HXLPE acetabular liners were introduced to reduce wear-related complications in THA. However, post-irradiation thermal free radical stabilization can compromise mechanical properties, leave oxidation-prone residual free radicals, or both. Reports of mechanical failure of HXLPE acetabular liner rims raise concerns about thermal free radical stabilization and in vivo oxidization on implant properties. The purpose of this study is to explore the differences in the mechanical, physical and chemical properties of HXLPE acetabular liner rims after extended time in vivo between liners manufactured with different thermal free radical stabilization techniques. Remelted, single annealed and sequentially annealed retrieved HXLPE acetabular liners with in vivo times greater than 4.5 years were obtained from our implant retrieval laboratory. All retrieved liners underwent an identical sanitation and storage protocol. For mechanical testing, a total of 55 explants and 13 control liners were tested. Explant in vivo time ranged from 4.6 – 14 years and ex vivo time ranged from 0 – 11.6 years. Rim mechanical properties were tested by microindentation hardness testing using a Micromet II Vickers microhardness tester following ASTM standards. A subset of 16 explants with ex vivo time under one year along with five control liners were assessed for oxidation by FTIR, crystallinity by Raman spectroscopy, and evidence of microcracking by SEM. No significant difference in in vivo or ex vivo was found between thermal stabilization groups in either set of explants studied. In the mechanically tested explants, there was no significant correlation between in vivo time and Vickers hardness in any thermal stabilization group. A significant correlation was found between ex vivo time and hardness in remelted liners (r=.520, p = .011), but not in either annealed cohort. ANCOVA with ex vivo time as a covariate found a significant difference in hardness between the thermal free radical stabilization groups (p 0.1) was found in retrieved remelted (25%), single annealed (100%) and sequentially annealed (75%) liner rims. Crystallinity was increased in the subsurface region relative to control liners for both annealed, but not remelted, liner rims. Hardness was increased in oxidized rims for both annealed cohorts but not in the remelted cohort. Microcracking was only found along the surface of one unoxidized remelted liner rim. Mechanical properties were reduced at baseline and worsened after in vivo time for remelted HXLPE liner rims. Rim oxidation was detected in all groups. Oxidation was associated with increased crystallinity and hardness in annealed cohorts, but not remelted liners. Increased crystallinity and oxidation do not appear to be directly causing the worsened mechanical behavior of remelted HXLPE liner rims after extended in vivo time

Introduction. HXLPE acetabular liners were introduced to reduce wear-related complications in THA. However, post-irradiation thermal free radical stabilization can compromise mechanical properties, leave oxidation-prone residual free radicals, or both. Reports of mechanical failure of HXLPE acetabular liner rims raise concerns about thermal free radical stabilization and in vivo oxidization on implant properties. The purpose of this study is to explore the differences in the mechanical, physical and chemical properties of HXLPE acetabular liner rims after extended time in vivo between liners manufactured with different thermal free radical stabilization techniques. Material and Methods. Remelted, single annealed and sequentially annealed retrieved HXLPE acetabular liners with in vivo times greater than 4.5 years were obtained from our implant retrieval laboratory. All retrieved liners underwent an identical sanitation and storage protocol. For mechanical testing, a total of 55 explants and 13 control liners were tested. Explant in vivo time ranged from 4.6 – 14.0 years and ex vivo time ranged from 0 – 11.6 years. Rim mechanical properties were tested by microindentation hardness testing using a Micromet II Vickers microhardness tester following ASTM standards. A subset of 16 explants with ex vivo time under one year along with five control liners were assessed for oxidation by FTIR, crystallinity by Raman spectroscopy, and evidence of microcracking by SEM. Results. No significant difference in in vivo or ex vivo time was found between thermal stabilization groups in either set of explants studied. In the mechanically tested explants, there was no significant correlation between in vivo time and Vickers hardness in any thermal stabilization group. A significant correlation was found between ex vivo time and hardness in remelted liners (r=.520, p=.011), but not in either annealed cohort. ANCOVA with ex vivo time as a covariate found a significant difference in hardness between the thermal free radical stabilization groups (p<.0005, η. 2. = 0.322). Post hoc analysis revealed hardness was significantly lower in the retrieved remelted group compared to both the single annealed (p=.001) and sequentially annealed (p<.0005) cohorts. Hardness was significantly higher in the retrieved remelted liners compared to controls (p=.007), with no different in either annealed cohort. Detectable subsurface oxidation (OI > 0.1) was found in retrieved remelted (25%), single annealed (100%) and sequentially annealed (75%) liner rims. Crystallinity was increased in the subsurface region relative to control liners for both annealed, but not remelted, liner rims. Hardness was increased in oxidized rims for both annealed cohorts but not in the remelted cohort. Microcracking was only found along the surface of one unoxidized remelted liner rim. Conclusion. Mechanical properties were reduced at baseline and worsened after in vivo time for remelted HXLPE liner rims. Rim oxidation was detected in all groups. Oxidation was associated with increased crystallinity and hardness in annealed cohorts, but not remelted liners. Increased crystallinity and oxidation do not appear to be directly causing the worsened mechanical behavior of remelted HXLPE liner rims after extended in vivo time. For any figures or tables, please contact authors directly

