Superfund Research Program

Research Support Core: Analytical Core

Project Leader: Keri C. Hornbuckle
Co-Investigator: Hans-Joachim Lehmler
Grant Number: P42ES013661
Funding Period: 2006-2025

Project-Specific Links

Final Progress Reports

Year:   2019  2014  2009 

Revised Aims:

The Aims for the Analytical Core have been modified to accommodate a funding level 10% lower than proposed. The impact on the specific aims has been to reduce the pace of sample analysis and reporting, especially for air samples analyzed for Atmospheric Sources of PCB Congeners and Characterization of Exposures of Urban and Rural Cohorts to Airborne PCBs. At this time, air samples for both projects accumulate for a longer period than planned and both projects have had to re-prioritize their budgets and analytical priorities. As expected, the Analytical Core depends on regular communications with each of the Project and other Core leaders to appropriately and fairly distribute its limited resources.

Studies and Results:

The Analytical Core of the Iowa Superfund Research Program provides assistance to the Project Directors and their staff in measuring PCB congeners and their metabolites in laboratory and field samples. Researchers provide advice and assistance in the development of laboratory experiments that involve PCBs, designing field studies for PCBs in the environment, in determining auxiliary measurements, and in the interpretation of the PCB data. Researchers provide instrumental metrology on a variety of essential instruments, increase sample through-put through method development on new instruments.

Sample analysis is a major Aim of the Analytical Core. In 2014, the Analytical Core supported Atmospheric Sources of PCB Congeners by analyzing air samples for all 209 PCBs and selected OH-PCBs in a gas-phase air samples, atmospheric particles, and sediments from the Indiana Harbor and Ship Canal; assisted Phytoremediation to Degrade Airborne PCB Congeners from Soil and Groundwater Sources by analyzing selected PCB congeners and assisting the measurement of selected OH-PCBs in plant tissues, soil, water and laboratory media; assisted Characterization of Exposures of Urban and Rural Cohorts to Airborne PCBs by analyzing for all 209 PCBs and selected OH-PCBs in human blood serum samples and air samples; and assisted the Inhalation Toxicology Core by analyzing PCB11 and OH-PCB11 in animal tissues. The Analytical Core assisted the Synthesis Core by providing GC-MS analyses of reaction mixtures and final synthetic products. These measurements were augmented by hundreds of quality control measurements and method development measurements (Table 1).

Table 1. Summary of samples analyzed by the Analytical Core in 2014 (approx.)

	Shipped PUFs	Received Air Samples	Analyzed samples for PCB congeners	Analyzed samples for OH-PCBs	Other
Atmospheric Sources of PCB Congeners (all samples analyzed for 209 congeners)	306	269	100 sediment samples	232 standard reference material, sediment, and ballast	100 sediment samples for musks
Characterization of Exposures of Urban and Rural Cohorts to Airborne PCBs (all samples analyzed for 209 congeners)	719 (365 for CJ; 354 for EC)	78 (0 for CJ; 78 for EC) *Samples are now being now received	509 air samples 93 human blood serum	172 human blood serum
Phytoremediation to Degrade Airborne PCB Congeners from Soil and Groundwater Sources			174 plants, soil, water samples	60 GC-ECD analysis of PCBs and OH-PCB (as methoxylated derivatives)	120 enantioselective GC-ECD analysis to determine enantiomeric fractions of PCBs and OHPCBs (as methoxylated derivatives)
Inhalation Toxicology Core			245 samples by GC-MS
Synthesis Core			112 samples by GC-MS

Normal quality control measurements include QC samples run with every batch of 10 samples including: instrument and standard solutions calibration standards, instrumental and field blanks, laboratory reference solutions, and standard reference materials. Researchers inject surrogate standards and internal standards in every sample, matrix spikes every 20 samples, and analyze standard reference material every set of 10 for blood samples and once for every sample matrix annually. Researchers also participate in international round-robin comparison of blind samples and conduct annual confirmation of instrument linearity for all target compounds on all instruments.

Method development is a major Aim of the Analytical Core. In 2014, Researchers participated in many experiments and collaborations that resulted in new analytical methods. The following are representative of 2014:

1. Developed and applied a LC-MS method for atropisomeric determinations of OH-PCBs.
2. Continue to develop methods for efficient and rapid determination PCBs and OH-PCBs in environmental samples. This year researchers focused on improvements in human blood serum analysis using tandem mass spectrometry. In 2012, researchers increased the number of OH-PCBs that can be quantified in environmental samples from 12 to 65.
3. In collaboration with Atmospheric Sources of PCB Congeners, developed a new method for detection and quantification of 80 OH-PCB congeners in atmospheric aerosol particles, sediments and sediment pore water using GC/MS/MS. Preliminary results from air samples show evidence of airborne decay of PCBs to the hydroxlated metabolites.
4. With Atmospheric Sources of PCB Congeners, developed a method for comparing the results from active and passive air sampling of flame retardants, chlorinated pesticides, and polycyclic aromatic hydrocarbons using the method previously developed for PCB congeners.
5. Developed a new method for determining the uptake rate of any semivolatile organic pollutant using the passive air sampling system originally designed for PCBs.
6. Developed a confirmation method using dual gas capillary columns for OH-PCBs.

Instrument maintenance is a major Aim of the Analytical Core. In 2014, researchers provided skilled support for the following instrumentation: Agilent 7000 triple quad mass spectrometer (GC/MS/MS); Agilent 6890 dual tower dual electron capture detector gas chromatograph (GC/ECD); Agilent 5973 single quad mass spectrometer (GC/MSD); Water Quattro micro gas GC/MS/MS; Agilent 6240 liquid chromatograph mass spectrometer (LC/MSD); Agilent 5975 GC/MSD; Agilent 6890 GC/ECD; Agilent 6850 GC/FID: Shimadzu10aVP LC; and two Dionex Accelerated Solvent Extraction Systems (ASE). The Core purchased and installed a new Agilent 7000 triple quad mass spectrometer (GC/MS/MS).

Significance:

The Analytical Core is dedicated to continuous improvement in the accuracy, precision, speed, and completeness of the services provided to the Research Cores of the Iowa Superfund Research Program.

Plans to Address Specific Aims:

The Core continues to develop methods that allow faster delivery of results to the projects and expects to develop a new method for sample extraction using solid phase automation.