催化动力学光度法测定痕量钒(Ⅴ)的研究

研究了在 p H=4及没食子酸存在下 ,微量钒 ( )催化溴酸钾氧化邻苯二胺的动力学条件 ,建立了催化动力学光度法测定痕量钒 ( )的新方法。方法的测定范围为 0～ 0 .0 2 5 μg· 2 5 m L- 1 ,检出限为 1.18× 10 - 6 g·L- 1 ,相对标准偏差为 4 .6 3% (n=10 ) ,线性回归方程为△ A=2 5 .6 6 c(μg· 2 5 m L- 1 ) - 0 .0 15 7(r=0 .9997) ,表观摩尔吸光系数ε4 6 0 nm=3.2 7× 10 7L· m ol- 1 · cm- 1 。该法灵敏度高 ,选择性好 ,直接应用于水样和食品样中痕量钒( )的测定 ,结果满意     

分光光度法测定微量表面活性剂在油/水体系中的分配系数

测定微量阴离子表面活性剂浓度的分光光度法被推广到测定油相中的微量阴离子表面活性剂浓度,进而用于表面活性剂在油/水体系中分配系数的测定.两种情形下氯仿层的吸光度只取决于测量体系中自由阳离子表面活性剂的浓度,因此可用单一阳离子的标准曲线作工作方程.用该法测定油相和水相中的阴离子表面活性剂浓度,工作方程斜率不同,测量下限分别可达2.5×10-5 mol·L-1和1×10-6mol·L-1.     

Parameter Estimation for Periodically Stationary Time Series

Abstract. The innovations algorithm can be used to obtain parameter estimates for periodically stationary time series models. In this paper, we compute the asymptotic distribution for these estimates in the case, where the innovations have a finite fourth moment. These asymptotic results are useful to determine which model parameters are significant. In the process, we also develop asymptotics for the Yule–Walker estimates.     

4-(6′甲基苯并噻唑-2′-偶氮)-3,5-二氨基吡唑与钯显色反应的研究和应用

对6种苯并噻唑偶氮吡唑化合物的分析特性进行了探讨,着重研究了4—(6′—甲基苯并噻唑-2′-偶氮)-3,5-二氨基吡唑(MBTAP)与钯离子显色反应的光度性质。在非离子表面活性剂 Brij35存在下与钯离子形成橙红色的配合物。适宜的 pH 值范围为9.0～10.5.配合物的最大吸收波长为510nm,表观摩尔吸光系数为3.01×10~4L·mol~(-1)·cm~(-1)。钯在0～14μg/25mL,范围内服从比尔定律.显色体系可稳定11h。在柠檬酸存在下可消除 Fe~(3+)、Co~(2+)、Cu~(2+)、Ni~(2+)等离子的干扰。     

Study on the polymerization of ϵ‐caprolactam in the interlamellar spaces of [TEACOOH]–montmorillonite intercalations complex and its characterization

The polymerization of ?‐caprolactam between the interlamellar spaces of the [TEACOOH]–montmorillonite intercalations complex was attempted using Na–montmorillonite and 10‐carboxy‐n‐decyltriethylammonium bromide to achieve [TEACOOH]–polycaprolactam–montmorillonite, in which montmorillonite (inorganic polymer) is chemically bonded with the polycaprolactam (organic polymer). The results of X‐ray and IR analysis for the samples obtained after polymerization showed that the polymerization reaction has been successfully accomplished. For the purpose of studying the polymeric reaction product more precisely, we have isolated the polymerized product from the silicate layers and analyzed it with X‐ray diffractometer and IR spectrometer. Comparison of the results of X‐ray and IR analysis between the isolated polymer and the polymer that was synthesized by the reaction of ?‐caprolactam only with the organic cation without montmorillonite showed that both obtained polymers are the same compounds. © 2003 Wiley Periodicals, Inc. J Appl Polym Sci 88: 1904–1910, 2003     

Quantitative preparation of long chain thioethers from an oxo-trans-2-enoic ester and a 9,12-dioxo-trans-10-enoic acid

Branched-chain thioethers have been prepared from methyl 4-oxo-trans-2-hexadecenoate and 9,12-dioxo-trans-10-octadecenoic acid. The reagents involved in these preparations were mercaptoacetic and mercaptopropionic acids. The yields of these thioethers are almost quantitative.     

