Study on Chemiluminescence Reactions of L ucigenin and Reductants by Flow Injection Analysis

The chemiluminescence reactions between lucigenin and reductants such as Mo(LII),V( II), U(III), W(III), Cr(II), Ti(III) and Fe( II), which were produced on-line by passing Mo(VI),V(V),U(VI), W(VI), Cr(VI,III),Ti(IV) and Fe(III) through a micro Jones column, are studied in detail. Results show that the reactions can be used directly for the determination of these substances. The mechanism of the reactions is also investigated.

Kinetic-spectrophotometric determination of free cyanide by stopped-flow reversed flow injection analysis

A stopped-flow reversed flow injection method for the determination of free cyanide is proposed. Pyridine-barbituric acid mixture is injected in the flow system as reagent to form the colour species with cyanide. The flow is stopped when the reagent zone comes in the flow cell, where absorbance-time data are collected at 580nm wavelength. The linear range of the determination is 0.1 -10μg/ml CN-. The sampling rate is 60h-1 and the relative standard deviation is 1.6% (n=16) at 5.0 μg/ml CN-1 level. With satisfactory results, the proposed method was applied to the determination of free cyanide in wastewater without sample pretreatment.

Flow Injection Analysis of Histidine with Enhanced Electrogenerated Chemiluminescence of Luminol

A simple and sensitive flow injection method is presented for the determination of histidine based on its enhancement of electrogenerated chemiluminescence (ECL) of luminol. After optimization of the experimental parameters, the working range for histidine was in 1.0 x 10-6 to 1.0 x 10 -3 mol/L with a detection limit (S/N = 3) of 0.56 mmol/L. The relative standard deviation was 1.6% for 11 measurements of 5 x 10 5 mol/L histidine solution. The proposed method has been successfully applied to the determination of histidine in real pharmaceutical preparation.

SELECTIVE SULFUR DIOXIDE DETERMINATION BY GAS DIFFUSION FLOW INJECTION ANALYSIS WITH CHEMILUMINESCENT DETECTION

Sulfur dioxide has been found to decrease the chemiluminescence of luminol-iodine system.A new determination method for sulfur dioxide in atmosphere is developed by applying this reaction to a flow injection gas diffusion separation system.This permits the determination of sulfur dioxide selectively and rapidly.

An analysis method of injection and production dynamic transient flow in a gas field storage facility

A dynamic transient flow analysis method considering complex factors such as the cyclic injection and production history in a gas field storage facility was established in view of the limitations of the existing methods for transient flow analysis and the characteristics of the injection-production operation of strongly heterogeneous gas reservoirs, and the corresponding theoretical charts were drawn. In addition, an injection-production dynamic transient flow analysis model named "three points and two stages" suitable for an underground gas storage(UGS) well with alternate working conditions was proposed. The "three points" refer to three time points during cyclic injection and production, namely, the starting point of gas injection for UGS construction, the beginning and ending points of the injection-production analysis stage;and the "two stages" refer to historical flow stage and injection-production analysis stage. The study shows that the dimensionless pseudo-pressure and dimensionless pseudo-pressure integral curves of UGS well flex downward in the early stage of the injection and production process, and the dimensionless pseudo-pressure integral derivative curve is convex during the gas production period and concave during the gas injection period, and the curves under different flow histories have atypical features. The new method present in this paper can analyze transient flow of UGS accurately. The application of this method to typical wells in Hutubi gas storage shows that the new method can fit the pressure history accurately, and obtain reliable parameters and results.

