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Lead Analysis Report #1: Soils AEC 3-3, AEC 9-3, and AEC10-1
DuPont HLR 581-94
Analysis ofPb in Blood, Soil, and Associated Materials in Support ofHaskell Lab Medical Research ProjectNo. MR9727*001
Author Keith A. McCieary
Study Completed: 1/26/94
Performed By: DuPont Specialty Chemicals Trace Metals Analysis Group Quality Control Laboratory
Chambers Works Deepwater, NJ 08023
Date
-88*
Lead Analysis Report #1: Soils AEC 3-3, AEC 9-3, and AEC10-1
DuPont HLR 581-94
Summary
The purpose ofthis study was to determine the amount oflead that was contained in samples associated with MR9727-001. There were essentially three type ofsamples: blood (microswine), aqueous (drinking water, dosing solutions), and solid (soil, bedding, etc.). Blood samples were prepared by dilution with a modifier solution (to digest sample and break viscosity) and analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS), Aqueous and solid samples were prepared using microwave assisted digestion and analyzed using inductively Coupled Plasma Atomic Emission Spectometry (ICP-AES). All samples were run in duplicate and average answers reported. In the case ofthe blood, each sample and duplicate was spiked and checked for recovery. Ifthe spike recovery was greaterthan 10% in error, a one point standard additions calculation was performed.
Methodology
The descriptions listed below are summaries ofthe actual methods used to analyze samples. The actual methods are documented in the GLP Protocols Notebook, archived at QCL and copies are available upon request
Sample Preparation: Blood
Blood samples were received in small polyethylene vails. Approximate sample volumewas 100-300 uL. 100 uL ofblood is diluted to 1.0 mL with modifiersolution. The modifier solution is a solution ofnitric add (digests sample), Triton X-100 (surfactant,'' breaks viscosity), methanol (antifoatmng agent), and ammonium phosphate (GFAAS modifier) in water.
Sample Analysis: Blood
-
Blood samples are analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS), In GFAAS, a 20 microliter volume ofsample+modifier is injected into a small graphite tube. This tube is electromagneticaliy heated to dry, char, and atomize the -
sample. A hollow cathode lamp (HCL) shines light corresponding to the atomic emission
ofPb (283.3 nni) through the tube. As free Eb atoms are generated by the sample atomization, they absorb the radiation, attenuating the amount ofsignal from the HCL. The degree ofattenuation ofthe HCL radiation is proportional to the concentration ofPb in the sample. Calibration standards of 10,20 .and 30 ng/mL are prepared by serial dilution ofa 1000 ug/mL stock. Each blood sample is analyzed twice. Each sample and duplicate is then spiked with lOng Pb mid reanalyzed to check for recovery. Ifrecovery is less than 90% or greater than 110%, a one point standard addition calculation is
-89-
DUP040004244
Lead Analysis Report #1: Soils AEC 3-3, AEC 9-3, and AEC10-1
DuPont HLR 581-94
performed to determine the amount ofPb in the sample. Each result is the average of the two replicates.
Sample Preparation: Aoueous Samples Samples that are primarily aqueous are prepared by acidifying 1Q.00 mL ofsample with 2.00 mL concentrated HN03. The sample is then diluted to a final volume of20.00 mL and analyzed by ICP-AES.
Sample Preparation: Solid Samples Solid Samples are prepared by microwave assisted digestion. 0.1 -0.2 g ofsample are digested with 5.00 mL concentrated HN03 in a Teflonlined pressure vessel The vessels are placed in a microwave digestion apparatus and cooked for 10 minutes at 300@W power. The samples are allowed to cool and are thenfiltered into a SO mL volumetric flask and diluted to volume with deionized water.- Samples are analyzed for Pb content by ICP-AES.
Sample Analysis: Anueous and Solid Samples These samples are analyzed by Inductively Coupled Plasma-Atomic Emission . Spectrometry (ICP-AES).' The prepared samples are pumped into an sample introduction system where afiae spray ofaerosol is generated. Ibis sample aerosol flows along a stream ofargon gas into the plasma. The plasma is a highly energetic discharge sustained in argon by applied radio-frequency power in excess of 1000 W. This discharge is energetic enough to desolvate, atomize, and excite the sample species to radiative emission. The intensity ofthe characteristic emissionwavelength ofPb (220.35 nm) is proportional to the amount ofPb in the sample.
