A novel high-temperature (360 degrees C)/high-pressure (30 MPa) flow system for online sample digestion applied to ICP spectrometry.
A flow injection sample digestion system has been developed comprising an indirectly electrically heated Pt/Ir capillary. Such a capillary allows reaction temperatures of up to 360 degrees C and pressures of up to 30 MPa (300 bar) and withstands concentrated acids. This temperature is 130 degrees C to 160 degrees C higher compared to the operating temperatures of microwave heated flow systems. A combination of an ultrasonic nebulizer and membrane desolvator serves as an interface between the flow digestion system and an ICP/AES spectrometer. The membrane desolvator removes interfering gaseous digestion products so effectively before the sample stream enters the plasma that the measured residual carbon concentration falls in the region of the detection limit of ICP/OES measurements. Sewage sludge samples were digested using nitric acid and the elemental traces online determined. The detection limits related to the original dry substances amount to the lower microg/g range.
Haiber
S
S
Institut für Spektrochemie und angewandte Spektroskopie, Dortmund, Germany.
Berndt
H
H
D002851:Chromatography, High Pressure Liquid; D017942:Nitric Acid / Q000378:metabolism; D011312:Pressure; D012722:Sewage / Q000737:chemistry*; D013057:Spectrum Analysis / Q000295:instrumentation / Q000379:methods*; D013696:Temperature; D014131:Trace Elements / Q000032:analysis*; D014835:Volatilization
D012722:Sewage; D014131:Trace Elements; D017942:Nitric Acid