INTRODUCTION - SR99_120007
Table 1. Analytes of interest for two applications of analytical methods for explosives in soil: Hazardous waste characterization and mine detection.
Extraction
Instrumentation - SR99_120010
Figure 1. Correlation analysis of GC-ECD concentration (mg/kg) estimates with those from HPLC-UV analysis using splits of the same acetonitrile extract (2 g soil:10 mL acetonitrile) from archived soils.
Figure 1. Correlation analysis of GC-ECD concentration (mg/kg) estimates with those from HPLC-UV analysis using splits of the same acetonitrile extract (2 g soil:10 mL acetonitrile) from archived soils. - continued
Figure 2. Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile).
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile).
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120015
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120016
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120017
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120018
Confirmation columns - SR99_120019
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery.
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120021
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120022
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120023
Drying of samples
Table 3. Concentrations of analytes found in dry and moist AEC soil exposed at room temperature for one week to vapor from Kodak TNT.
Table 3. Concentrations of analytes found in dry and moist AEC soil exposed at room temperature for one week to vapor from Kodak TNT. - continued
Drying of samples - continued
Table 4. Concentrations of analytes found in dry and moist Fort Leonard Wood soil exposed at room temperature for 68 days to vapor from Yugoslavian TNT.
Minefield samples
Minefield samples - continued
Table 6. Most common analytes detected in soils collected from an experimental minefield at Fort Leonard Wood two months after the mines were emplaced. The relative percent differences (%) are shown in parentheses for replicates.
Figure 6. GC-ECD chromatograms of soil extracts from a minefield sample.
Figure 7. Correlation analysis of GC-ECD concentration (g/kg) esti- mates with those from HPLC-UV analysis using splits of the same acetonitrile extracts from soils collected from an experimental minefield.
Table 7. Comparison of concentration estimates obtained using small (2-g) soil subsamples to those obtained from large (20-g) subsamples.
LITERATURE CITED - SR99_120035
APPENDIX A: DATA.
Table A1. HPLC and GC concentration estimates (mg/ kg) for field-contaminated soils using the Method 8330 extraction procedure (2 g soil:10 mL acetonitrile).
Table A1. HPLC and GC concentration estimates (mg/ kg) for field-contaminated soils using the Method 8330 extraction procedure (2 g soil:10 mL acetonitrile). - continued
Table A2. GC concentration estimates (g/kg) for field-contaminated soils and matrix spikes/ matrix spike duplicates (MS/MSD). 25-g soil subsamples were extracted with 50 mL of acetonitrile. Spiked concentration was 10 g/kg for the nitroaromatics and 40 g/kg for RDX.
Table A2. GC concentration estimates (g/kg) for field-contaminated soils and matrix spikes/ matrix spike duplicates (MS/MSD). 25-g soil subsamples were extracted with 50 mL of acetonitrile. Spiked concentration was 10 g/kg for the nitroaromatics and 40 g/kg for RDX. - continued
Table A3. Retention times (min) on analytical and confirmation columns.
Table A4. Found concentrations (g/kg) and method detection limits determined from spiked soils (2 g soil:10 mL acetonitrile) after 18 hr of sonication.
Table A5. Found concentrations (g/kg) and recoveries determined from 2-g spiked soil samples extracted with 10 mL acetonitrile by 18 hr of sonication. Target concentration was 50 g/kg.
Table A6. NG and PETN concentrations (g/kg) found in spiked soils (2 g) extracted with 10 mL acetonitrile for 2 hr and 18 hr in a cooled sonic bath. Target concentration was 50 g/kg.
Table A7. Method detection limits from 25 g Ottawa sand aged 1 hr after spiking and then extracted with 50 mL acetontrile (3,4-DNT internal standard).
Table A9. Recovery (%) from 25-g soil samples spiked at 10 g/kg and aged 24 hr prior to extraction with 50 mL acetonitrile.
REPORT DOCUMENTATION PAGE - SR99_120047
SR99_12
Table 1. Analytes of interest for two applications of analytical methods for explosives in soil: Hazardous waste characterization and mine detection.
