离子选择电极法测定对氟聚苯乙烯聚合体中的氟含量

本文研究了分解对氟聚苯乙烯聚合体的条件,建立了用离子选择电极法测定对氟聚苯乙烯聚合体中氟含量的方法,对氟苯甲酸加标回收率为９９．９％,对氟聚苯乙烯分析结果的相对标准偏差为２．７％,方法简便,准确。     

Determination of trace bismuth by flow injection-hydride generation collection-atomic absorption spectrometry

Bismuth hydride gas was collected on-line and determined via a new flow injection-hydride generation collection-flame atomic absorption spectrometry system. The performance of the gas-liquid separator, hydride gas collection time, acidity of the sample solution, NaBH(4) concentration, and the effects of concomitant interferents were investigated to optimize the conditions of this new method. Interferences from concomitant elements were investigated, and recoveries of 94.7-105.3% for 10 ng mL(-1) Bi were obtained after the addition of 0.2% ascorbic acid-thiourea masking reagents. The sensitivity of this new method was one order of magnitude higher than the continuous flow-hydride generation-flame atomic absorption method with a detection limit of 0.25 ng mL(-1) and a precision of 2.3%. The method was evaluated by determining trace bismuth in standard biological reference material human hair GBW07601, and the results were consistent with the certified value. The proposed method was then employed to determine trace bismuth in ten colored gelatin samples; recoveries of 94.2-105.8% were obtained.     

Daubechies小波主成分回归法机理及算法研究

将小波变换与主成分回归相结合,提出一种新型多元校正算法---小波基主成分回归法。理论分析和仿真实验表明,该法可更有效地去除噪声,提取有用信息。将其用于氯霉素及甲硝唑实际药物体系分析,与主成分回归法(PCR)相比,得到的回收率总平均相对误差由1.70%下降到0.90%。此外,通过将统计判据和小波多尺度分析相结合,发展了一种新的因子数判定方法。理论和实验研究表明,该法比传统因子数判定法具有更高的可靠性。     

New refractive index method for measurement of alcoholic strength of small volume samples

A study of the correlation between the refractive index (RI) method adopted by the European Community (EC) and a reference pycnometric method for the measurement of alcoholic strength was undertaken. A new RI method with greater accuracy was also developed. Alcoholic strength measured by both RI methods presented a relatively constant negative bias compared with results by the pycnometric method. Differences found between the RI methods and the pycnometric method were 0.6-0.9% (v/v) when RI was measured by the EC method and 0.4-0.5% (v/v) when the new RI method developed in our laboratory was used. Statistical analysis of the results showed that differences between the 2 RI methods and the reference pycnometric method were statistically significant at the 95% confidence level. Correction factors are proposed for the accurate use of measurements of alcoholic strength obtained for small volume samples.     

A novel method for quantitative determination of tea polysaccharide by resonance light scattering

A new method for the determination of tea polysaccharide (TPS) in green tea (Camellia sinensis) leaves has been developed. The method was based on the enhancement of resonance light scattering (RLS) of TPS in the presence of cetylpyridinium chloride (CPC)-NaOH system. Under the optimum conditions, the RLS intensity of CPC was greatly enhanced by adding TPS. The maximum peak of the enhanced RLS spectra was located at 484.02 nm. The enhanced RLS intensity was proportional to the concentration of TPS in the range of 2.0-20 μg/ml. It showed that the new method and phenol-sulfuric acid method give some equivalent results by measuring the standard compounds. The recoveries of the two methods were 96.39-103.7% (novel method) and 100.15-103.65% (phenol-sulfuric acid method), respectively. However, it showed that the two methods were different to some extent. The new method offered a limit of detection (LOD) of 0.047 μg/ml, whereas the phenol-sulfuric acid method gives a LOD of 1.54 μg/ml. Interfered experiment demonstrated that the new method had highly selectivity, and was more suitable for the determination of TPS than phenol-sulfuric method. Stability test showed that new method had good stability. Moreover, the proposed method owns the advantages of easy operation, rapidity and practicability, which suggested that the proposed method could be satisfactorily applied to the determination of TPS in green tea.     

Determination of tertiary amines and salts of organic acids in acetic acid by catalytic thermometric titration

A new method of determination of tertiary amines and salts of organic adds in acetic acid solution, to which about 2 % of water and 8% acetic anhydride are added, is described. After the equivalence point, the excess of perchloric acid catalyses the exothermic reaction of water with acetic anhydride. The end-point is determined from the graph of temperature against volume of added titrant. If a slightly soluble compound is produced during the titration, the precision of the new method is superior to that of the potentiometric method.     

