EQUIPMENT
- Thermo Jarrell-Ash Model 61E ICP
- Thermo Jarrell-Ash Autosampler 300
- 48 position rectangular sample racks
ICP PARAMETERS
1 | Units: | ppm |
2 | Integration time: | 10 seconds |
3 | Flush time: | 45 seconds |
4 | Background correction: | Yes |
5 | Blank subtraction: | No |
6 | Torch gas: | High Flow |
7 | Auxiliary Gas Flow: | Medium (1.0L/min.) |
8 | Nebulizer Press. (PSI): | 33 (adjustable) |
9 | Approximate RF Power: | 1150 watts |
10 | Analysis Pump Rate: | 70-130 rpm (adjustable) |
11 | Flush Pump Rate: | 70-130 rpm (adjustable) |
12 | Purge: | On |
ICP WAVELENGTHS
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STANDARDS
- Stock Solutions: Use 1000 ppm certified, NIST traceable, plasma grade standards for the 12 listed elements.
- Instrument Calibration Standards:
- WAT1 - deionized water.
- EPA2 - Pipet 10 mL of Sb, Ba, Be, Cd, Cr, Cu, Pb, Ni, and Tl stock solutions into a 1 liter volumetric flask. Add 5 mL of nitric acid. Dilute to volume with deionized water and mix well.
- EPA3 - Pipet 10 mL of Ag, Al, and Fe stock solutions into a 1 liter volumetric flask. Add 5 mL of nitric acid. Dilute to volume with deionized water and mix well.
- Instrument Calibration Verification Standards:
- A second set of calibration standards obtained from a different supplier.
ICP PROCEDURE
- Follow the manufacturer's instructions in order to initiate the plasma and the autosampler.
- Select EPA from the methods menu.
- Setup an autosampler table for the set being analyzed.
- Analyze the samples using the autosampler table.
- This table includes instrument calibration standards, the calibration verification standard, quality control sample, as well as client samples.
QUALITY CONTROL
- Following calibration, analyze one EPA2 standard, one EPA3 standard, one calibration verification standard, and one quality control sample.
- EPA2 and EPA3 Standards: Values must be within 2% of the known values.
- Instrument Calibration Verification Standard: All values must be within 10% of the known value.
- Quality Control Sample: Values on at least 10 of the 12 elements reported must be within the "advisory range" established by the supplier of the sample.
- Analyze one EPA2 and one EPA3 standard following the last client sample.
- Values for all elements must be within 8% of the known value.
NOTE
- Fe and Al are not TCLP metals. They are included in the matrix because of inter element interferences observed at the Sb, Tl, and Pb wavelengths.
REFERENCE
- Maxfield, R. and B. Mindak. 1985. EPA Method Study 27, Method 200.7 (Trace Metals by ICP). EPA-600/S4-85/05. National Technical Information Service.