Numerical Assessment of PE 80 and PE 100 Pipe Lifetime Based on Paris-Erdogan Equation

Summary: A novel accelerated fracture mechanics extrapolation procedure based on cyclic test with cracked round bar (CRB) specimens was verified by a correlation of real pipe failure time to simulated failure times at a temperature of 60 °C. The procedure was applied to predict the long-term failure of modern PE 80 and PE 100 pipes 23 °C. Moreover, the used stress intensity factor concept also allows to consider the impact of arbitrary additional loading situations like soil loads or point loads and to assess pipe lifetime under complex loading situations.     

Determination of slow crack growth behaviour of polyethylene pressure pipes with cracked round bar test

In this work, a short time test method to determine the slow crack growth behaviour of samples made out of pipes was evaluated. The cracked round bar (CRB) method used provides results below 48 h with brittle fracture surfaces, which indicates the type of slow crack growth failure. To evaluate the usability of the method, the results were compared with well-known tests such as notch pipe test, 2 notch creep test and instrumented Charpy impact tests. The results indicate that the CRB test can be used to predict long term slow crack growth behaviour of PE pipes.     

Synthesis of 2,6-Dimethoxyhydroquinone-3-mercaptoacetyl-peptide-chlorambucil Conjugates

In previous paper, we had reported the synthesis of three conjugates of the cytotoxicity agents: 2,6-Dimethoxyhydroquinone-3-mercaptoacetic acid (DMQ-MA)1, which is a derivative of 2,6-dimethoxy-p-benzoquinone (DMQ). DMQ is a naturally fermented product of wheat germ and was found to have a wide spectrum of cytotoxicity against various tumor cell lines under the synergistic activation of L-ascorbic acid2-5 . Owing to the very low aqueous solubility of DMQ, we prepared derivatives of the …     

Analysis of Molecular and Morphological Effects on Slow Crack Growth in Modern PE Pipe Grades by Cyclic Fracture Mechanics Tests

Summary: Three different polyethylene (PE) pipe grades as well as three different lots of one of the grades were investigated by cyclic tests with cracked round bar (CRB) specimens, concerning resistance to slow crack growth. To enhance the test sensibility and proof its applicability for a quick quality assurance method various molecular and morphological characterizations on compression molded plates were carried out, with special attention on the influence of molecular and morphological differences, as well as lot to lot variations on the resistance to slow crack growth. The cyclic CRB tests allowed a ranking of the different pipe grades and lots with short testing times per material and testing machine, as a function of failure time as well as of crack initiation time with further reduction of testing time of about 50%. Moreover the ranking corresponded to the expectations based on the molecular and morphological properties of the materials, where only minor changes in the molecular mass distribution and the co-monomer concentration in case of lot to lot variations were proofed reliably.     

Cyclic tests on cracked round bars as a quick tool to assess the long term behaviour of thermoplastics and elastomers

The aim of this work is to demonstrate the applicability of the cracked round bar test recently developed for PE-HD to other polymeric materials. The main advantage of this new test method are rather short testing times for PE-HD materials used in long-term applications such as piping. Therefore, this test is of high interest for other polymers used in similar applications.Five thermoplastic materials used for plumbing (PE-HD, PP-B, PB, PVC-U, PA12), a technical polymer (POM) and an elastomeric material (H-NBR) have been tested. Scanning electron microscopy has been applied to investigate fracture surfaces.Results show that the test method seems to be basically applicable to all tested materials. Most materials showed similar fracture behaviour as postulated in literature, despite the high acceleration factor of the cyclic CRB test.     

Evaluation of hybrid laser-cut and cast miniature fracture specimens

This paper presents a new hybrid laser-cutting method for producing fracture test specimens from thermosetting materials. The hybrid approach combines casting of a sheet of material with subsequent laser-cutting of the test specimens. The new approach was compared to the traditional casting method using a fracture toughness test. For this study, a compact version of the tapered double cantilever beam (cTDCB) was used as a specimen geometry for both manufacturing methods. The cTDCB specimen is crack length independent, and crack length investigations were performed to ensure the crack length independence of the cTDCB specimens. The specimens that were made by the hybrid laser-cut method were found to be comparable to the specimens obtained by the traditional casting method. Moreover, the laser-cut method provides a fast and accurate method to make a significant number of samples in a reasonable time. These tests show that the hybrid laser-cut method could be a good alternative to the traditional casting method.     

