亚硝化—厌氧氨氧化处理猪场废水研究

猪场废水COD浓度高、氨氮浓度高、悬浮物浓度高，已成为农村面源污染的主要来源，并严重威胁到农村饮用水安全。猪场废水氨氮浓度高、处理难度大，如何采用经济高效的方法，去除氨氮使其达到排放标准，一直是猪场废水处理中面临的重要难题。 厌氧氨氧化是近年受到国内外水处理研究者广泛关注的新型生物脱氮技术，具有不需要外加有机碳源、节省供氧量、降低能耗等优点。虽然国内外研究者对厌氧氨氧化过程的脱氮机理、厌氧氨氧化菌的生理生化特性等进行了多方面的研究，但已有的报道大多以模拟废水为研究对象，以猪场废水为研究对象的报道，在国内外文献中极少有报导。 本论文以猪场废水为主要研究对象，考察了猪场废水的亚硝化过程、厌氧氨氧化的启动过程，并对亚硝化和厌氧氨氧化联合用于猪场废水脱氮进行了探索。 1．论文首先研究了猪场废水的亚硝化过程，考察了废水水质和主要运行条件对亚硝化过程的影响。实验表明：（1）亚硝化阶段反应时间为8到10h时，出水中氨氮和亚硝酸盐浓度比可达到1：1～1：1.23，满足厌氧氨氧化反应对二者比例的要求；达到前述要求时，氨氮去除率达到58.3～65.6 %，亚硝化率在整个过程均保持在97 %以上，COD去除率在59.2～68.6 %；（2）曝气量（溶解氧）对亚硝化过程影响显著，随着曝气量增大，达到厌氧氨氧化要求的氨氮与亚硝酸盐氮浓度比例所需水力停留时间τ越短，pH出现明显下降的时间越短；（3）τ对应的pH在7.8～8.1之间，无需进行pH调节即可满足厌氧氨氧化反应对pH的要求；（4）氨氮和COD降解过程遵循一级反应动力学，氨氮和COD降解的速率常数分别为0.0656～0.0724 1/h和0.0491～0.0664 1/h。 2．在进行亚硝化过程研究的同时，以模拟废水为试验对象，进行厌氧氨氧化启动研究。以反硝化污泥和养殖厂储水池厌氧底泥的混合污泥作为接种污泥，历时大约100天，培育出具有厌氧氨氧化活性的污泥，氨氮和亚硝酸盐氮最高进水浓度分别为223.8 mg/L和171.4 mg/L，去除率最高分别达48%和41.5%，此时二者消耗比例为1.33：1。 3．在猪场废水的亚硝化研究完成和厌氧氨氧化过程初步启动成功后，在模拟废水中逐步加入猪场废水的亚硝化处理出水，逐步实现亚硝化和厌氧氨氧化的组合。亚硝化出水添加到厌氧反应器后，厌氧氨氧化反应仍可继续进行，且去除效率逐步提高。研究发现添加的亚硝化出水中携带的亚硝化细菌在厌氧氨氧化菌膜外层生长并累积，增加了厌氧氨氧化反应基质的传质阻力，妨碍了厌氧氨氧化效率的提高。 4．亚硝化－厌氧氨氧化实际工程应用探索中，生物接触氧化池可在有效去除废水中的有机物的同时实现亚硝化，出水中氨氮和亚硝酸盐比例平均为1.10，可满足后续厌氧氨氧化的要求；在适宜的进水浓度和温度下，ABR池出现了厌氧氨氧化启动的迹象；研究同时发现，水质的波动和气温的变化是工程中影响厌氧氨氧化菌活性的重要因素。 论文的主要创新点在于：（1）以猪场废水为研究对象，以实现厌氧氨氧化为目标，对亚硝化过程进行了比较详细的考察，获得了亚硝化出水满足厌氧氨氧化要求的工艺条件，通过对其COD和氨氮降解过程的考察，得出亚硝化阶段COD降解和氨氮去除的动力学模型；（2）对亚硝化－厌氧氨氧化处理猪场废水进行了探索，确立了影响其污染物去除率稳定的重要因素。 论文的上述研究成果，为厌氧氨氧化技术的实用性研究提供理论依据。 Piggery wastewater, which is characterized by high concentration of COD、ammonium and suspend substance, has become a most important source of non-point source pollution and also severely threats drinking water security in rural area. How to discharge piggery wastewater with the ammonium concentration meeting standard by economical and effective method? This is the most urgent problem in piggery wastewater treatment. As a new biological nitrogen removal technology, Anammox process has been paid more and more attention by researchers all over the world. Anammox has advantages of no need of organic carbon addition, low oxygen consumption and energy consumption. Plenty of investigations have been carried out to the mechanism, physiological and biochemical characteristic of bacteria about Anammox. Most of researches focused on synthetic wastewater, there is rare report about its application in piggery wastewater. In this paper，experimental studies were performed to investigate Sharon process in treatment of piggery wastewater，the start up process of Annammox using synthetic wastewater were studied, the feasibility of applying Sharon-Anammox process in the nitrogen removal of piggery wastewater was evaluated. 