The TQ-ICP-MS can be used for the determination of metals and semi-metals in the trace and ultra-trace range in aqueous solutions.
Equipment
Supported by the German Research Foundation (FKZ INST 275/441-1 FUGGExternal link).
8900 Triple Quadrupole ICP-MS (Fa. Agilent, Waldbronn, Deutschland)
For feeding of liquid samples an autosampler (prepFAST4DX System, Fa. Elemental Scientific, Mainz, Germany) is available.
Sample preparation
Liquid samples (a volume of at least 5 mL is required, if less volume is available please contact Dirk Merten in advance) must be free of particles (filtration < 0.45 μm or suitable centrifugation).
Subsequent to filtration samples must be acidified to pH<2 using HNO3. Samples must delivered with a list of electrical conductivities prior to acidification. If samples originate from extractions or the digestion of solid samples the used weight of the solid samples and the volume, concentration and kind of extracting solutions have to be delivered.
Quality Assurance
Calibration is performed using multi element standards having concentrations of 0, 1, 5, 10, 50 and 100 μg/L of each element to be analysed. For details please see heredocx, 14 kb · de
Accuracy of the measurements is verified using standard reference materials:
20 μg/L Ru and 10 μg/L Re are added as internal standards to all blanks, calbration standards, refrence materials and samples for drift corection. Alle solutions have a final concnetration of at least 2% HNO3
Samples will be diluted to a total dissolved solids below 1 g/L according to their matrix or their electrical conductivity for water samples, respectively.
For each sample three replicate measurements are performed, an outlier test according to Grubbs (sgnificance 90%) is carried out and subsequently mean and the single absolute standard deviation are calculated and reported with the results.
The detection limit is calculated for each measurement based on the 3 σ crteroin, taking the dilution of the sample into account.
Detection limits are reported with the results if concentration of one or more of the elements is below the respective detection limit.