Automated stopped-in-dual-loop flow analysis system for catalytic determination of vanadium in drinking water.

An automated stopped-in-dual-loop flow analysis (SIDL-FA) system is proposed for the determination of vanadium in drinking water. The chemistry is based on the vanadium-catalyzed oxidation reaction of p-anisidine by bromate in the presence of Tiron as an activator to produce a dye (lambda(max)=510 nm). A SIDL-FA system basically consists of a selection valve, three pumps (one is for delivering of standard/sample, and others are for reagents), two six-way injection valves, a spectrophotometric detector and a data acquisition device. A 100-microL coiled loop around a heated device is fitted onto each six-way injection valve. A well-mixed solution containing reagents and standard/sample is loaded into the first loop on a six-way valve, and then the same solution is loaded into the second loop on another six-way valve. The solutions are isolated by switching these two six-way valves, so that the catalytic reaction can be promoted. The net waste can be zero in this stage, because all pumps are turned off. Then each resulting solution is dispensed to the detector with suitable time lag. A touchscreen controller is developed to automatically carry out the original SIDL-FA protocol. The proposed SIDL-FA method allows vanadium to be quantified in the range of 0.1-2 microg L(-1) and is applied to the determination of vanadium in drinking water samples.

[Case of intracerebral hemorrhage due to amphetamine abuse].

We report a case of intracranial hemorrhage due to amphetamine abuse in a young adult. A 34-year-old, confused woman was transferred to our emergency room with right hemiparesis and aphasia. CT at admission demonstrated intracerebral hemorrhage in the left frontal and parietal lobes, associated with subarachnoid hemorrhage. MRA shortly after admission revealed no intracerebral vascular anomaly. Cerebral angiography following admission showed irregularity of the vessel wall in the left anterior and middle cerebral arteries. Later, a toxicology screen test for urine was found to be positive for amphetamines and metamphetamines. These findings suggested that cerebral vasculitis and hypertensive surge induced by amphetamines caused intracranial and subarachnoid hemorrhage. Amphetamine abuse should always be considered as a cause of intracranial hemorrhage in young adults.

Stopped-in-loop flow analysis of trace vanadium in water.

The new concept of stopped-in-loop flow analysis (SIL-FA) is proposed, and an SIL-FA method for the catalytic determination of vanadium is demonstrated. In an SIL format, a sample solution merges with reagent(s), and the well-mixed solution is loaded into a loop. The solution in the loop is separated by a six-way switching valve from the main stream. While the reaction proceeds in the stationary loop, the SIL-FA system does not need to establish a baseline continuously. This leads to a reduction in reagent consumption and waste generation compared with traditional flow injection analysis.

Sequential injection lab-on-valve simultaneous spectrophotometric determination of trace amounts of copper and iron.

A sequential injection (SI) method in a lab-on-valve (LOV) format for simultaneous spectrophotometric determination of copper and iron has been devised. The detection chemistry is based on the complex formation of 2-(5-bromo-2-pyridylazo)-5-[N-n-propyl-N-(3-sulfopropyl)amino]aniline (5-Br-PSAA) with copper(II) and/or iron(II) at pH 4.6. Copper(II) reacts with 5-Br-PSAA to form the complex which has an absorption maximum at 580 nm but iron(III) does not react. In the presence of a reducing agent only iron(II)-5-Br-PSAA complex is formed and detected at 558 nm. Under the optimum experimental conditions, the determinable ranges are 0.1-2 mg l(-1) for copper and 0.1-5 mg l(-1) for iron, respectively, with a sampling rate of 18 h(-1). The limits of detection are 50 microg l(-1) for copper and 25 microg l(-1) for iron. The relative standard deviations (n=15) are 2% for 0.5 mg l(-1) copper and 1.8% for 0.5 mg l(-1) iron when determined in standard solutions. The recoveries range between 96 and 105% when determining 0.25-2 mg l(-1) of copper and 0.2-5 mg l(-1) of iron in artificial mixtures at copper/iron ratios of 1:10 to 5:1. The proposed SI-LOV method is successfully applied to the simultaneous determination of copper and iron in multi-element standard solution and in industrial wastewater samples.

Successive determination of copper and iron by a flow injection-catalytic photometric method using a serial flow cell.

A flow injection-catalytic spectrophotometric method using a serial flow cell was proposed for the successive determination of trace amounts of copper and iron. This method is based on the oxidation coupling of p-anisidine with N,N-dimethylaniline in the presence of hydrogen peroxide to form a dye, which has an absorption maximum at 740 nm. In this indicator reaction, ligands such as 1,10-phenanthroline (phen) and diphosphate were achieved to improve the sensitivity and selectivity. Under the optimal experimental conditions, the determinable ranges were 0.05-5 ppb for copper and 0.5 - 100 ppb for iron, respectively. The RSDs (n = 10) were 0.78% for 0.5 ppb copper(II) and 0.5% for 200 ppb iron(III). The sample throughput was 30 h(-1). The present flow-injection method was applied to the determination of copper and iron in standard river water, tap water, and other natural water samples, and also to the analysis of labile and inert complexes in synthesized samples containing humic acid with copper(II) or iron(III).

Catalytic flow-injection determination of sub-ppb copper(II) using the redox reaction of cysteine with iron(III) in the presence of 2,4,6-tris(2-pyridyl)-1,3,5-triazine.

A kinetic-catalytic spectrophotometric flow-injection method was developed for the rapid and sensitive determination of trace amounts of copper(II). The method is based on the catalytic effect of copper(II) on the redox reaction of cysteine with iron(III). Iron(II) produced by the catalytic reaction reacts with 2,4,6-tris(2-pyridyl)-1,3,5-triazine (TPTZ) to form the iron(II)-TPTZ complex (lambda(max) = 593 nm). By measuring an absorbance of the complex, one could determine 0.05-8 ppb copper(II) with the relative standard deviations (n = 10) of 1.6%, 1.3%, and 0.8% for 0.5 ppb, 1 ppb, and 2 ppb copper(II), respectively. The limit of detection (S/N = 3) was 0.005 ppb. The sample throughput was 30 h(-1). The proposed method was successfully applied to the determination of copper in natural water and serum samples.

Utilization of activating and masking effects by ligands for highly selective catalytic spectrophotometric determination of copper and iron in natural waters.

A kinetic-catalytic spectrophotometric method is proposed for the successive determination of nanogram levels of copper and iron, which is based on their catalytic effects on the oxidative coupling of p-anisidine with N,N-dimethylaniline (DMA) to form a colored compound (lambda(max)=740 nm) in the presence of hydrogen peroxide at pH 3.2. 2,9-Dimethyl-1,10-phenanthroline (neocuproine) acted as an activator for the copper catalysis, and 1,10-phenanthroline (phen) acted as an activator for the iron catalysis. The selectivity was improved in the presence of diphosphate as a masking agent. The determinable ranges were 0.16-10 ppb for copper and 1-100 ppb for iron, respectively. The relative standard deviations of copper and iron were 1.1 and 0.97% for five determinations of 10 ppb copper and 40 ppb iron. The method was successfully applied to the analyses of copper and iron in tap, well, river and pond waters.