Flow Injection Analysis of Hydrazine in the Aqueous Streams of Purex Process by Liquid Chromatography System Coupled with UV-Visible Detector

Present study describes the development of a rapid, sensitive and selective flow injection analysis of hydrazine in the aqueous streams of purex process by liquid chromatography system coupled with UV-Visible detector. The method is based on the formation of yellow coloured azine complex by reaction of hydrazine with para-dimethy laminobenzaldehyde (pDMAB). The formed yellow coloured complex is stable in acidic medium and has a maximum absorption at 460 nm. The presence of uranium in hydrazine solution is not interfering in the analysis. Under optimum condition, the absorption intensity linearly increased with the concentration of hydrazine in the range from 0.05-10 mg?L–1 with a correlation coefficient of R2=0.9999 (n=7). The experimental detection limit is 0.05mgL–1. The sampling frequency is 15 samples h–1 and the relative standard deviation was 2.1% for 0.05 mg?L–1. This method is suitable for automatic and continuous analysis and successfully applied to determine the concentration of hydrazine in the aqueous stream of nuclear fuel reprocessing.

Simultaneous Biparametric Determination of Total Calcium and Potassium in Biological Fluids by Flow Injection Analysis──Use of Powell＇s Method in the System Optimization

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Flow Injection Analysis Technique for Online Preconcentration of Lead Ions in Airborne Particulate Matter Using Imprinted Polymer as the Sorbent

This work reported a simple and sensitive flow injection analysis(FIA)technique coupled with a Flame Atomic Absorption Spectrophotometer(FAAS)for online preconcentration of lead(Ⅱ)ions in the airborne particulate matter samples(PM_(2.5))using ion-imprinted polymers as adsorbent packed in minicolumn.A bulk polymerization method was chosen to synthesize the polymer based on a ternary complex of lead ions with 4-2-pyridilazo resorcinol and 4-vinyl pyridine with methacrylic acid as a functional monomer.The optimum pH for sorption was 6,and other variables for the FIA system were optimized,including breakthrough volume,eluent concentration,and eluent volume.The optimum conditions were reached with a breakthrough volume of 4.45 mL,calculated as a dynamic retention capacity of 5.20 mg/g of Pb(II)40 mg/L,with a 1.5 mL/min flow rate.The eluent used for the FIA system was 0.5 mL HNO_(3)of 3 mol/L.Linearity,precision,and limits of detection of the FIA system were determined before being applied to preconcentration and analysis of lead ions in PM_(2.5)samples.The precision of the method was determined to be 3.09%by calculating the coefficients of the variant.Linearity of the method in the concentration range of 50-1000μg/L gave a coefficient correlation of 0.9925,showing a good response,and the limit of detection of the system was 5.11μg/L,better than that of the FAAS method.Performances of the FIA system were evaluated and showed good results with an enrichment factor of more than 20 times higher and a concentration efficiency of 11.65 min^(-1)with a consumptive index of 4.5 mL.Preconcentration and analysis of the PM_(2.5)samples in Bandung City showed the concentrations of Pb(II)were 26.67μg/L and 33.3μg/L with the accuracy of the method for each sample of104.75%and 107.86%.

Flow injection chemiluminescence determination of meloxicam using potassium permanganate and formaldehyde system

A simple, rapid and sensitive flow injection chemiluminescence （FI-CL） method has been developed for the determination of meloxicam. The method is based on the CL-emitting reaction between meloxicam and potassium permanganate in a hydrochloric acid medium, enhanced by formaldehyde （HCHO）. Under optimum conditions, calibration curve over the range of 1.0-20.0μg/mL was obtained. The proposed method was successfully applied to the determination of meloxicam in capsules with no evi- dence of interference from common excipients. The detection limit of this method was 25.6 ng/mL. The relative standard deviation was 2.1% for 10.0 μg/mL meloxicam. The sample throughput was found to be 120 samples/h.

