VOC sampling locations table for Ground Zero area, Jan 2002

NYC 9/11 Public Portal Document

exposure study. The bulk solid PM53 sample was side- E. Chemical analysis of liquid extracts of bulk and drifted into an aluminum holder and mounted into the Alter samples. Siemens D-500 Diffractometer (Bruker Analytical X-Ray I. pH. The pH of samples isolated by aqueous Systems, Madison, WI). The generator, set at 45 kilovolts extraction was determined immediately after the extraction (kV) and 40 milliamperes (mA), generated x-rays from a procedure with an audited calibrated Coming 440 pH copper-target x-ray tube. The filament current was 3.46 meter (audited by Research Triangle Institute, Research mA. Intensities were collected by a lithium-drifted silicon Triangle Park, NC). detector fitted with a monochromator riding on a 2. Endotoxin. Aliquots of samples isolated by goniometer in the coupled 0/20 mode. Peaks were aqueous extraction were frozen on dry ice and sent by collected in the range 20 = 5 to 85 degrees. Collection overnight delivery to Associates of Cape Cod, Inc. software used was Materials Data, Inc. (MDI, Livermore, (Falmouth, MA) for analysis of endotoxin content using CA) Datascan, Version 3.2. Evaluation software was MDI the Limulus Amebocyte Lysate (LAL) gel-clot method. Jade 5 using the pattern library Powder Diffraction File LAL-reagent water (lot # 308-331) was used to (PDF), release 2000 (International Centre for Diffraction reconstitute or dilute Pyrotell lysate, endotoxin, and Data). XRD analysis was performed by the National Risk samples, and served as the negative control. Samples were Management Research Laboratory, Research Triangle titered using a twofold dilution scheme against control Park, NC. standard endotoxin (CSE; lot #85, Escherichia coli 0113, J. X-ray fluorescence (XRF) analysis. Five 5 EU/ng). Preliminary inhibition tests (positive product polycarbonate filters (Isopore 0.8um #ATTP04700, controls) were performed on the undiluted samples spiked Millipore Corporation, Bedford, MA) loaded with the with CSE equivalent to twice the sensitivity (X; 0.03 WTC3 PM2 5 sample used in the inhalation exposure study, EU/ml). The error of the gel-clot method is ± one twofold along with five lot-matched blank filters, were loaded into dilution. liquid-type polyethylene sample cups, placed in a stainless 5. Inductively coupled plasma - atomic emission steel sample holder, and analyzed. No film was used to spectrometry (ICP-AES) and - mass spectrometry (ICP- cover blanks or samples in the analysis. X-ray intensities MS). WTC2001 PM2 5 samples, control dust PM25 were collected with the Philips PW2404 XRF (Philips samples, and polycarbonate filters taken during an Analytical, Inc., Natick, MA), and the loaded particulate inhalation exposure using WTC3 PM2 5 were extracted was analyzed using the “standardless” software, UniQuant with deionized (d.i.) water or IM HCl, and analyzed for 4, after subtraction of the counts due to the blank filter their elemental content. The two extraction liquids are system (includes filter, polyethylene liquid sample cup and used to estimate easily bioavailable and total bioavailable stainless steel sample holder). The intensities were metal content, respectively. While this speciation scheme averaged in each channel needed for background is a rough approximation of bioavailability, it has proved subtraction. The blank filter analysis showed slightly useful in characterizing inhalation toxicology endpoints elevated counts due to Fe, Cr, Cu, Ca, Cl, S, and Si. The for various source and ambient particulates (Costa and constituents of the dust were evaluated as oxides, but are Dreher, 1997; Kodavanti et al., 1998). Milligram-sized reported quantitatively as elements with the oxygen aliquots of bulk samples were extracted with 1.6 ml of stripped. XRF analysis was performed by the National either liquid. Polycarbonate filters were extracted with 13 Risk Management Research Laboratory, Research ml of either liquid. High-speed centrifugation was used to Triangle Park, NC. separate the liquid and solids (17000 x g for 1.6 ml 4. Carbonfraction analysis. Carbon fraction analysis samples, 51000 x g for 13 ml samples). After dilution, was used to speciate the carbon content of samples into extraction solutions were analyzed quantitatively using organic, elemental, and carbonate carbon. Analysis was ICP-AES (Model P40, PerkinElmer Instruments, Shelton, performed on bulk WTC2001 and control dust PM2.5 CT) operated closely following EPA Method 200.7 (EPA, samples, and on quartz filters taken during an inhalation 2002a), and ICP-MS (ELAN 6000, PerkinElmer exposure using WTC3 PM2 5. The thermo-optical method, Instruments, Shelton, CT) operated closely following EPA based upon sequential pyrolytic vaporization and detection Method 6020 (EPA, 2002b). Blank Gehnan Teflo and of the three carbon fractions (Birch and Cary, 1996; Millipore Isopore filters (used in the inhalation study) Sunset, 2002), was performed by Simset Laboratory, were run through the extraction procedure. Filter blanks Forest Grove, OR (bulk samples), and Hillsborough, NC levels for all elements were negligible compared to the (filter samples). levels in the PM samples. Gelman Zefluor and Teflo filters and Millipore Isopore filters are of known, similar

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