同位素稀释高分辨气相色谱-高分辨质谱法检测烟道气中的低氯代二恶英

建立了同位素稀释高分辨气相色谱-高分辨质谱检测烟道气中痕量低氯代二恶英的分析方法。采用索氏提取富集烟道气样品中的目标物,提取液经过复合硅胶柱和碱性氧化铝柱净化后,进行高分辨气相色谱-高分辨质谱检测。采用DB-5MS毛细管色谱柱（30 m×0.25 mm×0.25 μm）分离,以保留时间和同位素特征离子丰度比定性,以与同位素的峰面积比值定量。实验结果表明,方法的回收率为66.6%~112.5%,相对标准偏差（RSD）的范围为19.9%~40.5%（n=5）,方法的检出限（LOD）为0.027~0.485 μg/L。应用该方法检测了3个焚烧炉烟道气样品,回收率在85.7%~137.0%范围内,样品中目标物含量分布在11.4~9183 pg/Nm³之间。结果表明该方法适合用于烟道气中痕量低氯代二恶英的检测。     

高效PLOT碳分子筛石英毛细管柱的研制及其性能研究

选用碳分子筛作吸附剂 ,用液相沉淀法涂渍出高效PLOT碳分子筛石英毛细管色谱柱 ,并对其色谱性能进行了考察。结果表明 ,该色谱柱具有良好的分离特性 ,1次进样可分离出O2、N2、CO、CO2、CH4、C2H2、C2H4、C2H6 等组分;适用于炼厂气、烟道气、水煤气及变压器油溶解气等的分析。     

FCC硫转移复合助剂的研究

以Mg-Al元素为基础,引入Fe、稀土等元素,制备了一系列FCC（流化催化裂化）液体硫转移复合助剂,负载于FCC平衡剂上,得待评价的催化剂。利用工业模拟装置考察了复合助剂降低FCC烟道气和FCC产品油总硫质量分数的效果。结果表明,同时加入稀土、Fe元素的复合助剂在烟道气和汽油中的降硫效果都较好,经热重仪分析发现,稀土,Fe元素的加入加强了复合助剂吸附氧并转化为结晶氧的能力,使SO2更易被氧化吸收,达到脱硫目的。此复合助剂在烟道气中最高脱硫率可达85.7%,FCC产品油的最高降硫量达到15.8%。通过酸性数据分析和产品油分布对比实验,发现加入少量复合助剂,对FCC催化剂活性和选择性均无不良影响。     

Determination of Speciation of Antimony in Fly Ash by HG-AFS

以某垃圾焚烧厂焚烧炉产生的烟道气为研究对象,采用酒石酸提取,对烟道气中Sb形态进行了分析,用HG - AFS分别测出样品中Sb(Ⅲ)和总Sb的量,差减法得到Sb(Ⅴ)的量.结果表明,Sb(Ⅲ)和总Sb检出限分别为0.13μg/L和0.11μg/L,相对标准偏差(RSD,n=11)分别为5.8％和6.3％,加标回收率在84.8％～113％.     

有机聚合物整体柱及其在生物大分子色谱分离中的应用

整体柱是近年发展起来的一种新型的色谱分离分析技术，与传统的色谱柱相比，具有制作简单、背压低、分辨率高、柱容量大等优点。本文介绍了有机聚合物整体柱及其在生物大分子色谱分离领域的应用，分析了其存在的问题，并展望了其应用前景。     

HG-AFS测定垃圾焚烧炉烟道气中锑的形态

以某垃圾焚烧厂焚烧炉产生的烟道气为研究对象,采用酒石酸提取,对烟道气中sb形态进行了分析,用HG-AFS分别测出样品中Sb（Ⅲ）和总Sb的量,差减法得到Sb（V）的量。结果表明,sb（Ⅲ）和总sb检出限分别为0．13μg／L和0．11μg/L,相对标准偏差（RSD,n=11）分别为5．8％和6．3％,加标回收率在84．8％-113％。     

锥型与圆柱型液相色谱制备柱的比较研究

用可视化柱上图形分析对入口内径大于出口内径的锥型液相色谱制备柱的样品谱带流型进行了研究。在一定的实验条件下，锥型柱与圆柱型柱的流动相流型曲线相反。对与锥型柱有相同长度、相同容积的圆柱型色谱柱的柱效、样品容量及峰高的比较研究表明：锥型柱优于圆柱型柱。锥型柱的样品容量约为圆柱型柱的2倍，柱效比圆柱型的高36％，色谱流出曲线峰值高于圆柱型柱12％。     

煤制活性焦性质对其脱除烟道气中二氧化硫性能的影响

讨论了四种煤制活性焦的性质对其脱除烟道气中SO2性能的影响,活性焦的表面碱性与微孔面积决定了其对烟道气中SO2的吸附与氧化。生成的硫酸主要贮存在活性焦的微孔内。活性焦内的硫酸在脱附温度为300℃时达到最大脱附速率。     