基于 Moldflow 的汽车中控台框架翘曲变形分析及优化

以某汽车中控台框架为研究对象,测量试模样品发现其翘曲变形量超过了装配要求。通过Moldflow软件模拟了该塑件实际的注塑过程,翘曲变形量的模拟值与实测平均值的最大误差为5.98%,发现该塑件翘曲变形的主要因素为冷却不均和收缩不均。本文在原物料中添加质量分数为25%的玻璃纤维以及优化工艺参数后,翘曲变形量的模拟值与初始方案相比降低了86.22%。试模验证表明,优化后的翘曲变形量模拟值与实测平均值的最大误差为4.35%,证明了Moldflow软件模拟分析的准确性。试模后各检测点的最大翘曲变形量降到了1.6 mm以下,较优化之前降低了80%以上,为类似大型复杂注塑件的翘曲变形分析及优化提供了思路。

Flow-injection Spectrophotometric Determination of Uric Acid in Urine via Prussian Blue Reaction

A simple and sensitive flow injection（FI） spectrophotometric method was reported for the determination of uric acid based on the reduction of Fe（III）/ferricyanide in the presence of uric acid. The in situ reduced ions reacted with unreduced portion of ferricyanide/Fe（III） to form soluble Prussian blue, which was monitored at an absorption wavelength of 735 nm. The optimized conditions allow a linear calibration graph in a concentration range of 1―100 μmol/L. The relative standard deviation was in a range of 0.5%―2.5%, with a detection limit（3σ blank） of 0.3 μmol/L and a sampling frequency of 60 injection/h was obtained. The effect of common substances present in human physiological fluids on the determination of uric acid was examined. The method was applied to determining uric acid in human urine samples with the recoveries in a range of 96%―105%. The results agree well with those by spectrophotometric reference method at a confidence level of 95%. Spectrophotometric procedures for uric acid determination in clinical samples were reviewed briefly.

Chemiluminescence Determination of Molybdenum by on-Line Reduction with a Flow Injection System

The chemiluminescence (CL) reaction between lucigenin (Lu) and molybdenum (III) produced by a Jones reductor was investigated using a flow injection system. On the basis of this, a novel method for the determination of trace amount of molybdenum has been established. The emission intensity was linear with molybdenum concentration in the range of 0.1-1000 ng/mL; the detection limit was 0.02 ng/mL molybdenum; the relative standard deviation was less than 2% for the determination of 0.1 ng/mL molybdenum (n=11). The method has been applied successfully to the analysis of trace molybdenum in water and steel samples.

基于Moldflow的绗缝机夹子注塑模设计

以绗缝机夹子的短板为例,基于Moldflow有限元分析软件,合理确定了塑件的浇口位置和浇口形式,精确预测出塑件的充型时间、注射压力、锁模力等工艺参数,并分析出塑件的体积收缩率及熔接线、气穴等潜在缺陷的位置。有限元模拟结果为注塑成型设备的选型和成型工艺参数的合理制定提供了可靠依据,为模具的优化设计提供了方向。基于Moldflow分析结果,设计出一套一模两腔侧浇口、带斜导柱侧向分型与抽芯机构的注塑模具并一次性试模成功。Moldflow有限元分析软件在注塑模设计中的应用不仅有效降低了模具设计的成本和周期,也为同类零件的模具优化设计提供了参考。

Study on the Flow Injection Micro-Column Pre-Separation System Coupled With High Performance Liquid Chromatography for the Determination of Ecdysterone in Traditional Chinese Medicine

A flow injection (FI) micro-column system coupled with high performance liquid chromatography (HPLC) was proposed for the pre-separation and determination of active organic component (ecdysterone) in traditional Chinese medicine, Loulu. The factors influencing separation performance were investigated and optimized. Under the optimal conditions, the contents of ecdysterone in Loulu were determined by HPLC system using MeOH-H_2O (40: 60,V/V) as the mobile phase at a flow rate of 1. 0 mL/min. The calibration curve was linear in the range of 0. 5~ 100 mg/L of ecdysterone concentrations. The detection limit of the analyte was 0. 11mol/L(3) with a precision of 0. 38% RSD (n=7 f c= 10. 0 mg/L). The average recovery of the method was 98. 7%. The proposed method has been applied to determine ecdysterone in practical samples, and the determined values by both external standard method and standard addition method were in good agreement. Compared to the traditional solid extraction method, the system proposed has the advantages of simple procedure, good reproducibility, minimum volume requirement, reduction of matrix interference and low contamination risk.

