微波消解测定环境水样中化学需氧量的研究

本文介绍了一种在密闭容器内，进行微波消解、快速测定环境水样中化学需氧量的新方法，并研究了微波功率、消解时间、酸等因素对分析结果的影响。对不同水样的化学需氧量进行了测定，与标准Ｋ２Ｃｒ２Ｏ７回流法相对照，大大提高了分析速度，用Ｆ检验法及ｔ－检验法检验，没有显著性差异。     

水中总磷量的密闭微波增压消解快速测定

研究了用聚四氟乙烯密封带密封容器，利用微波加热技术，在较高的温度和压力下消解样品，快速测定环境水样中总磷量的方法；讨论了微波功率、微波消解时间、酸度等因素对测定结果的影响，与标准方法对照，经t检验法及F检验法检验，测定结果没有显著性差异，多次加标回收率在98％－103％之间，相对标准偏差≤1．3％，结果令人满意；该法具有操作简便、快速、不污染环境、宜于大批量样品的测定、便于推广普及等优点，可用于其它样品的分析测定。     

尿碘标准物质测量方法的评价

将快速尿碘试剂盒法和标准方法对尿碘标准物质的测定结果与其标准值比较，观测结果有无差异，再用正态分布小样本容量的简化检验法和方差检验法判定快速尿碘试剂盒法与标准方法对尿碘标准物质测定结果的差异，以评价不同方法对尿碘标准物质测定结果的一致性。     

钛硅分子筛的结构表征及催化性能研究

以ＴＰＡＢｒ为模板剂，氨水等为碱源合成了钛硅分子筛ＴＳ－１，并利用ＸＲＤ，ＩＲ，元素分析，ＵＶ－ＶＩＳ，热分析等手段对合成的分子筛进行了表征，通过丙烯环氧化反应合成的ＴＳ－１催化性能。结果结果，ＴＳ－１凝胶与产品的硅钛与基本一致；随着硅钛比的降低，ＴＳ－１由单斜晶系过渡为正交晶系，在硅钛比为１２９－１６．７的范围内，随着进入骨架的钛量增加，单胞体积增大；     

吡咯等离子体聚合产物分析

用色谱－质谱、裂解色谱－质谱、电子自旋共振、红外光谱及元素分析等方法鉴定了吡咯等离子体聚合过程中气相冷凝物和聚合物的组成，根据分析结果提出了吡咯等离子体聚合的自由基反应历程。     

等吸收点—多波长线性回归—导数分光光度法同时测定重油中的铜,镍,锌

本文提出了一种同时测定多组分的新方法，即等吸收点－多波长线性回归－导数分光光度法。利用金属离子－５－Ｂｒ－ＰＡＤＡＰ－ＣＰＢ三元络合显色体素，同时测定了重油中的铜、镍、锌，相对标准偏差小于２．６％，分析结果与ＩＣＰ－ＡＥＳ及ＧＦ－ＡＡＳ法吻合。与常规分光光度法比较，灵敏度提高１０倍左右。     

环境水样中无机阴离子的高效毛细管电泳分析

本工作着重研究了阳离子表面活性剂的种类、浓度、电解液的ｐＨ值等参数对高效毛细管电泳分离分析的影响。采用间接紫外分光光度检测法，在选择的最佳实验条件下，对环境水样中的Ｃｌ＾－离子和ＮＯ＾－３离子进行了分析。分析结果与用标准环境监测分析方法所测试的结果相比较，令人满意。     

量子化学的Gaussian－2理论及其应用与化合物的标准生成焓预测

本文较为全面地综述了Ｇａｕｓｓｉａｎ－１，Ｇａｕｓｓｉａｎ－２（简称Ｇ１，Ｇ２）理论以及简化的Ｇ２（ＭＰ２），Ｇ２（ＭＰ３）理论，将其主要结果进行了比较分析。关于Ｇ２理论的应用，除了较为详细地综述了几年来理论在重现实验数据、评价实验数据、预测实验数据及研究化学反应途径等方面的应用外，还结合我们近期研究结果的主要结论讨论了该理论在研究等电子－等自旋，价层等电－等旋，等旋及非等旋化学反应的能量计算中的应用情况，以及该理论在预测化合物的标准生成焓方面的应用情况。     

新型侧链液晶聚氨酯扩链剂的合成与表征

本文合成了用以制备侧链型液晶聚氨酯的扩链剂二醇－４（４－甲氧基苯酰氧基）苯甲酸－双（β－羟乙基）氨基乙酯（ＩＶ），并以ＨＮＭＲ。ＦＴＩＲ、元素分析等测试手段对此二醇进行了表征，测试结果与设定结构相一致     