类水滑石复合氧化物在烟道气催化脱SO2、脱NOX方面的研究进展

以类水滑石为前驱体的复合氧化物作为环境友好的催化材料，在烟道气催化脱SO2、脱NOx方面具有抗水蒸气中毒能力强等特性。本文综述了类水滑石复合氧化物在这方面的特点和最新研究进展。     

石英Al2O3 PLOT柱在油气化探中的应用

报导了采用石英Ａｌ２Ｏ３ＰＬＯＴ柱分析油气化探样品的组成，在同一色谱条件下，该柱既能用于野外采样后现场直接分析游离烃，又能在室内分析酸解烃。具有分析周期短，重复性好，柱寿命长等优点，为石油勘探取样迅速准确的分析发挥了重要作用。     

气相色谱法测定黑色PMMA燃烧产物中的一氧化碳和二氧化碳含量

利用气相色谱法检测黑色PMMA完全燃烧烟气中的常量二氧化碳和微量一氧化碳,建立了双气路双检测器的检测方法。恒定色谱柱温度,通过定量管进样,Poropak T色谱柱预分离后,采用阀切换及柱反吹技术使不同组分分别流入5A分子筛色谱柱和Poropak N色谱柱中。5A分子筛色谱柱用于分离一氧化碳,经Ni催化甲烷化转化后用FID检测器测定;Poropak N色谱柱分离二氧化碳后进入电导检测器测定。采用峰面积法建立标准曲线,一氧化碳和二氧化碳的线性相关系数分别为0.999 9和0.999 6。用该法测定标准气体,其测定值与标准值的相对误差小于2%,测定结果的相对标准偏差小于1%。该方法可用于烟气毒性的分析。     

Constrained photophysics of an ESIPT probe within β-cyclodextrin nanocavity and chaotrope-induced perturbation of the binding phenomenon: implication towards hydrophobic interaction mechanism between urea and the molecular probe

Geological sequestration of pure carbon dioxide (CO(2)) in coal is one of the methods to sequester CO(2). In addition, injection of CO(2) or flue gas into coal enhances coal bed methane production (ECBM). The success of this combined process depends strongly on the wetting behavior of the coal, which is function of coal rank, ash content, heterogeneity of the coal surface, pressure, temperature and composition of the gas. The wetting behavior can be evaluated from the contact angle of a gas bubble, CO(2) or flue gas, on a coal surface. In this study, contact angles of a synthetic flue gas, i.e. a 80/20 (mol%) N(2)/CO(2) mixture, and pure CO(2) on a Warndt Luisenthal (WL) coal have been determined using a modified pendant drop cell in a pressure range from atmospheric to 16 MPa and a constant temperature of 318 K. It was found that the contact angles of flue gas on WL coal were generally smaller than those of CO(2). The contact angle of CO(2) changes from water-wet to gas-wet by increasing pressure above 8.5 MPa while the one for the flue gas changes from water-wet to intermediate-wet by increasing pressure above 10 MPa.     

水泥干法窑尾烟气中二氧化硫测试方法比对研究

针对水泥干法窑尾排放烟气的特点,采用非分散紫外吸收法、定电位电解法与在线CEMS系统常用的非分散红外吸收法对烟气中SO2进行现场比对测试。测试结果表明,非分散紫外吸收法能够较好地避免烟气中CO对SO2监测的干扰,其测定结果与非分散红外吸收法测定结果差异较小,而定电位电解方法与非分散红外吸收法测定结果差异较大。非分散紫外吸收法适用于水泥干法窑尾高CO浓度条件下低浓度SO2的测试。     

丙烯氨氧化合成丙烯腈过程中的尾气分析

在丙烯氨氧化合成丙烯腈过程中，尾气内含有因反应而生成的ＣＯ２，ＣＯ，Ｃ２Ｈ４，未反应完全的Ｃ３Ｈ６，Ｏ２和不参与反应的Ｎ２以及丙烯原料气中少量的Ｃ３Ｈ８。使用含有双阀、双检测器、双色谱柱的气相色谱系统可使上述所有气体得到分离，而且分离效果好，定量准确，操作简单，实用性强     

Determination of carbon monoxide,methane and carbon dioxide in refinery hydrogen gases and air by gas chromatography

This paper illustrates a method for determining trace amounts of CO, CH4 and CO2 with the detection limit of 0.15, 0.15 and 0.20 microg/l, respectively, in refinery hydrogen gases or in air. A simple modification of a gas chromatograph equipped with a flame-ionization detector is presented. A Porapak Q column, additionally connected with a short molecular sieve 5A packed column and a catalytic hydrogenation reactor on the Ni catalyst have been applied. The principle of the analytical method proposed is the separation of CO from O2 before the introduction of CO to the methanizer. The analytical procedure and examples of the results obtained have been presented. The modification applied makes it possible to use the GC instrument for other determinations, requiring utilization of the Porapak Q column and the flame-ionization detector. In such cases, the short molecular sieve 5A column and the methanizer can be by-passed.     

