基质固相分散—高效液相色谱法测定玉米中痕量呋喃丹

本文研究了应用基质固相分散－高效液相色谱法测定玉米中痕量呋喃丹残留物的新方法，并讨论了应用ＭＳＰＤ技术进行前处理与传统残留分析的区别。本实验首次将ＭＳＰＤ技术用于玉米中呋喃丹残留物的高效液相色谱分析，并对定量检测条件作了详细的研究。     

基质固相分散—高效液相色谱法测定痕量异丙威和溴氰菊酯

研究了基质固相分散处理复杂样品技术与高效液相色谱法相结合测定食物中痕量异丙威和溴氰菊酯残留物的新方法，研究了ＭＳＰＤ技术进行实验条件并讨论了与传统残留分析的区别，首次将ＭＳＰＤ技术应用于水果，粮食等食物中异丙威和溴氰菊残留物的高效液相色谱分析，并对定量检测条件作了详细的研究。     

（PSF—PDMS—PHS）n／PSF共混物的相容性及表面组成

利用ＤＳＣ、ＤＭＡ、ＴＥＭ和ＸＰＳ对［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ／ＰＳＦ共混物的相容性及表面组成进行了研究．结果表明，ＰＤＭＳ在共混物表面的富集与ＰＳＦ均聚物和［ＰＳＦ－ＰＤＭＳ－ＰＨＳ］ｎ中硬段的相容性有关；ＰＤＭＳ在相容的共混物体系表面的富集与对应的多嵌段共聚物组成基本相近；不相容共混物体系表面ＰＤＭＳ的富集程度相对较高，当共混物本体中有机硅含量从１％增至５％，表面层ＰＤＭＳ的含量迅速增加，可达到嵌段共聚物中ＰＤＭＳ的含量．     

含有机硅三元多嵌段共聚物的研究5.含有机硅三元多嵌段共聚物的形态结构

利用ＤＭＡ，ＴＥＭ和ＳＡＸＳ对ＰＳＦ－ＰＤＭＳ－ＰＨＳｎ，ＰＳＦ－ＰＤＭＳ－ＰＨＥｎ，ＰＰＯ－ＰＤＭＳ－ＰＨＳｎ和ＰＨＳ－ＰＤＭＳ－ＰＢＥｎ四种三元多嵌段共聚物的形态结构进行了研究，结果表明，不同三元多嵌段共聚物中三种链段的相互作用情况不同，其动态力学性能和形态结构有很大差异，并与嵌段共聚物微相分离的几种基本形态不同，特别是通过ＴＥＭ在ＰＳＦ－ＰＤＭＳ－ＰＨＳｎ和ＰＰＯ－ＰＤＭＳ－ＰＨＳｎ中观察到清晰的互容界面相。     

反相高效液相色谱法半制备分离[T(4-MOP)PS4]卟啉的研究

本文研究了新水溶性５，１０，１５，２０－四（４－甲氧基－３－磺酸苯基）卟啉［Ｔ（４－ＭＯＰ）ＰＳ４］的反相高效液相色谱（ＨＰＬＣ）分离条件。采用ＳｈｉｍｐａｃｋＰＲＥＰ－ＯＤＳ半制备色谱柱，用含有１０ｍｍｏｌ／Ｌ四乙基碘化铵的乙腈－水（体积比２５：７５）为流动相，流速１８ｍＬ／ｍｉｎ，于４１８ｎｍ波长下检测。［Ｔ（４－ＭＯＰ）ＰＳ４］与合成中生成的杂质组分完全分离。经此制备的卟啉纯度高，已成功地应用于自来水样中微量钴、锌、铜离子的ＨＰＬＣ测定中。     

Ni-P/SiO2催化剂晶化过程及其加氢活性研究

采用化学还原法制备了负载型Ｎｉ－Ｐ／ＳｉＯ２非晶态合金催化剂,应用ＩＣＰ、ＢＥＴ、氢氧滴定法、ＸＲＤ、ＳＥＭ、ＸＰＳ研究了上述催化剂在高温晶化过程中的表面结构、表面形貌和表面电子态的变化。测定了Ｎｉ－Ｐ／ＳｉＯ２非晶态合金晶化前后对其液相苯甲醛加氢反应催化活性和选择性。并讨论了非晶态合金催化剂晶化过程中结构变化对催化性能的影响。     

