Gamma radiation used for sterilization of medical devices is challenged by cobalt-60 supply and commercial capacity. To maintain a robust radiation sterilization marketplace for the rapidly growing single-use medical device industry, investigation of potential alternatives to gamma technology, such as electron beam (e-beam) and X-ray technology, is critical. In this work, we directly compare the effects of radiation source and absorbed dose level on the polymeric materials and function of a commercial pulsed lavage device used for wound care. Product functionality, polymer mechanical, and polymer optical properties were evaluated using standard methods and input from the device manufacturer. Test results show that functionality of the product was not inhibited by radiation although the battery in the device exposed to X-ray exhibited greater voltage loss compared to batteries in products exposed to gamma or e-beam. Statistically significant differences between gamma and e-beam exposure and between gamma and X-ray exposure were also observed for product appearance in terms of yellowness index of several of the polymers considered. Overall, the results of this study support the viability of e-beam and X-ray radiation technologies as alternatives to cobalt-60 gamma technology for sterilization of the single-use pulsed lavage medical device investigated.

A new technique, termed the stirred-reactor coupon analysis (SRCA) method, has been developed to measure the rate of glass dissolution in forward-rate conditions. Monolithic glass coupons are partially masked with an inert material before placement in a large volume of well-mixed solution with known chemistry and temperature for a predetermined duration. After the test, the mask is removed, and the difference in step height between the protected area and the exposed corroded portions of the sample coupon is measured to determine the extent of glass dissolution. The step height is converted to a rate measurement using the test duration and glass density. Test parameters such as sample surface preparation and test duration were evaluated to determine their effects on the measured rates. Additionally, results from an interlaboratory study (ILS) consisting of 12 laboratories from 11 different institutions are presented, where each laboratory performed 12 independent tests. When removing experimental outlier data, the 95% reproducibility limits for the SRCA method has no statistical difference with previously published standardized test methods used to determine the forward rate of glass dissolution. Overall, this paper describes steps necessary to perform the test method and provides the statistical calculations to evaluate test accuracy.

The medical device industry has been investigating ways to increase the use of alternatives to cobalt-60 gamma radiation and ethylene-oxide gas sterilization, such as electron beam (E-beam) and X-ray radiation, due to regulatory and market pressures. One impediment to switching to E-beam or X-ray technology for sterilization is the lack of data on the effects of these radiation sources on medical device polymers. To provide such data this work considers irradiation and testing of a common single-use medical bone cement mixing system, the Stryker Advanced Cement Mixer (ACM (R)), that is composed of seven polymer materials. The ACM (R) devices considered here were processed to sterilization-relevant doses (15, 25, 50, and 70 kGy) using three radiation technologies: gamma, E-beam, and X-ray. The system and its polymer components were tested for product functionality, as well as mechanical and visual properties to determine how exposure effects may be influenced by radiation technology and dose level. We found that although there were instances of statistically significant differences in effects between the gamma-irradiated products and those irradiated with E-beam and X-ray, those effects were negligible in terms of retained functionality of the product and retained mechanical properties of the polymer components. Overall, results of this study demonstrate that, for of the effects studied, E-beam and X-ray are viable alternatives to cobalt-60 gamma radiation for sterilization of the polymer-based device investigated.

Nuclear grade high-efficiency particulate air (HEPA) filter service life is generally limited to 10 years from the date of manufacture at Department of Energy facilities. Filter life extension offers a substantial cost savings and decreased facility downtime. This study compared tensile strength results between unused new and unused aged filters (7, 10, and 13 years old) to discern age related differences. Unused HEPA filters were disassembled. The filter sheets were preconditioned in a controlled environment for 24 h to resolve any atmospheric history of the filter media and to remove any effects of hysteresis on the results. Media used in HEPA filters are fragile, and damage occurs outside of the sample area when the material is cut. Basis weight measurements were recorded. Machine direction (MD) and cross direction (CD) tensile strength specimens were taken from the top or bottom of each filter pleat. Tensile strength specimens were also obtained of the pleat fold in the machine direction. Burst strength specimens were taken from across each filter pleat from top to bottom. Analysis of the raw data suggests that differences in tensile strength between new and aged HEPA filters are not significant. These results complement previous studies that have evaluated the relationships between the postulated 10-year HEPA filter lifespan, other performance indicators, and assessed cohort of aged filters as a function of normal operations. Those results along with the tensile strength results reported here suggest that HEPA filters, when properly maintained, can reasonably operate safely and efficiently for extended periods beyond 10 years when managed with well-defined performance and operational requirements.

