LF-NMR结合化学模式识别鉴别油脂种类及餐饮废弃油脂

应用主成分分析(Principal component analysis,PCA)和聚类分析法(Cluster analysis,CA)对9种(27个)常见食用植物油及100个餐饮废油的低场核磁共振(Low-field nuclear magnetic resonance,LF-NMR)(T2)弛豫特性数据进行分析。结果表明:在正常食用油种类区分方面,主成分分析的效果较优,9种食用油在主成分分布图上按种类正确分组,边界清晰。而在正常食用油与餐饮废油的区分方面,聚类分析效果较优,引入30个待测样本后,聚类分析(127个样品,欧式距离=5)的正确率为94.49%,分析误判率为5.51%,分组效果良好。LF-NMR结合化学模式识别可实现对油脂种类及餐饮废弃油脂的鉴别。     

凝胶净化–气相色谱法测定植物油脂中特丁基对苯二酚

采用凝胶净化色谱进行样品前处理,气相色谱法定量测定油脂样品中特丁基对苯二酚。研究了二次净化对测定结果的影响,结果显示在16.5~32.5 min进行二次净化,方法回收率在92.6%~94.1%之间,特丁基对苯二酚的检出限为1μg/m L,线性相关系数为0.999 8,4水平加标样品测定结果的相对标准偏差为2.34%~6.19%(n=6)。该法测量精密度和准确度满足方法学要求,适用于大批量植物油样品中特丁基对苯二酚的检测。     

气相色谱法测定学生用品胶黏剂中水分含量的样品处理

采用气相色谱法测定学生用品胶黏剂中水分含量，对样品处理条件进行优化。称取0.6 g样品和0.2 g异丙醇，置于预先加入玻璃珠的具塞玻璃瓶中，加入10 mL的N,N-二甲基甲酰胺，在摇床上以400 r/min速率震荡90 min，静置沉淀，取1μL上清液进行气相色谱分析。水的质量分数在5%～95%范围内线性关系良好，相关系数为0.999 8，方法检出限为3%。样品加标回收率为90%～110%，测定结果的相对标准偏差为0.11%～0.41%(n=6)。该样品处理方法操作简便，适合大批量样品检测，提高了检测效率，测定结果稳定、可靠。     

电化学预处理碳纤维电极用于毛细管电泳安培检测局部麻醉药

本文研究了电化学预处理碳纤维的各种条件,如处理电压、处理时间、处理后稳定时间、溶液条件等对局部麻醉药普鲁卡因、利多卡因电化学行为的影响.找出的电化学预处理最佳条件是在2.0V进行1.5min阳极化处理并在缓冲液中保持10min.普鲁卡因在pH=4~5之间,利多卡因在pH=6~7之间有较低的峰电位.运用最佳条件,普鲁卡因和利多卡因在毛细管电泳上5min内可获得很好的分离和检测.     

气相色谱法测定树脂工艺品中的半挥发性有机物残留

建立了树脂工艺品中半挥发性有机物(SVOCs)的超声萃取–气相色谱检测方法。对超声萃取条件进行了研究,优化了气相色谱参数。结果表明,样品用三氯甲烷在60℃下超声萃取40 min,选择HP–5色谱柱时,气相色谱(FID)测定半挥发物总量时可获得良好的灵敏度和准确的定量结果。方法的相对标准偏差小于5%(n=6),检测限为2 mg/kg。4个含量水平样品的6个实验室3次平行测定结果表明,实验室内测定结果的相对标准偏差为1.61%~2.94%,实验室间测定结果的相对标准偏差为5.96%~8.35%。     

甲烷动态反应-电感耦合等离子体质谱标准加入测定高纯钛中痕量铁

建立了电感耦合等离子体质谱(ICP-MS)快速测定高纯钛中痕量铁的方法。采用氢氟酸和硝酸溶解高纯钛样品,稀释、定容后直接进入ICP-MS检测;采用标准加入法消除基体效应,避免了离子交换、热水解沉淀等去除基体复杂的样品处理方式;以甲烷(CH_4)为反应气,在实际样品中优化确定了动态反应池的最佳工作条件,CH_4流量为0.7 L/min,低截取质量参数(RPq)为0.55,高截取质量参数(RPa)为"0",有效消除了ArO~+(m/z=56)对~(56)Fe~+的干扰。在确定的检测条件下,绘制了一高纯钛样品中的标准加入工作曲线,线性方程为y=2745.53x+1708.19,相关系数r~2为0.9999,此曲线可转换为"外标法"的校准曲线,线性方程为y=2745.53x+136.19,其它样品可在此曲线下检测,无需再进行标准加入操作,不会降低检测效率;方法的检出限和测定下限分别为0.029和0.097μg/g,精密度(RSD,n=11)小于7%,回收率为97.5%～106.0%。对3个实际高纯钛样品中痕量铁进行了测定,含量分别为0.53、0.96和4.74μg/g,测定过程及结果均表明本方法适用于高纯钛中痕量铁的快速准确测定。     

振荡浸提——原子吸收光谱法测定土壤中交换性钙镁

试验结果可知,取1 0份GBW0 7 4 1 6土壤标准样品在2 0℃左右条件下,在振荡机上浸提振荡3 0 min,采用原子吸收光谱法测定土壤中交换性钙镁.经精密度及正确度检验,该检测原理及检测过程的准确度水平符合要求.     

