Shrinkage behaviour of semi-crystalline polymers in laser sintering: PEKK and PA12

This is the author accepted manuscript. The final version is available from Elsevier via the DOI in this recordShrinkage is extensively mentioned in the literature as one of the main causes for dimensional instability or poor performance in Laser Sintering (LS). This study proposes and examines a methodology to describe shrinkage in cooling from a material perspective. Thermal behaviour and crystallisation effects were measured to determine the influence of powder structure and density on overall LS shrinkage. PEKK and PA12 powders were used to assess such behaviour in LS. The shrinkage parameter associated with powder bulk properties has the greatest impact in PEKK, contributing to 57% of the total shrinkage observed in cooling for this material as supported by the low values of bulk density, irregular morphology and internal porosity observed for these particles. For PA12, crystallisation is responsible for 60% of the overall shrinkage observed. In LS, PEKK shows an overall shrinkage approximately 30% lower than PA12, which makes it a promising material for maintaining final part dimensions.Arkema Innovations Chemistr

Methods for evaluating particle coalescence and their implications in laser sintering

This is the author accepted manuscript. The final version is available from Elsevier via the DOI in this recordAn experimental study on the melt and coalescence of different Poly(aryl ether ketones) (PAEK) powders was carried out. The study consisted of evaluating individual particles and neck growth using a hot stage platform. Three different methods of assessing particles dimensions were evaluated, and the coalescence was compared for the grades on three different substrates: glass, glass coated silicone and amorphous PEKK films, the last substrate with the intent to relate with the laser sintering process. It was found that all individual particles shrink prior to melting, achieving up to 30% reduction in perimeter at temperatures just above melting. This shrinkage is followed by an increase in size, mostly driven by viscous flow. Shrinkage is expected to affect neck growth by delaying coalescence, as particles are pulled away whilst neck increases. This is a plausible explanation for why neck growth occurs at a lower rate than predicted by most coalescence models. The use of different substrates does not seem to affect particle coalescence or change in dimension. Viscosity and particle size influence overall particle behaviour and melt, whilst morphology and porosity do not have a great impact in particles coalescence.The authors would like to acknowledge the financial support of Arkema Innovations Chemistry for this study

A route to improving elongation of high-temperature laser sintered PEKK

This is the author accepted manuscript. The final version is available from Elsevier via the DOI in this recordData availability: The dataset generated during the current study is not publicly available due to confidentiality reasons but can be made available on reasonable request with the approval of all authors.Laser sintering (LS) is one of the most popular additive manufacturing (AM) techniques as it produces parts of complex geometry with high dimensional accuracy and good mechanical strength. However, the nature of the LS process often leads to brittle behavior characterized by a low elongation at break if compared to conventional polymer processing techniques, e.g., injection molding (IM). For poly(ether ketone ketone) (PEKK), such elongation is currently below 3%. This study determines and then optimizes the relationship between cooling time and crystallization of PEKK during LS and the resulting elongation at break. The elongation at break of PEKK was successfully improved by using shorter cooling times. The combination of the slow crystallization kinetics of PEKK and a short cooling time of 1 h increased elongation at break to 14%; this is a striking result never achieved for PAEKs in LS before. A calibration curve was developed that can be used to correlate PEKK structure and mechanical properties to cooling conditions according to the application. This methodology can also be applied to select and optimize the mechanical properties of other LS polymers sharing similar kinetics of crystallization and processing temperatures. This work suggests a great potential for a wide range of “post-processing” heat treatments to be used in AM to tailor the ultimate mechanical properties.Arkema Innovations Chemistr

Micro-computed tomography of pulmonary fibrosis in mice induced by adenoviral gene transfer of biologically active transforming growth factor-β1

<p>Abstract</p> <p>Background</p> <p>Micro-computed tomography (micro-CT) is a novel tool for monitoring acute and chronic disease states in small laboratory animals. Its value for assessing progressive lung fibrosis in mice has not been reported so far. Here we examined the importance of in vivo micro-CT as non-invasive tool to assess progression of pulmonary fibrosis in mice over time.</p> <p>Methods</p> <p>Pulmonary fibrosis was induced in mice by intratracheal delivery of an adenoviral gene vector encoding biologically active TGF-ß1 (AdTGF-ß1). Respiratory gated and ungated micro-CT scans were performed at 1, 2, 3, and 4 weeks post pulmonary adenoviral gene or control vector delivery, and were then correlated with respective histopathology-based Ashcroft scoring of pulmonary fibrosis in mice. Visual assessment of image quality and consolidation was performed by 3 observers and a semi-automated quantification algorithm was applied to quantify aerated pulmonary volume as an inverse surrogate marker for pulmonary fibrosis.</p> <p>Results</p> <p>We found a significant correlation between classical Ashcroft scoring and micro-CT assessment using both visual assessment and the semi-automated quantification algorithm. Pulmonary fibrosis could be clearly detected in micro-CT, image quality values were higher for respiratory gated exams, although differences were not significant. For assessment of fibrosis no significant difference between respiratory gated and ungated exams was observed.</p> <p>Conclusions</p> <p>Together, we show that micro-CT is a powerful tool to assess pulmonary fibrosis in mice, using both visual assessment and semi-automated quantification algorithms. These data may be important in view of pre-clinical pharmacologic interventions for the treatment of lung fibrosis in small laboratory animals.</p

