N,O-羧甲基壳聚糖的合成和性质研究

采用多段升温法将壳聚糖改性,合成了取代度为1.84、平均分子量为3.08×105、等电点为7.28的N,O-羧甲基壳聚糖(CMC),分别用紫外光谱、红外光谱、荧光光谱对其结构进行了表征,并对其水溶液的Zeta电位、电导率、表面张力以及水分散体系中羧甲基壳聚糖微粒的粒径分布进行了研究.结果表明, N,O-羧甲基壳聚糖具有表面活性;介质的pH值和浓度对羧甲基壳聚糖溶液的稳定性有很大的影响.     

用计算全息法检测卡塞格林系统主镜

为实现对卡塞格林光学系统中的非球面主镜表面面形的高精度检测,设计了一种二元位相型计算全息图(CGH)。介绍了工作原理,对CGH的相位模型参数的优化设计、衍射次级分离以及台阶位置与深度计算等关键问题进行了讨论。通过引入虚拟玻璃的概念快速建立非球面检测模型,针对卡塞格林系统主镜中心开孔的特点,通过加入同轴载波实现了衍射次级的完全分离,相比目前常用的倾斜载波方法简化了相位量化复杂度,数值仿真计算出了最优的台阶深度,降低了加工难度。给出了相应的设计方法及实例,研制投产了CGH。测试得到主镜面形的均方根误差为0.018λ,并与传统补偿器结果(RMS=0.019λ)进行对比,两者测试结果吻合,验证了该设计与检测方法的正确性,该设计方法简单快捷,适用于卡塞格林光学系统主镜面形检测。     

Wastewater treatment using nanomaterial quaternary photocatalyst ZrCdPbO4 - Removal of colour pollutant by an eco friendly process

Pollution of environment is a major issue and has drawn attention of researchers throughout the globe. Water is polluted by various means like excretion of various industries and house releases, for example release of yarn, paper, and cloth industries etc. Present investigation consists of removal of such a pollutant. For this, synthesis of a novel quaternary nano particle sized photocatalyst ZrCdPbO₄ is carried and its characterization by different analytical techniques is also carried out. This is further used for removal of colour pollutants from the environment and Erythrosine-B is considered as a role model. Effect of various operational parameters like pH, concentration of dye, amount of photocatalyst, irradiation power etc. is studied, maximum degradation condition is extracted, and it is observed that reaction follows pseudo first order kinetics. Scavenger study suggests the participation of OH free radical in the reaction. Complete degradation of the dye in presence of light and photocatalyst is reported here by. Reusability of the photocatalyst is tested and is found to work up to five cycles efficiently.     

水性聚氨酯的制备及其性能的研究

本文以琥珀酸酐与三羟甲基丙烷反应,制得了含有羟基和羧基的酯类亲水性单体,并以此单体与ＴＤＩ和ＰＰＧ－１０００反应,制得了含有羧基的聚氨酯预聚体,在三乙醇胺水溶液中分散得到了水性聚氨酯（简称ＷＰＵ）。本文对预聚体的溶剂种类和用量,对乳胶粒的大小及形状的影响进行了研究,确认溶剂的用量越大,乳胶的粒径就越小;以丙酮作溶剂,乳胶粒为棒状或橄榄球状,而以丁酮为溶剂,得到的乳胶粒为圆球状。通过改变亲水单体的用     

On-line water removal during enzymatic triacylglycerol synthesis by means of pervaporation

Triacylglycerols can be synthesized from glycerol and fatty acids. During this equilibrium reaction water is produced, therefore a mixture of mono-, di- and triesters is obtained. One way to produce an excess of triacylglycerols is to remove the water produced during synthesis. This can be realized in an immobilized enzyme pervaporation system. The enzyme is immobilized onto the lumen side of a cellulose membrane where the organic phase is present. Air circulates at the shell side and the water activity is controlled with the use of a condenser. The lipase catalyzed esterification of decanoic acid and partial glycerides is studied in this reactor. The system is reaction limited. Only at low water activity conditions, an excess of triacylglycerols is obtained. The enzyme activity at the start of the experiments is independent of the water activity within the range studied. Stability is influenced: After 600 hours the activity is 26% of the activity at the start at a_w = 0.1 and 71% at a_w = 0.45.     

聚苯胺薄膜电极上示差脉冲伏安法可逆波理论研究

本文提出了聚苯胺(PANI)薄膜电极上示差脉冲伏安法可逆波理论,经验证理论和实验结果相符合.     

