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PHASE CHANGE LIQUIDS

Description: Work is being performed to develop a new shipping system for frozen environmental samples (or other materials) that uses an optimal phase change liquid (PCL) formulation and an insulated shipping container with an on-board digital temperature data logger to provide a history of the temperature profile within the container during shipment. In previous work, several PCL formulations with temperatures of fusion ranging from approximately -14 to -20 C were prepared and evaluated. Both temperature of fusion and heat of fusion of the formulations were measured, and an optimal PCL formulation was selected. The PCL was frozen in plastic bags and tested for its temperature profile in a cooler using a digital temperature data logger. This testing showed that the PCL formulation can maintain freezer temperatures (< -7 to -20 C) for an extended period, such as the time for shipping samples by overnight courier. The results of the experiments described in this report provide significant information for use in developing an integrated freezer system that uses a PCL formulation to maintain freezer temperatures in coolers for shipping environmental samples to the laboratory. Experimental results show the importance of the type of cooler used in the system and that use of an insulating material within the cooler improves the performance of the freezer system. A new optimal PCL formulation for use in the system has been determined. The new formulation has been shown to maintain temperatures at < -7 to -20 C for 47 hours in an insulated cooler system containing soil samples. These results are very promising for developing the new technology.
Date: March 1, 2006
Creator: Sorini, Susan S. & Schabron, John F.
Partner: UNT Libraries Government Documents Department

Mercury CEM Calibration

Description: Mercury continuous emissions monitoring systems (CEMS) are being implemented in over 800 coal-fired power plant stacks. The power industry desires to conduct at least a full year of monitoring before the formal monitoring and reporting requirement begins on January 1, 2009. It is important for the industry to have available reliable, turnkey equipment from CEM vendors. 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 generators are used to calibrate mercury CEMs at power plant sites. The Clean Air Mercury Rule (CAMR) which was published in the Federal Register on May 18, 2005 requires that calibration be performed with NIST-traceable standards (Federal Register 2007). Traceability procedures will be defined by EPA. An initial draft traceability protocol was issued by EPA in May 2007 for comment. In August 2007, EPA issued an interim traceability protocol for elemental mercury generators (EPA 2007). The protocol is based on the actual analysis of the output of each calibration unit at several concentration levels ranging initially from about 2-40 {micro}g/m{sup 3} elemental mercury, and in the future down to 0.2 {micro}g/m{sup 3}, and this analysis will be directly traceable to analyses by NIST. The document is divided into two separate sections. The first deals with the qualification of generators by the vendors for use in mercury CEM calibration. The second describes the procedure that the vendors must use to certify the generator models that meet the qualification specifications. The NIST traceable certification is performance based, traceable to analysis using isotope dilution inductively coupled plasma/mass spectrometry performed by NIST in Gaithersburg, MD. The outputs of mercury generators ...
Date: February 29, 2008
Creator: Schabron, John; Rovani, Joseph & Sanderson, Mark
Partner: UNT Libraries Government Documents Department

Enhanced Oil Recovery: Aqueous Flow Tracer Measurement

Description: A low detection limit analytical method was developed to measure a suite of benzoic acid and fluorinated benzoic acid compounds intended for use as tracers for enhanced oil recovery operations. Although the new high performance liquid chromatography separation successfully measured the tracers in an aqueous matrix at low part per billion levels, the low detection limits could not be achieved in oil field water due to interference problems with the hydrocarbon-saturated water using the system's UV detector. Commercial instrument vendors were contacted in an effort to determine if mass spectrometry could be used as an alternate detection technique. The results of their work demonstrate that low part per billion analysis of the tracer compounds in oil field water could be achieved using ultra performance liquid chromatography mass spectrometry.
Date: February 1, 2009
Creator: Rovani, Joseph & Schabron, John
Partner: UNT Libraries Government Documents Department