Human papillomavirus infection in women with and without cervical cancer in Karachi, Pakistan

BACKGROUND: No data exist on the population prevalence of, or risk factors for, human papillomavirus (HPV) infection in predominantly Muslim countries in Asia. METHODS: Cervical specimens were obtained from 899 married women aged 15-59 years from the general population of Karachi, Pakistan and from 91 locally diagnosed invasive cervical cancers (ICCs). HPV was detected using a GP5+/6+ PCR-based assay. RESULTS: The prevalence of HPV in the general population was 2.8%, with no evidence of higher HPV prevalence in young women. The positivity of HPV was associated with women's lifetime number of sexual partners, but particularly with the age difference between spouses and other husbands' characteristics, such as extramarital sexual relationships and regular absence from home. The HPV16/18 accounted for 24 and 88% of HPV-positive women in the general population and ICC, respectively. CONCLUSION: Cervical cancer prevention policies should take into account the low HPV prevalence and low acceptability of gynaecological examination in this population

Touchdown General Primer (GP5+/GP6+) PCR and optimized sample DNA concentration support the sensitive detection of human papillomavirus

BACKGROUND: The GP5+/GP6+ PCR assay is a well-established HPV detection technique. This study has examined the effects of incorporating 'hot start' and 'touchdown' steps into the protocol. In addition, dTTP was substituted with dUTP to permit contamination control measures against carry-over PCR product. METHODS: Firstly, HPV-16 was amplified from SiHa cell DNA (0.1 ng–100 ng) diluted in a background of C-33A DNA (100 ng-2 μg). Secondly, the detection of small quantities (15ag-1.5pg) of HPV recombinant plasmids (types 16, 31, 33, 45, 51, 52, and 56) diluted in C-33A DNA was investigated. Thirdly, clinical sample DNA extracts (cervical smears, formalin-fixed vaginal lesions and breast tumors) were tested for HPV. Six different PCR protocols were assessed. HPV was detected by gel electrophoresis, and by Southern and dot blot hybridization. RESULTS: HPV detection sensitivity was dependent on the total amount of DNA in a PCR. Touchdown protocols supported HPV-16 detection from 1 ng or 0.5 ng SiHa cell DNA in a background of 2 μg or 1 μg C-33A DNA respectively, and from 0.1 ng of SiHa cell DNA (~28 copies HPV-16) in 500 ng or 100 ng background DNA. Under standard GP5+/GP6+ annealing conditions, HPV-16 went undetected when the DNA content of a PCR was 2 μg or 1 μg, and with 500 ng C-33A DNA the sensitivity limit was 1 ng SiHa cell DNA. HPV recombinant plasmids were each detected with high (albeit varying) sensitivity by a touchdown protocol. HPV-31 was better amplified under standard annealing conditions (1.5fg in 100 ng background DNA) than by a touchdown approach (15fg detection limit). HPV-52 was not amplified by the standard protocol at the dilutions tested. Seventeen different HPV types were demonstrated in 47/65 (72%) abnormal cytology samples recorded as HPV negative by standard GP5+/GP6+ conditions. Twenty-one different HPV types were recorded in 111/114 (97%) vaginal lesions. Multiple infections were also detectable using a touchdown approach. Of 26 breast tumors, 5 (19%) tested HPV positive by the standard assay and 15/26 (58%) using a touchdown protocol. CONCLUSION: Touchdown modification of the GP5+/GP6+ PCR assay enables the detection of HPV undetected under regular assay conditions. The use of standardized DNA quantities in a PCR rather than standard sample volumes containing arbitrary amounts of DNA is supported. A touchdown approach may be beneficial as an analytical test for the re-evaluation of (apparently) HPV negative abnormal cervical cytological or histological samples, and for investigating the association of HPV with disease conditions at diverse organ sites. The clinical utility of a touchdown approach for HPV detection requires further investigation as increased assay analytical sensitivity may not necessarily equate with improved clinical sensitivity or specificity

Prevalence and determinants of human papillomavirus genital infection in men

Four-hundred-forty-five husbands of women with invasive cervical carcinoma, 165 of women with in situ cervical cancer, and 717 of control women (age range 19–82 years) were interviewed and a sample of exfoliated cells from the penis obtained in seven case–control studies conducted by the International Agency for Research on Cancer. The characteristics of human papillomavirus-positive and human papillomavirus-negative husbands were compared using odds ratios and 95% confidence intervals. Thirteen per cent of the husbands of control women, 18% of the husbands of women with invasive cervical carcinoma, and 21% of the husbands of in situ cervical carcinoma women were positive for penile human papillomavirus DNA. Human papillomavirus 16 was detected in 45 husbands, human papillomavirus 18, 31 or 33 in 19, and human papillomavirus 6/11 in 6, but the majority of human papillomavirus infection (158) was with other or unspecified human papillomavirus types. The same human papillomavirus type was seldom identified in both husband and wife. The strongest variation in penile human papillomavirus infection was by country, with percentages among the husbands of control women ranging between 3% in Spain and 39% in Brazil. Having had over 50 lifetime sexual partners, compared with only one, was associated with an odds ratio of 2.3