对Al—4Ti—3La合金中微量镉测定方法研究

采用碳酸锶共沉淀富集火焰原子吸收法成功地测定了Ａｌ－４Ｔｉ－３Ｌａ合金材料中微量镉，其灵敏度、精密度、分析速度大为提高，检出限可至０．０２ｍｇ·ｍｌ＾－１。同时对载体选择、酸度影响、沉淀剂用量、沉淀放量时间以及共存离子的干扰等方面进行了较系统的研究。方法用于Ａｌ－４Ｔｉ－３Ｌａ合金材料中镉的测定，获满意结果。     

Analysis of siliceous materials and coal by atomic absorption spectrophotometry with fusion for sample decomposition

The oxalic acid-lithium carbonate-lithium tetraborate (1:1:1) fusion agent proposed previously for cement analysis is applied to determine the composition of various siliceous samples including granite, clay, flyash, sand and silica fume. For samples with silica content higher than 70%, the sample size had to be reduced from 0.10 to 0.01 g and a recovery factor was needed in silica determination to account for the precipitation of silica during acid dissolution. Attempt has also been made to determine the major metallic elements in coal by fusion directly without the ashing procedure, and the results obtained were good. Further, the ash content of coal was proposed to be determined by establishing a relation between the ash content and the sum of the concentrations of four major oxides (i.e. the oxides of Si, Al, Fe and Ca), and the proposed method is accurate and is time saving compared with that determined by direct ashing at 800 degrees C.     

高效液相色谱法分离测定生物样品中吲哚类荧光化合物

本文提出一种用于吲哚类荧光化合物分离测定的高效液相色谱方法。本法采用２个洗脱液、固定柱温及荧光检测，检测灵敏度可达ｐｍｏｌ／Ｌ级，方法重现性良好。适用于生物样品中吲哚类荧光化合物的测定，样品不需复杂的预处理，因而或节省时间，避免样品中微量成份的损失。     

电感耦合等离子体质谱法测定煤矸石中微量锗和镓

建立了测定煤矸石中微量锗和镓的电感耦合等离子体质谱法。煤矸石试样经高温灰化,用硝酸-氢氟酸-高氯酸-磷酸分解,以电感耦合等离子体质谱法测定其中的锗和镓。通过在线三通加入内标元素铑,消除非质谱干扰;通过选择干扰元素的异质同位素进行定量测定,采用数学公式在线校正,消除质谱干扰。与分光光度法进行比对,锗、镓测定结果的相对偏差为-0.63%~0.28%。克服了常规化学分析方法步骤繁琐、耗时长、工作量大的不足。该法测定结果的相对标准偏差小于3%(n=6),加标回收率为97.4%~102.5%。该方法具有检出限低、快速、简便、线性范围宽、多元素同时测定等优点,分析误差满足化学分析法的要求,可用于煤矸石中锗和镓的测定。     

气相色谱分析过程的计算机仿真模拟与优化

以色谱法的ＬＥＳ模型作为气相色谱分析过程的计算机仿真模拟与优化的理论基础，提出了把两次多阶程度升温实验保留时间作为基本数据进行模拟优化的方法，拓宽了模拟优化方法在复杂组分样品中的应用。软件编程采用了计算数学方法，提高了模拟优化的精度和速度，节省了分析样品的时间。     

Identification of olive pollen allergens using a fluorescence‐based 2D multiplex method

Olive (Olea europaea L.) pollen is a major health concern in the Mediterranean countries and some olive growing regions in America and Australia. The molecular variability of pollen allergens constitutes a handicap for commercial extract standardization, which is the base of current diagnosis and vaccination procedures. In this paper, we report a time‐saving and plant material saving multiplex detection method for the rapid and simultaneous analysis of Ole e 1, Ole e 2, and Ole e 5 allergen polymorphism on a single blot. This method combines high‐resolution 2DE techniques with high‐sensitive fluorescence‐based detection methods. Using this strategy, we were capable to identify a higher number of allergen forms compared with classical 1D approach. The use of fluorescent probes and the increased resolution of 2D blots avoided overlapping effects, and allow estimating the amount of individual allergen forms. In addition, the pattern and identity of the IgE‐reactive proteins of either a population or individual patients allergic to olive pollen was also effortlessly determined in a single additional step. This flexible method might be extended to a higher number of olive allergens and cultivars, and is also applicable to other allergogenic plant species and sources.     