VALIDATION OF A NEW SOIL VOC SAMPLER

Description: The overall objective of this project is to facilitate national acceptance of the EnCore{trademark} sampling/storage device by conducting product tests, method development, and method validation activities. The specific goals for the initial six-month period of the project are listed: (1) Evaluate and become familiar with the stainless steel EnCore{trademark} sampling/storage device for collecting and holding soil samples for determination of volatile organic compounds (VOCs); (2) Initiate interaction with American Society for Testing and Materials (ASTM) Committee D-34 on Waste Management to begin the ASTM standard preparation and approval process; (3) Prepare an ASTM drall practice for using a device fitting the description of the EnCore{trademark} sampler for sampling and storing soil for volatile organic analysis. Under ASTM guidelines, the procedure describing the use of a device, such as the EnCore{trademark} sampler, is referred to as a practice rather than a method because it is a definitive set of instructions for performing one or more specific operations that does not produce a test result (ASTM 1996a); and (4) Plan testing needed to establish maximum storage temperatures and times for inclusion in the ASTM practice.
Date: April 1, 1997
Creator: Sorini, Susan S. & Schabron, John F.
Partner: UNT Libraries Government Documents Department

CHEMICAL SENSOR AND FIELD SCREENING TECHNOLOGY DEVELOPMENT: FUELS IN SOILS FIELD SCREENING METHOD VALIDATION

Description: A new screening method for fuel contamination in soils was recently developed as American Society for Testing and Materials (ASTM) Method D-583 1-95, Standard Test Method for Screening Fuels in Soils. This method uses low-toxicity chemicals and can be used to screen organic-rich soils. In addition, it is fast, easy, and inexpensive to perform. The screening method calls for extracting a sample of soil with isopropyl alcohol following treatment with calcium oxide. The resulting extract is filtered, and the ultraviolet absorbance of the extract is measured at 254 nm. Depending on the available information concerning the contaminant fuel type and availability of the contaminant fuel for calibration, the method can be used to determine the approximate concentration of fuel contamination, an estimated value of fuel contamination, or an indication of the presence or absence of fuel contamination. Fuels containing aromatic compounds, such as diesel fuel and gasoline, as well as other aromatic-containing hydrocarbon materials, such as motor oil, crude oil, and coal oil, can be determined. The screening method for fuels in soils was evaluated by conducting a collaborative study on the method and by using the method to screen soil samples at an actual field site. In the collaborative study, a sand and an organic soil spiked with various concentrations of diesel fuel were tested. Data from the collaborative study were used to determine the reproducibility (between participants) and repeatability (within participant) precision of the method for screening the test materials. The collaborative study data also provide information on the performance of portable field equipment versus laboratory equipment for performing the screening method and a comparison of diesel concentration values determined using the screening method versus a laboratory method. Data generated using the method to screen soil samples in the field provide information on the performance of the method ...
Date: April 1, 1997
Creator: Sorini, Susan S. & Schabron, John F.
Partner: UNT Libraries Government Documents Department

ACCU Core Sampling/Storage Device for VOC Analysis

Description: The Accu Core sampler system consists of alternating cylindrical clear acrylic sections and one-inch cylindrical stainless steel sections arranged in clear shrink wrap. The set of alternating acrylic and stainless steel sections in the shrink wrap are designed to fit in a Geoprobe dual-tube penetrometer for collection of continuous soil cores. The clear acrylic sections can have 1/2-inch access holes for easy soil headspace screening without violating the integrity of the adjacent stainless steel sections. The Accu Core sampler system can be used to store a soil sample collected in the stainless steel section by capping the ends of the section so it becomes a sample storage container. The sampler system can also be used to collect a subsurface soil sample in one of the sections that can be directly extruded from the section into a container for storage during shipment to the laboratory. In addition, the soil in a sampler section can be quickly sub-sampled using a coring tool and extruded into a storage container so the integrity of the soil is not disrupted and the potential for VOC loss during sub-sampling is greatly reduced. A field validation study was conducted to evaluate the performance of the Accu Core sampler to store VOC soil samples during transportation to the laboratory for analysis and to compare the performance of the Accu Core with current sampling and storage techniques, all of which require sub-sampling when the soil sample is brought to the surface. During some of the validation testing, the acrylic sections having access holes for headspace screening were included in the Accu Core sampler configuration and soil in these sections was screened to show the usefulness of the sample screening capability provided by the Accu Core system. This report presents the results of the field validation study as well as ...
Date: April 30, 2007
Creator: Sorini, Susan S.; Schabron, John F. & Sanderson, Mark M.
Partner: UNT Libraries Government Documents Department