流动注射分光光度法测定矿物浸提液中的游离氰化物

在氢氧化钠介质中游离的氰化物与苦味酸钠反应生成玫瑰红酸钠，并进行升温改善反应条件。双流路系统与单流路相比，峰形规范、光滑，能有效消除鬼峰，优化了显色条件，工作波长为５１０ｎｍ。按生产工艺要求的线性范围为４．０￣４０．０ｍｍｏｌ／Ｌ。进样频率为１３０次／ｈ。已成功地用于矿物浸提液中游离氰化物的现场分析。     

An improved LCAO SCF method for three-dimensional solids and its application to polyethylene,graphite, diamond,and boron nitride

An improved semi-empirical self-consistent scheme is described for calculating the band structures of three-dimensional solids. The basic level is that of CNDO theory. The non-orthogonality of the Bloch functions is recognised and allowance is made for all degrees of involvement of the overlap matrix. The calculation of the electron-repulsion integrals is formulated in a way suitable for solid-state problems. The method is tested on the standard systems; polyethylene, graphite, diamond, and hexagonal and cubic boron nitride. It is found that the valence band properties are satisfactorily reproduced. For optical spectra a configurational interaction scheme is required.     

电位滴定法快速测定磷肥中的水溶性磷

建立了电位滴定法快速测定磷肥中水溶性磷含量的方法。用蒸饮水溶解磷肥中的水溶性磷,通过硝酸钡和阳离子交换树脂除去干扰离子,用六次甲基四胺-硝酸缓冲溶液制试液的酸度（pH=5.4),在乙醇体系中,用一定浓度的硝酸铅标准溶液进行电位滴定,用二阶微分法确定硝酸铅标准溶液的滴定终点体积。方法的RSD为0.66%-0.97%,回收率为100.00%-100.10%。     

单脉冲激波管中1,2-二氯乙烷的热裂解

在单脉冲激波管上,研究了1,2-二氯乙烷的热裂解.实验的激波条件为:温度区间1020 K＜T＜1190 K, 压力: P=0.12 MPa,实验时间τ=0.5 ms;实验气体为1,2-二氯乙烷稀释于Ar气中(3.95 mmol/L).以4-甲基-1-环己烯作为对比速率法实验的内标物,用4-甲基-1-环己烯开环反应的速率常数k=1015.3exp(-33400/T) s-1,以及从其产物的浓度推定出实验温度.经激波加热后的实验气体的终产物用气相色谱分析出主要成分为C2H3Cl,指示出主要反应通道为β消去反应.如把所有产物C2H3Cl都归于β消去反应,则可推定出表观之反应速率常数k1a=5.0×1013exp(-30000/T) s-1.对于由C-Cl键断键反应引发的链反应的可能影响做了分析研究.用了一种简便分析可推知在实验的温度范围内的低端(1020 K)链反应的影响可以忽略,而在其高端(1190 K)链反应将给出10%的终产物C2H3Cl的附加浓度,获得真实的β消去反应速率常数则必须把这部分予以扣除.经过这样的校正之后,最后得到CH2ClCH2Clβ消去反应速率常数为k1c=2.3×1013exp(-29200/T) s-1.     

山东省主栽果树生殖器官中稀土与微量营养元素的相关性研究

通过对山东省5大类主栽果树20余个树种的花粉、种子和果实稀土与微量元素自然含量进行分析比较, 认为稀土(RE)与微量元素在各树种花粉中平均含量顺序为Fe＞Zn＞B＞Cu＞Mn＞RE, 种子中B＞Fe＞Zn＞Mn＞Cu＞RE, 果实中Fe＞B＞Zn＞Cu＞Mn＞RE. 各元素在各生殖器官中的自然分布因树种而有很大差异. 但基本规律类同, 即花粉＞种子＞果实. 花粉富集各种微量营养元素的能力都很强. 花粉和果实稀土与微量元素之间绝大多数呈正相关, 种子大多呈负相关, 但相关性均不显著.     

Characterization of a urea optical sensor based on polypyrrole

A new optical sensor for urea determination is presented. It is based on the enzymatic reaction with urease, which is first photoimmobilized with polyacrylamide onto a chemically polymerized polypyrrole (PPy) film. The main advantage of this sensor is that no indicator dye or pH indicator is needed, because PPy itself acts as the support and the indicator. These PPy films show an absorbance spectrum in the near IR range which is pH dependent. The variation of absorbance is thus directly related to the change of pH caused during the enzymatic reaction, which is also dependent on the urea concentration. The linear range of the sensor is from 0.06 to 1 M of urea, which is the common level of urea concentration found in blood and urine samples.     

