Document 93jN63EBLnMZdVXxVZZx4YbX5

ES-80-SS-27 Page I MEASUREMENT OF SELECTED CHEMICALS IN SOIL FROM THE DEAD CREEK SITE QUALITY ASSURANCE INTRODUCTION Following media reports and subsequent Illinois EPA concern about hazardous chemicals at the Dead Creek site near Sauget, Illinois, personnel from Monsanto's W. G. Knmmrich Plant sampled several areas at the site. Samples were submitted to Environmental Sciences for analyses for polychlorinated biphenyls, elemental phosphorus, chlorinated benzenes, chlorinated phenols, phosphate esters, and metals. During the various determinations, replicates and spiked samples were analyzed to evaluate the performance of the method used for these particular samples. SUMMARY This report suaeearlzes the quality assurance results obtained for various samples analyzed during the course of this project. The accuracy (recovery from spiked samples) and precision (relative standard deviation of replicate determinations) results are tabulated herein. Although It would be difficult to summarize the overall performance of the methods for all the analytes. In general, the methods performed at the recovery and precision levels established during method valida tion. DETAILS Analytical Methods The soil samples were analyzed for the various chemicals using established pro cedures or methods developed and validated for the chemicals of Interest In soil. The following list tabulates the methods which were used. Analyte Method No. Title Polychlorinated 81phenyls ES-80-M-28 Determination of Polychlorinated Biphenyls In Soil and Sediment Chlorinated Benzenes ES-80-M-29 Determination of Chlorinated Benzenes in Soil and Sediment Chlorinated Phenols ES-80-M-30 Determination of Chlorinated Phenols in Soil and Sediment Elemental E5-80-M-24 Phosphorus (P,,) Determination of Elemental Phosphorus (P*) in Soil and Sediment Phosphate Esters ES-80-M-5 Determination of Group I Compounds in Sediments . . . Metals Ref. 1, 2 Inductively Coupled Plasma (ICP) . . . Method for Trace Element Analysis of Water and Wastes Arsenic Ref. 3 Methods for Chemical Analysis of water and Wastes - Arsenic HONS 022344 ES-80-SS-27 Page 2 Ml determinations were carried out in strict accordance with these methods, except that the polychlorinated biphenyls, chlorinated benzenes and phosphate esters were measured In extracts from acidified samples to facilitate determi nation of chlorinated phenols in the same extracts. Results The results for the determinations of the compounds of interest have been report ed In Special Studies ES-80-SS-24, 25, and 26, Measurement of Selected Chemicals In Soil from the Dead Creek Site . . . This Special Study is a compilation of the quality assurance results for all three Special Studies. Quality Assurance The recovery and precision results for the determinations are tabulated in Tables I-V. Each table contains the results for all quality assurance samples for a specific group of compounds. Recovery results are reported as percent recovery, calculated as S Recovery * Concentr*tion (sample + spike)- average concentration x 1Q0 Concentration (spike added) Precision results are reported as percent relative standard deviation (RSD) for replicate determinations. The tables present the recovery and precision results In concentration ranges (1-10 ppm to 10,000 - 100,000 ppm). The entries are averages of all values for all samples which had either recovery or precision evaluated In that range. All values are for actual samples except the metals recovery results, which are for spiked blank soil. In the recovery column, NE means Not Evaluated, l.e., no samples were spiked In that concentration range, and NO means Not Determinable, l.e., the spiking level was too low (usually <501) compared to the level actually In the sample. In the precision columns, NE means Not Evaluated, i.e., no repli cates were analyzed which contained the analyte in that concentration range. More detailed compilations of the accuracy and precision results can be found in Reference 4. REFERENCES 1. Methods for Chemical Analysis of Waters and Wastes, EPA-600/4-79-020, page: Metals - 6, Section 4.1.3. 