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

Description: 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 ...
Date: June 1, 2002
Creator: Sorini, Susan S.; Schabron, John F. & Rovani, Joseph F.
Partner: UNT Libraries Government Documents Department

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

Description: 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 ...
Date: September 15, 2003
Creator: Sorini, Susan S.; Schabron, John F. & Rovani, Joseph F.
Partner: UNT Libraries Government Documents Department

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

Description: 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 ...
Date: June 1, 2006
Creator: Sorini, Susan S.; Schabron, John F. & Jr, Joseph F. Rovani
Partner: UNT Libraries Government Documents Department

Petroleum Processing Efficiency Improvement

Description: A series of volatile crude oils was characterized using the Asphaltene Determinator oncolumn precipitation and re-dissolution method developed at Western Research Institute (WRI). Gravimetric asphaltenes and polars fractions from silica gel chromatography separation of the oils were characterized also. A study to define the differences in composition of asphaltenes in refinery desalter rag layer emulsions and the corresponding feed and desalter oils was conducted. Results indicate that the most polar and pericondensed aromatic material in the asphaltenes is enriched in the emulsions. The wax types and carbon number distributions in the two heptaneeluting fractions from the Waxphaltene Determinator separation were characterized by repetitive collection of the fractions followed by high temperature gas chromatography (GC) and Fourier transform infrared spectroscopy (FTIR). High resolution Fourier transform ion cyclotron resonance mass spectrometry (FT-ICRMS) was conducted by researchers at the Florida State University National High Magnetic Field laboratory in a no-cost collaboration with the study.
Date: September 1, 2012
Creator: Schabron, John; Rovani, Joseph; Sanderson, Mark & Loveridge, Jenny
Partner: UNT Libraries Government Documents Department

Mercury CEM Calibration

Description: 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.
Date: March 31, 2007
Creator: Schabron, John F.; Rovani, Joseph F. & Sorini, Susan S.
Partner: UNT Libraries Government Documents Department

FIELD SCREENING FOR HALOGENATED VOLATILE ORGANIC COMPOUNDS: THE NEW X-WAND HVOC SCREENING DEVICE

Description: Western Research Institute (WRI) has developed new methodology and a test kit to screen soil or water samples for halogenated volatile organic compounds (HVOCs) in the field. The technology has been designated the X-Wand{trademark} screening tool. The new device uses a heated diode sensor that is commonly used to detect leaks of refrigerants from air conditioners, freezers, and refrigerators. This sensor is selective to halogens. It does not respond to volatile aromatic hydrocarbons, such as those in gasoline, and it is not affected by high humidity. In the current work, the heated diode leak detectors were modified further to provide units with rapid response and enhanced sensitivity. The limit of detection for trichloroethylene TCE in air is 0.1 mg/m{sup 3} (S/N = 2). The response to other HVOCS relative to TCE is similar. Variability between sensors and changes in a particular sensor over time can be compensated for by normalizing sensor readings to a maximum sensor reading at 1,000 mg/m{sup 3} TCE. The soil TCE screening method was expanded to include application to water samples. Assuming complete vaporization, the detection limit for TCE in soil is about 1 ug/kg (ppb) for a 25-g sample in an 8-oz jar. The detection limit for TCE in water is about 1 ug/L (ppb) for a 25-mL sample in an 8-oz jar. This is comparable to quantitation limits of EPA GC/MS laboratory methods. A draft ASTM method for screening TCE contaminated soils using a heated diode sensor was successfully submitted for concurrent main committee and subcommittee balloting in ASTM Committee D 34 on Waste Management. The method was approved as ASTM D 7203-05, Standard Test Method for Screening Trichloroethylene (TCE)-Contaminated Soil Using a Heated Diode Sensor.
Date: March 1, 2006
Creator: Schabron, John F.; Sorini, Susan S. & Jr, Joseph F. Rovani
Partner: UNT Libraries Government Documents Department

