Southern Maryland Wood Treating
US Army Corps
Of Engineers,
Baltimore District
Contract Number
DACW 31-01-C-0018
Post-closure Monitoring Report
Quarter 3, September 2002
Southern Maryland Wood Treating
Hollywood, Maryland
- Prepared for
- United States Army Corp of Engineers
- Prepared by
- Resource Management Concepts, Inc.
Lexington Park, Maryland 20653
Appendix D: Data Validation Reports
This data validation report is for the groundwater samples collected for the Post-Closure Monitoring at SMWT Site (Hollywood, MD) on September 10-13, 2002. Samples were analyzed for PAHs compounds using SW-846 Method 3510C/8310. A total of 11 aqueous samples were validated; the sample IDs are:
| Field Sample ID | Lab. Sample ID |
|---|---|
| MW21D | C2I130265-001 |
| MW13 | C2I130265-002 |
| MW14 | Not Sampled |
| MW27R | Not Sampled |
| MW37D | C2I120209-003 |
| MW38 | C2I120209-001 |
| MW32 | C2I130265-005 |
| MW36 | C2I160145-001 |
| MW17R | C2I130265-004 |
| MW20D | C2I130265-003 |
| MW33 | C2I110240-001 |
| MW34D | C2I110240-002 |
| MW35 | C2I120209-002 |
| EQUIP. RINSATE BLANK | C2I160145-002 |
| FIELD BLANK | C2I160145-003 |
The data was reviewed by RMC, Inc. personnel and validated using a combination of method-specific criteria, laboratory Standard Operatingon Procedures (SOPs), and the Innovative Approach to Data Validation for USEPA Region III (June 1995). Parameters evaluated under data validation procedure Level M3 are presented in Table 5. Data associated with parameters in compliance with quality control specifications have not been qualified. Data associated with parameters that did not comply with quality control specifications and directly impacted project data have been qualified in accordance with USEPA Region III specifications.
Table 5: Laboratory Performance Criteria
| Qualified | Parameter | |
|---|---|---|
| Yes | No | |
| X | Holding Times | |
| X | Blank Analysis | |
| X | Initial Calibration | |
| X | Continuing Calibration | |
| X | System Monitoring Compounds | |
| X | Laboratory Control Sample/LCS Duplicate | |
| X | Quantitation Verification | |
The quality of data collected in support of this sampling activity is considered acceptable with applicable qualifications.
I Holding Times
Form 1
The objective is to ascertain the validity of results based on the holding time of the sample from time of collection to time of sample extraction and analysis. For PAH compounds in cooled (@4º C + 2º C) aqueous samples, the maximum holding time is seven days from sample collection to extraction and 40 days from extraction to analysis.
- The samples were collected on September 10 through September 13, 2002, and analyzed on September 18 through September 19, 2002. All criteria were met. No qualifiers were applied.
II Initial Calibration
Form V1 and Chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for PAH target compounds. Initial calibration demonstrates that the instrument is capable of acceptable performance in the beginning of the analytical run and of producing a linear curve. The percent relative standard deviation of the calibration factors (%RSD) should be < 20%. If linear regression is used, the correlation coefficient must be > 0.990 for all target compounds.
- For initial calibrations performed on instrument GC7 (column 1) on September 17, 2002, all criteria were met. No qualifiers were applied.
III Continuing Calibration
Form VII and Chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for target compounds. Continuing calibration establishes that the initial calibration is still valid. It also establishes the 12-hour relative response factors on which the quantitations are based and checks satisfactory performance of the instrument on a day-to-day basis. The percent difference (%D) between the initial calibration factor (CF) and the continuing CF must be < 15 %.
- For continuing calibration performed on instrument GC7 (Columns 1 and 2) on September 17, 2002, @1129, all qualifications were met. No qualifiers were applied.
- For continuing calibration performed on instrument GC7 (Columns 1 and 2) on September 18, 2002, @1731, all qualifications were met. No qualifiers were applied.
