Substoichiometric determination of phosphorus

Phosphorus in orchard leaves (NBS SRM-1571) and spinach (SRM-1570) was determined by various substoichiometric analytical methods such as the direct method, GRASHCHENKO's method and the method of carrier amount variation. All samples were labelled with³²P radioisotope. The data obtained by the method of carrier amount variation were also treated by the method of least squares instead of De VOE's method. Phosphorus concentration in orchard leaves was 0.206±0.011% by the direct method, 0.219±0.011% by GRASHCHENKO's method, 0.211±0.011% by the method of carrier amount variation and 0.207±0.007% by the method of least squares, respectively. These values agree with the value reported by NBS (0.21±0.01%). Furthermore, these concentrations obtained by various substoichiometric methods were compared with those by radioactivation reported in a prevoius paper.     

Comparison study of two procedures for the determination of emamectin benzoate in medicated fish feed

A new method has been developed for the determination of emamectin benzoate in fish feed. The method uses a wet extraction, cleanup by solid-phase extraction, and quantitation and separation by liquid chromatography (LC). In this paper, we compare the performance of this method with that of a previously reported LC assay for the determination of emamectin benzoate in fish feed. Although similar to the previous method, the new procedure uses a different sample pretreatment, wet extraction, and quantitation method. The performance of the new method was compared with that of the previously reported method by analyses of 22 medicated feed samples from various commercial sources. A comparison of the results presented here reveals slightly lower assay values obtained with the new method. Although a paired sample t-test indicates the difference in results is significant, this difference is within the method precision of either procedure.     

Disintegration test to measure lot-to-lot variations of vaginal tablets

Attempts were made to investigate the disintegration test for vaginal tablets. Disintegration tests were done for four different commercial vaginal tablets (three lots each) by the watch glass method and Japanese Pharmacopoeia (JP) disintegration method, and the resulting profiles were compared to those by the modified British Pharmacopoeia (BP) method on a point of lot-to-lot variation of the disintegration times. The disintegration time of every tablet by the modified BP method was longest, followed by the watch glass method, and finally by the JP disintegration method. The results for lot-to-lot differences in disintegration times by the modified BP method were similar to those by the watch glass method. However, such lot-to-lot differences as found by the modified BP method and watch glass method were not always observed by the JP disintegration method. It was concluded from these results that the modified BP method was most suitable for investigating lot-to-lot differences in the disintegration of vaginal tablets.     

Development of effective Stokesian dynamics method for ferromagnetic colloidal dispersions (cluster-based Stokesian dynamics method)

We have developed a new Stokesian dynamics (SD) method for nondilute colloidal dispersions, which enables us to reduce drastically the computation time. To verify the validity of the present method, which is called the "cluster-based SD method," three-dimensional simulations of a ferromagnetic colloidal dispersion have been carried out for a simple shear flow. The correlation function and viscosity have been evaluated to compare the results obtained by the present method with those obtained by the ordinary SD method and by the method of ignoring hydrodynamic interactions between particles. The results obtained here are summarized as follows. The transient properties from an initial state obtained by the present method agree well with those obtained by the ordinary method, even if a radius r(clstr), which defines the cluster formation, is taken as a small value such as r(clstr)=1.2d (d is the particle diameter). Also, the equilibrium properties such as the pair correlation function and viscosity obtained by the present cluster-based method are in satisfactory agreement with those obtained by the ordinary SD method. Furthermore, the cluster-based method drastically reduces the computation time to about one-fourteenth to one-seventieth that of the ordinary method. It is clear from these results that the cluster-based SD method is significantly superior to the ordinary SD method for ferromagnetic colloidal dispersions for which a large model system such as N=1000 or 10,000 is indispensable in simulations.     

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.     

Cell surface proteins of Candida albicans: preparation of extracts and improved detection of proteins

We have reexamined the detection of the components in a beta-mercaptoethanol and ammonium carbonate buffer extract of surface proteins of Candida albicans and the effects of postextraction manipulation of the extract on recovery of extract components. Following sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE), preferential staining of some moieties was observed when bands detected by a commercial silver staining method or a Coomassie Brilliant Blue (CBB) staining method were compared. Additional protein bands that were either not detected or poorly detected by a single method alone were readily observed by a combined silver-CBB staining method. This method also detected alterations in the profile of extracted proteins from organisms grown in the presence of galactose or hemoglobin rather than glucose. Two-dimensional electrophoresis (2-DE) gel analysis by double stain showed better detection of several acidic and basic protein spots. Less than 10% of the extract as determined by a dye-binding assay was lost following either or both lyophilization and dialysis. These manipulations of the extract did not change the protein profile following SDS-PAGE as determined by the combined staining or Western blot analysis of a 70 kDa protein. These observations suggest that soluble cell wall proteins are not unusually sensitive to procedures routinely used in protein purification. In addition, these studies suggest that a modified staining method that combines both silver stain and CBB stain provides improved detection of cell wall proteins compared to either method alone.     

A simple method of judging the acceptability of analytical methods

The method is based on calculation of the relative differences between values obtained for calibration standards by a sequential leave-one-out technique and accurate values obtained by a reference method. The method is suitable, namely, for comparing analytical procedures when a limited number of standards of accurately known composition is available.     

Synthesis of radioiodinated labeled peptides

This report covers optimization of radioiodination of peptides by both a direct method in which a constituent tyrosine residue is labeled and indirect method by using an iodinated derivative (SIB) of N succinimidyl 3-(tri-n-butylstannyl) benzoate (ATE) as the intermediate. Radioiodination of IgG and FMLF were performed by direct method using Chloramine-T as an oxidant but since Formyl-Methyl-Leucyl-Phenylalanine, FMLF, does not lend itself for direct radioiodination we performed labeling of FMLF by indirect method via radioiodined SIB at different pH.     