On a Mixture GARCH Time‐Series Model

Abstract. Recently, there has been a lot of interest in modelling real data with a heavy‐tailed distribution. A popular candidate is the so‐called generalized autoregressive conditional heteroscedastic (GARCH) model. Unfortunately, the tails of GARCH models are not thick enough in some applications. In this paper, we propose a mixture generalized autoregressive conditional heteroscedastic (MGARCH) model. The stationarity conditions and the tail behaviour of the MGARCH model are studied. It is shown that MGARCH models have tails thicker than those of the associated GARCH models. Therefore, the MGARCH models are more capable of capturing the heavy‐tailed features in real data. Some real examples illustrate the results.     

白细胞介素-10基因多拷贝表达盒的构建及在毕赤酵母中的表达

目的构建白细胞介素-10(IL-10)基因多拷贝表达盒,提高IL-10在毕赤酵母中的表达水平。方法体外构建重组表达载体αIL-10/pAO815,BamHⅠ和BglⅡ双酶切获得目的基因表达盒(AOX-αIL-10),再连接到BglⅡ酶切位点处,依次构建多拷贝重组载体n(AOX-αIL-10)/pAO815。从质粒pPIC9K上用NdeⅠ和SalⅠ双酶切获得Kan抗性基因,重组到多拷贝表达载体n(AOX-αIL-10)/pAO815上。重组载体n(AOX-αIL-10)/pAO815电转化毕赤酵母,PCR筛选含有IL-10基因的酵母转化子,甲醇诱导表达,对表达量高的转化子再次经重组载体n(AOX-αIL-10)/pAO815-Kan电转化,高浓度G418抗性筛选二次酵母转化子,使用甲醇诱导表达。ELISA测定IL-10含量,MC/9细胞测定IL-10活性。结果所构建的8拷贝表达盒的重组载体8(AOX-αIL-10)/pAO815和4拷贝表达盒4(AOX-αIL-10)/pAO815-Kan,转化子分泌表达IL-10水平最高,为(8.25±1.65)mg/L,比活性为1.465×105U/mg。结论已成功构建了高拷贝表达盒,并提高了IL-10在毕赤酵母中的表达水平。     

孔雀绿分光光度法测定炭素制品中微量铅的研究

采用分光光度法来测定炭素制品中微量铅的含量。经比较实验确定了该方法最佳的实验奈件。该方法操作简便、快速、检出限低、灵敏度高，是检测微量铅含量一种较理想的方法。     

新显色剂4—（2—苯并噻唑偶氮）邻苯二酚—钼（Ⅵ）—OP体系的分光光度研究

在ｐＨ５．０～５．７范围内，新显色剂４－（２－苯并噻唑偶氮）邻苯二酚（ＢＴＡＰＣ）与钼（Ⅵ）和非离子表面活性剂ＯＰ反应，形成稳定的、带负电荷的、紫红色三元胶束配合物。该配合物中Ｍｏ（Ⅵ）与ＢＴＡＰＣ的组成比为１∶２；其λｍａｘ为５６０ｎｍ，对比度（Δλ）为１２８ｎｍ；在２０℃、ｐＨ５．２和μ０．１时，配合物的表观稳定常数为３．０２×１０１０，表观摩尔吸光系数ε５６０为８．１１×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，真实ε５６０为７．６７×１０４Ｌ·ｍｏｌ－１·ｃｍ－１。钼含量在０～０．７２ｍｇ／Ｌ范围内遵从比耳定律。建议了配合物的结构。本法简便、快速、准确，用于合金钢试样中痕量或小量钼的测定，取得了满意的结果。