重金属离子富集检测的微量热研究

采用微量热技术对重金属离子的富集检测过程进行了研究. 采用流动注射分析法研究了重金属离子进样顺序、 样品进样流速和载体树脂颗粒粒径对重金属离子抑制脲酶催化反应的影响, 优化了脲酶及重金属离子进样量, 获得了脲酶固定化及重金属离子富集条件的优化参数. 结果表明, 在低流速(0.1 mL/min), 载体树脂颗粒粒径为0.5～0.6 mm, 脲酶进样量为3 mL, 重金属离子进样量为5 mL的条件下, 先进行重金属离子的富集, 再检测其对固定化脲酶催化反应的影响可得到较好的检测效果. 在实验浓度范围内, 4种重金属离子对脲酶催化反应的影响顺序为砷离子>铜离子>镉离子>铅离子. 本文对重金属离子进行了适当的富集, 降低其检测下限, 为采用微量热法进行重金属离子的快速检测提供了理论依据.     

气体中合成辣椒素的检测方法研究

研究了气体中合成辣椒素(OC)的固体吸附-气相色谱检测方法,建立了气体样品经XAD-2吸附后于CH_2Cl_2溶液中解析,采用毛细管色谱柱分离,FTD检测器进行检测的技术途径.色谱柱:HP-5;载气:高纯氮气(1.2 mL/min);进样口温度:250℃;检测器温度:280℃;程序升温:初始温度180℃,保持0.5 min后以30℃/min的速率升至250℃保持5 min;对影响样品采集和检测的条件进行了选择研究,方法平均回收率为91.5%;平均相对标准偏差为3.2%(n=6);对气态OC的最低检出浓度为10 μg/m~3;在5.0～1000.0 μg/mL范围内有良好的线形关系(r=0.9996).     

气相色谱-质谱联用法测定食品中3-氯丙醇酯及缩水甘油酯

建立了气相色谱-质谱联用同时测定多种植物油和油脂类食品中3-氯丙醇酯(3-MCPDE)和缩水甘油酯(GE)的检测方法。通过对样品提取、酯交换、衍生化和GC-MS检测条件的优化,植物油、奶粉、油炸膨化类食品以及焙烤类食品中3-MCPDE的定量下限分别为100、25、125、20μg/kg。方法的平均回收率为81.2%~109%,相对标准偏差(RSD,n=6)为0.77%~7.3%,样品在较宽的线性范围内呈良好线性关系,相关系数(r)大于0.999。采用该方法对30个食品样品进行了检测,其中3-MCPDE和GE的检出含量范围为未检出~8.04 mg/kg。该法具有高效、灵敏和可操作性强等特点,能够满足日常食品,特别是油脂和油脂食品中3-MCPDE和GE的定性及定量检测要求。     

Dichroism of absorption and polarization of phosphorescence of molecules of the closed form of nitrobenzospirothiopyran

The spectral-polarization characteristics of absorption and phosphorescence of molecules of the initial form of nitro-substituted indolinospirobenzothiopyran were studied in oriented polyethylene films and in solutions with different polarity. An oscillator model of the electron transitions responsible for the formation of absorption and luminescence spectra was suggested. It was established that the principal differences in the spectral and photophysical properties of the compound studied and its oxygen-containing analog are associated with the fact that the electronegativity of the S atom is lower than that of the O atom. Translated fromIzvestiya Akademii Nauk. Seriya Khimicheskaya, No. 6, pp. 1143–1146, June, 1997.     

非那雄胺合成工艺改进

非那雄胺能抑制5α-还原酶的活性,明显降低二氢睾酮水平,是一种治疗良性前列腺增生的有效药品。该合成工艺以甾烯酮酸为原料,将其与氯化亚砜反应,无须分离即与叔丁胺反应得17β-酰胺化合物,再氧化开环,环合,氢化,脱氢合成了非那雄胺。经元素分析、IR、1HNMR、13CNMR、MS分析表征了其结构。该法无须使用昂贵的2,2-二吡啶二硫化物和剧毒药品苯亚硒酸酐,且以乙酸铵代替氨气,降低了对设备的要求和腐蚀,更适用于工业生产。     

Synthesis of phenolic components of Grains of Paradise

Two vanilloids, (5E)-8-(4-hydroxy-3-methoxyphenyl)oct-5-en-4-one (1) and 4-[3-hydroxydecyl]-2-methoxyphenol (2), isolated from the dried seeds of Grains of Paradise (Aframomum melegueta), were synthesized; the latter compound was made as the S-enantiomer and the material derived from the seeds was found to be a 1:1.7 mixture of the R and S isomers. The synthetic route used should allow the preparation of analogs having extended alkyl chains and consequently different lipophilicity, and 3, a homolog of 2, was also prepared.     