Results
The results for all samples subnutted under MR9727-001 are listed in Appendix L
-90-
DUP040004245
Lead Analysis Report #1: Soils ABC 3-3, AEC 9-3, and AEC10-1
DuPont HLR 581-94
2531 2101
4051
PB_PHS2.XLS MR9727-001
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Lead Analysis Report #2; Soils PLW and EC1
DuPont HLR 581-94
Analysis ofPb in Blood, Soil, and Associated Materials in Support ofHaskell Lab Medical Research Project No. MR 9740-001
Author Keith A. McCleaiy
Study Completed: 1/26/94
Performed By: DuPont Specialty Chemicals Trace Metals Analysis Group Quality Control Laboratory
Chambers Works Deepwater, NT 08023
DUP040004248
Lead Analysis Report #2: Soils PLW and EC1
DuPont HLR 581-94
Summary
The purpose ofthis study was to determine the amount oflead that was contained in samples associated with MR9740-001. There were essentially three type ofsamples: blood (microswine), aqueous (drinking water, dosing solutions), and Solid (soil, bedding, etc.). Blood samples were prepared by dilution with a modifier solution (to digest sample and break viscosity) and analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Aqueous and solid samples were prepared using microwave assisted digestion and analyzed using Inductively Coupled Plasma Atomic Emission Spectrometry (CCP-AES). All samples were run in duplicate and average answers reported In the case ofthe blood, each sample and duplicate was spiked and checked for recovery. Ifdie spike recovery was greater than 10% in error,.a one point standard additions calculation was performed.
Methodology
The descriptions listed below are summaries ofthe actual methods used to analyze samples. The actual methods are documented in the CLP Protocols Notebook, archived at QCL and copies are available upon request
SamplePreparation: Blood
Blood samples were received in small polyethylene vials. Approximate sample volume was 100-300 uL. 100 uL ofblood is diluted to 1.0 mL with modifier solution. The modifier solution is a solution ofnitric acrid (digests sample), Triton X-I00 (surfactant, breaks viscosity), methanol (andfoaming agent), and ammonium phosphate (GFAAS ' modifier) in water.
Sample Analysis: Blood
Blood samples are analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS). In GFAAS, a20 microliter volume ofsample + modifier is injected into a small graphite tube. This tube is eiectromagneticaliy heated to dry, char, and atomize the sample. A hollow cathode lamp (HCL) shines light corresponding to the atomic emission ofPb (283.3 nm) through'the tube. As free Pb atoms are generated by the sample atomization, they absorb the radiation, attenuating the amount ofsignal from the HCL. The degree ofattenuation ofthe HCL radiation is proportional to the concentration ofPb in the sample. Calibration standards of 10,20 ,and 30 ng/mL are prepared by serial dilution ofa 1000 ug/mL stock. Each blood sample is analyzed twee. Each sample and duplicate is then spiked with lOng Pb and reanalyzed to check for recovery. Ifrecovery is less than 90% or greater than 110%, a one point standard addition calculation is
-94-
DUP040004249
Lead Analysis Report #2: Soils PLW and EC1
performed to determine the amount ofPb in the sample. Each result is the average ofthe two replicates.
Sample Preparation: Aqueous Samples Samples that are primarily aqueous are prepared by acidifying 10.00 mL ofsample with 2.00 mL concentrated HN03. The sample is then diluted to a final volume of20.00 mL and analyzed by ICP-AES. Sample Preparation: Solid Samples Solid Samples are prepared by microwave assisted digestion. 0.1 - 0.2 g ofsample are digested with 5.00 mL concentrated HNQ3 in a Teflon lined pressure vessel. Thevessels are placed in a microwave digestion apparatus and cooked for 10 minutes at 300@W power. The samples are allowed to cool and are then filtered into a SO mL volumetric . flask and diluted to volumewith deionized water. Samples are analyzed for Pb content by ICP-AES. Sample Analysis: Aqueous and Solid Samples These samples are analyzed by Inductively Coupled Plasma - Atomic Emission Spectrometry (ICP-AES). The.prepared samples are pumped into an sample introduction systemwhereafinesprayofaerosolisgenerated. This sample-aerosol flows along a stream ofaigon gas into the plasma. The plasma is a highly energetic discharge sustained in argon by applied radio-frequency power in excess of 1000 W. This.discharge d energetic enough to desolvate, atomize, and excite the sample species to radiative emission. The intensity ofthe characteristic emission-wavelength ofPb (220.35 pm) Is
proportional to the amount ofPb in the sample.
Results The results for all samples submitted under MR9740-00I are listed in Appendix L
-95-
Lead Analysis Report #2: Soils PLW and EC1
DuPont HLR 581-94
MR_9740.XLS 7/29/94 ~ MR 9740-001 '
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-96-
DUP040004251
Lead Analysis Report #2: Soils PLW and EC1
DuPont HLR 581-94
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Pago 2 OF 2
DUP040004252
Lead Analysis Report #3: Soils FM (Fort Madison) and PLW1
DuPont HLR 581-94
Analysis ofPb in Blood, Soil, and Associated Materials in Support ofHaskell Lab Medical Research ProjectHo. MR-9905
Author KeithA-McCieary
Study Completed: 8/22/94
Performed By: DuPont Specialty Chemicals Trace Metals Analysis Group Quality Control Laboratory
Chambers Works Deepwater, NJ 0S023
Keith A. McCleary, PhJD.