1. Sharon process of piggery wastewater was firstly investigated to analyze the effects of water quality and main running parameters, which meet the NH4+-N to NO2--N ratio requirement of successive Anammox. Results showed: (1)During Sharon Process，after 8～10 hours’ reaction the NH4+-N to NO2--N ratio in effluent reached 1:1.0～1:1.23, when the removal percentage of NH4+-N was 58.3～65.6 %, a semi-nitration rate of above 97 % was achieved during the process; meanwhile 59.2～68.6 % of the COD was also removed. (2)The aeration rate（oxygen） had obvious effect on the hydraulic retention time(τ) which met the NH4+-N to NO2--N ratio requirement of Anammox. As aeration rate increased, the hydraulic retention time(τ) was shortened. (3) The pH corresponding to τ was between 7.8 and 8.1, thus it needed no artificial adjustment. (4) The reduction of ammonia and COD followed the first-order reaction kinetics. The velocity constants of ammonia and COD were 0.0656～0.0724 1/h and 0.0491～0.0664 1/h, respectively. 2. The startup of Anammox process using the artificial wastewater was performed simultaneously with Sharon. The aim was to investigate the running parameters of Anammox and make foundation for the combination stage. By using the mixture of denitrifying sludge and anaerobic sludge in tank of the breeding factory, sludge of Anammox activity was cultivated in UASB after 100 days. The removal percentage of NH4+-N and NO2-N were up to 48% and 41.5%, respectively, when the NH4+-N and NO2-N influent concentration were 223.8 mg/L and 171.4 mg/L, respectively, the NH4+-N and NO2-N removal rate was 1.33:1. 3. After investigation of Sharon and startup of Anammox, effluent of Sharon process was added into the synthetic wastewater to combine Sharon and Anammox step by step. It took some time after the addition of Sharon effluent that Anammox reaction continued and the removal rate kept increasing. It indicated that nitrifying bacteria were carried by the Sharon effluent cumulated in the outer layer of Anammox. This enhanced transfer resistance of Anammox reaction and the increasing removal rate was restrained. 4. In the bio-contact oxidation pond of practical project, Sharon process were carried out successfully and organic compounds were removed effectively. An average NO2-N/ NH4+-N rate of 1:1.0 was achieved in the effluent, which met the requirement of successive Anammox. Under condition of suitable influent concentration and temperature, there was evidence that Anammox could start up in ABR. The variety of wastewater and temperature had great affects on Anammox activity in practical engineering. Innovation of this paper: (1) The Sharon process for treating piggery wastewater was discussed in details. Technological parameters that met requirement of Anammox were obtained. The dynamic models of COD and ammonium removal in the process were educed. (2) Sharon-Ananmmox for treatment of piggery wastewater was investigated, and the primary influencing factors was studied. This paper could be a theoretical consult for research of Anammox utility.

