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| Author(s): |
Felisberto Gonçalves Santos Junior
Total Authors: 1
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| Document type: | Doctoral Thesis |
| Press: | Piracicaba. |
| Institution: | Universidade de São Paulo (USP). Centro de Energia Nuclear na Agricultura (CENA/STB) |
| Defense date: | 2016-12-07 |
| Examining board members: |
Boaventura Freire dos Reis;
Eder Tadeu Gomes Cavalheiro;
Pedro Sérgio Fadini;
Carlos Eduardo Saraiva Miranda;
Ivo Milton Raimundo Junior
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| Advisor: | Boaventura Freire dos Reis |
| Abstract | |
In this thesis, automated photometric analytical procedures for simultaneous determination of sulfate and chloride in petroleum coke, molybdenum in plants without pre-concentration step and zinc in water using liquid-liquid microextraction were developed. All procedures reported in this thesis, employed flow analysis modules based on multicommuted process, syringe pump for fluid propulsion and solenoid three-way valves as commutation devices the insertion aliquots of sample and reagents solutions in the analytical path. Photometric detections were performed, using LEDs-photometers, built for this project, equipped with flow cells with long optical path (50.0 mm for chloride, sulfate and zinc, 200.0 mm for molybdenum) and the high intense radiation beam LEDs with maximum emission at 472 nm for chloride, sulfate and molybdenum and 525 nm for zinc. The procedures for simultaneous determination of sulfate and chloride showed linear response between 10 to 700 mg L-1; 0.25 to 10 mg L-1; detection limit of 5.3 mg L-1; 0.16 mg L-1; variation coefficient of 3.0%; 0.9% (n = 10), respectively, and sampling throughput of 75 determinations per hour for each analyte. The procedure for molybdenum presented a linear response between 50 to 500 ?g L-1, detection limit of 9.1 ?g L-1, variation coefficient of 1.07% (n = 10) and sampling throughput of 51 determinations per hour. The procedure for zinc showed linear response between 10 to 100 ?g L-1, detection limit of 8.3 ?g L-1, variation coefficient of 3.3% (n = 10) and sampling throughput of 19 determinations per hour (AU) | |
| FAPESP's process: | 13/05728-2 - Development of fluid propelling device and flow analysis module with ability to implement the processes of sequential injection analysis and multicommutation flow analysis |
| Grantee: | Felisberto Gonçalves Santos Junior |
| Support Opportunities: | Scholarships in Brazil - Doctorate |