Study on Quenching Effect of Holmium (Ⅲ) Ion in Chemiluminescence System of Luminol H_2O_2-Cr(Ⅲ) by Flow Injection Technique

A new chemiluminescence (CL) analytical method for determination of rare earth Ho(Ⅲ) ion is reported. It is based on the quenching effect of Ho(Ⅲ) ion on CL intensity of Luminol H 2O 2 Cr(Ⅲ) system. The detection limit is 3×10 -8 mol/L, the linear range is from 1×10 -7 to 1×10 -4 mol/L; the relative standard deviation is less than 3% (for 2×10 -7 mol/L Ho, n=11). The method was applied to determination of Ho(Ⅲ) in pure samples with satisfactory results.

Flow-injection spectrophotometric determination of vanadium with malachite green oxalate by bromate in acidic and micellar medium

A flow injection method is proposed for determining vanadium（V）. The method is based on its catalytic effect on the oxidation of malachite green oxalate by bromate. The reaction was monitored spectrophotometrically by measuring malachite green oxalate absorbance at λmax = 625 nm. The reagents and manifold variables, which have influences on the sensitivity, were investigated and the optimum conditions were established. The optimized conditions made it possible to determine vanadium in the ranges of 10-140 ng/mL with a detection limit of 5.2 ng/mL and a sample rate of 20 ± 5 samples/h.

Determination of Lanthanu m in Lu minol- H_2 O_2- Cr( Ⅲ) Syste m by Flow Injection Chemilu minescence

A novel method of flow injection chemiluminescence (CL) analysis for the determination of rare earth La(Ⅲ) ion is prensented. It is based on the quenching effect of La(Ⅲ) ion in the CL system of Luminol H 2O 2 Cr(Ⅲ). The CL emission intensity is linear with La(Ⅲ) concentration in the range 1×10 -7 ～1×10 -4 mol/L; the detection limit is 4×10 -8 mol/L, the relative standard deviation is less than 3% (for 2×10 -7 mol/L La, n =11).

Flow Injection Determination of Tramadol Based on Its Sensitizing Effect on the Chemiluminescent Reaction of Permanganate-Sulfite

In this paper, a novel chemiluminescence (CL) method for the determination of tramadol has been developed by combining the flow injection technique and its sensitizing effect on the weak CL reaction between sulfite and acidic KMnO4. A mechanism for the CL reaction has been proposed on the basis of fluorescent and CL spectra. Under the optimized conditions, the proposed method allows the measurement of tramadol hydrochloride over the range of 0.04 - 4 ?g/mLwith a correlation coefficient of 0.9995 (n = 8) and a detection limit of 0.01 ?g/mL (3σ), and the relative standard deviation for 2.0 ?g/mL tramadol (n = 11) is 2.1%. The utility of this method was demonstrated by determining tramadol hydrochloride in tablets and injections.

Determination of ribavirin by flow injection chemiluminescence

Objective： To establish a rapid and precise continuous flow-injection chemiluminescence （CL） method to determine ribavirin. Methods： The ribavirin could restrain strongly CL reaction of luminol in sodium hydroxide （NaOH） solution with potassium chlorate （KClO3）. The different experimental parameters affecting the CL intensity were studied carefully. Results： Under optimum conditions （The concentrations of luminol, KClO3, and NaOH were at 0.1 mmol/L, 0.5μmol/L, and 0.2 mol/L, respectively）, the linear range of the working curves was 0.01-7.00μg/ml with a detection limit of 0.004μg/ml. Conclusion： The method is simple, rapid and sensitive, and successfully applied to the determination of ribavirin in pharmaceutical preparations and biological fluids.