Document xjXEbDyNJ34Ly5rDagjmz319Q
Memorandum
To: Hanan Ghantous, H-l
From:
Keith A. McCleary, Jackson Lab
Date:
July 29,1994
Subject: Final Report, Lead in Blood Analysis
Ce: C. J. Hensler, Jackson Lab
M. S. Bogdanfiy, Haskell Toxicology
R. C. Rhea, Haskell Quality Assurance
R. L. Sobocinski, QCL
Enclosed please find three copies ofthe final report for the analysis ofPb in blood as conducted by the Du Pont Specially Chemicals' Trace Metals Analysis Group as part of Medical Research Project No. MR 9727-001: "Absolute Bioavailability of Soil Lead in Microswine: Soils AEC 3-3, AEC 9-3, and AEC 10-1",
A copy ofthis report is to be kept with those materials relating to the analyses performed (SOP's, methods, and copies of sample logs) under GLP guidelines here at Jackson Lab. If you have any questions, please feel free to call me (Ducom 540-2467).
DUP040005107
Diana Lead Data Entry Coding Form:|
Decontrol*] 282.01 j
BatesBegin DUP040005108
jDoc Type: Research Report
BatesEnd: DUP040005112
TotalPages
J JYear Date
19941 Month Date. |
5 Attmnt?# 0
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Title
Analysis of Pb in Blood. Soil, and Associated Materials in Support of HasKell Lab. Medical Research
Reference: Project No. MR-9727-001
Primary Author Last Name I McCleary
Secondary Authors:
Primary Hanan N. Ghantous Recipient ts)-
First Name. Middle Initial: Keith A Publication:
CC's.
C J Hensler, M S Bogdanffy. R.C. Rhea R.L Sobosinski
Names Stated:
DuPont Specialty Chemicals Trace Metals Group, Chambers Works Plant, Deepwater, NJ, Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Inductively Coupled Atomic Emission Spectrometry
DCP-AFfil
Doc Problems
jCase Produced In Steven Thomas j Produced By | DPT
Dup/Cross Ref#'s
Doc Control Comments-
Disk, Box 1. January 2002, SH001001 - SH001002
jSource: Responsive to Plaintiffs 1st Re
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jObj. Coder Nam D Green
Obj Data Entry Nam | D Green
ObjDataDate 8/22/2002
N 26929.01
Analysis ofPb in Blood, Soil, and Associated Materials in Support ofHaskell Lab Medical Research Project No. MR 9727-001
Author Keith A McCleaiy
Study Completed: 1/26/94
Performed By: DuPont Specialty Chemicals Trace Metals Analysis Group Quality Control Laboratory
Chambers Works.. Deepwater, NJ 08023
Signature:
Keith A. McCleaiy, Pn.D.
^ ^Date 6 10
DUP040005108
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 of samples: 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 of the 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 vails. 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 of nitric acid.(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 20 microliter volume of sample + modifier is injected into a small graphite tube. This tube is electromagneticaUy heated to dry, char, and atomize the sample. A hollow cathode lamp (HCL) shines light corresponding to the atomic emission of Pb (283.3 nm) 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 of attenuation of the 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. Each blood sample is analyzed twice. Each sample and duplicate is then spiked with lOng Pb and reanalyzed to check for recovery. If recovery is less than 90% or greater than 110%, a One point standard addition calculation is
DUP040005109
performed to determine die 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 of sample 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 of sample are digested with 5.00 mL concentrated HN03 in a Teflon lined 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 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 of aerosol is generated. This sample aerosol flows along a stream of argon 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 of the characteristic emission wavelength of Pb (220.35 nm) is proportional to the amount ofPb in the sample.
Results
The results for all samples submitted under MR9727-001 are listed in Appendix I.
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PB_PHS2.XLS MR 9727-001
NON BLOOD SAMPLES (ug/mL) AEC10-1
516 513;
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AEC 9-3
AEC 3-3
PIG DOSE 11 (AEG 3-3) PIG DOSE II (AEC 3-3) GRPII 202 GRPII 203 I GRPII 205
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1686 1776 1411
884 603 596 753
1962 1366 1116
385 536 985 543
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ASPEN LAB SHAVINGS BASAL CHOW di WATER Rm. 211 NITRIC ACID Pb ACETATE DOS. SOI
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Pb SOIL 10-1 Pb SOIL 3-3
4868 1590 1869
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2005 1876 1787 1668
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