纳米羟基磷灰石/溶菌酶复合体的原位合成及酶活性研究

利用一种新的溶菌酶的组装方法, 湿法合成原位组装了羟基磷灰石/溶菌酶复合体, 对组装体进行多种表征并与浸渍组装的方法进行了对比.     

Evaluation of effective thermal conductivity of fireworks compositions

Effective thermal conductivity of fireworks raw materials and their mixture have been measured by the temperature modulated DSC and the hot wire method, in order to predict spontaneous ignition properties precisely. As a result, an excellent linear correlation has been obtained between the density and the λ_e by the TMDSC method. Moreover, the low-density data by the hot wire method lie on the extrapolated point of the linear correlation. Thus, the λ_e within the ordinary limit of fireworks composition can be measured by the TMDSC method. Krupiczka’s estimation method shows a good agreement with the experimental values.     

Identification of areas of absence of adhesive bonding between layers in multilayer structures

The theoretical foundations of the acoustic impedance method for controlling multilayer structures by means of a self-vibration mode are considered. It is shown that the self-vibration mode allows the range of application of the impedance method to be significantly extended because of the possibility of controlling of new material types, to halve a deep uncontrolled area, and to control structures—which was previously impossible by the impedance method—by means of one-way access from a thicker layer.     

恒电量瞬态扰动测量Tafel斜率及数据积分处理

提出了一个三参数积分法拟合恒电量强极化数据以测定Tafel斜率的新方法.实验证明,恒电量瞬态扰动测量碳钢在酸溶液中的腐蚀,获得的Tafel斜率与消除了溶液电阻影响的Tafel外推结果有很好的一致性,说明恒电量法有效地消除了溶液电阻对该体系测量结果的影响,并且通过电化学和失重实验验证表明,这种快速测量可以获得准确的腐蚀速率.这种新的恒电量强极化积分算法相对微分法的优势体现在算法简捷和用于数值计算的数据具有较高的信噪比,因此能够提高测量精度.     

The Methodological Studies on the Determination of Propofol by HPLC

Propofol injection is a new veinal narcotic medicine which was produced by Finland Leiras company. The former method examined of propofol is by GC method. Now a new HPLC method was developed for the determination of propofol. The method is rapid, accurate and stable.     

Analysis of gamma-ray spectra by using fast Fourier transform (author's transl)]

In order to simplify the mass data processing in a response matrix method for gamma-ray spectral analysis, a method using a Fast Fourier Transform devised. The validity of the method was confirmed by a computer simulation for spectra of a NaI detector. The method uses the fact that spectral data can be represented by Fourier series with reduced number of terms. The estimation of intensities of gamma-ray components is performed by a matrix operation using the compressed data of an observation spectrum and standard spectra in Fourier coefficients. The identification of gamma-ray energies is also easy. Several features in the method and a general problem to be solved in a response matrix method are described.     

A comparison of photopeak area computation methodologies

The accuracy and precision of photopeak area calculation methods has been studied by comparison of a digital method of computation with the fitting of a mathematical function to the data. In the present study, peak areas for 16 replicate photopeaks were computed both by the total peak area method any by the peak fitting method of program SAMPO. Both methods worked well with the fitting method showing somewhat smaller spread in the results.     

Modified liquid displacement method for determination of pore size distribution in porous membranes

A new method called constant pressure liquid displacement method (CPLM) was developed and tested to measure the pore size distribution of porous membranes. The permeability, defined as a ratio of the flow rate to the pressure applied, used to be assumed constant either for a conventional liquid displacement method or for a bubble point method, leading to the erroneous interpretation of the pore size distribution. However, it was possible to eliminate such an assumption by measuring the flow rates experimentally at a standard low pressure through the pores penetrated with a permeating liquid according to the proposed method. The pore size distribution for a hydrophobic PVDF membrane was successfully measured by the CPLM and compared with those measured by two different methods such as the conventional liquid displacement method and the mercury intrusion method.     

茶碱抗体的制备及鉴定

茶碱在临床上是一种非常有用的药剂。本文报道一种新的茶碱抗血清的制各及鉴定方法．用混合酸酐法合成抗原，借助于紫外光谱对其进行定性和定量分析。用混合免疫法免疫兔子，用免疫扩散法对抗血清进行鉴定。     

合成方法对MCM-22分子筛的结构、性质及催化性能的影响

在水热条件下分别以动态法和静态法合成了高纯度和高结晶度的MCM-22分子筛.采用N2吸附、XRD、TEM和FTIR等方法研究了制备方法对分子筛的结构及性质的影响.结果表明,动态法合成的MCM-22比静态法合成的分子筛的晶粒小,酸量低.在丙酮一步法合成甲基异丁基酮反应中,静态条件下合成的MCM-22为载体的催化剂的丙酮转化率较高,这是由于该分子筛的酸量较高所致.而MIBK的选择性则呈相反趋势,这可能与动态条件下合成的分子筛粒径小、孔道短有关.     

Metrological assessment of the high-accuracy RNAA method for determination of cobalt in biological materials

The paper summarizes work on the development of the high-accuracy RNAA method for the determination of trace amounts of cobalt in biological materials. The method is based on a combination of neutron activation with selective and quantitative isolation of the analyte in a state of high radiochemical purity by use of column chromatography followed by gamma-ray spectrometric measurements. The method was devised according to a set of rules, which were formulated to obtain high accuracy of the method. The procedure has been also equipped with several criteria as key factors in quality assurance. Qualification of the high-accuracy RNAA method as a primary ratio method has been demonstrated and its usefulness in the certification of the candidate reference materials tea leaves and mixed Polish herbs is presented.