HEAVY OIL PROCESS MONITOR: AUTOMATED ON-COLUMN ASPHALTENE PRECIPITATION AND RE-DISSOLUTION

Description: About 37-50% (w/w) of the heptane asphaltenes from unpyrolyzed residua dissolve in cyclohexane. As pyrolysis progresses, this number decrease to below 15% as coke and toluene insoluble pre-coke materials appear. This solubility measurement can be used after coke begins to form, unlike the flocculation titration, which cannot be applied to multi-phase systems. Currently, the procedure for the isolation of heptane asphaltenes and the determination of the amount of asphaltenes soluble in cyclohexane spans three days. A more rapid method to measure asphaltene solubility was explored using a novel on-column asphaltene precipitation and re-dissolution technique. This was automated using high performance liquid chromatography (HPLC) equipment with a step gradient sequence using the solvents: heptane, cyclohexane, toluene:methanol (98:2). Results for four series of original and pyrolyzed residua were compared with data from the gravimetric method. The measurement time was reduced from three days to forty minutes. The separation was expanded further with the use of four solvents: heptane, cyclohexane, toluene, and cyclohexanone or methylene chloride. This provides a fourth peak which represents the most polar components, in the oil.
Date: June 1, 2006
Creator: Schabron, John F.; Jr, Joseph F. Rovani & Sanderson, Mark
Partner: UNT Libraries Government Documents Department

Heavy Oil Process Monitor: Automated On-Column Asphaltene Precipitation and Re-Dissolution

Description: An automated separation technique was developed that provides a new approach to measuring the distribution profiles of the most polar, or asphaltenic components of an oil, using a continuous flow system to precipitate and re-dissolve asphaltenes from the oil. Methods of analysis based on this new technique were explored. One method based on the new technique involves precipitation of a portion of residua sample in heptane on a polytetrafluoroethylene-packed (PTFE) column. The precipitated material is re-dissolved in three steps using solvents of increasing polarity: cyclohexane, toluene, and methylene chloride. The amount of asphaltenes that dissolve in cyclohexane is a useful diagnostic of the thermal history of oil, and its proximity to coke formation. For example, about 40 % (w/w) of the heptane asphaltenes from unpyrolyzed residua dissolves in cyclohexane. As pyrolysis progresses, this number decrease to below 15% as coke and toluene insoluble pre-coke materials appear. Currently, the procedure for the isolation of heptane asphaltenes and the determination of the amount of asphaltenes soluble in cyclohexane spans three days. The automated procedure takes one hour. Another method uses a single solvent, methylene chloride, to re-dissolve the material that precipitates on heptane on the PTFE-packed column. The area of this second peak can be used to calculate a value which correlates with gravimetric asphaltene content. Currently the gravimetric procedure to determine asphaltenes takes about 24 hours. The automated procedure takes 30 minutes. Results for four series of original and pyrolyzed residua were compared with data from the gravimetric methods. Methods based on the new on-column precipitation and re-dissolution technique provide significantly more detail about the polar constituent's oils than the gravimetric determination of asphaltenes.
Date: March 31, 2007
Creator: Schabron, John F.; Rovani, Joseph F. & Sanderson, Mark
Partner: UNT Libraries Government Documents Department

