| Chapter 1 This chapter reviews the environmental sample pretreatment methods and inorganic chemiluminescence system application in the field of environmental analysis, then summarizes the advantages and disadvantages of the proposed environmental sample pretreatment methods and chemiluminescence analysis. The combination of sample pretreatment methods with chemiluminescence analysis is feasible and necessary.Chapter 2 Chemiluminescence flow injection system combined with on-line solid phase extraction has been developed for the determination of phenol in water samples. The principle is based on the enhancement of phenol on luminol/NaOH-KMnO4 chemiluminescent system. Installation of SPE column in the manifold provides a convenient pathway to simultaneous sample preparation and sample introduction for analysis. The on-line SPE was introduced to this system which can greatly enrich phenol, improved the detection limit, and effectively alleviate the matrix interference. Parameters that influenced the efficiency of the proposed method, including solution concentration, flow rate and extraction time, ratio of eluant were optimized. HPLC was also be used to confirm the adsorption and elution ability and reused capability of the SPE particles.The proposed method has been successfully applied to determinate phenol in tap water, lotus pool water, reclaimed water and seawater. Under the optimal conditions, the linear range of this method is 0.01-15 mg L-1 for phenol. The detection limits is 0.005 mg L-1.Chapter 3 An on-line solid phase extraction device combined with flow-injection chemiluminescence system was presented for the enrichment and determination of humic acid (HA) in water samples. The chemiluminescence principle was based on the enhancement effect of HA on Ce(Ⅳ)/H2SO4-rhodanmine 6G chemiluminescence system. For sample treatment, the on-line solid-phase extraction (SPE) material was packed into a cartridge first and then the cartridge was installed in the manifold. Parameters that influenced the efficiency of the proposed method, including reagent concentration, flow rate and extraction time, were optimized. Under the optimized conditions, the relative standard deviation was 3.6% for determining 2 mg L-1 HA standard and the detection limit was 3μg L-1. The proposed method was successfully applied to the determination of HA in the range of 0.1 mg L-1 to 35 mg L-1. The results were validated by spiked standard experiment. The recovery was from 73.6% to 121%. Chapter 4 An auto analytical instrument for the detection of trace phenol and humic acid was developed. The principle of the analyzer is based on flow injection chemiluminescence analysis. The light signal was detected by a photomultiplier tube (PMT) and converted to analog signal. Then the analog signal was pre-amplified by ultralow input bias current operational amplifier AD 549 and subsequently converted into digital signal by a ADS1258. The analyzer collected data via STM32 F103 as a microprocessor, sends data to software by USB interface. The software translated by Visual C++ 6.0 is used for real-time monitoring. I/O interface in microprocessor is to control the eight solenoid valves open/close and the rates of the five peristaltic pumps are determined by the RS 485 interface. RS 232 serial interface and central control system are made to finish data communication. An analytical method based on this instrument was established and it can determine the amount of the trace phenol and humic acid in surface, middle and bottom seawater within 34 min. The phenol and humic acid was detected using CL system of luminol/NaOH-KMnO4 and acidic Ce(IV), respectively. The limit of detection (LOD) was 0.01 mg L-1 for phenol) and 0.005 mg L-1 for humic acid. The analyzer has been applied for seawater detection on-line. |
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