- For continuing calibration performed on instrument GC7 (Columns 1 and 2) on September 19, 2002, @0552, the standard benzo(a)pyrene was outside the +/- 15% D criteria. The average of all standards were with in the criteria. No qualifiers were applied.
- For continuing calibration performed on instrument GC7, (Columns 1 and 2) on September 20, 2002, @1010, all qualifications were met. No qualifiers were applied.
- For continuing calibration performed on instrument GC7 (Columns 1 and 2) on September 20, 2002, @1724, all qualifications were met. No qualifiers were applied.
IV Blank Analysis
Form I, IV, and Chromatograms
The purpose of blank analysis is to determine the presence and magnitude of contamination problems resulting from field or laboratory activities. No contaminants should be detected in any of the associated blanks. Positive sample results are qualified "B" if the concentration of analyte is < five times (5x) the absolute maximum blank concentration.
No contaminants were detected in the intra lab blank. All criteria were met. No qualifiers were applied.
V System Monitoring Compounds (Surrogates)
Form II and Chromatograms
Laboratory performance on individual samples is established by means of spiking activities. All samples are spiked with surrogate compound(s) prior to sample preparation. Surrogate-spiked recoveries must be within the specified control limits. When surrogates have percent recoveries below the control limit, positive sample results are qualified as biased low ("L") and non-detects ("UL"). Table 6 summarizes the surrogate recovery analysis.
Table 6: Surrogate Recovery Analysis
| Field Sample # | S1-Column 1% R* | S1-Column 2% R* | S2-Column 1% R* | S2-Column 2% R* | Qualifiers |
|---|---|---|---|---|---|
| MW21D | 94 | 95 | 100 | 95 | |
| MW13 | 88 | 89 | 93 | 89 | |
| MW14 | Not sampled. | ||||
| MW27R | Not sampled. | ||||
| MW37D | 94 | 94 | 102 | 94 | |
| MW38 | 87 | 87 | 92 | 86 | |
| MW32 | 91 | 92 | 95 | 92 | |
| MW36 | 82 | 82 | 87 | 83 | |
| MW17R | 91 | 92 | 96 | 92 | |
| MW20D | 92 | 92 | 97 | 92 | |
| MW33 | 93 | Not analyzed | 95 | Not analyzed | |
| MW34D | 93 | Not analyzed | 94 | Not analyzed | |
| MW35 | 93 | 93 | 98 | 92 | |
| EQUIP. RINSATE BLANK | 91 | 91 | 95 | 91 | |
| FIELD BLANK | 87 | 87 | 92 | 88 | |
* % R = % Recovery
Control Limit
- (S1) p-Terphenyl
- (75-138%R)
- (S2) Benzo (e) pyrene
- (71-131%R)
VI Laboratory Control Sample/LCS Duplicate
Form III and Chromatograms
Data for laboratory control samples are generated to determine long-term precision and accuracy of the analytical method on various matrices. Percent recoveries must be within the specified method control limits.
- All criteria were met. No qualifiers were applied.
VII Quantitation Verification
Form 1 and Chromatograms
The accuracy of the analytical results is verified through the calculation of several parameters. The percent difference (%D) between the calculated and reported values must be within 10%. Any positive value < RL (reporting limit) and > MDL (method detection limit) is reported as estimated "J." Positive results must be confirmed on a secondary chromatographic column. When the percent difference between the results calculated from each column is more than 40%, the reported results are qualified as estimate "J."
