利用连续流动分析仪测定水溶肥料硝态氮的方法研究

探讨了利用连续流动分析仪测定水溶肥料中的硝态氮的方法。选择含腐植酸、有机、微量元素、大量元素等4类水溶肥料样品,采用水振荡浸提试样,利用连续流动分析仪对浸提液中硝态氮的含量进行测定,并与紫外分光光度计测定数据进行对比,探讨利用连续流动分析仪测定化学肥料中硝态氮含量可行性。结果表明,流动分析仪法的方法检出限为0.008 g/kg;加标回收率在93.2%~101%;测定结果的相对标准偏差在1.7%~8.3%;所得数据与紫外分光光度计测定结果对比分析,t检验结果表明两种方法无显著差异;两种方法测定数据之间拟合方程为y=0.9782x+0.0768,R²=0.9966。结果表明,连续流动分析仪测试速度快,试剂消耗量少,精密度和准确度满足要求,可用于水溶肥料硝态氮含量的分析测定。     

差示火焰光度法测定硼酸盐中钾和钠

研究了火焰光度法测定硼酸盐中钾和钠含量的方法.分别在0～100 mg·L-1和0～200 mg·L-1的浓度范围内,采用差示测量法测定样品中钾和钠含量.考察了硼对钾、钠测定的影响以及钾、钠的相互影响.与四苯硼钠重量法(国家标准)相比,方法测定钾含量相对误差的绝对值≤3.91%,t检验和F检验也表明两种方法无显著性差异.与原子吸收光谱法相比,方法测定钾相对误差的绝对值≤3.63%.测定钠含量相对误差的绝对值≤3.76%,t检验和F检验表明两种方法无显著性差异.钾、钠的加标回收试验结果分别在97.5%～102.5%和97.1%～99.1%之间.     

血脂生化检验中采用分级检验方法的检验效果观察

目的研究并探讨在血脂生化检验中采用分级检验方法的检验效果。方法选取2014年1月—2016年12月期间温州医科大学检验学院、生命科学学院实验室收集的160份血液标本作为研究对象,采取数字随机分组法随机分为两组,每组80份血液标本,对照组血液标本采用传统拉网式检验方法进行检测,观察组血液标本采用分级检验方法进行检测,比较两组血液标本的血脂生化检验结果。结果两组血液标本经血脂生化检验后,其总胆固醇、甘油三酯、高密度脂蛋白胆固醇比较,差异均无统计学意义(P0.05),但观察组的低密度脂蛋白胆固醇、载脂蛋白A-1、载脂蛋白B与对照组比较具有统计学差异(P0.05);阳性率方面,两组总胆固醇、甘油三酯、高密度脂蛋白胆固醇的阳性率比较无统计学差异(P0.05),而观察组低密度脂蛋白胆固醇、载脂蛋白A-1、载脂蛋白B的阳性率均高于对照组(P0.05)。结论在血脂生化检验中采用分级检验方法可有效提高血脂异常的检出率,有利于提高血脂生化检验的准确性。     

蒙古药阿木日－6中金属元素的原子光谱分析

测定了常用蒙古药阿木日－６中金属元素的含量，为将来进一步探讨该药中金属元素，特别是微量元素与其药效的关系以及准确检验此种药物提供了实验数据．     

蒙古药阿木日—6中金属元素的原子光谱分析

测定了常用蒙古药阿木日—6中金属元素的含量，为将来进一步探讨该药中金属元素，特别是微量元素与其药效的关系以及准确检验此种药物提供了实验数据。     

银盐法测定饮用水中砷的含量

为测定饮用水中砷的含量并探讨其最佳测定条件,用银盐法测定了饮用水中砷的含量,并改变温度、酸度、锌粒大小和加入量进行了实验.结果表明,测定饮用水中砷的含量的最佳条件是:最佳温度25℃,在50 mL测量液中加入1:1的硫酸4mL,5g锌粒.该法操作快速、简便,结果准确、可靠,加标回收率为98%-103%.     