碱法草浆造纸蒸煮黑液厌氧生物降解性及其主要微生物类群研究

造纸行业是造成我国水环境有机污染物的重要污染源之一，其水污染的特点是小厂多、草浆多、工艺落后、污染扩散面广、造成废 水排放量大，每年排放的废水量约39亿立方米，占全国工业废水排放量的1/6，其中有机污染物（以BOD5计）160万吨左右，约占全 国工业废水中有机污染物总量的1/4。尤以占全国制浆造纸行业90%以上的碱法草浆造纸厂的蒸煮黑液量大面广，除含有机物外，还 含有木质素、残碱、硫化物、氯化物等污染物，属于PH值高、色度深、难于治理的高浓度有机废水，对水体污染特别严重，各地要 求治理呼声很高，急待研究并尽快找出各种有效的治理途径。对于碱法草浆蒸煮，黑液高浓度废水的治理，有各种方法，根据国内 的研究进展和我们已有试验工作表明，最经济有效，具有实用价值，在生产上可获得成功是厌氧处理法。近10多年来，国外关于高 效厌氧处理技术研究进展迅速，并出现了多种多样的工艺设备，如高效厌氧生物反应器，并在实用化方面取得了很大成绩，建立了 生产性装置，达到了高负荷运行，效果良好。本试验是根据我们已有研究基础，针对我国国情，对小型制浆造纸厂水污染防治除了 开发碱回收及各种综合利用技术外，要特别加强废水(废液)实用技术研究的指导思想，本试验采用改进型的上流式厌氧污泥床反应 器，设计了两种试验方案，通过试验结果如下。1. 试验方案I—碱法草浆黑液酸化和厌氧发酵I号UASB反应器动态模型试验结果表 明：(1). 采用中温35℃±1℃高效厌氧反应器USAB内装有填料(陶粒)和三相分离器，具有保持高浓度生物量和防止污泥流失的特点 ，污泥浓度Vs 可达30%以上，因而具有高效、节能、产能、滞留期短的优点，当进水CODcr在7500-10000mg/l，HRT由7天缩短到3天 ，有机容积负荷在1.22gCODcr/l·d-3.43gCODcr/l·d时，CODcr平均去除率可达55%-45.5%，最高CODcr去除率可达60.2-63.5%， BOD5去除率可达75.9-83.2%,沼气容积产气率可达0.29-0.67l/l·d，每克CODcr转化为沼气产率达0.39-0.48l/gCODcr·d，CH4含量 65.8-75.5%。厌氧发酵出水再用化学法进行后处理脱除难降解的木质素，CODcr总去除率达80%以上。(2). 动态试验结果表明：采 用酸化—厌氧发酵处理黑液工艺合理，技术路线可行。2. 试验方案II—黑液用化学法(Hcl)去除木质素进行厌氧发酵，II号UASB反 应器动态模型试验结果表明：(1). 采用中温35℃±1℃高效厌氧反应器UASB(内有软填料)，当进水CODcr7000-13000mg/l左右，HRT 由6天缩短到1天，有机负荷由0.98gCODcr/l·d增加到11gCODcr/l·d时，COD平均去除率均可稳定在70-77%，BOD5去除率为87.3- 93.1%，沼气容积产气率0.21-2.6l/l·d，每克CODcr转化为沼气产率为0.39-0.48l/gCODcr·d，高的可达0.53l/gCODcr·d，转化 率较高，CH4含量63-70%。(2). 试验证明碱法草浆黑液物化预处理—厌氧发酵处理的技术路线也是可行的，工艺合理、效果较好。 在有条件的工厂可采用。3.厌氧发酵阶段几大类群微生物计数表明：(1). 当发酵工艺和运行处于相对稳定状态时，微生物群体的 组成也达到相对的稳定，各类微生物之间保持动态平衡关系。当产乙酸菌的数量为107-108个/ml时，产甲烷菌的数量为105-106 个/ml，当产乙酸菌数量为106-107个/ml时，产甲烷菌的数量为103-105个/ml。(2).稳态运行条件下，黑液预处理为甲烷发酵创造 了有利的生态环境，获得了较好的处理效果和较高的COD转化为沼气的产率0.39-0.48l/g·CODcr·d，反应器中形成较为稳定而数 量较下水污泥中高1-2个数量级的厌氧发酵微生物区系组成。这一结果为黑液厌氧发酵提供了微生物理论依据。Paper industry is one of the important pollution source of water environment in our country. Its character of water pollution is many small factories, much grass pulp, disadvantageous technique, large preading area of pullution. Its effluent makes up 1/6 of whole country's industry wastwater. Its organic pollutant accounts 1/4 of whole country's. Alkaline grass paper pulp effluent with pollutants such as ligoin, remaining alkali sulfide, chloride besides organic material, is a kind of high concentrate organic wastewater which has high PH walug, dark colour and is difficult in treatment. There is urgent require to find ways to treat the wastewater. There are different ways to treat alkaline paper grass pulp effluent. According to the research advances and our experiment work, the most economical and useful way is anaerobic degradation which was advanced quick in last ten years. In the control of waste water of small pulp paper mill, the study of wastewater utilization technology should be emphasized, besides alkaline retrieving and different kinds of comprehensive utilization technology. Our experiment used modified UASB(Upflow Anaerobic Sludge Blanket Reactor). Two kinds of plan were disgned. The results are lined below. 