Sample: MW36 (C2I160145-001) Column 1, p-terphenyl
Conc. μg/L = Amt * DF * Vt / Vo / Vi
where:
- Amt is the amount on-column (ng)
- DF is the dilution factor
- Vt is the volume of final extract (μL)
- Vo is the volume of the sample extracted (μL)
- Vi is the injection volume (μL)
Conc. μg/L = 8.15697 ng * 1 * 1,000 μL / 1,000 mL / 1.0 μL = 8.15697μg/L
- Reported Concentration = 8.157 μg/L
- %D = (1-| Concentration Calculated (μg/L) / Reported Concentration (μg/L)|) * 100
- %D = -0.00037%
- Values were within 10% difference
Sample: MW36 (C2I160145-001) Column 2, p-terphenyl
Conc. μg/L = Amt * DF * Vt / Vo / Vi
where:
- Amt is the amount on-column (ng)
- DF is the dilution factor
- Vt is the volume of final extract (μL)
- Vo is the volume of the sample extracted (μL)
- Vi is the injection volume (μL)
Conc. μg/L = 8.23902 ng * 1 * 1,000 μL / 1,000 mL / 1.0 μL = 8.23902 μg/L
- Reported Concentration = 8.239 μg/L
- %D = (1-| Concentration Calculated (μg/L) / Reported Concentration (μg/L)|) * 100
- %D = -0.00024%
- Values were within 10% difference
This data validation report for groundwater samples collected for the Post-Closure Monitoring at SMWT Site (Hollywood, MD) on September 10 through September 13, 2002. Samples were analyzed for gas chromatography/mass spectrometry (GC/MS) semivolatile compounds using SW-846 Method 8270C. A total of 11 aqueous samples were validated; the sample IDs are:
| Field Sample ID | Lab. Sample ID |
|---|---|
| MW21D | C2I130265-001 |
| MW13 | C2I130265-002 |
| MW14 | Not Sampled |
| MW27R | Not Sampled |
| MW37D | C2I120209-003 |
| MW38 | C2I120209-001 |
| MW32 | C2I130265-005 |
| MW36 | C2I160145-001 |
| MW17R | C2I130265-004 |
| MW20D | C2I130265-003 |
| MW33 | C2I110240-001 |
| MW34D | C2I110240-002 |
| MW35 | C2I120209-002 |
| EQUIP. RINSATE BLANK | C2I160145-002 |
| FIELD BLANK | C2I160145-003 |
The data was reviewed by RMC, Inc., personnel and validated using a combination of method-specific criteria, laboratory SOP, and the Innovative Approach to Data Validation for USEPA Region III (June 1995). Parameters evaluated under data validation procedure Level M3 are presented in Table 7. Data associated with parameters in compliance with quality control specifications have not been qualified. Data associated with parameters that did not comply with quality control specifications and directly impacted project data have been qualified in accordance with USEPA Region III specifications.
Table 7: Laboratory Performance Criteria
| Qualified | Parameter | |
|---|---|---|
| Yes | No | |
| X | Holding Times | |
| X | Blank Analysis | |
| X | Initial Calibration | |
| X | Continuing Calibration | |
| X | System Monitoring Compounds | |
| X | Laboratory Control Sample/LCS Duplicate | |
| X | Quantitation Verification | |
The quality of data collected in support of this sampling activity is considered acceptable with applicable qualifications.
I Holding Times
Form 1
The objective is to ascertain the validity of results based on the holding time of the sample from time of collection to time of sample extraction and analysis. For semivolatile compounds in cooled (@4º C + 2º C) aqueous samples, the maximum holding time is seven days from sample collection to extraction and 40 days from extraction to analysis.
- The samples were collected on September 10 through September 13, 2002 and analyzed on September 25 through October 1, 2002. All criteria were met. No qualifiers were applied.
II Initial Calibration
Form V1 and Chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for semivolatile target compounds. Initial calibration demonstrates that the instrument is capable of acceptable performance in the beginning of the analytical run and of producing a linear curve. The percent relative standard deviation of the calibration factors (%RSD) should be < 20%. If linear regression is used, the correlation coefficient must be > 0.990 for all target compounds.
- For initial calibration performed on instrument GC 731 (column 1) on September 25, 2002, the %RSD for standards dinitrophenol, 2-naphthylamine and benzaldehyde was > 20%. No qualifiers were required.
III Continuing Calibration
Form VII and Chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for target compounds. Continuing calibration establishes that the initial calibration is still valid. It also establishes the 12-hour relative response factors on which the quantitations are based and checks satisfactory performance of the instrument on a day-to-day basis. The percent difference (%D) between the initial CF and the continuing CF must be < 15 %.