六氟化硫中痕量一氧化碳和二氧化碳的气相色谱检测及其在断路器故障分析中的应用

为了准确分析高浓度SF₆中痕量的CO及CO₂,发展了可靠的气相色谱-火焰离子化检测器（GC-FID）方法。通过双Porapak Q色谱柱结合阀切换将SF₆从待测样品中分离并排出检测系统,从而避免SF₆可能造成的在线转化柱中毒现象,同时实现CO和CO₂的完全分离;通过在线镍催化将CO和CO₂的检测转化为对CH₄的检测,极大地提高检测灵敏度。结果显示,该方法对CO和CO₂的检测互不干扰,两者都可在2~500 μL/L范围内呈现良好的线性相应,测定重复性好（RSD小于2%）,准确度高。建立的GC-FID方法可直接用于SF₆高压断路器中痕量CO及CO₂的检测,为SF₆相关电气设备潜伏性故障诊断提供了研究手段。     

Temperature programmed decomposition studies: high-sensitivity determination of carbon monoxide,carbon dioxide and methane by gas chromatography

Carbon monoxide, carbon dioxide and methane, evolved in very low amount during temperature programmed decomposition of transition metal cluster catalysts, can be determined quickly (<3 min) by gas chromatography on a Porapak S column. Catalytic conversion of the CO and CO₂ to methane makes it possible to use a hydrogen fiame ionization detector. The advantages are that the limit of detection is about 1 ppm (ca. 4.4 × 10^?11 mol cm^?3, STP) and that the procedure is applicable to decompositions studied in helium/oxygen or other reactive gas mixtures.     

电厂废气中饱和水蒸气对活性炭变压吸附捕集CO2的影响

由于热电厂废气中含有高湿饱和水蒸气,选用疏水材料活性炭为吸附剂,利用真空变压吸附技术研究了活性炭分离电厂废气中水蒸气和二氧化碳的可行性和优越性,研究了水对CO₂捕集的影响。实验分析表明,水在活性炭上的“S”型等温吸附曲线有利于真空条件下被解吸。同时,圆锥模型描述了水蒸气在吸附床内的浓度分布。结果表明,即使水蒸气可以被活性炭吸附,但它的存在不影响CO₂的捕集。每个循环操作可在相对较短的解吸时间和较高的解吸压力下完成。实验中单床三步变压吸附工艺可以使CO₂回收率高达80%,CO₂纯度达43%。     

Stability effects on CO2 adsorption for the DOBDC series of metal-organic frameworks

Metal-organic frameworks with unsaturated metal centers in their crystal structures, such as Ni/DOBDC and Mg/DOBDC, are promising adsorbents for carbon dioxide capture from flue gas due to their high CO(2) capacities at subatmospheric pressures. However, stability is a critical issue for their application. In this paper, the stabilities of Ni/DOBDC and Mg/DOBDC are investigated. Effects of steam conditioning, simulated flue gas conditioning, and long-term storage on CO(2) adsorption capacities are considered. Results show that Ni/DOBDC can maintain its CO(2) capacity after steam conditioning and long-term storage, whereas Mg/DOBDC does not. Nitrogen isotherms for Mg/DOBDC show a drop in surface area after steaming, corresponding to the decrease in CO(2) adsorption, which may be caused by a reduction of unsaturated metal centers in its structure. Conditioning with dry simulated flue gas at room temperature only slightly affects CO(2) adsorption in Ni/DOBDC. However, introducing water vapor into the simulated flue gas further reduces the CO(2) capacity of Ni/DOBDC.     

Methods to adjust for the interference of N2O on delta13C and delta18O measurements of CO2 from soil mineralization

In this paper we present an overview of the present knowledge relating to methods that avoid interference of N2O on delta13C and delta18O measurements of CO2. The main focus of research to date has been on atmospheric samples. However, N2O is predominantly generated by soil processes. Isotope analyses related to soil trace gas emissions are often performed with continuous flow isotope ratio mass spectrometers, which do not necessarily have the high precision needed for atmospheric research. However, it was shown by using laboratory and field samples that a correction to obtain reliable delta13C and delta18O values is also required for a commercial continuous flow isotope ratio mass spectrometer. The capillary gas chromatography column of the original equipment was changed to a packed Porapak Q column. This adaptation resulted in an improved accuracy and precision of delta13C (standard deviation(Ghent): from 0.2 to 0.08 per thousand; standard deviation(Lincoln): from 0.2 to 0.13 per thousand) of CO2 for N2O/CO2 ratios up to 0.1. For delta18O there was an improvement for the standard deviation measured at Ghent University (0.13 to 0.08 per thousand) but not for the measurements at Lincoln University (0.08 to 0.23 per thousand). The benefits of using the packed Porapak Q column compared with the theoretical correction method meant that samples were not limited to small N(2)O concentrations, they did not require an extra N2O concentration measurement, and measurements were independent of the variable isotopic composition of N2O from soil.