Anthony D. Cinson

High‐Performance, Superparamagnetic, Nanoparticle‐Based Heavy Metal Sorbents for Removal of Contaminants from Natural Waters

We describe the synthesis and characterization of high-performance, superparamagnetic, iron oxide nanoparticle-based, heavy metal sorbents, which demonstrate excellent affinity for the separation of heavy metals in contaminated water systems (i.e., spiked Columbia River water). The magnetic nanoparticle sorbents were prepared from an easy-to-synthesize iron oxide precursor, followed by a simple, one-step ligand exchange reaction to introduce an affinity ligand to the nanoparticle surface that is specific to a heavy metal or class of heavy metal contaminants. The engineered magnetic nanoparticle sorbents have inherently high active surface areas, allowing for increased binding capacities. To demonstrate the performance of the nanoparticle sorbents, river water was spiked with specific metals and exposed to low concentrations of the functionalized nanoparticles. In almost all cases, the nanoparticles were found to be superior to commercially available sorbent materials as well as the unfunctionalized iron oxide nanoparticles.

Preliminary Assessment of NDE Methods on Inspection of HDPE Butt Fusion Piping Joints for Lack of Fusion

Studies at the Pacific Northwest National Laboratory in Richland, Washington, are being conducted to evaluate nondestructive examination approaches for inspecting butt fusion joints in high density polyethylene (HDPE) pipe for lack of fusion (LOF). The work provides information to the United States Nuclear Regulatory Commission on the effectiveness and need for volumetric inspection techniques of HDPE butt fusion joints in Section III, Division 1, Class 3, buried piping systems in nuclear power plants. This paper describes results from preliminary assessments using ultrasonic nondestructive techniques and high-speed tensile impact testing for determining joint integrity. A series of butt joints were fabricated in 3408, 12-inch IPS DR-11 material by varying the fusion parameters in attempts to provide good joints and joints containing LOF. These butt joints were visually examined and volumetrically examined with time-of-flight diffraction (TOFD) and phased-array (PA) ultrasound. A limited subset of pipe joint material was destructively analyzed by either slicing through the joint and visually examining the surface or by employing a standard high-speed tensile impact test. Initial correlation of the fusion parameters, nondestructive, and destructive evaluations have shown that areas with gross LOF were detected with both TOFD and PA ultrasound and that the tensile impact test showed a brittle failure at the joint. There is still some ambiguity in results from the less obvious LOF conditions. Current work is targeted on assessing the sensitivity of the ultrasonic volumetric examinations and validating the results with a destructive analysis. It is expected that on-going and future work will lead to quantifying the ultrasonic responses in terms of joint integrity.Copyright

Improved explosive collection and detection with rationally assembled surface sampling materials

Sampling and detection of trace explosives are critical steps in the analytical process necessary for modern transportation safety. In this work we have explored some of the fundamental aspects that influence collection and detection of trace levels of explosive residues from surfaces. We compared the analyte-release performance of standard muslin sampling swipes to that of rationally assembled fiberglass cloth, and used thermal-desorption ion mobility spectroscopy for detection. This collection–detection system is widely used for analyzing the trace chemical residues. The fiberglass cloth was chemically modified by covalently bonding phenyl-functional groups to the surface. The rationally assembled sampling materials provide significantly performance improvements over standard muslin sampling materials for detection of TNT, NG, RDX, TATP, and PETN. The phenyl-functionalized fiberglass swipes showed over 10 times greater TNT release, compared to muslin sampling swipes, as well as improved response and repeatability after multiple uses of the same swipe. The improved TNT release from the functionalized-fiberglass swipes resulted in significantly improved detection limits over muslin. To better understand the improvement offered by the phenyl-functionalized fiberglass, several commercially available fiberglass materials, each offering specific characteristics, were also compared, allowing several physical and chemical properties to be systematically explored to determine their influence on performance. These results are relevant to improving the detection of other explosive compounds, and potentially to a wider range of chemical sampling from surfaces.

Waterless coupling of ultrasound from planar contact transducers to curved and irregular surfaces during non-destructive ultrasonic evaluations

The Applied Physics group at the Pacific Northwest National Laboratory (PNNL) in Richland, WA has evaluated a method for waterless/liquidless coupling of ultrasonic energy from planar ultrasonic contact transducers to irregular test surfaces for ultrasonic non-destructive evaluation applications. Dry couplant material placed between a planar transducer face and a curved or uneven steel or plastic surface allows for effective sound energy coupling and preserves the integrity of the planar transducer sound field by serving as an acoustic impedance matching layer, providing good surface area contact between geometrically dissimilar surfaces and conforming to rough and unsmooth surfaces. Sound fields radiating from planar ultrasonic contact transducers coupled to curved and uneven surfaces using the dry coupling method were scanned and mapped using a Pinducer receiver connected to a raster scanner. Transducer sound field coverage at several ultrasonic frequencies and several distances from the transducer contact locations were found to be in good agreement with theoretical beam divergence and sound field coverage predictions for planar transducers coupled to simple, planar surfaces. This method is valuable for applications that do not allow for the use of traditional liquid-based ultrasonic couplants due to the sensitivity of the test materials to liquids and for applications that might otherwise require curved transducers or custom coupling wedges. The selection of dry coupling material is reported along with the results of theoretical sound field predictions, the laboratory testing apparatus and the empirical sound field data.