2. Federal Register, Vol. 44, No. 233, Oecember 3, 1979. 3. Methods for Chemical Analysis of Water and Wastes, EPA-600/4-79-020, Method 206 - Arsenic, pages: 206.2-1 to 206.5-2. 4. RGK NBP 1914831 HONS 022345 RECOVERY ANO PRECISION IR1C I. PC ANO ELEMENTAL PHOSPHORUS (PQ IN DEAD CREEK SOU SAMPLES ANALYTE LEVEL 1-10 ppm X lltec USO PCI** (Cl, to Cl* HnmIqos) NO NE 10-100 pn X Ntc MSP 100-1,000 mm X Rac ijgO 70S 171 120X 18X 1,000-10,000 pp 10,000-100,000 w I Rec XNSO tc X USD 77X S8X NC OX P* 561 NE NE NE RE NC NE NE NE NE c **' SS-Ot-SJ U HONS Oi2346 RECOVERY AMD PRECISION INKE II. CIIMMENZENES IN DEAD CREEK SOIL SAMPLES MMIVH X level X 1-10 % dec PtPRSO NOROCM.OROKHZENE 1051 he r-UICHLOROKHZENC 120% 2IX 0-UIO8.0R0KHZIHE 125% 16% 1RICHL0R0REHZEHES (3) 961 14% K1IMCI10MRER2EHES (3) 110% 9% KRTACM.0MSEH2CHE 1401 12% M OCHIOROWRZERE 135% 13% RI1ROCM.OROKNZCHES (O-.P-) 125% 37% 10-100 ppa 1 Roc % RSO 110% RE 125% 64% 120% ME 110% 13% 120% RE 120% RE 90% RE 120% RE 100-1 ,000 ppm % Rec % RSO 100% RE 120% RE 120% 8% 120% RE 1301 RE 140% HE 110% HE 120% 26% i i s i Io i-u HONS 022347 RECOVERY ANO PRECISION in. CHLowmwis m dead creek sou swus ANALYTE x\LEVEL 1-IO I Arc pf % RSO O-CWOAOPttAOl H-CMLOAOPHENOL 2.4-DICHLOROfHEHOL PENIACMLOROPHENOt 19% 34% 36% 26% 66% 47% 160% 46% 10-100 PfMR % Rec % RSO 64% HE 16% HE 59% HE 40% HE 100-1,000 pm % Ik % RSO 50% HE 30% HE 50% HE 36% 20% (i-s sSo rHiad HONS 0223W RECOVERY AMO PRECISION MAIVH S\UVU 1-10 ppM \ 1 Rk 1 ASO DltUtVlPHENYL PHOSPHATE mnnmmm PHOSPHATE 751 1201 NE 421 lNIPHCNVl PHOSPHATE 1201 891 2-ETHUHllYlDIPHENYl PHOSPHATE 901 471 iswtcnoiPHum. PHOSPHATE T-BHTYLPHENYIOIPHENYI PHOSPHAIC NE 701 NE HE 01 - T-IUTYIPMENYIPHENU PHOSPHATE 881 NE NDHYIPHEHYIDIPHENYI PHOSPHATE 841 ax UOfftPHENYlDIPHENYl PHOSPHATE 621 211 10 100 ppM 1 Rk 1 RSD 1301 1151 1201 1101 NE NE NE NE NE NE 921 1001 961 NE 761 NE 761 NE 100-1 ,000 PPM 1 Rtc 1 RSD 1201 121 NE 1151 1151 NE NE NE NE 1001 NE NE NE NE 961 NE 881 NE 1,000-10,000 1 Rm 1 RSD NE NE NE NE NE 61 NE NE NE NE NE NE NE NE HI NE NE NE I *t>4 M-M-S3 - a HONS 022349 RECOVERY ARO PRECISION 1*RL!:_, NRTW.S IN OEM) CREEK SOIL SAMPLES ANALYTE . level \ I 1-10 R*c T,so SILVER HE NE ALUMINUM NO NE BARIUM NO NE BERYLLIUM 90S NE IORON 01 NE CALCIUM NO NE CRMIW COBALT 891 5.2S Sit NE CHROMIUM com* 271 NE OS NE IRON NO NE MAGNESIUM MHWEX NO NE NO NE MOLYBDENUM 531 NE SODIUM NO NE NICKEL OS NE LEAD OS NE MOSPNURUS NO NE ANTIMONY OS NE SILICON NO NE TIN 80S NE STRONTIUM TITANIUM 81S NE NO HI VANADIUM NO NE /INC NO NE ARSENIC (By AA) NE NE 1-TOO S tec Trsd NE 461 NO NE NO NE 90S NE 65S 19S NO NE 97S 1TSS 21S 6.St 109S ms 20S 66S NO NE NO NE NO in 831 ns NO NE 100S MS tfiSK 21S NO NE 27S 2.9S NO 85X lost NE 5.fit 3.31 99S 30S NO 1391 13S 34S NE NE 100-1 S tec "SSSS NE NE NO NE 89S 37S 941 NE BIS 31 NO NE 961 NE 97S 5.IS 91S 6.41 90S NE NO NE NO NE NO 101 831 NE NO MS 91S 131 93S NE NO 101 27S 131 OS 491 96S SMS 94S 6.51 301 1.31 1201 87S 111 NE NE NE . 1000-10 ,000 pfM S Rec 1 RSD NE NE NE 6.51 NE OX NE NE NE NE NE 8.31 NE m NE NE NE NE NE NE NE NE NE 7.81 NE NE NE NE NE NE NE 4.51 NE 6.5S NE 171 NE NE NE NE NE NE NE NE NE NE NE NE NE 8.91 NE NE 10,000-100,008 pfm 1 Rk 1 RSD NE RE NE NE NE NE NE NE NE NE NE 7.51 NE NE NE NE NE NE NE 111 NE 8.11 NE NE NE NE NE NE NE NE NE NE NE NE NE 7.91 NE NE NE NE NE NE NE NE NE NE NE NE NE 161 NE NE i *U HONS 022350 Submitted by: Prepared by: Approved by: ES-80-SS-27 Page 8 Monsanto Industrial Chemicals Company Environmental Sciences Section - HIE 800 North Lindbergh Boulevard St. Louis, Missouri 63166 Robaerrt G. Kaley, Yr ' Research Group Leader dJtu James P. Miieduuire Manager, Environmental Sciences MONS 022351