聚二甲基硅氧烷／聚氨酯共混体系的增容作用（I）

采用二甲基硅氧烷－ｂ－乙二醇嵌段共聚物（ＤＭＳ－ｂ－ＯＥ）对聚二甲基硅氧烷／聚氨酯（ＰＤＭＳ／ＰＵ）共混体系的增容，重点研究了增容共混体系的微观形态结构和软科学性能之间的关系。扫描电子显微镜、动态力学分析和力学性能测试结果表明：ＤＭＳ－ｂ－ＯＥ对ＰＤＭＳ／ＰＵ具有优良的增容作用，改善了ＰＤＭＳ／ＰＵ共混体系的相容性，提高了该共混物的力学性能。其抗张强度由３．４ＭＰａ提高到７．６ＭＰａ。     

聚砜、聚二甲基硅氧烷、聚对羟基苯乙烯三元多嵌段共聚物的形态结构

利用动态力学分析（ＤＭＡ）．透射电子显微镜（ＴＥＭ）和小角Ｘ 光光散射（ＳＡＸＳ）对聚砜（ＰＳＦ）、聚二甲基硅氧烷（ＰＤＭＳ）和聚对羟基苯乙烯（ＰＨＳ）三元多嵌段共聚物ＰＳＦ—ＰＤＭＳ—ＰＨＳｎ的形态结构进行了研究．结果表明，ＰＳＦ—ＰＤＭＳ—ＰＨＳｎ的形态结构出现了许多新的现象，除具有微相分离的基本特征外，还出现双连续相双分散相的特征．在适当的嵌段长度和组成下，通过ＴＥＭ观察到一种新的特殊形态 蜂窝状形态结构，并在嵌段共聚物两相界面处直接观察到非常清晰的界面相．同时，对该形态的形成过程作了初步讨论．     

PVC／SBR／MBS三元共混合金的研究

对ＰＶＣ／ＳＢＲ／ＭＢＳ三元共混合金作了研究。在ＰＶＣ／ＳＢＲ体系中加入ＭＢＳ，ＰＶＣ的冲击强度可提高５．５倍，弯曲强度的保留率在８０％左右。电镜和ＤＤＶ测试表明ＭＢＳ的加入提高了ＳＢＲ对ＰＶＣ的相容性，增强了橡胶对ＰＶＣ的界面粘结力。     

聚四甲基亚苯基硅氧烷及其共聚物的亚微观结构与性能的关系

用ＳＡＸＳ法和偏光显微镜研究了ＰＴＭＰＳ均聚物和ＰＴＭＰＳ ＤＭＳ多嵌段共聚物熔体结晶的亚微观结构．结果表明ＰＴＭＰＳ和ＰＴＭＰＳ ＤＭＳ的亚微观结构参数，和球晶形态、晶体界面自由能表观积及基本物性参数等存在密切相关性．当ＤＭＳ含量为５０％时亚微观结构参数均显示一个转折变化过程，此时，球晶形态、晶体界面自由能、熔点、玻璃化温度和结晶度指数亦呈现一个突变过程．     

海水中铜锌铅镉的萃取-反萃取法同时提取-原子吸收光谱法测定

采用萃取-反萃取法同时提取出海水中Cu、Zn、Pb、Cd,Cu、Pb、Cd石墨炉法测定,Zn用火焰法测定.对样品的前处理方法和最佳仪器条件进行了研究,并通过加标实验验证了方法的可靠性.结果表明:萃取-反萃取法能完全满足海水中Cu、Zn、Pb、Cd的前处理要求,可节省一半前处理时间,有溶液稳定、环保、节省试剂等优点.     

溴酸钾滴定法测定铜冶炼烟尘中的砷含量

研究了测定铜冶炼烟尘中砷含量的溴酸钾滴定方法。对测定体系中的各共存元素进行研究,探讨了测定方法的各项测定条件,方法的相对标准偏差RSD为0.13%～0.61%,样品加标回收率在99.5%～100%,方法精密度高,准确度好,适用于铜冶炼烟尘中砷含量为1.00%～50.00%的测定。     

ICP-AES法测定塑料中镉含量的不确定度评定

介绍了用ICP-AES法测定塑料中镉含量的不确定度的评定方法.分析了测量不确定度的主要来源,对测试不重复性、工作曲线非线性、标准溶液、样品质量、定容体积等5个不确定度分量进行分析计算,最后合成ICP-AES法测定塑料中镉含量的相对标准不确定度为1.709%,并计算求得扩展不确定度.     

Determination of platinum and iridium in reforming catalysts by second derivative and absorptiometric spectrophotometry

Summary Investigations on the spectrophotometric determination of platinum as a complex formed by tin(II)chloride in hydrochloric acid are reported. The determination of platinum was found to be interfered with by iridium, because it also forms a complex with tin(II) chloride. The features of the derivative absorption spectrophotometry for the quantitative determination of platinum and iridium was also studied. The analytical application of the method for the determination of platinum and iridium in catalysts was investigated.     