1. The first experiment plant-aciding black pulp effluent and methanogenic digestion. The dynamic model experiment results of I-UASB reactor showed: (1)The mesophilic(35℃±1℃)high effect UASB reactor having haydite and threee state seperation in it had the character of keeping high bioimass concentration and preventing losss of sludge. It had advantages of high effect, energe saving, energe prodcing and short HRT(Hydroulic retention time). When the influent COD was 7500-10000mg, HRT was shortened from 7 days to 3days, organic loading rate was 1.22g-3.43COD/l· d, the average COD removal efficiency was 55%-45%. The highest COD efficiency was 60.2-63.5%, BOD removal of 75.9 -83.4% was achieved. Biogass production rate were up to 0.29-0.67l/l·d. Biogass converted efficiency from every gram of COD could reach 0.39-0.48l/gCOD·d. Methane content was 65.0-75.5%. Chemical method was used to deplate lignin in anaerobic digestion effluent. Total COD removal efficiency could be more than 80%. (2)Using aciding annaerobic digestion to treat the black effluent was reseanable in technique and technology. 2. The second experiment plan-anaerobic digestion was used after the chemical method was used to deplate lignin in the black effluent. The result of dynamic experiment of II-UASB reactor showed: (1)High effect mesophilic (35℃±1℃)UASB reactor having soft slaffing in was used. When influent COD was about 7000-13000mg/l, HRT was shortened from 6 days to 1 day and organic loading rate was increased from 0.90 to 11g COD /l·d, average COD removal efficiency remained stable on 70-77%. BOD, removal efficiency was between 87.3-93.1%. Biogass production rate was 0.2-2.6l/l ·d .Biogass converted efficiency from a gram of COD was 0.39-0.481/gCOD·d with the high value of 0.53l/gCOD·d. Methane content was 63-70%. (2)The way that using physical, chemical Pre-treatment-anaerobic digestion to treat alkaline black effluent is feasible and can be used in some factories when the condition exists. 3. Counting of several class of microoganisms in anaerobic digestion stage showed: (1)As the disgestion was in stable motion, the compositon of microorganic colony could get relative stable. Dynamic balance was remaining among different kinds of microorganism such as methanogenic bacteria, Acidogenic bacteria, sulfate reducing bacteria, and heterotrophic bacteria. (2)Under stable motion, the pre-treatment of black effluent produced favourable eco-enviroment for methanegenic digestion. Good treatment effect and high biogass convertent efficiency from COD(0.39-0.48l/g·COD· d)were gotten. Some stable and high quantity(10-100times more than sewage sludge)microorganism colony were formed in the reactor. This result provided theoretical basis for anaerobic digestion of black effluent.

