Validation of a New Soil VOC Sampler: Precision of the Performance of the En Core Sampler to Store Low VOC Concentrations

Soil sampling and storage practices for volatile organic analysis must be designed to minimize loss of volatile organic compounds (VOCs) from samples. The En Core{reg_sign} sampler is designed to collect and store soil samples in a manner that minimizes loss of contaminants due to volatilization and/or biodegradation. An American Society for Testing and Materials (ASTM) standard practice, D 6418, Standard Practice for Using the Disposable En Core Sampler for Sampling and Storing Soil for Volatile Organic Analysis, describes use of the En Core sampler to collect and store a soil sample of approximately 5 grams or 25 grams for volatile organic analysis. To support the ASTM practice, four studies have been performed to evaluate the performance of the En Core sampler for storage of soil samples spiked with VOCs. The first study was conducted to evaluate the performance of the device to store soil samples spiked with VOCs at high-level concentrations of approximately 2,500 {micro}g/Kg under various conditions. This analyte concentration in the soil was selected to limit the influence of the analytical method on the data. A second study was conducted to answer questions on the performance of the En Core sampler for storage of soil samples containing low-level (<200 {micro}g/Kg) concentrations of VOCs. In this study, soil samples were spiked with concentrations of VOCs at approximately 100 {micro}g/Kg and stored under various conditions prior to analysis. The third study was performed to generate data on the performance of the 25-gram En Core sampler to store soil samples spiked with EPA Method 1311, Toxicity Characteristic Leaching Procedure (TCLP), volatile organic analytes under various conditions for 14 days. The low-level performance data and TCLP analyte storage data are included in appendices to the ASTM practice, and the ASTM research report describing the high-level study is referenced in the practice. The fourth study, which is described in this report, was performed to estimate the precision of the performance of the 5-gram and 25-gram En Core samplers to store soil samples spiked with low concentrations of VOCs. This was done so that information on the precision of the performance of the devices can be added to the ASTM practice. Data generated in the precision validation study show very good precision of the performance of the En Core samplers to store soil samples spiked with low concentrations of a variety of VOCs

Validation of a New Soil VOC Sampler: Revision of ASTM Practice D 6418, Standard Practice for Using the Disposable En Core Sampler for Sampling and Storing Soil for Volatile Organic Analysis, and Development of a Subsurface Sampling/Storage Device for VOC Analysis

Soil sampling and storage practices for volatile organic analysis must be designed to minimize loss of volatile organic compounds (VOCs) from samples. The En Core{reg_sign} sampler is designed to collect and store soil samples in a manner that minimizes loss of contaminants due to volatilization and/or biodegradation. An American Society for Testing and Materials (ASTM) standard practice, D 6418, Standard Practice for Using the Disposable En Core Sampler for Sampling and Storing Soil for Volatile Organic Analysis, describes use of the En Core sampler to collect and store a soil sample of approximately 5 grams or 25 grams for volatile organic analysis. To support the ASTM practice, a study was performed to estimate the precision of the performance of the 5-gram and 25-gram En Core samplers to store soil samples spiked with low concentrations of VOCs. This report discusses revision of ASTM Practice D 6418 to include information on the precision of the En Core devices and to reference an ASTM research report on the precision study. This report also discusses revision of the ASTM practice to list storage at -12 {+-} 2 C for up to 14 days and at 4 {+-} 2 C for up to 48 hours followed by storage at -12 {+-} 2C for up to 5 days as acceptable conditions for samples stored in the En Core devices. Data supporting use of these storage conditions are given in an appendix to the practice and are presented in the research report referenced for the precision study. Prior to this revision, storage in the device was specified at 4 {+-} 2 C for up to 48 hours. The En Core sampler is designed to collect soil samples for VOC analysis at the soil surface. To date, a sampling tool for collecting and storing subsurface soil samples for VOC analysis does not exist. Development of a subsurface VOC sampling/storage device was initiated in 1999. This device, which is called the Accu Core sampler, is designed so that a soil sample can be collected below the surface using a penetrometer and transported to the laboratory for analysis in the same container. During the past year, prototype devices have been tested for their performance in storing soil samples containing low concentrations of VOCs. The Accu Core sampler testing is also described in this report