A finite element method based comparative fracture assessment of carbon black and silica filled elastomers: Reinforcing efficacy of carbonaceous fillers in flexible composites

This study is focused on numerical investigation on fracture behaviors of carbon black (CB) and silica filled elastomeric composites. Finite element analysis (FEA) in compliance with multi-specimen method is used to calculate J-integral and geometry factor of the rubber composites up to a displacement of 20 mm for single edge notch in tension (SENT) and double edge notch in tension (DENT) specimens. An empirical relationship between crack tip opening displacement (CTOD) and crack advancement is established depending on notch to width ratio (NWR). The stress contours across the notches for SENT and DENT specimens is discussed briefly. It is found that fracture propagation resistance of CB filled elastomer is 125% more than that of silica filled elastomer. Although, Silica filled elastomer have good tensile strength and crosslink density but it fails to replace carbon black in terms of fracture properties. The critical J-integral for CB filled elastomer is 18.7% and 32.2% more than silica filled elastomer for SENT and DENT specimens respectively. The effect of specimen type on various fracture properties is also explored. The factor of safety is found to be significantly more in case of CB filled elastomers making them less vulnerable to crack propagation and catastrophic failure.     

Strain and damage sensing in additively manufactured CB/ABS polymer composites

In this study, an experimental investigation is performed to observe the electromechanical response of CB (carbon black)/Acrylonitrile butadiene styrene (ABS) additive manufactured composite under quasi-static (tensile, shear, and mode-I fracture) and dynamic (mode-I fracture) loading conditions for the potential damage sensing applications. Dog bone tensile, double v-notch shear, and single edge notch bending (SENB) specimen printed with three different configurations (0°/90°, +45°/-45°, and 0°) are considered for the quasi-static condition. A modified split Hopkinson pressure bar along with high-speed video camera is used for dynamic fracture experiments. Four-point probe technique coupled with a high-resolution data acquisition system is employed to obtain the real-time electrical response. In the case of tensile loading, +45°/-45° printed specimens show a nonlinear change of electrical resistance due to unique failure mode. Under the shear loading, electrical resistance remains unchanged during the elastic deformation. After the damage evolution, +45°/-45° printed specimens exhibit a higher rate of change in electrical resistance due to alignment of the filaments along the maximum principle shear stress direction. For both static and dynamic fracture loading, a minimal change of electrical resistance is observed before crack initiation. However, after the crack initiation, a sharp change of electrical resistance for 0°/90° printed specimens indicates a faster crack propagation as compared to the +45°/-45° printed specimens.     

Fracture mechanics of laser sintered cracked polyamide for a new method to induce cracks by additive manufacturing

This paper presents an experimental investigation on specimens manufactured by Selective Laser Sintering (SLS), with the purposes of giving designers advice when designing 3D printed parts, and laying the basis for a step forward in the field of fracture mechanics of 3D complex parts.The aim is to investigate the effect of building direction in Polyamide (PA) 3D printed samples and to assess whether a crack can be initiated directly from the sintering process for fracture mechanics study purposes.Six different configurations of Mode I Compact Tension (CT) specimens were manufactured and tested; the experiments were monitored by Digital Image Correlation (DIC) and fractured surfaces were analyzed using microscopy.Results showed that samples with better mechanical performance are those in which all the layers contain a portion of the crack. On the other hand, those with layers parallel to the crack plan offer a preferential pathway for the crack to propagate. DIC and fractography investigations showed that, under certain conditions, small-radius geometries, or too-close surfaces may bond together depending on printer resolution. Experiments also showed that SLS is capable of printing specimens with internal cracks that can be used to study fracture mechanics of complex parts or parts with internal cracks.     

Fracture resistance measurement of fused deposition modeling 3D printed polymers

A method is presented to characterize the fracture resistance and interlayer adhesion of fused deposition modeling (FDM) 3D printed materials. Double cantilever beam (DCB) specimens of acrylonitrile butadiene styrene (ABS) were designed and printed with a precrack at the layers' interface. The DCBs were loaded in an opening mode and the load-displacement curves were synchronized with the optical visualization of the crack tip to detect the critical load at the crack initiation. A finite element model, coupled with J-integral method and fracture surface analysis was then developed to obtain the apparent fracture resistance (J_cr,a) and the interlayer fracture resistance (J_cr,i), as a measure of the interlayer adhesion. The maximum J_cr,i was measured to be 4017 J/m², a value close to the fracture resistance of bulk ABS. Both J_cr,a and J_cr,i increased with the printing temperature. This method can find a great importance in the structural applications of printed materials.     

Determination and comparison of the plane stress essentialwork of fracture of three polyesters PET, PPT and PBT

The essential work of fracture (EWF) method has been used to study the relationship between molecular structure and thin film fracture toughness for three ductile polyesters at ambient temperature. The fracture toughness of PPT is of particular interest. Successful fracture characterisation of thin film polyesters has been achieved by the EWF method using double edge notched tension (DENT) specimens. The specific essential work of fracture, w _e, for polyethylene terephthalate (PET), polypropylene terephthalate (PPT) and polybutylene terephthalate (PBT) films is found to be 35.54±2.56, 41.03±3.23 and 31.34±8.60 kJ m^–2, respectively. Differential scanning calorimetry (DSC) has been employed to investigate the crystallinity of the polymers concerned and the effect of this on their EWF values.     

