Sources of Error in Analysis of Municipal Sludges and Sludge-Amended Soils for Di(2-ethylhexyl) Phthalate
1989
Eiceman, G. A. | Gardea-Torresdey, J. L. | O'Connor, G. A. | Urquhart, N. S.
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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