NEW SOIL VOC SAMPLERS: EN CORE AND ACCU CORE SAMPLING/STORAGE DEVICES FOR VOC ANALYSIS

Soil sampling and storage practices for volatile organic analysis must be designed to minimize loss of volatile organic compounds (VOCs) from samples. The En Core{reg_sign} sampler is designed to collect and store soil samples in a manner that minimizes loss of contaminants due to volatilization and/or biodegradation. An ASTM International (ASTM) standard practice, D 6418, Standard Practice for Using the Disposable En Core Sampler for Sampling and Storing Soil for Volatile Organic Analysis, describes use of the En Core sampler to collect and store a soil sample of approximately 5 grams or 25 grams for volatile organic analysis and specifies sample storage in the En Core sampler at 4 {+-} 2 C for up to 48 hours; -7 to -21 C for up to 14 days; or 4 {+-} 2 C for up to 48 hours followed by storage at -7 to -21 C for up to five days. This report discusses activities performed during the past year to promote and continue acceptance of the En Core samplers based on their performance to store soil samples for VOC analysis. The En Core sampler is designed to collect soil samples for VOC analysis at the soil surface. To date, a sampling tool for collecting and storing subsurface soil samples for VOC analysis is not available. Development of a subsurface VOC sampling/storage device was initiated in 1999. This device, which is called the Accu Core{trademark} sampler, is designed so that a soil sample can be collected below the surface using a dual-tube penetrometer and transported to the laboratory for analysis in the same container. Laboratory testing of the current Accu Core design shows that the device holds low-level concentrations of VOCs in soil samples during 48-hour storage at 4 {+-} 2 C and that the device is ready for field evaluation to generate additional performance data. This report discusses a field validation exercise that was attempted in Pennsylvania in 2004 and activities being performed to plan and conduct a field validation study in 2006. A draft ASTM practice describing use of the Accu Core sampler is being prepared. An update on the status of the ASTM practice is given in this report

Mercury CEM Calibration

The Clean Air Mercury Rule (CAMR) which was published in the Federal Register on May 18, 2005, requires that calibration of mercury continuous emissions monitors (CEMs) be performed with NIST-traceable standards. Western Research Institute (WRI) is working closely with the Electric Power Research Institute (EPRI), the National Institute of Standards and Technology (NIST), and the Environmental Protection Agency (EPA) to facilitate the development of the experimental criteria for a NIST traceability protocol for dynamic elemental mercury vapor generators. The traceability protocol will be written by EPA. Traceability will be based on the actual analysis of the output of each calibration unit at several concentration levels ranging from about 2-40 ug/m{sup 3}, and this analysis will be directly traceable to analyses by NIST using isotope dilution inductively coupled plasma/mass spectrometry (ID ICP/MS) through a chain of analyses linking the calibration unit in the power plant to the NIST ID ICP/MS. Prior to this project, NIST did not provide a recommended mercury vapor pressure equation or list mercury vapor pressure in its vapor pressure database. The NIST Physical and Chemical Properties Division in Boulder, Colorado was subcontracted under this project to study the issue in detail and to recommend a mercury vapor pressure equation that the vendors of mercury vapor pressure calibration units can use to calculate the elemental mercury vapor concentration in an equilibrium chamber at a particular temperature. As part of this study, a preliminary evaluation of calibration units from five vendors was made. The work was performed by NIST in Gaithersburg, MD and Joe Rovani from WRI who traveled to NIST as a Visiting Scientist

Prototype ATLAS IBL Modules using the FE-I4A Front-End Readout Chip

The ATLAS Collaboration will upgrade its semiconductor pixel tracking detector with a new Insertable B-layer (IBL) between the existing pixel detector and the vacuum pipe of the Large Hadron Collider. The extreme operating conditions at this location have necessitated the development of new radiation hard pixel sensor technologies and a new front-end readout chip, called the FE-I4. Planar pixel sensors and 3D pixel sensors have been investigated to equip this new pixel layer, and prototype modules using the FE-I4A have been fabricated and characterized using 120 GeV pions at the CERN SPS and 4 GeV positrons at DESY, before and after module irradiation. Beam test results are presented, including charge collection efficiency, tracking efficiency and charge sharing.Comment: 45 pages, 30 figures, submitted to JINS

Characterization of HV-CMOS detectors in BCD8 technology and of a controlled hybridization technique

Radiation detectors built in high-voltage and high-resistivity CMOS technology are an interesting option for the large area pixel-trackers sought for the upgrade of the Large Hadron Collider experiments. A characterisation of the BCD8 technology by STMicroelectronics process has been performed to evaluate its suitability for the realisation of CMOS sensors with a depleted region of several tens of micrometer. Sensors featuring 50 7250 \u3bcm2 pixels on a 125 \u3a9cm resistivity substrate have been characterized. The response to ionizing radiation is tested using radioactive sources and an X-ray tune, reading out the detector with an external spectroscopy chain. Irradiation tests were performed up to proton fluences exceeding 5 c51015 p/cm2 and they show the depletion and breakdown voltages increases with irradiation. A hybridization process for capacitive coupling has been developed. Assemblies have been performed using the ATLAS FE-I4 readout ASIC and prototype CMOS sensors. Measurements show a planarity better than 1.5 \u3bcm peak-to-peak on the 5 mm length of the HV-CMOS chip. To evaluate more precisely the achievable uniformity dummy chips of FE-I4 sizes have been made on 6-inch wafers. The measurement of the 24 capacitors on each chip is expected to achieve a precise estimation of the real thickness uniformity. The goal is to achieve less then 10% variation on the glue thickness ( 3c0.5 \u3bcm)

ATLAS pixel detector electronics and sensors

The silicon pixel tracking system for the ATLAS experiment at the Large Hadron Collider is described and the performance requirements are summarized. Detailed descriptions of the pixel detector electronics and the silicon sensors are given. The design, fabrication, assembly and performance of the pixel detector modules are presented. Data obtained from test beams as well as studies using cosmic rays are also discussed