盐碱法提取酵母核酸的工艺研究

对盐碱法提取酵母核酸进行了研究。结果表明,最佳提取条件为提取温度85℃,提取pH为7.5,NaCl的含量为6.5%,提取时间180 min,对酵母核酸的平均提取率达到5.70%。     

微量进样火焰原子吸收法测定高血脂患者血清中Ca,Mg,Cu含量及其统计分析

为降低血清用量,设计了简单的连续微量进样装置,每次进样量可准确控制在250～300μL,即提高试液利用率6～8倍。用微量进样原子吸收法对混合血清中Ca,Mg,Cu的含量进行了重复测定,求出测定的相对标准偏差分别为:4.5%(Ca),3.2%(Mg),5.8%(Cu),可完全满足测定要求。用此方法测定了无其他疾病单纯高血脂患者和正常人血清中Ca,Mg,Cu的含量,并用u检验,Kruskal and Wallis法及扩大的t检验对测定数据进行了统计分析,结果表明,高血脂患者与正常人对比,血清中Ca含量无差别;Mg含量较高;Cu含量较低,且TG值越高,血清Cu含量越低。此结果可为医学科研和临床提供参考。     

高硫煤镜质组热解过程中结构变化及有机硫形态变迁规律研究

用手选富集与离心分离相结合的方法,从两种全硫含量相近的新西兰煤(NXL;St,ad=1.84%)和山西煤(SX;St,ad=1.80%)中分离出高纯度镜质组。在高纯Ar气氛下,分别制备了300、500、700和1 000℃下的镜质组焦。用FT-IR研究了两种镜质组中的脂肪氢、芳香氢随温度的变化,结果表明,SX镜质组中脂肪氢的相对含量较高,在热解过程中活性高于同温度下的NXL镜质组;两种镜质组中的脂肪氢相对含量都随温度升高而降低,温度高于500℃时,SX镜质组中脂肪氢相对含量基本不变,当温度高于700℃时,NXL镜质组中的脂肪氢相对含量基本保持不变;热解过程芳香氢都表现出先增大后减小的趋势。用XPS研究了镜质组中的有机硫含量及形态随温度的变化,结果表明,SX镜质组中易分解的有机硫化物较多,在300℃以下即可分解完全;NXL镜质组中的有机硫化物分解完全在700℃左右,两种镜质组中的噻吩类硫的含量都随热解温度的升高而增加,砜类硫的含量随热解温度的升高而降低。     

130名哈萨克族牧民血清铁、血红蛋白含量与高血压关系的分析

为探讨乌鲁木齐南山130名哈萨克族牧民血清铁及血红蛋白含量与原发性高血压的关系,给哈萨克族原发性高血压的病因学研究提供科学依据,对这些牧民进行了血压测定和血清铁、血红蛋白含量分析。结果表明,130名哈萨克族牧民高血压检出率为53.3%;高血压组血清铁水平明显高于正常组(P=0.000);高血压组血红蛋白含量也明显高于正常组(P=0.004);进一步分析表明,高血压组男性和女性血清铁水平明显高于正常组男性和女性(P0.01和P0.001);血红蛋白含量高血压组女性较正常血压组女性高,差异有统计学意义(P0.05),而男性两组差异不明显。提示哈萨克族高血压患者血清铁和血红蛋白的含量与高血压的发生可能有关。     

荧光淬灭法溶解氧测定仪校准方法的研究

介绍了荧光淬灭法溶解氧测定仪的工作原理,探讨了该类仪器计量特性和校准方法,提出了校准项目和技术指标,零值误差(≤0.10 mg/L)、溶解氧浓度示值误差(±0.50 mg/L)、重复性(≤0.20 mg/L)、响应时间(≤60 s)。用该校准方法对某些荧光淬灭法溶解氧测定仪进行了校准,证明该法是可行的。     