Mercury Calibration System

Description: U.S. Environmental Protection Agency (EPA) Performance Specification 12 in the Clean Air Mercury Rule (CAMR) states that a mercury CEM must be calibrated with National Institute for Standards and Technology (NIST)-traceable standards. In early 2009, a NIST traceable standard for elemental mercury CEM calibration still does not exist. Despite the vacature of CAMR by a Federal appeals court in early 2008, a NIST traceable standard is still needed for whatever regulation is implemented in the future. Thermo Fisher is a major vendor providing complete integrated mercury continuous emissions monitoring (CEM) systems to the industry. WRI is participating with EPA, EPRI, NIST, and Thermo Fisher towards the development of the criteria that will be used in the traceability protocols to be issued by EPA. An initial draft of an elemental mercury calibration traceability protocol was distributed for comment to the participating research groups and vendors on a limited basis in early May 2007. In August 2007, EPA issued an interim traceability protocol for elemental mercury calibrators. Various working drafts of the new interim traceability protocols were distributed in late 2008 and early 2009 to participants in the Mercury Standards Working Committee project. The protocols include sections on qualification and certification. The qualification section describes in general terms tests that must be conducted by the calibrator vendors to demonstrate that their calibration equipment meets the minimum requirements to be established by EPA for use in CAMR monitoring. Variables to be examined include linearity, ambient temperature, back pressure, ambient pressure, line voltage, and effects of shipping. None of the procedures were described in detail in the draft interim documents; however they describe what EPA would like to eventually develop. WRI is providing the data and results to EPA for use in developing revised experimental procedures and realistic acceptance criteria based on actual capabilities ...
Date: March 11, 2009
Creator: Schabron, John; Kalberer, Eric; Rovani, Joseph; Sanderson, Mark; Boysen, Ryan & Schuster, William
Partner: UNT Libraries Government Documents Department

Mercury Calibration System

Description: U.S. Environmental Protection Agency (EPA) Performance Specification 12 in the Clean Air Mercury Rule (CAMR) states that a mercury CEM must be calibrated with National Institute for Standards and Technology (NIST)-traceable standards. In early 2009, a NIST traceable standard for elemental mercury CEM calibration still does not exist. Despite the vacature of CAMR by a Federal appeals court in early 2008, a NIST traceable standard is still needed for whatever regulation is implemented in the future. Thermo Fisher is a major vendor providing complete integrated mercury continuous emissions monitoring (CEM) systems to the industry. WRI is participating with EPA, EPRI, NIST, and Thermo Fisher towards the development of the criteria that will be used in the traceability protocols to be issued by EPA. An initial draft of an elemental mercury calibration traceability protocol was distributed for comment to the participating research groups and vendors on a limited basis in early May 2007. In August 2007, EPA issued an interim traceability protocol for elemental mercury calibrators. Various working drafts of the new interim traceability protocols were distributed in late 2008 and early 2009 to participants in the Mercury Standards Working Committee project. The protocols include sections on qualification and certification. The qualification section describes in general terms tests that must be conducted by the calibrator vendors to demonstrate that their calibration equipment meets the minimum requirements to be established by EPA for use in CAMR monitoring. Variables to be examined include linearity, ambient temperature, back pressure, ambient pressure, line voltage, and effects of shipping. None of the procedures were described in detail in the draft interim documents; however they describe what EPA would like to eventually develop. WRI is providing the data and results to EPA for use in developing revised experimental procedures and realistic acceptance criteria based on actual capabilities ...
Date: March 11, 2009
Creator: Schabron, John; Kalberer, Eric; Rovani, Joseph; Sanderson, Mark; Boysen, Ryan & Schuster, William
Partner: UNT Libraries Government Documents Department

Mercury Continuous Emmission Monitor Calibration

Description: Mercury continuous emissions monitoring systems (CEMs) are being implemented in over 800 coal-fired power plant stacks throughput the U.S. 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 calibrators/generators. These devices are used to calibrate mercury CEMs at power plant sites. The Clean Air Mercury Rule (CAMR) which was published in the Federal Register on May 18, 2005 and vacated by a Federal appeals court in early 2008 required that calibration be performed with NIST-traceable standards. Despite the vacature, mercury emissions regulations in the future will require NIST traceable calibration standards, and EPA does not want to interrupt the effort towards developing NIST traceability protocols. The traceability procedures will be defined by EPA. An initial draft traceability protocol was issued by EPA in May 2007 for comment. In August 2007, EPA issued a conceptual interim traceability protocol for elemental mercury calibrators. The protocol is based on the actual analysis of the output of each calibration unit at several concentration levels ranging initially from about 2-40 {micro}g/m{sup 3} elemental mercury, and in the future down to 0.2 {micro}g/m{sup 3}, and this analysis will be directly traceable to analyses by NIST. The EPA traceability protocol document is divided into two separate sections. The first deals with the qualification of calibrator models by the vendors for use in mercury CEM calibration. The second describes the procedure that the vendors must use to certify the calibrators that meet the qualification specifications. The NIST traceable certification is performance based, traceable to analysis using isotope dilution inductively coupled plasma/mass spectrometry (ID/ICP/MS) performed by NIST in Gaithersburg, MD. The outputs ...
Date: March 12, 2009
Creator: Schabron, John; Kalberer, Eric; Boysen, Ryan; Schuster, William & Rovani, Joseph
Partner: UNT Libraries Government Documents Department