气相色谱内标法测定皮革中五氯酚残留量不确定度评估

采用气相色谱内标法测定皮革中五氯酚残留量,对整个测量过程的不确定度来源进行了分析,并对不确定度各个分量进行了评估和合成,结果显示,样品重复性测量不确定度分量对总不确定度的贡献最大。当五氯酚测定结果为1.021 mg/kg时,扩展不确定度为0.056 mg/kg。按照相关计量规范要求,给出了五氯酚测量结果不确定的表达式。     

非标记铕配合物荧光免疫分析法研究: 测定血清中的金属硫蛋白

本文报告一种新型非同位素免疫分析法, 非标记稀土铕配合物荧光免疫分析。它仍以免疫反应为基础, 所不同的是无须制备标记物。较标记免疫分析法简便、快速、在所建立的方法中, 金属硫蛋白(MT)的量与Eu-β-二酮配合物的荧光强度成负相关。测定范围为0-1.3μg/mL, 测定血清中MT的回收率为95%-100%, 相对标准偏差<10%。     

铅锡合金准二维电沉积的微结构研究

铅锡合金的准二维电沉积物具有伪共晶-固溶体双层结构.研究表明,这种奇特的结构是由生长界面上电流密度自发变化引起的.当生长界面处于整个沉积物前端时,电流密度大,铅和锡共同沉积形成伪共晶组织;当生长界面处于整个沉积物后端时,电流密度小,铅沉积成为主要反应,此时沉积物是含铅较多的固溶体组织.     

石墨炉原子吸收分光光度法测定大气颗粒物中的镉

将大气颗粒物样品采集在有机滤膜上(或滤筒中)，用硝酸、高氯酸消解，以石墨炉原子吸收分光光度法测定其中镉的含量。在0．00～8．00μg/L范围内对镉的质量浓度与吸光度数据进行回归，得线性方程为A：0．016 0．041X，相关系数r=0．9991，回收率为90％～94％，测定结果的相对标准偏差为2．1％～7．5％，检出限为0．366μg/L，该方法适用于大气和固定污染源排气中镉的测定。     

钕掺杂磷酸盐微晶玻璃的制备及表征

利用熔融和晶化技术制备掺钕磷酸盐玻璃陶瓷。 采用差热分析、X射线衍射、扫描电子显微镜、紫外 可见 近红外分光光度计及荧光光谱仪对材料进行表征和分析。 结果表明,在490～540 ℃核化1～2 h,在550 ℃晶化1～3 h,可制得主晶相为Al2SiO5的透明玻璃陶瓷。 其透过率可达69%,晶粒平均尺寸为90 nm,并随热处理时间的增加逐渐增大,但透过率降低。 由于Nd3+在热处理后进入到Al2SiO5晶相中,使荧光谱线在1 056 nm处峰值比原始玻璃强度大。     

由乳酸合成乳酸乙酯反应动力学的研究

研究了用强酸性阳离子交换树脂催化乳酸和乙醇酯化反应的动力学,通过对实验结果的分析,发现该反应正反应为二级反应,逆反应为零级反应,并由此推导出了反应动力学方程。同时还发现在温度较低时这一反应存在诱导期现象,并对这一现象进行了分析。     

渣油悬浮床加氢水溶性催化剂预硫化研究 Ⅱ 钼酸盐硫化产物的XPS分析

通过XPS分析法对钼酸盐的硫化行为进行了考察,分别考察了四价钼物种质量分数和硫钼元素的质量分数比，发现硫化产物的表面化学组成中四价钼质量分数和硫钼元素质量分数比不成正比，证实了该产物表面钼的硫化物不完全以MoS2形式存在。未经过临氢加热的硫化产物表面的四价钼物种的质量分数显著低于经过临氢加热的样品的质量分数，说明临氢加热在钼酸盐的硫化过程中起了重要作用。氯化铵是钼酸盐硫化过程中有效的助硫化剂，当它的用量增大时，硫化产物表面四价钼的质量分数也增大。以蒽为探针，使用化学探针法测定了硫化产物在渣油加氢过程中的催化活性，发现随着氯化铵用量的增加，产物的催化活性也相应提高，印证了XPS测定结果。     

Selective and sensitive detection of nitrite based on NO sensing on a polymer-coated rotating disc electrode

A new effective way of nitrite detection in complex samples is presented. It is based on chemical conversion of nitrite to nitric monoxide (NO) in acidic aqueous solution containing hexacyanoferrate(II) as a reductor. NO is then detected on a poly-eugenol coated platinum electrode. When the electrode is rotating and the reduction medium is continuously purged with nitrogen, the addition of a nitrite-containing sample produces narrowed current spikes. The peak current is proportional to nitrite content in the sample over the range of 5.0–100 μM and detection limit is 0.6 μM. The method is simple and highly reproducible. Relative standard deviation of 10 repetitions is less than 4%. Practical utility of the proposed approach is demonstrated by nitrite determination in human saliva.