The low-activity waste (LAW) fraction of Hanford tank waste will be converted to glass at the Waste Treatment and Immobilization Plant (WTP) and disposed on the Hanford site. The chemical durability of LAW glasses has been researched for decades to satisfy contract requirements. Most LAW glass durability data has been generated on non-radioactive simulant glasses fabricated via crucible melts. These non-radioactive glasses were chosen due to safety and cost reasons with confidence that radioactive waste glasses would exhibit similar behavior. To reduce the risk of significant differences in laboratory test response data between WTP melter waste glass and simulant glass, Product Consistency Tests (PCT, i.e., ASTM C1285-21) and Environmental Protection Agency (EPA) 1313 durability tests were performed on actual and simulant LAW glasses fabricated using laboratory-scaled melters. Actual and simulant glass durability test results are presented and statistically compared. Differences in test responses were found to be within experimental uncertainty.

Many polymer-based medical devices are sterilized by gamma irradiation. To reduce the use of cobalt-60 gamma-ray sources, transition from gamma ray to alternative irradiation technologies was proposed, namely electron beam (e-beam) and X-ray. A major impediment for such a transition is the knowledge gap in material compatibility with the different radiation sources. In this study, multi-layer films consisting of ethylene vinyl acetate (EVA) and ethylene vinyl alcohol (EVOH) components were irradiated to target doses of 30, 45, and 60 kGy by gamma-ray, e-beam, and X-ray sources. Effects of irradiation were evaluated on 12 material properties, and statistical comparisons between gamma irradiation and alternative technologies were conducted using the two one-sided t-test (or “equivalence test”) and classic t-test. Melting temperature and UV absorbance below 300 nm showed dose dependencies, while other investigated properties such as discoloration and mechanical durability did not change with dose up to 60 kGy. Based on these results, there is no material compatibility issue associated with the transition from gamma to e-beam or to X-ray as source of sterilization radiation of the studied multi-layer film.

Due to market and regulatory pressures, many healthcare manufacturers are considering alternatives to cobalt-60 gamma radiation, including accelerator-based electron beam (E-beam) and X-ray radiation for product sterilization. In this work, the effects of irradiation on a representative medical product, comprised of eight distinct polymer materials, were directly compared for three radiation technologies - cobalt-60 gamma, E-beam, and Xray - at four dose levels (15, 25, 50, and 70 kGy). The objective was to determine how radiation effects (deleterious or beneficial) are influenced by source and dose level, with the specific goal of determining whether E-beam radiation and/or X-ray radiation could be viable alternatives to gamma radiation for device sterilization. The specific product considered is a single-use medical device for orthopedic surgery, the Stryker Instruments MixeVac III bone cement mixer, which is currently sterilized using gamma radiation from cobalt-60 sources. Following ASTM International standards and input from the manufacturer, we characterized the effects of the three radiation sources on product functionality as well as on the mechanical and optical properties of the constituent polymers. Results indicate that although measurable differences in properties between the standard gamma irradiated materials and the alternative E-beam and X-ray irradiated materials were observed, those differences were small. Statistically significant differences were noted in the case of yellowness index for polyvinyl chloride, high-density polyethylene, and polycarbonate, and in the case of tensile elongation at break for high impact polystyrene and polyvinyl chloride. In general, the results of this study support the viability of Ebeam and X-ray radiation as alternative options to cobalt-60 gamma radiation for sterilization of Stryker singleuse universal bone cement mixer medical devices.

Abstract Many polymer-based medical devices are sterilized by gamma irradiation. To reduce the use of cobalt-60 gamma-ray sources, transition from gamma ray to alternative irradiation technologies was proposed, namely electron beam (e-beam) and X-ray. A major impediment for such a transition is the knowledge gap in material compatibility with the different radiation sources. In this study, multi-layer films consisting of ethylene vinyl acetate (EVA) and ethylene vinyl alcohol (EVOH) components were irradiated to target doses of 30, 45, and 60 kGy by gamma-ray, e-beam, and X-ray sources. Effects of irradiation were evaluated on 12 material properties, and statistical comparisons between gamma irradiation and alternative technologies were conducted using the two one-sided t-test (or “equivalence test”) and classic t-test. Melting temperature and UV absorbance below 300 nm showed dose dependencies, while other investigated properties such as discoloration and mechanical durability did not change with dose up to 60 kGy. Based on these results, there is no material compatibility issue associated with the transition from gamma to e-beam or to X-ray as source of sterilization radiation of the studied multi-layer film.