Migration of neutral solutes by double stepwise gradient elution in capillary electrochromatography

Characteristics of electroosmotic flow (EOF) and the migration of neutral solutes under double stepwise gradient elution in capillary electrochromatography were studied systematically. EOF velocity proved to be the function of operation time changing with the introduction of the second mobile phase. Accordingly, the retention of components also changed. The migration of neutral solutes was studied under the following three situations; A, components eluted when the column was filled only with the first kind of mobile phase; B, solutes eluted still in the first kind of mobile phase while at that time two kinds of mobile phase coexisted in the column and C, samples eluted in the second kind of mobile phase. Equations to describe the retention times of components under these three kinds of conditions were deduced and applied to predict the retention times of 12 aromatic compounds. Relative errors between experimental and calculated values were below 5.0%, which proved the reliability of the equations. In addition, parameters that might affect the retention time of solutes, such as the transferring time of mobile phase vials, the capacity factors of components and EOF velocities two steps were studied systematically (C) 2001 Elsevier Science B.V. All rights reserved.

Realization of write-once-read-many-times memory devices based on poly(N-vinylcarbazole) by thermally annealing

A nonvolatile write-once-read-many-time (WORM-time) memory device based on poly(N-vinylcarbazole) (PVK) films was realized by thermally annealing. The device can be fabricated using a simple spin coat method. It was found that the control of PVK film surface morphology by thermally annealing plays an important role in achieving the WORM memory properties. The memory device showed an ON/OFF current ratio as high as 10(4) and the retention time was over 2000 s without degradation.

The morphology control of pentacene for write-once-read-many-times memory devices

We realized write-once-read-many-times (WORM) memory devices based on pentacene and demonstrated that the morphology control of the vacuum deposited pentacene thin film is greatly important for achieving the unique nonvolatile memory properties. The resulted memory devices show a high ON/OFF current ratio (10(4)), long retention time (over 12 h), and good storage stability (over 240 h). The reduction of the barrier height caused by a large interface dipole and the damage of the interface dipole under a critical bias voltage have been used to explain the transition processes.

Identification of Phenylethanoid Glycosides in Plant Extract of Plantago asiatica L. by Liquid Chromatography-Electrospray Ionization Mass Spectrometry

The present work describes a liquid chromatography-electrospray ionization mass spectrometry (LC-ESI-MS) method for rapid identification of phenylethanoid glycosides in plant extract from Plantago asiatica L. By using a binary mobile phase system consisting of 0.2% acetic acid and acetonitrile under gradient conditions, a good separation was achieved on a reversed-phase C-18 column. The [M-H](-) ions, the molecular weights, and the fragment ions of phenylethanoid glycosides were obtained in the negative ion mode using LC-ESI-MS. The identification of the phenylethanoid glycosides (peaks 1-3) in the extract of P. asiatica L. was based on matching their retention time, the detection of molecular ions, and the fragment ions obtained by collision-induced dissociation (CID) experiments with those of the authentic standards and data reported in the literature.

Studies on principal components and antioxidant activity of different Radix Astragali samples using high-performance liquid chromatography/electrospray ionization multiple-stage tandem mass spectrometry

The principal components, isoflavonoids and astragalosides, in the extract of Radix Astragali were detected by a high-performance liquid chromatography Couple to electrospray ionization ion trap multiple-stage tandem mass spectrometry (HPLC-ESI-IT-MSn) method. By comparing the retention time (t(R)) of HPLC, the ESI-MSn data and the structures of analyzed Compounds with the data of reference compounds and in the literature, 17 isoflavonoids and 12 astragalosides have been identified or tentatively deduced. By Virtue of the extracted ion chromatogram (EIC) mode, simultaneous determination of isoflavonoids and astragalosides could be achieved when the different components formed overlapped peaks. And this method has been utilized to analyze the constituents in extracts of Radix Astragali from Helong City and of different growth years. Then the antioxidant activity of different samples has been Successfully investigated by HPLC-ESI-MS method in multiple selected ion monitoring(MIM) mode, applying the spin trapping technology, and the Ferric Reducing Antioxidant Power (FRAP) assay was applied to support the result.