Slow crack growth resistance of modern PA-U12 grades measured by cyclic cracked round bar tests and strain hardening tests

A critical failure mechanism in long-term applications of plastic structures, such as piping systems, is considered to be crack initiation and subsequent Slow Crack Growth (SCG). Thus, safe installation and operation during service lifetime of such structures are not conceivable without the knowledge of the resistance against SCG for any new material, like Unplasticized PolyAmide 12 (PA-U12). Unfortunately, long-term static tests at elevated temperatures lead to unreasonably long test times and measurements may also be affected by thermal aging and hydrolysis. Against this backdrop, the current study examines two accelerated test methods, namely the cyclic Cracked Round Bar (CRB) test as well as the Strain Hardening (SH) test, in order to characterize the SCG behavior. Both were originally developed for PolyEthylene (PE) and successfully implemented in recent years. While the cyclic CRB test measures SCG directly, accelerated through cyclic loading, the SH test quantifies the molecular disentanglement resistance, which determines craze formation and breakdown. The focus of this work was initially put on the extension of the CRB test towards PA-U12 grades, checking the occurrence of actual crack initiation and propagation. Afterwards a correlation to SH test results was done in terms of SCG resistance. Thereby, adequate test conditions were developed and the influence of the Molecular Weight (MW), expressed by the Viscosity Number (VN) of the PA-U12 grades, was considered. Results confirm the suitability of each method to rank SCG resistance and show a good correlation of the abovementioned SMall scale Accelerated Reliable Test (SMART) methods, highlighting their sensitivity to long-term relevant molecular parameters.     

Simultaneous UPLC‐MS/MS determination of antiepileptic agents for dose adjustment

Therapeutic drug monitoring (TDM) of anti‐epileptic drugs (AED) is a routine application. Carbamazepine (CRB) is monitored as the parent drug while oxcarbazepine (OXC) and eslicarbazepine acetate (ESL) are monitored as their active metabolite (eslicarbazepine; MHD). We have developed a UPLC‐MS/MS method for determining CRB, OXC, ESL and MHD in plasma or serum with a simplified extraction protocol. The developed method detects sildenafil (SLD), which clinically interferes with AED and is likely to be co‐administered in epileptic patients suffering from sexual insufficiency (60%). MHD was prepared in‐house. AED were simultaneously determined in presence of SLD using gatifloxacin as an internal standard (IS). Separation was achieved using acetonitrile, methanol and 100 mm ammonium acetate in water (32:3:65, v /v/v) on an Intersil^®RP‐HPLC column (250 × 4.6 mm, 5 μm). A one‐step extraction was performed by simultaneous protein and phospholipids precipitation. Detection was done by tandem mass spectrometry. No relative matrix effect was observed. The method was linear (0.5–40 μg/mL for CRB, ESL and MHD and 0.05–4 μg/mL for OXC), accurate and selective. Recoveries were 64.41 ± 5.07, 45.62 ± 1.73, 61.41 ± 4.77 and 60.33 ± 1.36 for CRB, OXC, ESL and MHD, respectively. The method was successfully applied for TDM of AED.     

Relevance of the femtolaser notch sharpening to the fracture of ethylene-propylene block copolymers

The effect of the notch sharpening on the fracture toughness measured under Linear Elastic Fracture Mechanics (LEFM), Elastic-Plastic Fracture Mechanics (EPFM) and Post-Yielding Fracture Mechanics (PYFM) approaches has been evaluated. Bulk and film specimens of an ethylene-propylene block copolymer have been analyzed. The samples for fracture characterization were sharpened using a steel razor blade and the femtosecond laser ablation technique. Both notching techniques give rise to crack tip radii of the very same size. The fracture toughness of the specimens sharpened via femtolaser were ∼10%, ∼75% and ∼90% lower than that of the specimens sharpened via razor blade when determined with the help of LEFM, the EPFM approach as the multiple specimen method, and by the Essential Work of Fracture, respectively. Both in the bulk samples as in the films, the presence of plastic deformation, either large or small, occurring ahead of the crack tip during the sharpening seems to be the reason for the difference in the fracture values.     