Introduction. HXLPE acetabular liners were introduced to reduce wear-related complications in THA. However, post-irradiation thermal free radical stabilization can compromise mechanical properties, leave oxidation-prone residual free radicals, or both. Reports of mechanical failure of HXLPE acetabular liner rims raise concerns about thermal free radical stabilization and in vivo oxidization on implant properties. The purpose of this study is to explore the differences in the mechanical, physical and chemical properties of HXLPE acetabular liner rims after extended time in vivo between liners manufactured with different thermal free radical stabilization techniques. Material and methods. Remelted, single annealed and sequentially annealed retrieved HXLPE acetabular liners with in vivo times greater than 4.5 years were obtained from our implant retrieval laboratory. All retrieved liners underwent an identical sanitation and storage protocol. For mechanical testing, a total of 55 explants and 13 control liners were tested. Explant in vivo time ranged from 4.6 – 14.0 years and ex vivo time ranged from 0 – 11.6 years. Rim mechanical properties were tested by microindentation hardness testing using a Micromet II Vickers microhardness tester following ASTM standards. A subset of 16 explants with ex vivo time under one year along with five control liners were assessed for oxidation by FTIR, crystallinity by Raman spectroscopy, and evidence of microcracking by SEM. Results. No significant difference in in vivo or ex vivo was found between thermal stabilization groups in either set of explants studied. In the mechanically tested explants, there was no significant correlation between in vivo time and Vickers hardness in any thermal stabilization group. A significant correlation was found between ex vivo time and hardness in remelted liners (Δ=.520, p=.011), but not in either annealed cohort. ANCOVA with ex vivo time as a covariate found a significant difference in hardness between the thermal free radical stabilization groups (p<.0005, η. 2. = 0.322). Post hoc analysis revealed hardness was significantly lower in the retrieved remelted group compared to both the single annealed (p=.001) and sequentially annealed (p<.0005) cohorts. Hardness was significantly higher in the retrieved remelted liners compared to controls (p=.007), with no different in either annealed cohort (figure 1). Detectable subsurface oxidation (OI > 0.1) was found in retrieved remelted (25%), single annealed (100%) and sequentially annealed (75%) liner rims (figure 2). Crystallinity was increased in the subsurface region relative to control liners for both annealed, but not remelted, liner rims. Hardness was increased in oxidized rims for both annealed cohorts but not in the remelted cohort. Microcracking was only found along the surface of one unoxidized remelted liner rim. Conclusion. Mechanical properties were reduced at baseline and worsened after in vivo time for remelted HXLPE liner rims. Rim oxidation was detected in all groups. Oxidation was associated with increased crystallinity and hardness in annealed cohorts, but not remelted liners. Increased crystallinity and oxidation do not appear to be directly causing the worsened mechanical behavior of remelted HXLPE liner rims after extended in vivo time. For any tables or figures, please contact the authors directly