Extraction
Instrumentation - SR99_120010
Figure 1. Correlation analysis of GC-ECD concentration (mg/kg) estimates with those from HPLC-UV analysis using splits of the same acetonitrile extract (2 g soil:10 mL acetonitrile) from archived soils.
Figure 1. Correlation analysis of GC-ECD concentration (mg/kg) estimates with those from HPLC-UV analysis using splits of the same acetonitrile extract (2 g soil:10 mL acetonitrile) from archived soils. - continued
Figure 2. Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile).
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile).
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120015
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120016
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120017
Figure 2 (cont'd). Chromatograms from field-contaminated soils (25 g extracted with 50 mL acetonitrile). - continued - SR99_120018
Confirmation columns - SR99_120019
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery.
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120021
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120022
Figure 5. GC-ECD chromatograms of blank and spiked soils used for determination of method detection limits and spike recovery - continued - SR99_120023
Drying of samples
Table 3. Concentrations of analytes found in dry and moist AEC soil exposed at room temperature for one week to vapor from Kodak TNT.
Table 3. Concentrations of analytes found in dry and moist AEC soil exposed at room temperature for one week to vapor from Kodak TNT. - continued
Drying of samples - continued
Table 4. Concentrations of analytes found in dry and moist Fort Leonard Wood soil exposed at room temperature for 68 days to vapor from Yugoslavian TNT.
Minefield samples
Minefield samples - continued
Table 6. Most common analytes detected in soils collected from an experimental minefield at Fort Leonard Wood two months after the mines were emplaced. The relative percent differences (%) are shown in parentheses for replicates.
Figure 6. GC-ECD chromatograms of soil extracts from a minefield sample.
Figure 7. Correlation analysis of GC-ECD concentration (g/kg) esti- mates with those from HPLC-UV analysis using splits of the same acetonitrile extracts from soils collected from an experimental minefield.
Table 7. Comparison of concentration estimates obtained using small (2-g) soil subsamples to those obtained from large (20-g) subsamples.
LITERATURE CITED - SR99_120035
APPENDIX A: DATA.
Table A1. HPLC and GC concentration estimates (mg/ kg) for field-contaminated soils using the Method 8330 extraction procedure (2 g soil:10 mL acetonitrile).
Table A1. HPLC and GC concentration estimates (mg/ kg) for field-contaminated soils using the Method 8330 extraction procedure (2 g soil:10 mL acetonitrile). - continued
Table A2. GC concentration estimates (g/kg) for field-contaminated soils and matrix spikes/ matrix spike duplicates (MS/MSD). 25-g soil subsamples were extracted with 50 mL of acetonitrile. Spiked concentration was 10 g/kg for the nitroaromatics and 40 g/kg for RDX.
Table A2. GC concentration estimates (g/kg) for field-contaminated soils and matrix spikes/ matrix spike duplicates (MS/MSD). 25-g soil subsamples were extracted with 50 mL of acetonitrile. Spiked concentration was 10 g/kg for the nitroaromatics and 40 g/kg for RDX. - continued
Table A3. Retention times (min) on analytical and confirmation columns.
Table A4. Found concentrations (g/kg) and method detection limits determined from spiked soils (2 g soil:10 mL acetonitrile) after 18 hr of sonication.
Table A5. Found concentrations (g/kg) and recoveries determined from 2-g spiked soil samples extracted with 10 mL acetonitrile by 18 hr of sonication. Target concentration was 50 g/kg.
Table A6. NG and PETN concentrations (g/kg) found in spiked soils (2 g) extracted with 10 mL acetonitrile for 2 hr and 18 hr in a cooled sonic bath. Target concentration was 50 g/kg.
Table A7. Method detection limits from 25 g Ottawa sand aged 1 hr after spiking and then extracted with 50 mL acetontrile (3,4-DNT internal standard).
Table A9. Recovery (%) from 25-g soil samples spiked at 10 g/kg and aged 24 hr prior to extraction with 50 mL acetonitrile.
REPORT DOCUMENTATION PAGE - SR99_120047
SR99_12