This study developed a model for predicting viscosity of alkali-alumino-borosilicate glass melts as functions of composition and temperature. The model is based on a total of 3935 viscosity-temperature data from 574 glasses with viscosity values ranging from 2.53 to 7260 Poise (P) in the temperature range of 900-1260 degrees C. Several different model forms were surveyed, including those based on Arrhenius, Vogel-Fulcher-Tammann, Avramov-Milchev, and Mauro-Yue-Ellison-Gupta-Allen. For each of these models, combinations of the temperature-independent parameters were fitted to composition. It was found that generally fitting more than one temperature-independent parameter as functions of composition resulted in overfitting. The Avramov-Milchev-based model was found to best represent the Hanford low-activity waste glass melt viscosity data based on model fit and validation statistics. A 21-term partial quadratic mixture model was recommended for use. This model predicts melt viscosity with a root-mean square error of .1736 ln(P), which is similar to the error in viscosity measurements from replicate glass analyses of .1383 ln(P). Viscosity was found to be most increased by SiO2 > Al2O3 > ZrO2 > SnO2 and most decreased by Li2O > Na2O > B2O3 > CaO > K2O > MgO, at temperatures from 900 to 1260 degrees C.

Abstract High-efficiency particulate air (HEPA) filters are widely employed by nuclear facilities to remove radiological particulate matter from their effluent exhaust streams. The purpose of this study is to evaluate the relationships between the 10-y HEPA filter lifetime deployment and its other performance indicators. This 10-y-long endeavor to collect and analyze data regarding the service life of HEPA filters at the Pacific Northwest National Laboratory began in 2010. A set of HEPA filters was selected, and the filters have been surveyed and analyzed at least annually to verify compliance with permit conditions. The study suggests the frequency of filter replacement should be based on the actual operational requirements, such as fume hood face velocity and/or efficiency test results, instead of on the prescribed filter “age limit” of 10 y from the date of manufacture (e.g., birth date) when operating under dry conditions. The study has now been completed, and over the past decade, all the HEPA filters have been replaced due to either technical issues as listed in this report or the previously recommended filter “age limit” of 10 y as prescribed by the oversight bodies. Experimentally determined failure rates are also determined from the data set and can be used to estimate the chances of HEPA filters surviving 15, 20, or even 30 y.

The objective of this task was to determine the precision of the SRCA technique when used to determine the dilute condition corrosion rate. To this end, an interlaboratory round robin study was conducted per the instructions in ASTM Practice E691 to measure the precision with which the SRCA test method can be conducted. Twelve independent labs from eleven different institutions each evaluated four glass compositions in three different conditions. The ASTM procedures recommend at least 6 labs participate in a round robin testing the same 3 materials in the same conditions to determine precision. In this case, 12 labs each performed 12 independent tests. This was only possible thanks to the multi-glass testing capability of the SRCA test. A total of 108 duplicate pairs were used to calculate the repeatability of the tests, with the same glass tested in the same vessel, producing as identical conditions as possible for the replicates. These test results were quite tightly clustered, with a median difference from the average value of the pair of only 2.9%. Based on the calculations outlined in ASTM E177-20 and a measured standard deviation of 4.74%, the intralaboratory repeatability limit (r) was calculated to be within 13.3% of the expected value with 95% confidence level. The reproducibility limit (R) of the test was examined using all 277 data points from the round robin. Because of the differences in dissolution rates due to pH variability and intrinsically for the 12 conditions tested, the reproducibility limits for each condition and overall were calculated from the percent relative residual value for each test. The SRCA test is expected to be reproducible within 64% of the expected value with a 95% confidence level.