一种自动微量滴定新方法

本文依据传统滴定分析原理，利用流动注射装置提出一种新的自动微量滴定方法，它不仅具有流动注射滴定分析法简便快速，试剂和试样消耗少，仪器装置简单等优点，而且测定信号怀被测组分的浓度直接成线性关系，结果的准确度和精度优于一般流动注射滴定方法。通过用盐酸滴定氢氧化钠进行验证，相关系数为０．９９９９，相对标准偏差（ＲＳＤ）为０．４％。     

Direct determination of carnosic acid in a new active packaging based on natural extract of rosemary

A new antioxidant film is being developed that incorporates a natural extract of rosemary and is intended for contact with food. The rosemary extract has been screened and carnosic acid and carnosol have been determined as the major antioxidant components (6.96% and 0.88%, respectively) that are responsible for the antioxidant properties of the whole extract. Thus, a fast method for the direct determination of carnosic acid in the packaging material, in order to evaluate the antioxidant capacity of the new active plastic, has been developed and optimized. The method consists of extraction from the plastic with methanol, followed by anion exchange solid-phase extraction and final analysis by UPLC–MS. Using this process, the recovery of carnosic acid is about 99%. The complete analytical performance of the method developed here is also assessed. The analytical features of the method, such as the relative standard deviation, reproducibility, repeatability, linear range, and detection and quantification limits, are shown. This method can be subsequently modified to monitor other active components in different packages, and it constitutes a crucial step forward in research into new and improved commercial antioxidant packages.     

Quantitative analysis of chloride in brackish water: an application to the hyperchromic effect of copper(II) ion with chloride ion.

A new modified method was applied to the determination of chloride anion in brackish water by using a common copper(II) sulfate solution and a spectrophotometer. The result of the quantitative analysis demonstrated that chloride concentrations were 1.61% w/v and 1.74% w/v at ebb tide and flood tide, respectively, of the Muya River. On the other hand, chloride concentrations were 1.17% w/v at ebb tide and 1.65% w/v at flood tide of the Yoshino River. The new method proved that chloride concentration corresponded well with results from Mohr and conductive methods. Therefore, the newly developed method can be exploited as common means to measure chloride concentration in aqueous solutions. Moreover, it is also valuable for application to other types of environmental samples.     

反相高效液相色谱中流动相线性梯度洗脱条件下溶质保留时间预测的新方法

 在计算溶质的梯度保留时间时 ,根据流动相在色谱柱内的分布规律 ,对溶质在色谱柱内的迁移距离和流动相梯度同时进行校正 ,从而建立了一种预测溶质线性梯度洗脱条件下保留时间的新方法。该方法在不同的仪器系统中 ,对于弱保留和强保留溶质在不同线性梯度洗脱条件下保留时间的预测 ,都具有良好的准确度。以 15种氨基酸和 8种苯的同系物为例 ,该方法对于弱保留溶质保留时间的预测 ,相对平均误差分别为 3 70 %和 4 90 % ,远小于文献方法得到的结果 (2 3 6 1%和 31 16 % ) ;对于强保留溶质保留时间的预测 ,相对平均误差分别为 0 2 1%和6 0 1% ,略小于文献 。     

Quantitative genotyping of single nucleotide polymorphism by single-molecule multi-color fluorescence resonance energy transfer

We developed a new single nucleotide polymorphism (SNP) genotyping method based on single-molecule multi-color fluorescence resonance energy transfer (FRET). We demonstrated that this new method uses less than 1 fmol of sample and is also highly quantitative with a detection level of 1% or lower in the minor allele fraction.     

Determination of nitrogen solubility in dilute pepsin hydrochloric acid solution of fishmeal: interlaboratory study

A revised method to determine solubility of nitrogen in dilute pepsin, using 0.0002% pepsin in place of 0.2% in AOAC Official Method 971.09, was tested in 16 laboratories with 12 samples of fishmeal. Results were calculated according to 2 procedures: AOAC Official Method 971.09 and a method described in 1964 by researchers at the Torry Research Station (Aberdeen, Scotland), and generally referred to as the modified Torry method. Variations in the method of shaking and source of pepsin were also investigated. Pepsin solubility values were lower and more variable when calculated by the Torry procedure. The method of shaking apparently affected the result when calculated according to the Torry but not the AOAC method. The source of pepsin had no significant effect on between-laboratory variability, but a comparison of the 2 main sources within one laboratory resulted in highly significant differences. Based on this study, the International Fishmeal and Fish Oil Organization has adopted this new method, using 0.0002% pepsin but keeping the AOAC method of calculation. The type of shaker and source of pepsin are recommended but are not mandatory. The repeatability and reproducibility limits of this new method are 1.6 and 3.3% units of solubility, respectively.     