- For continuing calibration performed @ 1155 on instrument GC731 (Column 1) on September 25, 2002, the standards for 2-naphthylamine and benzidine were > 15% D. No qualifiers were applied.
- For continuing calibration preformed @ 0802 on instrument GC731 (Column 1) on October 1, 2002, the standards for benzoic acid, 2-naphthylamine, and benzaldehyde were > 15% D. No qualifiers were applied.
IV Blank Analysis
Form I, IV, and Chromatograms
The purpose of blank analysis is to determine the presence and magnitude of contamination problems resulting from field or laboratory activities. No contaminants should be detected in any of the associated blanks. Positive sample results are qualified "B" if the concentration of analyte is < five times (5x) the absolute maximum blank concentration.
- The intra lab blank showed a concentration of bis(2-Ethylhexyl)phthalate greater than the MDL and the reporting limit. All samples associated with the intra-lab blank showing a concentration of bis(2-Ethylhexyl)phthalate are qualified "B."
V System Monitoring Compounds (Surrogates)
Form II and Chromatograms
Laboratory performance on individual samples is established by means of spiking activities. All samples are spiked with surrogate compound(s) prior to sample preparation. Surrogate-spiked recoveries must be within the specified control limits. When surrogates have percent recoveries below the control limit, positive sample results are qualified as biased low ("L") and non-detects ("UL"). Table 8 summarizes the surrogate recovery analysis.
Table 8: Surrogate Recovery Analysis
| Field Sample # | Surrogate 1 %R* | Surrogate 2 %R* | Surrogate 3 %R* | Surrogate 4 %R* | Surrogate 5 %R* | Surrogate 6 %R* | Qualifiers |
|---|---|---|---|---|---|---|---|
| MW21D | 60 | 77 | 77 | 84 | 67 | 79 | |
| MW13 | 63 | 65 | 63 | 70 | 63 | 71 | |
| MW14 | Not sampled. | ||||||
| MW27R | Not sampled. | ||||||
| MW37D | 82 | 70 | 73 | 79 | 62 | 59 | |
| MW38 | 71 | 67 | 66 | 75 | 71 | 78 | |
| MW32 | 69 | 67 | 68 | 73 | 65 | 79 | |
| MW36 | 94 | 81 | 74 | 88 | 75 | 73 | |
| MW17R | 69 | 68 | 63 | 72 | 63 | 81 | |
| MW20D | 66 | 67 | 66 | 73 | 62 | 72 | |
| MW33 | 74 | 66 | 68 | 74 | 67 | 59 | |
| MW34D | 80 | 69 | 75 | 78 | 64 | 76 | |
| MW35 | 83 | 73 | 77 | 79 | 77 | 76 | |
| EQUIP. RINSATE BLANK | Not analyzed. | ||||||
| FIELD BLANK | 95 | 78 | 66 | 80 | 67 | 75 | |
* % R = % Recovery
Control Limit
- (Surrogate 1) 2,4,6-Tribromophenol
- (21-122 %R)
- (Surrogate 2) 2-Fluorobiphenyl
- (30-110 %R)
- (Surrogate 3) 2-Fluorophenol
- (13-110 %R)
- (Surrogate 4) Nitrobenzene-d5
- (32-112 %R)
- (Surrogate 5) Phenol-d5
- (10-113 %R)
- (Surrogate 6) Terphenyl-d14
- (10-144 %R)
- All criteria were met. No qualifiers were applied.
VI Laboratory Control Sample/LCS Duplicate
Form III and chromatograms
Data for laboratory control samples are generated to determine long-term precision and accuracy of the analytical method on various matrices. Percent recoveries must be within the specified method control limits.
- All criteria were met. No qualifiers were applied.
VII Quantitation Verification
Form 1 and chromatograms
The accuracy of the analytical results is verified through the calculation of several parameters. The percent difference (%D) between the calculated and reported values must be within 10%. Any positive value < RL (reporting limits) and > MDL (method detection limit) is reported as estimated "J". Positive results must be confirmed on a secondary chromatographic column. When the percent difference between the results calculated from each column is more than 40%, the reported results are qualified as estimate "J."