This report presents the results of testing two rods after heat treatment at 400C for 8 hours and compares to the results from FY 2021 of similar rods that were tested as baseline. The heat treatment resulted in a decrease in yield stress.

o} stab flank. The round thread had a 0{sup o} load flank and 20{sup o} stab flank. Most of the testing was performed on the round thread form. Both a coupled connection design and an integral connection design were tested. The coupling was a pin by pin (male) thread, with the pipe having a box (female) thread. Both designs have outside and inside diameters that are flush with the pipe body. Both designs also contain a small external shoulder. The test procedure selected for this evaluation was the newly written ISO 13679 procedure for full scale testing of casing and tubing connections. The ISO procedure requires a variety of tests that includes makeup/breakout testing, internal gas sealability/external water sealability testing with axial tension, axial compression, bending, internal gas thermal cycle tests and limit load (failure) tests. This test was performed with four coupled samples and included most of these loads. Two integral samples were also included for limit load testing ISO makeup/breakout tests are divided into three types--initial makeup, IML1, repeated makeup within the same sample, MBL, and repeated makeup using several samples called round robin, RR. IMU and MBL were performed in this project. The ISO sealing and structural procedure is divided into four primary tests and identified as Series A, B, C and Limit Load (failure). Series A and B test to 95% actual yield of the pipe and Series C uses 90% of actual yield. Samples 1 and 3 were tested to Series A and the loads are shown in Figure 1. For these samples, the axial compression was limited to 75% pipe body yield, which was set by Mr. Watts at the beginning of the test. Samples 2 and 4 were tested to Series B with loads shown in Figure 2. This series included 20 degrees per 100 feet bending but no external pressure. Due to premature leaks, no samples were subjected to Series C which included mechanical and thermal cycles. Samples 5 and 6 were tested to failure. The project started with the selection and purchase of a popular size of oilfield pipe, which was 7-inch OD, 32 pound per foot, P-110 casing. While the connections were being threaded, material tensile tests were performed to get the actual strength of the 7-inch pipe. The first samples contained a square thread form. Excessive galling was experienced during the first series of makeup/breakout tests and Mr. Watts decided to change the thread form and remachine the samples. The second samples had a round thread form and performed very well in the makeup/breakout tests. Basically no galling occurred of any consequence. Samples 1 and 3 were to be tested with external water (ISO Series A) while samples 2 and 4 were to be tested with bending (ISO Series B, no external pressure). Testing of all four samples started with tension and internal gas pressure. During this initial pressure testing, samples 1, 3 and 4 developed leaks and the test was stopped before any external pressure or bending was applied. Sample 2 successfully tested to ISO Load Point 5 which included bending before developing a leak. Figure 3 shows the loads at which the samples leaked and the relative pipe body performance capability. Sample 1 and end A of sample 2 held a high pressure while samples 3, 4 and end B of sample 2 leaked at relatively low pressures. All of these leaks were with nitrogen gas pressure. After reviewing the results, it was believed that several conditions may have contributed to the premature leaks: The BOL 2000 thread lubricant contains solid particles that are larger than the solid particles in API 5A2 compound. Possibly the large particles prevented tight thread contact necessary for gas leak tightness. The BOL 2000 lubricant may have caused or at least contributed to the yielding of the pin end during makeup. Pin inward deformation was found in some pins subsequent to testing and breakout. Excessive yielding of the pin or box will contribute to poor thread contact and leakage. The connections were made up to full or near full shoulder contact. This causes the end of the pin to be stressed near the yield strength. This along with the interference caused by the thread compound may cause excessive pin hoop stresses and yielding which in turn gives relatively loose thread contact. This behavior is present when repeated makeup and breakout occurs.

Resuscitation and detection of stressed total coliforms in chlorinated water samples is needed to assess and prevent health effects from adverse exposure. In this study, we report that the addition of a growth enhancer mix consisting of trehalose, sodium pyruvate, magnesium chloride, and 1× trace mineral supplement improved growth of microorganisms from chlorinated secondary effluent in the base medium with Colilert-18. Improving growth of chlorine stressed microorganisms from secondary effluent is crucial to decreased detection time from 18 to 8 h.