A new approach to decoupling of bacterial adhesion energies measured by AFM into specific and nonspecific components

A new method to decoupling of bacterial interactions measured by atomic force microscopy (AFM) into specific and nonspecific components is proposed. The new method is based on computing the areas under the approach and retraction curves. To test the efficacy of the new method, AFM was used to probe the repulsion and adhesion energies present between Listeria monocytogenes cells cultured at five pH values (5, 6, 7, 8, and 9) and silicon nitride (Si₃N₄). Overall adhesion energy was then decoupled into its specific and nonspecific components using the new method as well as using Poisson statistical approach. Poisson statistical method represents the most commonly used approach to decouple bacterial interactions into their components. For all pH conditions investigated, specific energies dominated the adhesion, and a transition in adhesion and repulsion energies for cells cultured at pH 7 was observed. When compared, the differences in the specific and nonspecific energies obtained using Poisson analysis and the new method were on average 2.2 % and 6.7 %, respectively. The relatively close energies obtained using the two approaches demonstrate the efficacy of the new method as an alternative way to decouple adhesion energies into their specific and nonspecific components.     

有机物燃烧热测定方法的改进

对有机物燃烧热的测定方法进行了改进。改变点火丝的安装方法,采用高性能量热计,改变氧弹内氧气的压力及燃烧样品的用量,确定了新的测定方法。采用新的测定方法测定萘的燃烧热,测定结果的相对误差为0．05％,相对标准偏差为0．077％。     

红外吸收法测定炼钢碳化硅类脱氧剂中的碳化硅

为了满足炼钢碳化硅类脱氧剂中碳化硅的分析,在参照国家标准方法的基础上,通过烧失率、助熔剂选择、线性化考核及精密度和准确度等条件试验,建立了红外吸收法测定炼钢碳化硅类脱氧剂中的碳化硅的分析方法。方法的回收率大于98%,相对标准偏差为0.5%～0.7%,准确度高,误差小,实用性强。     

多元弱酸(碱)溶液pH的简易通用计算方法

提出了计算多元弱酸(或碱)溶液pH的新方法.该计算方法具有以下特点:限制条件简单,即多项式中某一项小于最大项的5％即可忽略该项贡献;计算过程和步骤清晰易记;通用性好,一元或多元弱酸(碱)溶液pH计算均可适用.     

用氧瓶燃烧-电位滴定法测定煤中有机硫和橡胶总硫

研究了煤中有机硫和橡胶中总硫的微量测定方法,样品经氧瓶分解后所转变的ＳＯ４２－在Ｆｅ（ＣＮ）６３－／Ｆｅ（ＣＮ）６４－电对存在下用Ｐｂ２＋滴定。提出了采用Ｚｎ３［Ｆｅ（ＣＮ）６］２、微酸性溶液和低浓度Ｆｅ（ＣＮ）６４－存在下,消除磷干扰的新方法,应用于合成样品和实际样品的分析,结果满意。其回收率＞９８％,相对标准偏差＜２．３％,绝对误差＜０．１５％。     

基于离子色谱的有机电合成快速检测分析的新方法

在有机电化学合成中 ,实时准确地分析反应物、中间体和产物的组成及浓度变化十分重要 ,对特定体系研发一种快速、有效的检测方法 ,则有更加重要的应用价值 .电合成法以其原料价廉易得、反应条件温和、环境污染小等特点 ,成为生产乙醛酸等物种的重要途径和发展方向 .在草酸电合成乙醛酸过程中 ,已知电解液的主要物种是乙醛酸和草酸 ,对乙醛酸的定量检测将对电合成的过程评价和生产具有指导意义 .但由于它们较为相似的分子结构却给物种的分析与检测造成极大的麻烦 ,迄今尚未见到有关实时准确地分离检测乙醛酸的方法报道 .实际检测中人们仍不得…     

无汞盐密封法测定高氯浓度水样的化学需氧量

提出了一种以重铬酸钾为氧化剂,以6%硫酸银代替硫酸汞作为掩蔽-催化剂消除高氯离子干扰,测定化学需氧量(COD)的无汞密封新方法。研究了反应温度、反应时间和硫酸银浓度等测定条件。该法可以避免汞盐对环境的污染,适合测定多种类型的水样。该法测定结果的相对标准偏差为1.4%(n=8),平均加标回收率为98.5%.