With information about a patient's bone mechanical properties orthopaedic operations could be optimised to reduce intra- and post-operative complications. However, there is currently no reliable method of measuring a patient's bone mechanical properties in vivo. We have previously investigated microindentation, using a 1.5mm diameter spherical indenter tip, and found no correlation between these measurements and compression testing measurements. We hypothesised that by using a larger diameter indenter tip we would closer match bone millimetre-scale mechanical properties. 20 bone samples were taken from 20 patients undergoing hip replacement surgery. The samples were machined from the femoral neck calcar cortical bone into 6×3×3mm parallelepiped specimens, aligned with the osteons along the long axis. The samples were micro-computed tomography (CT) scanned to calculate porosity. Microindentation was performed using a 6mm diameter, sapphire, spherical indenter tip. 12 indentations were performed in a grid and the reduced moduli were calculated using the Oliver-Pharr method. Compression testing was then performed to failure and the apparent elastic modulus was calculated for each sample. A moderate correlation was found between the indentation reduced moduli and compression testing elastic moduli (r=0.52, r2=0.275, p=0.018). In addition, a moderate correlation was found between the indentation reduced moduli and CT-measured porosity (r=0.5, r2=0.251, p=0.025) and a strong correlation was found between compression testing moduli and porosity (r=0.75, r2=0.568, p<0.001). Using large-tip spherical microindentation, indentation reduced moduli correlated significantly with compression testing apparent elastic moduli in these 20 cortical bone specimens. Microindentation using a large, spherical indenter tip may predict the mechanical properties of bone at the millimetre length scale and shows promise as a potential future clinical decision aid in surgery

Objectives

Advanced glycation end-products (AGEs) are a post-translational modification of collagen that form spontaneously in the skeletal matrix due to the presence of reducing sugars, such as glucose. The accumulation of AGEs leads to collagen cross-linking, which adversely affects bone quality and has been shown to play a major role in fracture risk. Thus, intervening in the formation and accumulation of AGEs may be a viable means of protecting bone quality.

Objectives. Microindentation has the potential to measure the stiffness of an individual patient’s bone. Bone stiffness plays a crucial role in the press-fit stability of orthopaedic implants. Arming surgeons with accurate bone stiffness information may reduce surgical complications including periprosthetic fractures. The question addressed with this systematic review is whether microindentation can accurately measure cortical bone stiffness. Methods. A systematic review of all English language articles using a keyword search was undertaken using Medline, Embase, PubMed, Scopus and Cochrane databases. Studies that only used nanoindentation, cancellous bone or animal tissue were excluded. Results. A total of 1094 abstracts were retrieved and 32 papers were included in the analysis, 20 of which used reference point indentation, and 12 of which used traditional depth-sensing indentation. There are several factors that must be considered when using microindentation, such as tip size, depth and method of analysis. Only two studies validated microindentation against traditional mechanical testing techniques. Both studies used reference point indentation (RPI), with one showing that RPI parameters correlate well with mechanical testing, but the other suggested that they do not. Conclusion. Microindentation has been used in various studies to assess bone stiffness, but only two studies with conflicting results compared microindentation with traditional mechanical testing techniques. Further research, including more studies comparing microindentation with other mechanical testing methods, is needed before microindentation can be used reliably to calculate cortical bone stiffness. Cite this article: M. Arnold, S. Zhao, S. Ma, F. Giuliani, U. Hansen, J. P. Cobb, R. L. Abel, O. Boughton. Microindentation – a tool for measuring cortical bone stiffness? A systematic review. Bone Joint Res 2017;6:542–549. DOI: 10.1302/2046-3758.69.BJR-2016-0317.R2