微波消解-高分辨电感耦合等离子体质谱 (HR-ICP-MS)法测定煤炭中35种痕量金属元素

高分辨电感耦合等离子体质谱可以区分干扰元素和目标元素微弱的质量数差别,能解决大多数多原子、氧化物干扰问题,在煤炭痕量元素分析领域受到关注,但煤炭样品中痕量金属元素尤其是稀土元素受到的质谱干扰挑战未被系统地报道.采用HNO3-HF混酸微波消解煤炭样品,优化了消解时间、赶酸、复溶等前处理条件,研究了煤炭中V、Cr、Mn、C...     

A new electrochromatoscan method for the quantitative paper chromatography of amino acids

Summary A new electrochromatoscanning method has been developed for the quantitative analysis of micro-volume samples by paper chromatography. This method permitted the analysis of amino acid samples as small as 1 nmole. Amino acids such as -alanine, glycine, L-glutamic acid and L-aspartic acid in seaweeds were analyzed using this method.Studies on Porous Layer Electrochemistry Using Filter Paper. Part III.     

逐级酸处理对锡盟褐煤的结构及热解特性的影响

为了探讨高硫褐煤提质利用中酸洗处理对煤质特性的影响,以内蒙古锡盟褐煤为研究对象,依次用HF、HNO₃和HCl的酸溶液进行预处理,对原煤及其酸处理样品进行了傅里叶变换红外光谱的煤结构表征、程序升温差热-热重实验的煤热解特性研究及其反应过程的动力学分析。结果表明,HF处理对煤样的结构影响不大,HNO₃的处理明显改变了HF处理后煤样中有机质的结构,HCl处理又使HNO₃处理引起的煤样中脂肪基团CH₃的吸收峰强度变化减弱;逐级酸处理对锡盟褐煤的热解特性存在一定的影响,HF和HNO₃处理对褐煤的热解反应性具有促进作用,HCl处理对其热解反应性的影响不大。动力学分析显示,不同过程酸预处理对褐煤热解过程的影响不能单独采用热解过程的总包反应活化能进行描述,热解活化能不仅与指前因子存在着补偿效应,也与热解阶段的失重量存在一定的关联。     

Determination of mercury in mineral coal using cold vapor generation directly from slurries,trapping in a graphite tube,and electrothermal atomization

A rugged and reliable method for the determination of mercury in coal without sample digestion, based on chemical vapor generation (cold vapor technique) from slurried coal samples has been developed. It involves collection of the mercury vapor in a graphite tube, treated with gold or rhodium as permanent modifier, and determination by electrothermal atomic absorption spectrometry. Mercury quantitatively leached out of the investigated coal reference materials into 1 mol l⁻¹ nitric acid within 48 h when the coal was ground to a particle size of ≤50 μm, except for one sample (BCR 180), which had to be ground to ≤30 μm, or a leaching time of 72 h had to be used. No detectable quantity of mercury was generated directly from the slurry particles, but it was not necessary to filter the solution. The greatest advantage of the method is that only a minimum of reagents and sample handling steps are required, a prerequisite for accurate results in routine analysis. The results were well within the 95% confidence level of the certificate or close to the information value of the reference materials investigated. The characteristic mass of 110 pg obtained with gold as the permanent modifier is close to values reported for direct analysis of solutions, showing close to 100% trapping efficiency for mercury. A limit of detection (LOD) of 90 pg absolute was obtained with this modifier, which corresponds to an LOD of 0.009 μg g⁻¹ Hg in coal. This is based on 1 ml of slurry containing 10 mg of coal, and is an order of magnitude lower than the lowest mercury content in the investigated reference materials.     

Study on the structure and reactivity of COREX coal

COREX is the primary process in the current smelting reduction method. The process has strict coal quality standards. Combustion processes of coal used in the COREX operating system were analyzed using a synchronous thermogravimetric analyzer combined with a mass spectrometer. The microcosmic structure and macerals were observed by an electronic scanning microscope. The qualitative and quantitative determinations of oxygen functional groups, such as phenolic hydroxyl, carboxyl, carbonyl, and methoxy groups were detected by the Fourier Transform Infrared spectrometer (FT-IR) and through chemical analysis methods. In addition, the evolution of the chemical structure and transformation mechanism of organic oxygen functional groups during COREX coal combustion have been thoroughly investigated. This study proposes a new coal-requirement index system and coal blending method, which will increase the expansion of coal selection and decrease the overall usage of coal during COREX.