Date Infill
-98-
DUP040004253
Lead Analysis Report #3: Soils EM (Fort Madison) and PLW1
DuPont HLR 581-94
Summary
The purpose ofthis study was to determine the amount oflead that warcontained in samples associated with MR99Q5. There were essentially three type ofsamples: blood (microswine), aqueous (drinldng water, dosing solutions), and solid (soil, bedcfing, etc.). Blood samples were prepared by dilution with a modifier solution (to digest sample and break viscosity) and analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Aqueous and solid samples were prepared using microwave assisted digestion and analyzed using Inductively Coupled Plasma Atomic Emission Spectrometry (ICPAES). All samples were run in duplicate and average answers reported. In the case ofthe blood, each sample and duplicate was spiked and checked for recovery. Ifthe spike recovery was greater than 10% in error, a one point standard additions calculation was performed.
Methodology
The descriptions listed below are summaries ofthe actual methods used to analyze samples. The actual methods are documented in the GLP Protocols Notebook, archived at QCL and copies are available upon request
Sample Preparation: Blood Blood samples were received in small polyethylene vials. Approximate sample volume was 100-300 uL. 100 uL ofblood is diluted to 1.0 mL with modifier solution. The modifier solution is a solution ofnitric add (digests sample), Triton X-100 (surfactant, breaks viscosity), methanol (antifoaming agent), and ammonium phosphate (GFAAS modifier) in water.
Sample Analysis: Blood
Blood samples are analyzed using Graphite Furnace Atomic Absorption Spectrometry (GFAAS). In GFAAS, a 15 microliter volume ofsample+5 microliters ofmodifier is injected into a small graphite tube. This tube is dectromagnetically heated to dry, char, and atomize the sample. A hollow cathode lamp (HCL) shines light corresponding to the atomic emission ofPb (283.3 nra) through the tube. As free Pb atoms are generated by the sample atomization, they absorb the radiation, attenuating the amount of signal from the HCL The degree ofattenuation ofthe HCL radiation is proportional to the concentration ofPb in the sample. Calibration standards of 10,20 .and 30 ng/mL are prepared by serial dilution of a 1000 ug/mL stock. Bach blood sample is analyzed twice. Each sample and duplicate is then spiked with lOng Pb and reanalyzed to check for recovery. Ifrecovery is less than 90% or greater than 110%, a one point standard
-99-
DUP040004254
Lead Analysis Report #3: Soils FM (Fort Madison) and PLW1
DuPont HLR 581-94
addition calculation is performed to determine the amount ofPb in the sample. Each result is the average of the two replicates.
Sample Preparation: Aqueous Samples Samples that are primarily aqueous are prepared by acidifying 10,00 mi, ofsample with 2.00mL concentrated HN03. The sample is then diluted to a final volume of20.00 mL and analyzed by ICP-AES. Concentrated samples may require further dilution, or a higher initial dilution to prepare the sample to be analyzed within the standardized range ofthe instrument
Sample Preparation: Solid Samples Solid Samples are prepared by microwave assisted digestion, 0.1 - 0.2 g ofsample are digested with 5.00 mL concentrated HN03 in a Teflon lined pressure vessel The vessds are placed in a microwave digestion apparatus and cooked for 10 minutes at 3Q0@Wpower. The samples are allowed to cool and are then filtered into a 50 mL volumetric flask and diluted to volume with deionized water. Samples are analyzed for Pb content by ICP-AES.
Sample Analysis: Aqueous and Solid Samples These samples are analyzed by Inductively Coupled Plasma - Atomic Emission Spectrometry (ICP-AES). The prepared samples are pumped into an sample introduction system where a fine spray ofaerosol is generated. This sample aerosol flows along & stream ofargon gas into the plasma. The plasma is a highly energetic discharge sustained in argon by applied radio-frequency power in excess of 1000 W. Tins discharge is. energetic enough to desolvate, atomize, and excite the sample species to radiative emission. The intensity ofthe characteristic emission wavelength, ofPb (220.35 nm) is proportional to the amount ofPb in the sample.
Results
The results for ail samples submitted under MR9905 are listed in Appendix L
-100-
DUP040004255
Lead Analysis Report #3: Soils FM (Fort Madison) and PLW1
DuPont BLR 581-94
S0IL2 PUW1 DOS SOLNi
GROUP III 301J PLW1 f
GROUP III 303J PLWI I GROUP III 304J PLW1 I
10/19/94
APPENDIX 1 MR9905.XLS
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