Determination of Cysteine at Bismuth Nanostructure – Carbon Ionic Liquid Electrode by Square Wave Voltammetry

Bismuth nanostructure‐carbon ionic liquid electrode has been employed for sensitive determination of cysteine (Cys). Bismuth nanostructure was incorporated into the carbon ionic liquid electrode (CILE) and applied for determination of cysteine. An interaction was taking place between bismuth nanostructure and the thiol group of cysteine. The bismuth cysteinate complex oxidation potential occurred at more negative potential compared to the cysteine oxidation peak obtained at bare carbon ionic liquid electrode (CILE). Square wave voltammetry (SWV) was used for the determination of the cysteine and satisfactory results were obtained. The calibration curve was linear in the concentration range of 1 to 500 µM and 0.5–2 mM of Cys. A low detection limit of 0.5 µM was achieved for Cys. The electrode showed a good selectivity for determination of cysteine in the presence of other amino acids. The proposed electrode was satisfactory applied for the determination of cysteine in human serum plasma sample.     

Kinetic spectrophotometric determination of sulfide, using in-cuvette mixing and titration techniques with computerized data acquisition

In-cuvette mixing and titration techniques have been used for the kinetic determination of sulfide based on its inhibition effect on the oxidation of indigo carmine with hexacyanoferrate(III) in the presence of silver. The reaction was monitored spectrophotometrically by measuring the decrease in absorbance of indigo carmine at 612 nm. Both initial rate and fixed-time methods were applied to the in-cuvette technique. Using in-cuvette mixing, sulfide up to 1800 ng was determined and detection limit and relative standard deviation for the determination of 120 ng of sulfide were calculated as 23.0 ng and 1.59%, respectively. On the basis of the titration technique, the upper limit of determination was 25 μg of sulfide and detection limit and average relative standard deviation for the determination of 1 μg of sulfide were 0.025 μg and 4.95%, respectively. The effect of foreign ions on the sulfide determination was studied. The proposed methods were applied to the determination of sulfide in water.     

Chloride analysis in magnesium metal using ion chromatography with conductometric detection

A simple, rapid and accurate method for the determination of chloride in magnesium metal has been developed. The quantitative determination of chloride was accomplished by anion exchange chromatography with conductometric determination. A Metrosep Anion Dual 2 analytical column connected in series with a Metrosep RP guard column was used for chloride separation. A solution containing a mixture of 1.3 mM Na2CO3 and 2 mM NaHCO3 was used as eluent. The method requires a sample dissolution using nitric acid. The limit of detection for the determination of chloride is 50 mg kg(-1) and the relative standard deviation was 5% for the overall method. The recovery of chloride added was 99-102%. No interference was observed from either the closely eluting "system peak" or the nitrate peak in the determination of chloride.     

Study on Chemiluminescence System of Potassium Permanganate-Sodium Hydrosulfite-Aminopyrine

A new flow injection Chemiluminescence method for the determination of aminopyrine was studied. It is based on the chemiluminescence reaction of potassium permanganate-sodium hydrosulfite-aminopyrine. The main factors which affect the determination were investigated. Under the most favorable conditions. The linear range for the determination of amimopyrine was 2.0×10^-7~8.0×10^-5g/mL,the determination limit was 6.0×10^-8g/mL,the relative standard deviation was 1.8% for 11 mesurements to 4.0×10^-6g/mL aminopyrine standard solution. This method has been applied to the determination of aminopyrine in medicine.     

环氧琥珀酸(盐)测定方法探讨

本文以含0.1 mol/L盐酸的氯化镁饱和溶液为加成试剂,进行了环氧基测定的探讨,并考察了反应时间、反应温度对分析准确度的影响。实验结果标明,在反应温度60℃条件下,反应45 min后,分析相对误差降至1%以内;与离子色谱测定方法比较,其测定结果吻合,可用于工业化生产中环氧琥珀酸(盐)的测定。     

气相色谱法测定胰酶中的丙酮溶剂残留量

采用气相色谱测定了胰酶中残留的丙酮溶剂,并通过外标法定量分析其含量。气相色谱条件为:氢火焰离子化检测器(FID),DMF作为溶剂,DM-WAX色谱柱(30 m×0.53 mm×1μm),载气为氮气,进样口温度为200℃,检测器温度为300℃,柱温采取程序升温。气相色谱法检测丙酮的加标回收率为92.5%～98.0%,检出限(3S/D)为0.05μg/mL。