In 2020, PNNL completed a literature search for high-efficiency particulate air (HEPA) filter age information. HEPA filters are used in many operations to remove particulate matter from effluent exhaust streams. They are thought to degrade over time both during proper storage and during normal operational service; however, the rate at which the filters degrade remains unknown. This brings into question if age is an adequate indicator of HEPA filter performance. Data from six previous reports were obtained from the literature search and combined to create a data set of 1600 operating filters. Filter usage was identified from multiple facilities. The various types of filters (e.g., axial flow, self-contained, and standard 61 x 61 x 28 cm; and both separator and separatorless) reported were constructed to the requirements Section FC (HEPA Filters) or Section FK (Special HEPA Filters) of the American Society of Mechanical Engineers AG-1 code. Filters were presumed to have continuously met the operational criteria and in particular passed both annual efficiency tests and annual differential pressure measurements. The environmental conditions within the exhaust system were also assumed adequate for long-term filter operation. The data, by the nature of the reports, excludes rejected filters from quality assurance evaluations, intake, or installation testing. The collective data set shows over half of were operating past the recommended 10-year Department of Energy (DOE) lifetime. Data was evaluated for age lifetime using a linear trendline, survival function, probability functions, and failure rate; financial impacts were also addressed. This report supports the notion that HEPA filters can operate safely and efficiently under proper maintenance well past the 10-year lifetime established by DOE. Using the results of the four age evaluation approaches, they collectively point to the reasonableness of an operating HEPA filter lifetime of 20 years. The results are not necessarily definitive, but nevertheless, they are promising. The analysis provides reasonable assurance that when implemented using a graded approach with well-defined performance and operational requirements, extending the service life for HEPA filters beyond 10 years is low risk.

In 2020, PNNL completed a literature search for high-efficiency particulate air (HEPA) filter age information. HEPA filters are used in many operations to remove particulate matter from effluent exhaust streams. They are thought to degrade over time both during proper storage and during normal operational service; however, the rate at which the filters degrade remains unknown. This brings into question if age is an adequate indicator of HEPA filter performance. Data from six previous reports were obtained from the literature search and combined to create a data set of 1600 operating filters. Filter usage was identified from multiple facilities. The various types of filters (e.g., axial flow, self-contained, and standard 24 x 24 x 11.5 inches; and both separator and separatorless) reported were constructed to the requirements Section FC (HEPA Filters) or Section FK (Special HEPA Filters) of the American Society of Mechanical Engineers AG-1 code. Filters were presumed to have continuously met the operational criteria and in particular passed both annual efficiency tests and annual DP measurements. The environmental conditions within the exhaust system were also assumed adequate for long-term filter operation. The data, by the nature of the reports, excludes rejected filters from quality assurance evaluations, intake, or installation testing. The collective data set shows over half of were operating past the current 10-year Department of Energy (DOE) limit. Data was evaluated for age lifetime using a linear trendline, survival function, probability functions, and failure rate; financial impacts were also addressed. This report supports the notion that HEPA filters can operate safely and efficiently under proper maintenance well past the 10-year lifetime established by DOE. Using the results of the four age evaluation approaches, they collectively point to the reasonableness of an operating HEPA filter lifetime of 20 years. The results are not necessarily definitive, but nevertheless, they are promising. The analysis provides reasonable assurance that when implemented using a graded approach with well-defined performance and operational requirements, extending the service life for HEPA filters beyond 10 years is low risk.

The dissolution rate of some glasses accelerates after prolonged time spent at a slow, residual dissolution rate. This phenomenon is referred to as Stage III behavior. The acceleration in glass dissolution rate linked to Stage III behavior is significant and may be the most impactful behavior to long-term performance of glass in a repository. This work is aimed at understanding the effect of glass composition on Stage III behavior to add a level of technical defensibility to glass disposal. To this end, a set of 24 glass compositions were statistically designed, where eight glass components (SiO2, B2O3, Al2O3, CaO, Na2O, SnO2, ZrO2, and Others) have been independently varied in order to study the individual effects of each glass component. These glasses have been subjected to static dissolution tests at 90 degrees C in deionized water and then seeded with zeolite Na-P2 28 days into the testing to induce Stage III behavior. The response of the glasses to the zeolite seeds fell into four primary types: (1) no response to seeds; (2) an immediate linear sustained acceleration in the rate; (3) an immediate linear acceleration in the rate followed by a decrease; and (4) a progressive acceleration in the rate that is concurrent with the addition of the seeds. The main glass components observed to influence these behaviors were CaO, Al2O3, B2O3, and ZrO2, where (1) CaO influenced which glasses showed a Stage III response to seeds (high CaO: types 2, 3, and 4) or did not respond to seeds (low CaO: type 1), (2) Al2O3 and B2O3 influenced which glasses showed a sustainable Stage III response (high Al2O3: types 2 and 4) versus transitory response (low Al2O3 and high B2O3: type 3), and (3) ZrO2 concentration influenced whether glasses showed a linear (high ZrO2: type 2) versus progressive (low ZrO2: type 4) response to seeds.