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

Dep. of Chemistry, New Mexico State Univ., Box 30003, Las Cruces, NM 88003-0003

G. A. O'Connor^*

Dep. of Agronomy and Hortic., New Mexico State Univ., Box 30003, Las Cruces, NM 88003-0003

N. S. Urquhart

Dep. of Experimental Statistics, New Mexico State Univ., Box 30003, Las Cruces, NM 88003-0003.

^* Corresponding author.

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.