Ultrasonic Phased Array Evaluation of Control Rod Drive Mechanism (CRDM) Nozzle Interference Fit and Weld Region

Ultrasonic phased array data were collected on a removed-from-service CRDM nozzle specimen to assess a previously reported leak path. First a mock-up CRDM specimen was evaluated that contained two 0.076-mm (3.0-mil) interference fit regions formed from an actual Inconel CRDM tube and two 152.4-mm (6.0-in.) thick carbon steel blocks [1,2]. One interference fit region has a series of precision crafted electric discharge machining (EDM) notches at various lengths, widths, depths, and spatial separations for establishing probe sensitivity, resolution and calibration. The other interference fit has zones of boric acid (crystal form) spaced periodically between the tube and block to represent an actively leaking CRDM nozzle assembly in the field. Ultrasonic phased-array evaluations were conducted using an immersion 8-element annular 5.0-MHz probe from the tube inner diameter (ID). A variety of focal laws were employed to evaluate the interference fit regions and J-grove weld, where applicable. Responses from the mock-up specimen were evaluated to determine detection limits and characterization ability as well as contrast the ultrasonic response differences with the presence of boric acid in the fit region. Nozzle 63, from the North Anna Unit-2 nuclear power plant, was evaluated to assess leakage path(s) and was destructively dismantled to allow a visual verification of the leak path(s).Copyright

Ultrasonic phased array sound field mapping through large-bore coarse grained cast austenitic stainless steel (CASS) piping materials

A sound field beam mapping exercise was conducted to further understand the effects of coarse-grained microstructures found in cast austenitic stainless steel (CASS) materials on phased array ultrasonic wave propagation. Laboratory measurements were made on three CASS specimens with different microstructures; the specimens were polished and etched to reveal measurable grain sizes, shapes, and orientations. Three longitudinal, phased array probes were fixed on a specimens outside diameter with the sound field directed toward one end (face) of the pipe segment over a fixed range of angles. A point receiver was raster scanned over the surface of the specimen face generating a sound field image. A slice of CASS material was then removed from the specimen end and the beam mapping exercise repeated. The sound fields acquired were analyzed for spot size, coherency, and beam redirection. Qualitative analyses were conducted between the resulting sound fields and the microstructural characteristics of each specimen.

Ultrasonic Evaluation of Two Dissimilar Metal Weld Overlay Specimens

Two dissimilar metal weld (DMW) pipe-to-nozzle specimens were implanted with thermal fatigue cracks in the 13% to 90% through-wall depth range. The specimens were ultrasonically evaluated with phased-array probes having center frequencies of 0.8, 1.0, 1.5, and 2.0 megahertz (MHz). An Alloy 82/182 weld overlay (WOL) was applied and the specimens were ultrasonically re-evaluated for flaw detection and characterization. The Post-WOL flaw depths were approximately 10% to 56% through-wall. This study has shown the effectiveness of ultrasonic examinations of Alloy 82/182 overlaid DMW specimens. Phased-array probes with center frequency in the 0.8- to 1.0-MHz range provide a strong coherent signal but the greater ultrasonic wavelength and larger beam spot size prevent the reliable detection of small flaws. These small flaws had nominal through-wall depths of less than 15% and length in the 50-60 mm (2-2.4 in.) range. Flaws in the 19% and greater through-wall depth range were readily detected with all four probes. At the higher frequencies, the reflected signals are less coherent but still provide adequate signal for flaw detection and characterization. A single inspection at 2.0 MHz could provide adequate detection and sizing information but a supplemental inspection at 1.0 or 1.5 MHz is recommended.

Using Phased Array Ultrasonic Testing in Lieu of Radiography for Acceptance of Carbon Steel Plate Welds

The Pacific Northwest National Laboratory (PNNL) is conducting studies for the U.S. Nuclear Regulatory Commission (NRC) to assess the capability, effectiveness, and reliability of ultrasonic testing (UT) as a replacement method for radiographic testing (RT) for volumetric examination of nuclear power plant (NPP) components. This particular study focused on evaluating the use of UT on carbon steel plate welds. Welding fabrication flaws included a combination of planar and volumetric types, e.g., incomplete fusion, lack of penetration, cracks, porosity, and slag inclusions. The examinations were conducted using phased-array (PA) UT techniques applied primarily for detection and flaw type characterization. This paper will discuss the results of using UT in lieu of RT for detection and classification of fabrication flaws in carbon steel plate welds.

Phased Array Ultrasonic Sound Field Mapping in Cast Austenitic Stainless Steel

This study maps the phased array-generated acoustic sound fields through three types of CASS microstructure in four specimens to quantitatively assess the beam formation effectiveness in these materials.

Ultrasonic Sound Field Mapping Through Coarse Grained Cast Austenitic Stainless Steel Components

The Pacific Northwest National Laboratory (PNNL) has been involved with nondestructive examination (NDE) of coarse-grained cast austenitic stainless steel (CASS) components for over 30 years. More recent work has focused on mapping the ultrasonic sound fields generated by low-frequency phased array probes that are typically used for the evaluation of CASS materials for flaw detection and characterization. The casting process results in the formation of large grained material microstructures that are nonhomogeneous and anisotropic. The propagation of ultrasonic energy for examination of these materials results in scattering, partitioning and redirection of these sound fields. The work reported here provides an assessment of sound field formation in these materials and provides recommendations on ultrasonic inspection parameters for flaw detection in CASS components.