大青叶正丁醇提取物化学成分的HPLC/ESI-MSn研究

High performance liquid chromatography-electrospray ionization mass spectrometry(HPLC/ESI-MSn) was applied to analyze the chemical constituents from n-BuOH extract of Folium Isatidis.The data of retention time,UV spectra,molar masses and structural information on the compounds were obtained.Seventeen compounds are found in extract from n-BuOH.There are four nucleosides,two purines and eleven flavones.

Studies on lignan constituents from Schisandra chinensis (Turcz.) Baill. fruits using high-performance liquid chromatography/electrospray ionization multiple-stage tandem mass spectrometry

A reversed-phase high-performance liquid chromatography-diode array detector-electrospray ionization multiple-stage tandem mass spectrometry (RP-HPLC-DAD-ESl-MSn) method has been developed for the detection and analysis of lignan constituents in the methanol extract from the fruits of Schisandra chinensis (Turcz.) Baill. RP-HPLC-DAD-ESI-MSn and electrospray ionization Fourier transform ion cyclotron resonance multiple-stage tandem mass spectrometry (ESI-FT-TCR-MSn) have been applied to investigate the characteristic product ions of four lignan reference compounds. Then, the logical fragmentation pathways of the lignans have been proposed. By comparing the retention time (t(R)) of HPLC, the ESI-MSn data and the structures of analyzed compounds with the data of reference compounds and in the literature, 11 peaks in HPLC have been unambiguously identified and another 5 peaks have been tentatively identified or deduced. Also, in the present paper, the extracted ion chromatograms (EIC) have been used to analyze the lignan isomers. The experimental results demonstrate that RP-HPLC-DAD-ESI-MSn is a specific and useful method for the identification of the lignan constituents and their isomers.

Negative differential resistance and memory effect in diodes based on 1,4-dibenzyl C60 and zinc phthalocyanine doped polystyrene hybrid material

Negative differential resistance (NDR) and memory effect were observed in diodes based on 1,4-dibenzyl C60 (DBC) and zinc phthalocyanine doped polystyrene hybrid material. Certain negative starting sweeping voltages led to a reproducible NDR, making the hybrid material a promising candidate in memory devices. It was found that the introduction of DBC enhanced the ON/OFF current ratio and significantly improved the memory stability. The ON/OFF current ratio was up to 2 orders of magnitude. The write-read-erase-reread cycles were more than 10(6), and the retention time reached 10 000 s without current degradation.

Studies on enzymological properties of antibody elicited by meso-tetra(alpha, alpha, alpha, alpha-O-phenylacetyl benzene)porphyrin

meso-Tetra (alpha, alpha, alpha, alpha-O-phenylacetyl benzene) porphyrin was used as a complete antigen to elicit monoclonal antibody 1F2 through the immunization and cell fusion techniques. McAb 1F2 obtained was demonstrated very pure by HPLC and MALDI/TOFMS. The retention time of McAb 1F2 was 2. 63 min. The subtype of McAb 1F2 was IgG2a. The relative molecular weight was 156 678. 8. When the McAb 1F2-porphyrin was formed, the maximal absorption of the porphyrin soret region had a redshift from 408 to 416 nm and hyperchromical effect, showing that the antigen-antibody combination was rigid and intense, and the abzyme constancy was high. But compared with HRP, the activity of the abzyme was only 4. 687 5 U/mg and 1. 899 % of that of HRP. Its K-m was 20. 29 mmol/L, k(cat) 396. 82 min(-1), k(cat)/K-m. 1. 955 7 X 10(4) L . mol(-1) . min(-1).

