Document 5kmmJV7rGgmVwebrEpYJLvxQ0

Memorandum To: From: Date; Subject: Cc: Hanan Ghantous, H-l Keith A. McCleary, Jackson Lab October 19,1994 Final Report, Lead in Blood Analysis C. J. Hensler, Jackson Lab M. S. Bogdanffy, 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 Specialty Chemicals' Trace Metals Analysis Group as part of Medical Research Project No. MR 9905. A copy ofthis report is to be kept with those materials relating to the analyses performed (SQP's, methods, and copies of sample logs) under GLP guidelines here at Jackson Lab. Ifyou have any questions, please feel free to call me (Ducom 540-2467). DUP040004276 Diana Lead Data Entry Coding Form: BatesBegin: DUP040004277 Doc Type 1 Research Report BatesEnd' DUP040004280 TotalPages | Year Date- j 1994 J Month Date | DecControl#' | 235 011 4 Attmnt?# 0 101 Day Date J 19 j Title Analysis of Pb in Blood Soil and Associated Materials in Support of Haskell Lab Mecical Research Reference: Pioject No. MR 9905 Primary Author Last Name.I McCleary Secondary Authors. Primary Hanan Ghantous Recipient (s)- I First Name, Middle Initial.1 Keith A 1 Publication- j CC's C J Hensler M S Bogdanffy R C Rhea R L Sobosinski 1 Names Stated DuPont Specialty Chemicals Trace Metals Analysis Group, Quality Control Laboratory, Chambers Works Plant. Deepwater, NJ. Graphite Furnace Atomic Absorption Spectrometry (GFAAS). Inductively Coupled Plasma Atomic Fmis;inn Snprtrnmptrv /ICP-AFS1 Doc Problems:j j Case Produced In | Steven Thomas | Produced By. | DPT | Source. | Responsive to Plaintiffs 1st Re Dup/Cross Ref #'s I Doc Control Comments: Disk Boxl January 2002 SH001001 - SH001002 Obj. Coder Nam I C Green | Obj Data Entry Nam j D. Green | ObjDataDate | 8/21/2002 Analysis ofPb in Blood, Soil, and Associated Materials in Support ofHaskell Lab Medical Research Project No. MR 9905 Author Keith A. McCleary Study Completed: 8/22/94 Performed By: DuPont Specialty Chemicals Trace Metals Analysis Group Quality Control Laboratory Chambers Works Deepwater, NJ 08023 Signature: Keith A. McCleary, Ph.D. Date io[n DUP040004277 Summary The purpose ofthis study was to determine the amount oflead that was contained in samples associated with MR9905. 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 Ethission 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 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 15 microliter volume of sample + 5 microliters ofmodifier is injected into a small graphite tube. This tube is electromagnetically 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 of signal from the HCL. The degree of attenuation 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 ng/mL stock. Each 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 DUP040004278 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 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. 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 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 ofthe characteristic emission wavelength ofPb (220.35 nm) is proportional to the amount ofPb in the sample. Results The results for all samples submitted under MR9905 are listed in Appendix I. APPENDIX 1 MR9905.XLS E o> XI aa. 1cUe < in CinO V Q. 2 < m a o o CQ -J < u. O CHO Z =J PRE 0.5 HR 1.0 HR 2.0 HR 4.0 HR 8.0 HR 12 HR 24 HR 41 8 HR 72 HR 96 HR 120 HR 144 HR CO TT"-- IN rCM CCOM in *P f<0 *rP* Tin-* r 0CM0 CM CO rr*s* CCMM iinn uVo" CM rC*O CO C0O3 CM 0in5 CM oCO tCnO CCOM in 1101H <5 1 I102H I103H <5 | I104H I.105H <5 T~* o IP- 05 o o CO T-- Ti*; CO CO PCM" 03 oCM <5 <5 oCO CO 0in5 0CM5 CO o in 247 | 130 175 152 130 113 64 174 156 103 T-- 05 0CO5 0CO0 CCOO CPMN 0CD0 30 CinO co r* CO CO yCDt pC>M GinO CO CinM r-- 5 w or-. CrM- 12011 2021 2031 12041 12051 1 CO CO o r* ygmm CO r-- iro-. 441 529 509 167 37 177 1 1621 133 258 127 5291 469 336 302 223 166 344 225 C*pO 209 224 164 113 00 - CCOO oCO 0CO5 C0O3 iCnO tCnM 152 112 232 148 108 190 139 142 108 03 CO CCOO *in* 0CO3 113 1301J <5 1 302J <5 1303J | < 5 I304J <5 I305J [<5 1 96 L O) CO r- 00 780 I 443 C0M3 *C#O 1758 123 1167 | COCOO 132 1439 597 979 493 547 co CCMO Cc0Mo3 03 214 154 r-- iCnM 340 159 366 412 614 421 200 282 219 328 641 685 357 459 418 135 375 | 328 388 861 ccoo C0O3 70 iCnO C*pO 00 34 iCnM Tr>"- 0CO0 o03 aCO oCO _i -J -J =tb t" T-- T-- e> O a a. CL CC CC 0. CC 1Or* O X Xi 3C T-- COt CO* COi *0P5t 0*}3 4 0>M<3tft 1 B> g Qn. u. O z => z zU1 > o UCCl < 3UCOl co az Q C<UCJ J mJ < hui o Z (SOIL #1 FT MADISON 6/13 1SOIL #1 FT MADISON DOS SOLN 1duplicate [SOIL #1 GRP 1 102-H 6-14-94 ISOIL #1 GRP 1 105-H 6-14-94 354| 174 179 156 126 159 109 139 ASPEN SHAVINGS OREO COOKIES BLANK S0IL2 PLW1 S01L2 PLVV1 DOS SOLN GROUP III 301J PLW1 GROUP III 302J PLW1 [GROUP III 303J PLW1 GROUP 111304J PLW1 1GROUP HI 305J PLW1 Pb Acetate 6/17/94 Pb Acetate 9/20/94 113 tn 113 V 101H-240 --j n Oc) CM cCroO- 3079 i 1644 1729 1897 619 1296 102H-240 15ng/mL 103H-240 38 ng/mL 104H-240 15 ng/mL 105H-240 27ng/mL DUP040004280 10/19/94