated experimentally and theoretically for the separation of NH₃ from aqueous solutions containing NH₃ and CO₂. DTPA and D2EHPA were used as carriers and n-decanol was used as a diluent in this process. The membrane stripping experiments, as well as the extractive equilibrium experiments, indicate that DTPA is a better carrier than D2EHPA in relation to the increase in the NH₃ stripping rate. The influence of operating conditions, such as flow rate, the ratio of NH₃ to CO₂, and carrier concentration, on the membrane stripping rate were examined. The experimental data demonstrate that the NH₃ stripping rate by an SLM process is not significantly influenced by the amount of CO₂ present, as is that by the supported gas membrane. To predict the stripping of NH₃ from solutions containing NH₃ and CO₂, a mathematical model incorporating chemical equilibria and Nernst–Planck diffusion was developed to describe the mass transport. The experimental data suggested that the SLM process can effectively strip NH₃ from aqueous solutions containing NH₃ and CO₂.     

稀土浸矿氨氮废水的吹脱试验研究

针对稀土浸矿产生的高氨氮废水,采用吹脱法对其进行处理,通过单因素试验和正交试验对影响因素进行了研究。结果表明,各主要因素对吹脱效果的影响大小为p H吹脱温度气液比;最佳操作条件:p H=11,温度为40℃,气液比为5 555.6∶1,吹脱时间为100 min。吹脱出的NH_3用H_2SO_4吸收,形成(NH_4)_2SO_4溶液,可作为浸取剂返回生产中使用或者用于生产(NH_4)_2SO_4肥料,实现资源回收利用。该试验工艺可作为脱氮除磷二级生物处理或一级强化处理的预处理。     

曝气吹脱法去除水中三氯乙烯等有机污染物

在实验室洗气瓶试验条件下,研究了不同曝气流量以及曝气时间即气水比大小对三氯乙烯和四氯乙烯吹脱去除率的影响。结果表明三氯乙烯和四氯乙烯在曝气量为0．4～1．4L／min的试验条件下,气水比分别在2．24～4．71（气）／L（水）和1．10～2．43（气）／L（水）范围内能将初始浓度为国家标准5倍的三氯乙烯和四氯乙烯去除到国家标准限值以内,所需时间均在30min以内。试验结果表明曝气吹脱法能在较短短时间内有效去除三氯乙烯和四氯乙烯,可以作为有效去除挥发性污染物的应急处理技术。     

盐酸解析工艺在PVC废酸治理中的应用

介绍了将盐酸解析工艺应用于PVC副产废酸治理的生产技术 ,解析出的HCl气体作为合成VCM的原料气 ,每年回收量超过 1 80 0t,回收率达到 85 % ;产生的经济效益约 1 5 9.8万元 a;可节约水资源90 0 0m3 a。同时 ,治理了废酸和CaCl2 排放造成的水污染及H2 S对大气的污染。     

Electrochemical costripping models and mutual interferences of mutli-transition metal systems on the surface of boron-doped diamond

Electrochemical behaviors of electrodeposition stripping of some transition metals, such as Ag, Cu, Pb, Sn, and Cd were investigated on boron-doped diamond (BDD) film with differential pulse anodic stripping voltammetry (DPASV). The results show that the metal costripping process on the surface of BDD is influenced by deposition potential of transition metals, potential of hydrogen evolution reaction, mutual interferences between two transition metals, and so on. Electrochemical costripping models and mutual interferences of binary transition metals are proposed. (i) When the hydrogen evolution potential is higher or lower than the deposition potential of two transition metals, the metals do not form alloys and compound the cathode ions in the solution, and the costripping process conforms to metal 1 stripping-metal 2 stripping. (ii) When the hydrogen evolution potential is between the deposition potential of two transition metals, the metals do not form alloys and compound the cathode ions in the solution, and the costripping process conforms to metal 1 stripping-hydrogen evolution-metal 2 stripping. (iii) When two transition metals form alloys, the costripping process conforms to metal 1 stripping-alloy striping-metal 2 stripping. (iv) When the hydrogen evolution potential is between deposition potential of two transition metals, and transition metal 2 is complexed with one kind of cathode ion in the solution, the costripping process conforms to metal 1 stripping-hydrogen evolution-metal 2 complex formation-metal 2 stripping. Moreover, the electrochemical-costripping model of two transition metals in a solution with three or more transition metals, is similar to that in the binary system. It is also found that various metals electrodeposited on BDD film in the form of single metal or alloy can be completely stripped away by the constant-potential electrolysis technique at 2.8 V for 10 s.