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This article in JEQ

  1. Vol. 18 No. 3, p. 374-379
     
    Received: Oct 6, 1988


    * Corresponding author(s):
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doi:10.2134/jeq1989.00472425001800030023x

Sources of Error in Analysis of Municipal Sludges and Sludge-Amended Soils for Di(2-ethylhexyl) Phthalate

  1. G. A. Eiceman,
  2. J. L. Gardea-Torresdey,
  3. G. A. O'Connor * and
  4. N. S. Urquhart
  1. D ep. of Agronomy and Hortic., New Mexico State Univ., Box 30003, Las Cruces, NM 88003-0003
    D ep. of Experimental Statistics, New Mexico State Univ., Box 30003, Las Cruces, NM 88003-0003.

Abstract

Abstract

Rapid quantitative determination of di-(2-ethylhexyl) phthalate (DEHP) in municipal sludge is described for capillary gas chromatography/mass spectrometry (GC/MS) using selected ion monitoring with isotope dilution techniques. Propagation of error through a four-step technique is measured as an increase in variance with each additional step. Stepwise accumulated variation (as a percentage of total error) was GC/MS analysis with data reduction, 3%; analyst (sample preparation), 8%; heterogeneity of sludge, 30%; heterogeneity in sludge-amended soil, 77%; and errors between planters, 100%. The relative standard deviation (RSD) associated with analysis of sludge alone was 16% at 51 mg kg−1 DEHP. Analysis precision was dependent on sample size and DEHP concentration. The RSD for a 13 mg kg−1 DEHP loading in soil/sludge mixtures for a greenhouse study was 26.5%. Detection limits for DEHP in sludges with rapid screening procedures were fixed by interfering extractable matrices.

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