Mechanical evaluation of polymeric filaments and their corresponding 3D printed samples

3D printing technologies permits to produce functional parts with complex geometries, optimized topologies or enhanced internal structures. The relationship between mechanical performance and manufacturing parameters should be exhaustively analyzed to warrant the long term success of printed products. In this work, the mechanical performance of filaments based on acrylonitrile butadiene styrene (ABS), polylactic acid (PLA) and polylactic acid/polyhydroxyalkanoate (PLA/PHA) was investigated and also compared with their corresponding 3D printed samples. In general, the specimen dimensional deviations were found to be within the tolerances defined by the standard testing protocols. Density values revealed a high level of filament fusion promoting a nearly solid internal structure. The filaments exhibited improved tensile performance with respect to their corresponding printed samples. Tensile and bending performance looked quite independent of the raster angle. Izod impact behavior was increased, for ABS systems printed with the ±45° raster orientation. Quasi-static fracture tests displayed improved crack initiation resistance with the 0°/90° raster angle. The crack propagation observed for the ±45° specimens, through the bonding of the inter-layers, suggests weak entanglements.     

On the experimental measurement of fracture toughness in SENT rubber specimens

This work provides a direct comparison of several experimental approaches used in the literature to measure fracture toughness of rubber of rubber using single edge notched in tension (SENT) specimens, with the final aim to provide guidelines for an optimal testing procedure. Digital image correlation measurements were used to get new insights into the fracture process. SENT is experimentally advantageous because of the simple preparation from laboratory plates and the small amount of material required. The most common experimental approaches to measure fracture toughness of rubber rely on the energy release rate, measured by the tearing energy or the J-integral parameters. This work points out the importance of experimental conditions and test procedures: long specimens and short notches are preferred, identification of fracture initiation from the front view is necessary, strain energy density should not be evaluated from un-notched specimens at the critical stretch level, rather alternative strategies are shown in this work.     

Special fracture mechanics specimens for multilayer plastic pipes testing

Pipes consisting of layers of different materials (multilayer pipes) are considered. The fracture toughness value of the main pipe is taken into account as a parameter relevant to fracture assessment connected with the resistance of pipe material against slow crack growth. With the aim of simplifying estimation of main pipe material fracture toughness, non-homogeneous test specimens cut directly from multi-layer pipes are suggested and numerically analysed. The values of the corresponding stress intensity factor K_I and biaxiality factors B are calculated for the case of two and three layer test specimens. Based on the results obtained, the transferability of fracture toughness values measured on laboratory specimens to pipe systems is discussed. It is shown that in most cases of multi-layer commercial pipes and routine fracture toughness measurements the values of the stress intensity factor calculated on the basis of homogeneous specimens can be used.     

On the determination of the point of fracture initiation by the load separation criterion in J-testing of ductile polymers

The application of an experimental approach based on the load separation criterion for the determination of the point of fracture initiation in a fracture test on a ductile polymer was critically examined. To this aim, the fracture process outlined by the application of this method was related to that described by the visual analysis of the fracture surfaces obtained in fracture tests on nominally identical specimens, in which different levels of crack extension were produced. The material examined was an acrylonitrile-butadiene-styrene (ABS) resin, and the fracture tests were performed at low loading rate on single-edge notched in bending specimens.The results demonstrated that this load separation criterion based methodology is a promising approach for the determination of the point of fracture initiation, and for material fracture resistance, J_Ic, evaluation. The method also has experimental simplicity and a high degree of repeatability.     

Conformational change,intrachain aggregation and photophysical properties of regioregular poly(3‐octylthiophene) in alkanes

This study explores the role of segmental solubility of regioregular poly(3‐octylthiophene) (rr‐P3OT) on chain organization and its photophysical properties. In good solvent chlorobenzene (CRB), rr‐P3OT chain adopts an extended conformation, allowing long conjugation length of π‐electrons. Cyclohexane is a good solvent for octyl side chain but a poor solvent for the thiophene backbone. The selective segmental interactions of rr‐P3OT with this solvent induce conformational change of the polymer. Addition of cyclohexane into the CRB solution leads to chain coiling, which in turn causes significant decrease of the conjugation length. Absorption and photoluminescence spectra of the rr‐P3OT in cyclohexane exhibit a blueshift of about 16 nm compared to those of the CRB solution. The change of chain conformation is also detectable by monitoring the variation of quantum yield upon increasing cyclohexane ratio. The quantum yield drops from 0.17 ± 0.01 to 0.11 ± 0.01 when the extended rr‐P3OT chain transforms into coiled conformation. Hexane is a nonsolvent for rr‐P3OT due to its relatively low solubility parameter. The addition of hexane into rr‐P3OT solution in cyclohexane forces dense packing of thiophene rings within the coiled chain. An intrachain aggregation occurs in this system, leading to the appearance of three distinct redshift peaks in absorption spectra and the drastic drop of quantum yield. Correlation between the growth of redshift peaks and the decrease of quantum yield is clearly observed. © 2013 Wiley Periodicals, Inc. J. Polym. Sci., Part B: Polym. Phys. 2013 , 51, 1288–1297