New method for analysis of Chinese herbal complex prescription and its application

Traditional Chinese medicine (TCM) is a great treasure of China, the analysis of which is an arduous task. The viewpoint that all chemical constituents of Chinese herbal complex prescription should be analyzed as a black box is elucidated for the first time. Intelligent multi-mode multi-column chromatographic system (IMMCC) with its hybrids is the basic method and HPLC Unified Method is the breakthrough for the black box analysis. Dang-Gui-Bu-Xue-Tang was selected as a typical TCM and a systematic separation method from non-aqueous mobile phase to pure water mobile phase was put forward in order to convert unknown sample to known sample. The a, c values and UV spectra of 66 components of Astragalus, 78 components of Angelica and 71 components of Dang-Gui-Bu-Xue-Tang were obtained. Intelligent optimization and peak identification method and software for complex samples were developed and the optimum multi-step multi-binary gradient curve of mobile phase for Astragalus was ascertained. The maximum error and minimum error of predicted retention time for all components of Astragalus are 8.62% and 0.05% respectively. All components of Astragalus were compared with those of Angelica and it is found that many components of Astragalus are the same as those of Angelica, while the contents of these components are different. Many components of Dang-Gui-Bu-Xue-Tang are also the same as those of Astragalus and Angelica with different contents.

On-line concentration of proteins in pressurized capillary electrochromatography coupled with electrospray ionization-mass spectrometry

Pressurized capillary electrochromatography (pCEC) and electrospray ionization-mass spectrometry (ESI-MS) have been hyphenated for protein analysis. Taken cytochrome c, lysozyme, and insulin as samples, the limits of detection (LODs) for absolute concentrations are 10(-11) mol (signal-to-noise ratio S/N = 3) with relative standard deviations (RSDs) of retention time and peak area, respectively, of less than 1.7% and 4.8%. In order to improve the detection sensitivity, on-line concentration by field-enhanced sample-stacking effect and chromatographic zone-sharpening effect has been developed, and parameters affecting separation and detection, such as pH and electrolyte concentration in the mobile phase, separation voltage, as well as enrichment voltage and time, have been studied systematically. Under the optimized conditions, the LODs of the three proteins could be decreased up to 100-fold. In addition, the feasibility of such techniques has been further demonstrated by the analysis of modified insulins at a concentration of 20 mu g/mL.

Deconvolution of overlapped peaks based on the exponentially modified Gaussian model in comprehensive two-dimensional gas chromatography

Comprehensive two-dimensional gas chromatography (GC x GC) has attracted much attention for the analys is of complex samples. Even with a large peak capacity in GC x GC, peak overlapping is often met. In this paper, a new method was developed to resolve overlapped peaks based on the mass conservation and the exponentially modified Gaussian (EMG) model. Linear relationships between the calculated sigma, tau of primary peaks with the corresponding retention time (t(R)) were obtained, and the correlation coefficients were over 0.99. Based on such relationships, the elution profile of each compound in overlapped peaks could be simulated, even for the peak never separated on the second-dimension. The proposed method has proven to offer more accurate peak area than the general data processing method. (c) 2005 Elsevier B.V. All rights reserved.

Resolution prediction and optimization of temperature programme in comprehensive two-dimensional gas chromatography

A model is developed for predicting the resolution of interested component pair and calculating the optimum temperature programming condition in the comprehensive two-dimensional gas chromatography (GC x GC). Based on at least three isothermal runs, retention times and the peak widths at half-height on both dimensions are predicted for any kind of linear temperature-programmed run on the first dimension and isothermal runs on the second dimension. The calculation of the optimum temperature programming condition is based on the prediction of the resolution of "difficult-to-separate components" in a given mixture. The resolution of all the neighboring peaks on the first dimension is obtained by the predicted retention time and peak width on the first dimension, the resolution on the second dimension is calculated only for the adjacent components with un-enough resolution on the first dimension and eluted within a same modulation period on the second dimension. The optimum temperature programming condition is acquired when the resolutions of all components of interest by GC x GC separation meet the analytical requirement and the analysis time is the shortest. The validity of the model has been proven by using it to predict and optimize GC x GC temperature programming condition of an alkylpyridine mixture. (c) 2005 Elsevier B.V. All rights reserved.