Sample: MW36 (C2I160145-001) Column 1, Nitrobenzene-d5
Conc. μg/L = Amt * DF * UF * Vt (Vo * Vi) gpc
where:
- Amt is the amount on-column (ng)
- DF is the dilution factor
- UF is the unit correction factor (1.000)
- Vt is the volume of final extract (μL)
- Vo is the volume of the sample extracted (μL)
- Vi is the injection volume (μL)
- gpc is the gel permeation chromatography correction factor (1.000)
Conc. μg/L = 88.3011 ng * 1 * 1 * 1000μL / (1,060 μL * 2.0 μL) = 41.6515 μg/L
- Reported Concentration = 41.6 μg/L
- %D = (1-| Concentration Calculated (μg/L) / Reported Concentration (μg/L)|) * 100
- %D = -0.12%
- Values were within 10% difference
This data validation report for groundwater samples collected for the Post-Closure Monitoring at SMWT Site (Hollywood, MD) on September 10-13, 2002. Samples were analyzed for PCP herbicide compounds using SW-846 Method 8151A. A total of 11 aqueous samples were validated; the sample IDs are:
| Field Sample ID | Lab. Sample ID |
|---|---|
| MW21D | C2I130265-001 |
| MW13 | C2I130265-002 |
| MW14 | Not Sampled |
| MW27R | Not Sampled |
| MW37D | C2I120209-003 |
| MW38 | C2I120209-001 |
| MW32 | C2I130265-005 |
| MW36 | C2I160145-001 |
| MW17R | C2I130265-004 |
| MW20D | C2I130265-003 |
| MW33 | C2I110240-001 |
| MW34D | C2I110240-002 |
| MW35 | C2I120209-002 |
| EQUIP. RINSATE BLANK | C2I160145-002 |
| FIELD BLANK | C2I160145-003 |
The data was reviewed by RMC, Inc. personnel and validated using a combination of method-specific criteria, laboratory SOP, and the Innovative Approach to Data Validation for USEPA Region III (June 1995). Parameters evaluated under data validation procedure Level M3 are presented in Table 9. Data associated with parameters in compliance with quality control specifications have not been qualified. Data associated with parameters that did not comply with quality control specifications and directly impacted project data have been qualified in accordance with USEPA Region III specifications.
Table 9: Laboratory Performance Criteria
| Qualified | Parameter | |
|---|---|---|
| Yes | No | |
| X | Holding Times | |
| X | Blank Analysis | |
| X | Initial Calibration | |
| X | Continuing Calibration | |
| X | System Monitoring Compounds | |
| X | Laboratory Control Sample/LCS Duplicate | |
| X | Quantitation Verification | |
The quality of data collected in support of this sampling activity is considered acceptable with applicable qualifications.
I Holding Times
Form 1
The objective is to ascertain the validity of results based on the holding time of the sample from time of collection to time of sample extraction and analysis. For PCP herbicide compounds in cooled (@4º C + 2º C) aqueous samples, the maximum holding time is seven days from sample collection to extraction and 40 days from extraction to analysis.
- The samples were collected on September 10 through September 13, 2002, and analyzed on September 24 through September 27, 2002. All criteria were met. No qualifiers were applied.
II Initial Calibration
Form V1 and Chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for PCP herbicide target compounds. Initial calibration demonstrates that the instrument is capable of acceptable performance in the beginning of the analytical run and of producing a linear curve. The percent relative standard deviation of the calibration factors (%RSD) should be < 20%. If linear regression is used, the correlation coefficient must be > 0.990 for all target compounds.
- For initial calibrations performed on instrument GC2 on September 21, 2002, the standards MCPP and dichloroprop had a %RSD > 20%. No qualifiers were applied.
- For initial calibrations performed on instrument GC2 on September 26, 2002, all criteria were met. No qualifiers were applied.
III Continuing Calibration
Form VII and chromatograms
Compliance requirements for satisfactory instrument calibration are established to ensure that the instrument used is capable of producing acceptable qualitative and quantitative data for target compounds. Continuing calibration establishes that the initial calibration is still valid. It also establishes the 12-hour relative response factors on which the quantitations are based and checks satisfactory performance of the instrument on a day-to-day basis. The percent difference (%D) between the initial CF and the continuing CF must be < 15 %.