A flow system for calibration of dissolved oxygen sensors

Well-defined oxygen standard solutions were obtained by the electrolysis of water in a coulometric oxygen generator. The generator was integrated into a flow system that includes the degassing of the carrier electrolyte, the generation of dissolved oxygen and the temperature control of the carrier electrolyte. The current efficiency of oxygen generation was found to be 100% by the Winkler titration method. Calibrations of a home made laboratory sensor and a WTW CellOx dissolved oxygen sensor have been made in a concentration range of 0.02 to 8 mg/L at temperatures from 5°C to 30°C. The calibration of the WTW sensor on water vapour saturated air was compared with the electrochemical calibration method. Both methods gave reliable results provided that the temperature equilibration between the sensor and the ambient air was successful. Received: 24 March 1997 / Revised: 15 May 1997 / Accepted: 15 May 1997     

流动注射分光光度法研究壳聚糖树脂吸附阴离子染料

利用流动注射分光光度法技术，跟踪观察交联壳聚糖树脂吸附阴离子染料的行为，讨论了外加氯化钠或甲醇以及温度等因素对吸附的影响。利用固－液相互作用方程，求取了吸附剂－吸附质相互作用能。实验结果表明，交联壳聚糖树脂吸附 子染料，其表观吸附速率常数随体系中氯化钠浓度或甲醇含量的增大而减小，随温度的升高而增大；交联壳聚糖树脂吸附酸性铬蓝K染料的表观活化能力26.095kJ/mol。     

Influence of temperature, electrical conductivity, power and pH on ascorbic acid degradation kinetics during ohmic heating using stainless steel electrodes

Degradation kinetics of ascorbic acid was determined in pH 5.7 buffer solution using an isothermal batch ohmic heater with stainless steel electrodes. Variables included in this study were temperature (40, 60 and 80 degrees C); power (0, 100,150 and 300 W); and electrical conductivity (varied using 0.25%, 0.5% and 1.0% NaCl). Ascorbic acid concentration was detected by using a HPLC technique. The results indicate that ascorbic acid degradation can be described successfully by a first order model during both conventional and ohmic heating. The Arrhenius relation showed negative values for temperature coefficient (E(T)) during most ohmic treatments, due to a combination of factors that may alter the reaction mechanism. In particular, it appears that at a given power level, higher electric field strengths are conducive to increased incidence of faradaic reactions. Increasing NaCl concentration appears to significantly influence reaction rates via its influence on dissolved oxygen, and through its participation in electrolytic reactions. Contrary to expectations, increasing temperature tended to significantly reduce reaction rate, likely due to decreased dissolved oxygen concentration at high temperature. The results indicate the importance of using inert electrodes in ohmic heating processes.     

基于四苯乙烯自聚集膜增强电化学发光灵敏检测溶解氧

该文发展了一种基于四苯乙烯(TPE)在电极表面自聚集增强鲁米诺电化学发光信号的新技术,并实现了溶解氧的定量测定。将TPE分子修饰至金电极表面,在室温下形成多孔隙、无定形的聚集态自组装薄膜,有效增加了电极比表面积与孔隙的协同作用,高效捕获氧气分子O_2与超氧阴离子自由基O■,使鲁米诺的电化学发光信号得到显著增强。TPE修饰电极具有较高的稳定性与较好的重现性。利用氮气排除氧气,可改变鲁米诺电化学发光强度,进而测定溶液中溶解氧的含量。研究显示,通氮时间(1～6 min)与溶解氧浓度在1.63～0.190 mg/L范围内呈良好线性关系,相关系数(r~2)为0.990 9,溶解氧初始浓度的最低检出限为1.89 mg/L。方法操作简单、检测快速、信号变化灵敏,为溶解氧的灵敏检测提供了新方法。     

Epoxidation of styrene–butadiene–styrene block copolymer and use for gas permeation