Soil Samplers: New Techniques for Subsurface Sampling for Volatile Organic Compounds

Description: Soil sampling techniques for volatile organic analysis must be designed to minimize loss of volatile organic compounds (VOCs) from the soil that is being sampled. Preventing VOC loss from soil cores that are collected from the subsurface and brought to the surface for subsampling is often difficult. Subsurface bulk sample retrieval systems are designed to obtain intact cylindrical cores of soil ranging anywhere from one to four inches in diameter, and one to several feet in length. The current technique that is used to subsample these soil cores for VOC analysis is to expose a horizontal section of the soil core to the atmosphere; screen the exposed soil using a photoionization detector (PID) or other appropriate device to locate contamination in the soil core; and use a hand-operated coring tool to collect samples from the exposed soil for analysis. Because the soil core can be exposed to the atmosphere for a considerable length of time during screening and sample collection, the current sub-sampling technique provides opportunity for VOCs to be lost from the soil. This report describes three alternative techniques from the current technique for screening and collecting soil samples from subsurface soil cores for VOC analysis and field testing that has been done to evaluate the techniques. Based on the results of the field testing, ASTM D4547, Standard Guide for Sampling Waste and Soils for Volatile Organic Compounds, was revised to include information about the new techniques.
Date: March 31, 2009
Creator: Sorini, Susan; Schabron, John; Rovani, Joseph & Sanderson, Mark
Partner: UNT Libraries Government Documents Department

PETROLEUM RESIDUA SOLUBILITY PARAMETER/POLARITY MAP: STABILITY STUDIES OF RESIDUA PYROLYSIS

Description: A new molecular weight/polarity map based on the Scatchard-Hildebrand solubility equation has been developed for petroleum residua. A series of extractions are performed with solvents of increasing solubility parameter, and the fractions are analyzed by vapor pressure osmometry for number average molecular weight and by analytical-scale size exclusion chromatography for molecular weight spread. Work was performed for a heavy oil material subjected to three increasing severities of thermal treatment prior to and through the onset of coke formation. The results are diagnostic of the layers of solvations by resin-type molecules around a central asphaltene core. Two additional stability diagnostic methods were also used. These were the Heithaus titration ''P-index'' and Gaestel ''G'' index, which have been applied to paving asphalts for decades. The Heithaus titration involves the titration of three toluene solutions of a residuum at three concentrations with a poor solvent, such as isooctane, to the point of asphaltene flocculation. In the present work, the significance of the data are developed in terms of the Hildebrand solubility parameter. The Heithaus results are combined with data from the new molecular weight/polarity map. The solubility parameters for the toluene-soluble asphaltene components are measured, and the solubility parameters of the maltenes can be calculated. As thermal treatment progresses, the solubility parameters of asphaltene materials increase and the molecular weights decrease. A new coking index is proposed based on Heithaus titration data. Preliminary results suggest that an alternative, simpler coking index may be developed by measuring the weight percent of cyclohexane solubles in heptane asphaltenes. Coking onset appears to coincide with the depletion of these resin-type asphaltene solubilizing components of residua. The objective of the present study was to develop a mapping tool that will enhance understanding of the changes that occur in residua during upgrading and support the industry-sponsored work in which ...
Date: April 30, 1999
Creator: Schabron, John F.; Pauli, A. Troy & Joseph F. Rovani, Jr.
Partner: UNT Libraries Government Documents Department

