EQUIPMENT

  1. Thermo Jarrell-Ash Model 61E ICP
  2. Thermo Jarrell-Ash Autosampler 300
  3. 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

1Sb2068
2Ba4934
3Be3130
4Cd2265
5Cr2677
6Cu3247
7Pb2203
8Ni2316
9Tl1908
10Ag3082
11Al3082
12Fe2599

STANDARDS

  1. Stock Solutions: Use 1000 ppm certified, NIST traceable, plasma grade standards for the 12 listed elements.
  2. Instrument Calibration Standards:
    1. WAT1 - deionized water.
    2. 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.
    3. 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.
  3. Instrument Calibration Verification Standards:
    1. A second set of calibration standards obtained from a different supplier.

ICP PROCEDURE

  1. Follow the manufacturer's instructions in order to initiate the plasma and the autosampler.
  2. Select EPA from the methods menu.
  3. Setup an autosampler table for the set being analyzed.
  4. Analyze the samples using the autosampler table.
    1. This table includes instrument calibration standards, the calibration verification standard, quality control sample, as well as client samples.

QUALITY CONTROL

  1. Following calibration, analyze one EPA2 standard, one EPA3 standard, one calibration verification standard, and one quality control sample.
    1. EPA2 and EPA3 Standards: Values must be within 2% of the known values.
    2. Instrument Calibration Verification Standard: All values must be within 10% of the known value.
    3. 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.
  2. Analyze one EPA2 and one EPA3 standard following the last client sample.
    1. Values for all elements must be within 8% of the known value.

NOTE

  1. 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

  1. 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.