- For continuing calibration performed on instrument GC2 on September 24, 2002, at 0937, all qualifications were met. No qualifiers were applied.
- For continuing calibration performed on instrument GC2 on September 24, 2002, at 1838, all qualifications were met. No qualifiers were applied.
- For continuing calibration performed on instrument GC2 on September 27, 2002, at 0642, the standards Dalapon, dichloroprop, 2,4-D, 2,4,5-TP(Silvex), 2,4,5-T, and Dinoseb were outside the +/- 15% D criteria. No qualifiers were applied.
- For continuing calibration performed on instrument GC2 on September 27, 2002, at 1516, the standards Dalapon, dichloroprop, 2,4-D, 2,4,5-TP(Silvex), 2,4,5-T, and Dinoseb were outside the +/- 15% D criteria. No qualifiers were applied.
IV Blank Analysis
Form I, IV, and Chromatograms
The purpose of blank analysis is to determine the presence and magnitude of contamination problems resulting from field or laboratory activities. No contaminants should be detected in any of the associated blanks. Positive sample results are qualified "B" if the concentration of analyte is < five times (5x) the absolute maximum blank concentration.
- No contaminants were detected in the intra lab blank. All criteria were met. No qualifiers were applied.
V System Monitoring Compounds (Surrogates)
Form II and Chromatograms
Laboratory performance on individual samples is established by means of spiking activities. All samples are spiked with surrogate compound(s) prior to sample preparation. Surrogate-spiked recoveries must be within the specified control limits. When surrogates have percent recoveries below the control limit, positive sample results are qualified as biased low ("L") and non-detects ("UL"). Table 10 summarizes the surrogate recovery analysis.
Table 10: Surrogate Recovery Analysis
| Field Sample # | S1-Column 1% R* | Qualifiers |
|---|---|---|
| MW21D | 74 | |
| MW13 | 76 | |
| MW14 | Not sampled | |
| MW27R | Not sampled | |
| MW37D | 77 | |
| MW38 | 77 | |
| MW32 | 80 | |
| MW36 | 85 | |
| MW17R | 81 | |
| MW20D | 77 | |
| MW33 | 79 | |
| MW34D | 85 | |
| MW35 | 77 | |
| EQUIP. RINSATE BLANK | Not analyzed | |
| FIELD BLANK | 80 |
Control Limit
- (S1) DCAA
- (53-119 %R)
VI Laboratory Control Sample (LCS)/LCS Duplicate
Form III and Chromatograms
Data for laboratory control samples are generated to determine long-term precision and accuracy of the analytical method on various matrices. Percent recoveries must be within the specified method control limits.
- All criteria were met. No qualifiers were applied.
VII Quantitation Verification
Form 1 and Chromatograms
The accuracy of the analytical results is verified through the calculation of several parameters. The percent difference (%D) between the calculated and reported values must be within 10%. Any positive value < RL (reporting limit) and > MDL (method detection limit) is reported as estimated "J". Positive results must be confirmed on a secondary chromatographic column. When the percent difference between the results calculated from each column is more than 40%, the reported results are qualified as estimate "PG".
Sample: MW36 (C2I160145-001) Column B, DCAA
Conc. μg/L = Amt * DF * 20 * Vt / Vo / Vi
where:
- Amt is the amount on-column (ng)
- DF is the dilution factor
- UF is the unit correction factor (1.000)
- Vt is the volume of final extract (μL)
- Vo is the volume of the sample extracted (μL)
- Vi is the injection volume (μL)
Conc. μg/L = 0.04259 ng * 1 * 20 * 10,000μL / 1,000 μL / 1.0μL = 8.518 μg/L
- Reported Concentration = 8.518 μg/L
- %D = (1-| Concentration Calculated (μg/L) / Reported Concentration (μg/L)|) * 100
- %D = 0.00%
- There is no difference in the values.
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