RESIDUA UPGRADING EFFICIENCY IMPROVEMENT MODELS: COKE FORMATION PREDICTABILITY MAPS

Description: The dispersed particle solution model of petroleum residua structure was used to develop predictors for pyrolytic coke formation. Coking Indexes were developed in prior years that measure how near a pyrolysis system is to coke formation during the coke formation induction period. These have been demonstrated to be universally applicable for residua regardless of the source of the material. Coking onset is coincidental with the destruction of the ordered structure and the formation of a multiphase system. The amount of coke initially formed appears to be a function of the free solvent volume of the original residua. In the current work, three-dimensional coke make predictability maps were developed at 400 C, 450 C, and 500 C (752 F, 842 F, and 932 F). These relate residence time and free solvent volume to the amount of coke formed at a particular pyrolysis temperature. Activation energies for two apparent types of zero-order coke formation reactions were estimated. The results provide a new tool for ranking residua, gauging proximity to coke formation, and predicting initial coke make tendencies.
Date: May 1, 2002
Creator: Schabron, John F.; Pauli, A. Troy & Jr., Joseph F. Rovani
Partner: UNT Libraries Government Documents Department

FIELD SCREENING FOR HALOGENATED VOLATILE ORGANIC COMPOUNDS

Description: Western Research Institute (WRI) initiated exploratory work towards the development of new field screening methodology and a test kit to measure halogenated volatile organic compounds (VOCs) in the field. Heated diode and corona discharge sensors are commonly used to detect leaks of refrigerants from air conditioners, freezers, and refrigerators. They are both selective to the presence of carbon-halogen bonds. Commercially available heated diode and corona discharge leak detectors were procured and evaluated for halogenated VOC response. The units were modified to provide a digital readout of signal related to VOC concentration. Sensor response was evaluated with carbon tetrachloride and tetrachloroethylene (perchloroethylene, PCE), which represent halogenated VOCs with and without double bonds. The response characteristics were determined for the VOCs directly in headspace in Tedlar bag containers. Quantitation limits in air were estimated. Potential interferences from volatile hydrocarbons, such as toluene and heptane, were evaluated. The effect of humidity was studied also. The performance of the new devices was evaluated in the laboratory by spiking soil samples and monitoring headspace for halogenated VOCs. A draft concept of the steps for a new analytical method was outlined. The results of the first year effort show that both devices show potential utility for future analytical method development work towards the goal of developing a portable test kit for screening halogenated VOCs in the field.
Date: June 1, 2002
Creator: Schabron, John F.; Jr., Joseph F. Rovani & Bomstad, Theresa M.
Partner: UNT Libraries Government Documents Department

VALIDATION OF A NEW SOIL VOC SAMPLER: PERFORMANCE OF THE EN CORE SAMPLER AT -7 C AND -21 C AND DEVELOPMENT OF THE ACCU CORE SUBSURFACE SAMPLING/STORAGE DEVICE FOR VOC ANALYSIS

Description: 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 five grams or 25 grams for volatile organic analysis. Prior to the study described in this report, D 6418 specified sample storage in the En Core sampler at 4 {+-} 2 C for up to 48 hours; at -12 {+-} 2 C for up to 14 days; or at 4 {+-} 2 C for up to 48 hours followed by storage at -12 {+-} 2 C for up to five days to minimize loss of volatile compounds due to volatilization and/or biodegradation. The study described in this report was conducted to evaluate the performance of the disposable En Core sampler to store low concentrations of VOCs in soil at -7 {+-} 1 C and -21 {+-} 2 C. In the study, data on the performance of the En Core sampler to store soils spiked with low-level concentrations of VOCs at 4 {+-} 2 C for 48 hours followed by storage at -7 {+-} 1 C for five days, at -7 {+-} 1 C for 14 days, at 4 {+-} 2 C for 48 hours followed by storage at -21 {+-} 2 C for five days, and at -21 {+-} 2 C for 14 days were generated. Based on these data, a new revision of D 6418 was prepared and balloted in ...
Date: May 1, 2004
Creator: Sorini, Susan S.; Schabron, John F. & Jr., Joseph F. Rovani
Partner: UNT Libraries Government Documents Department