The epoxidation of styrene–butadiene–styrene triblock copolymer (SBS) by an in situ generated peracid method is discussed. The presence of an acid acting as catalyst led to side reaction. The reactivities of internal double bonds (the 1, 4-structure) were higher than those of the vinyl bonds (the 1, 2-structure). In the 1, 4-structure, the reactivities of cis-structure were higher than those of trans-structure. The oxirane weight content and total oxygen weight content were determined by titration and element analysis, respectively. The cohesive energy, solubility parameter, and the glass transition temperature of epoxidized SBS increased with increasing total oxygen weight content. But the molecular weight between crosslinking points decreased resulting in an increase of crosslinking density with increasing total oxygen weight content. The changes of properties of epoxidized SBS reduced the gas permeability of oxygen and nitrogen through epoxidized SBS membrane, but increased the gas selectivity between oxygen and nitrogen. When the operating temperature of gas permeation was increased, the permeability of oxygen and nitrogen increased but the selectivity decreased. For epoxidized SBS containing 7.35 wt % oxygen content, the activation energy was 9 and 12.2 kcal/mol for oxygen and nitrogen, respectively.     

Effect of Preparation Method on the Structural Characteristics of NiO-ZrO2 Oxygen Carriers for Chemical-looping Combustion

Chemical-looping combustion(CLC) offers an effective approach for power generation and CO₂ capture. In this work, an NiO-ZrO₂ oxygen carrier prepared by three methods was subjected to an optimal reaction temperature test, an optimal flow test and a cyclic redox reaction test to explore the most suitable reaction conditions. Through comparative analysis, it is noted that the coprecipitation method is not suitable for the preparation of this NiO-ZrO₂ oxygen carrier, while the oxygen carrier prepared by the mechanical mixing method and solution combustion method obtained a higher CH₄ conversion rate and CO₂ selectivity. In addition, these two oxygen carriers also showed high stability during successive CLC testing. Therefore, both the mechanical mixing method and the solution combustion method can be used to prepare NiO-ZrO₂ oxygen carriers.     

碘量法与电重法测定氧化铜矿中酸溶铜的方法比较

试料用含亚硫酸钠的硫酸(10%)溶液浸取,使铜的氧化物矿物选择溶解,过滤后加入溴饱和盐酸掩蔽砷和锑等金属,补加少量硫酸,蒸干后用硫酸溶解,用硫代硫酸钠标准溶液滴定测定氧化铜矿中酸溶铜的含量,此方法快速、稳定、准确。选取14个日常分析的样品进行测定,其结果与电解重量法比对,结果令人满意。     

重铬酸钾滴定法测定废杂铜中的铁含量

研究了废杂铜中铁含量的测定方法。试料采用盐酸、硝酸、高氯酸溶解,加入过量氨水生成氢氧化铁沉淀与铜、铬等干扰元素分离,沉淀用热盐酸溶解后,用氯化亚锡还原至溶液呈浅黄色,重铬酸钾滴定法测定铁含量。探讨了溶样方式、氯化铵用量、氨水过量的体积、硫磷混酸用量对测定结果的影响。对4个废杂铜样品中的铁含量进行测定,测定结果的相对标准偏差RSD(n=11)为0.38%～0.95%,加标回收率为99.4%～100%,方法准确可靠,能够满足测定要求。     

Method for simultaneous luminescence sensing of two species using optical probes of different decay time, and its application to an enzymatic reaction at varying temperature

Chemical sensing, imaging and microscopy based on the use of fluorescent probes has so far been limited almost exclusively to the detection of a single parameter at a time. We present a scheme that can overcome this limitation by enabling optical sensing of two parameter simultaneously and even at identical excitation and emission wavelengths of two probes provided (a) their decay times are different enough to enable two time windows to be recorded, and (b) the emission of the shorter-lived probe decays to below the detectable limit while that of the other still can be measured. We refer to this new scheme as the dual lifetime determination (DLD) method and show that it can be widely varied by appropriate choice of probes and experimental settings. DLD is demonstrated to work by sensing oxygen and temperature independently from each other by making use of two probes, one for oxygen (a platinum porphyrin dissolved in polystyrene), and one for temperature [a europium complex dissolved in poly(vinyl methylketone)]. DLD was applied to monitor the consumption of oxygen in the glucose oxidase-catalyzed oxidation of glucose at varying temperatures. The scheme is expected to have further applications in cellular assays and biophysical imaging. Figure Principle behind the dual lifetime determination (DLD) method