Acid hydrolysis of carboxymethylcellulose of low degree of substitution

Cotton cellulose was swollen in a sodium hydroxide solution and carboxymethylated by a two-bath method for different periods of time for each process. The kinetics of acid hydrolysis and the crystallinity of the swollen and carboxymethylated samples were measured. The proportion of broken bonds, rate constants for hydrolysis, and permeability of cellulose to hydrolyzing agents were calculated. The susceptibility of glycosidic linkages to acid hydrolysis was improved by carboxymethylation more than by swelling in alkali. The increased accessibility of carboxymethylcellulose to acid was regarded as a consequence of increased intra-and intercrystalline swelling and of the glycosidic bonds' weakness caused by the electron-attracting carboxymethyl group on the C-6 position.     

Study of hydration of two cements of different strengths

Main hydration products of two cement pastes, i.e. CSH-gel, portlandite (P) (and specific surface S) were studied by static heating, and by SEM, TEM and XRD, as a function of cement strength (C-33 and C-43) hydration time (th) and subsequent hydration in water vapour.Total change in mass on hydration and air drying, M_o, increased with strength of cement paste and with hydration time. Content of water escaping at 110 to 220°C, defined as water bound with low energy, mainly interlayer and hydrate water, was independent on cement strength but its content increased with (th). Content of chemically bound (zeolitic) water in CSH-gel, escaping at 220-400°C, was slightly dependent on strength and increased with (th). It was possibly derived from the dehydroxylation of CSH-gel and AFm phase. Portlandite water, escaping at 400-500°C, was independent on cement strength and was higher on longer hydration. Large P crystals were formed in the weaker cement paste C-33. Smaller crystals were formed in C-43 but they increased with (th). Carbonate formated on contact with air (calcite, vaterite and aragonite), decomposed in cement at 600-700^oC. It was high in pastes C-33(1 month) and C-43(1 month), i.e. 5.7 and 3.3%, respectively; it was less than 1% after 6 hydration months (low sensitivity to carbonation) in agreement with the XRD study showing carbonates in the air dry paste (1month), and its absence on prolonged hydration (6 months) and on acetone treatment. Water vapour treatment of (6 months) pastes or wetting-drying increased this sensitivity.Nanosized P-crystals, detected by TEM, could contribute to the cement strength; carbonate was observed on the rims of gel clusters.This revised version was published online in November 2005 with corrections to the Cover Date.     

恶臭嗅辨实验室建设探讨

针对恶臭测试的环境影响问题,提出了解决的实例方案,并对方案的要点及优缺点进行讨论,此方案在实际操作中具有较好的效果。     

Estimation of Kinetic Parameters of Thermal Oxidation of Ilmenite

The aim of the presented work was the investigation of thermal oxidation of ilmenite in static air atmosphere. The investigations were carried out by use of a derivatograph (MOM, Hungary). The changes of crystallographic structure of investigated samples were identified by X-ray diffractometry on Philips PW-1710 diffractometer. In temperature above 500°C appears structure of hematite Fe₂O₃. On the basis of the thermogravimetric measurements, the contracting area and contracting volume models were found as the best fitting experimental data. This revised version was published online in August 2006 with corrections to the Cover Date.     

Mechanism of action of base-catalyzed oxygenation of phenol derivatives

Cyclopropyl derivative of 2,6-di-tert-butylphenol is synthesized as a probe to investigate the mechanism of base-catalyzed autooxidation of phenol derivatives. Our study indicates that one electron reduction of molecular oxygen from phenolate gives phenoxyl radical 3, a key intermediate of autooxidation. The coupling of phenoxyl radical and superoxide radical gives peroxylate anion 4 and produces the final epoxy alcohol adduct 6.     

氯氧化镁生成热的研究

用氧化镁氯化镁水溶液制备了8水合氯氧化镁[nMg(OH)2·MgCl2·8H2O], 并测定了其在盐酸中的溶解热, 实验结果表明, 氯氧化镁溶解热与n值呈线性关系, 根据溶解热求出5Mg(OH)2·MgCl2·8H2O和3Mg(OH)2·MgCl2·8H2O的生成热分别为-7727.1和5888.1kJ·mol^1^-。