FIELD SCREENING FOR HALOGENATED VOLATILE ORGANIC COMPOUNDS

Description: Western Research Institute (WRI) is continuing work toward the development of new screening methodology and a test kit to measure halogenated volatile organic compounds (VOCs) in the field. Heated diode and corona discharge sensors are commonly used to detect leaks of refrigerants from air conditioners, freezers, and refrigerators. They are both selective to the presence of halogens. In prior work, the devices were tested for response to carbon tetrachloride, heptane, toluene, and water vapors. In the current work, sensor response was evaluated with sixteen halogenated VOCs relative to carbon tetrachloride. The results show that the response of the various chlorinated VOCs is within an order of magnitude of the response to carbon tetrachloride for each of the sensors. Thus, for field screening a single response factor can be used. Both types of leak detectors are being further modified to provide an on-board LCD signal readout, which is related to VOC concentration. The units will be fully portable and will operate with 115-V line or battery power. Signal background, noise level, and response data on the Bacharach heated diode detector and the TIF corona discharge detector show that when the response curves are plotted against the log of concentration, the plot is linear to the upper limit for the particular unit, with some curvature at lower levels. When response is plotted directly against concentration, the response is linear at the low end and is curved at the high end. The dynamic ranges for carbon tetrachloride of the two devices from the lower detection limit (S/N=2) to signal saturation are 4-850 vapor parts per million (vppm) for the corona discharge unit and 0.01-70 vppm for the heated diode unit. Additional circuit modifications are being made to lower the detection limit and increase the dynamic response range of the corona discharge unit. The ...
Date: July 1, 2003
Creator: Schabron, John F.; Joseph F. Rovani, Jr. & Bomstad, Theresa M.
Partner: UNT Libraries Government Documents Department

FUELS IN SOIL TEST KIT: FIELD USE OF DIESEL DOG SOIL TEST KITS

Description: Western Research Institute (WRI) has developed a new commercial product ready for technology transfer, the Diesel Dog{reg_sign} Portable Soil Test Kit, for performing analysis of fuel-contaminated soils in the field. The technology consists of a method developed by WRI (U.S. Patents 5,561,065 and 5,976,883) and hardware developed by WRI that allows the method to be performed in the field (patent pending). The method is very simple and does not require the use of highly toxic reagents. The aromatic components in a soil extract are measured by absorption at 254 nm with a field-portable photometer. WRI added significant value to the technology by taking the method through the American Society for Testing and Materials (ASTM) approval and validation processes. The method is designated as ASTM Method D 5831-96, Standard Test Method for Screening Fuels in Soils. This ASTM designation allows the method to be used for federal compliance activities. In June 2001, the Diesel Dog technology won an American Chemical Society Regional Industrial Innovations Award. To gain field experience with the new technology, Diesel Dog kits have been used for a variety of site evaluation and cleanup activities. Information gained from these activities has led to improvements in hardware configurations and additional insight into correlating Diesel Dog results with results from laboratory methods. The Wyoming Department of Environmental Quality (DEQ) used Diesel Dog Soil Test Kits to guide cleanups at a variety of sites throughout the state. ENSR, of Acton, Massachusetts, used a Diesel Dog Portable Soil Test Kit to evaluate sites in the Virgin Islands and Georgia. ChemTrack and the U.S. Army Corps of Engineers successfully used a test kit to guide excavation at an abandoned FAA fuel-contaminated site near Fairbanks, Alaska. Barenco, Inc. is using a Diesel Dog Portable Soil Test Kit for site evaluations in Canada. A small ...
Date: September 30, 2002
Creator: Sorini, Susan S.; Schabron, John F. & Joseph F. Rovani, Jr.
Partner: UNT Libraries Government Documents Department