Introduction. The increase in revision joint replacement surgery and fractures of bone around orthopaedic implants may be partly addressed by keeping bone healthy around orthopaedic implants by inserting implants with mechanical properties closer to the patient's bone properties. We do not currently have an accurate way of calculating a patient's bone mechanical properties. We therefore posed a simple question: can data derived from a micro-indenter be used to calculate bone stiffness?. Methods. We received ethical approval to retrieve femoral heads and necks from patients undergoing hip replacement surgery for research. Cortical bone from the medial calcar region of the femoral neck was cut into 3×3×6mm cuboid specimens using a diamond wafering blade. Micro-indentation testing was performed in the direction of loading of the bone using a MicroMaterials (MicroMaterials, UK) indenter, using the high load micro-indentation stage (see Figure 1). To simulate in vivo testing, the samples were kept hydrated and were not fixed or polished. From the unloading curve after indentation, the elastic modulus was calculated, using the Oliver-Pharr method using the indentation machine software. To assess which microindentation machine settings most precisely calculate the elastic modulus we varied the loading and unloading rates, load and indenter tip shape (diamond Berkovich tip, 1mm diameter Zirconia spherical tip and 1.5mm diameter ruby spherical tip). Following this, for 11 patients' bone, we performed compression testing of the same samples after they were indented with the 1.5mm diameter ruby spherical tip to assess if there was a correlation between indentation values of apparent elastic modulus and apparent modulus values calculated by compression testing (see Figure 2). Platens compression testing was performed using an Instron 5565 (Instron, USA) materials testing machine. Bluehill compliance correction software (Instron, USA) was used to correct for machine compliance. The strain rate was set at 0.03mm/s. The apparent elastic modulus was calculated from the slope of the elastic region of the stress-strain graph. The correlation between values of apparent modulus from compression testing and indentation were analyzed using IBM SPSS Statistics 22. Results. The most precise results were obtained using a spherical indenter tip (1.5 mm diameter ruby ball), rather than a sharp Berkovich tip, high load (10N), a loading rate of 100 mN/s and unloading rate of 300 mN/s with a pause of 60 seconds at maximum load. We also used multiple load cycles with a peak load of 10N (see Figure 3). Using these optimal settings we calculated the mean elastic modulus over 10 cycles of testing with six indents on one sample to be 11.8 GPa (+/− 1.01). There was a moderate correlation between indentation and compression values of apparent modulus (r=0.62, n=11, p=0.04). Discussion. By using a spherical indenter tip and fast unloading it was possible to get precise apparent modulus values. The apparent modulus derived from micro-indentation, correlated moderately with that derived from direct compression testing. This early data suggests that microindentation may become a clinically relevant test of bone quality in real time

The increase in revision joint replacement surgery and fractures of bone around orthopaedic implants may be partly addressed by keeping bone healthy around orthopaedic implants by inserting implants with mechanical properties closer to the patient's bone properties. We do not currently have an accurate way of calculating a patient's bone mechanical properties. We are therefore investigating whether microindentation can accurately calculate bone stiffness. We received ethical approval to retrieve femoral heads and necks from patients undergoing hip replacement surgery for research. Cortical bone from the medial calcar region of the femoral neck was cut into 3×3×6mm cuboid specimens. Micro-indentation testing was performed in the direction of loading of the bone using a MicroMaterials indenter. The samples were kept hydrated and were not fixed or polished. From the unloading curve after indentation, the elastic modulus was calculated, using the Oliver- Pharr method. To assess which microindentation machine settings most precisely calculate the elastic modulus we varied the loading and unloading rates, load and indenter tip shape. The most precise results were obtained by using a spherical indenter tip (rather than Berkovich tip), high load (10N), a loading rate of 100 mN/s and unloading rate of 300 mN/s with a pause of 60 seconds at maximum load and multiple load cycles with constant loads. Using these settings the mean elastic modulus over 12 cycles of testing was 13.0 GPa (+/- 2.47). By using a spherical indenter tip and fast unloading it was possible to get precise apparent modulus values. By unloading as fast as possible the effects of bone viscoelastic properties are minimised. By using a spherical indenter tip, plastic deformation at the tip is minimised (compared to the Berkovich tip). We are performing further standard compression tests on the samples to verify the accuracy of the indentation tests

Bone microhardness has been successfully correlated with important functional parameters such as mineralisation and stiffness. It provides a means of examining the mechanical competence of bone at a micron scale, averaging the effect of osteonal lamellae but sensitive to variation in mineral content within a bone, and, with careful selection of indentation site, able to obtain material characteristics separate from any effects of porosity. However, the effect of bone’s viscoelasticity on such measurements has been largely ignored. This preliminary study investigates the post-indentation size change of Vickers indentations on wet bone. 4 axial slices of bovine femur were harvested from the same shaft, and polished. Each sample was subjected to 4 sets of 10 Vickers indentations with a load of 50 g and holding period of 15 s. The indentation size was measured immediately after the load was removed, and then again at intervals for a period up to 24 hours after the indentation was made. To avoid dehydration, the bone stood in water during the indentation testing and during measurement, and between each measurement period it was fully immersed in water. Measured hardness significantly decreased with time, by approximately 30% in total. The rate of post-indentation recovery is difficult to analyse since the driving force of residual strain decreases as recovery takes place. However a simple exponential fit to the variation of HV with time in the form of H = H(final).(1−exp(−kt)) + H(initial) suggests that the size of the indentation tends towards a constant size between 5 and 24 hours after indentation. Thus we conclude that care should be taken when making “early” measurements given the rapid rate of change in indentation size. Caution should also be employed when interpreting such data.