Melting point and crystallinity of various UHMWPE with different molecular weight from DSC curves (1—the first scanning, 2—the second scanning).
\r\n\tWe dedicated a chapter to the principles of chest drainage which may be of cross-specialty interest from A&E to post-surgical procedures.
\r\n\r\n\tThe broad spectrum of the diseases of the pleura, which are to be considered heterogeneous by definition, may affect patients of different ages, require different treatment strategies, and have different outcomes (e.g. pneumothorax, mesothelioma).
\r\n\r\n\tIn this book, we will discuss most of the pleural diseases but we opted to analyze them from the surgical point of view because of the complexity of diagnosis, treatment, and care of such patients, which may be challenging but critically important.
",isbn:"978-1-83969-693-0",printIsbn:"978-1-83969-692-3",pdfIsbn:"978-1-83969-694-7",doi:null,price:0,priceEur:0,priceUsd:0,slug:null,numberOfPages:0,isOpenForSubmission:!0,hash:"679c752debe8c1edd8a489cc9731485e",bookSignature:"Dr. Alberto Sandri",publishedDate:null,coverURL:"https://cdn.intechopen.com/books/images_new/11045.jpg",keywords:"Pleural Ultrasonography, Pleural CT-scan, Chest Tubes, Small-bore Catheters, Pneumothorax, Air-leak, Empyema, Pleural Surgery, VATS, Pleurectomy, Bronchopleural Fistula, Pneumonectomy",numberOfDownloads:null,numberOfWosCitations:0,numberOfCrossrefCitations:null,numberOfDimensionsCitations:null,numberOfTotalCitations:null,isAvailableForWebshopOrdering:!0,dateEndFirstStepPublish:"March 12th 2021",dateEndSecondStepPublish:"April 9th 2021",dateEndThirdStepPublish:"June 8th 2021",dateEndFourthStepPublish:"August 27th 2021",dateEndFifthStepPublish:"October 26th 2021",remainingDaysToSecondStep:"2 days",secondStepPassed:!0,currentStepOfPublishingProcess:3,editedByType:null,kuFlag:!1,biosketch:"Dr. Alberto Sandri is qualified in Medicine from the University of Torino. During his fourth year of specialty, Dr. Sandri completed a fellowship in minimally invasive thoracic surgery at St. James's University Teaching Hospital in Leeds, the UK with a significant focus on minimally invasive thoracic surgery. In the years following his specialty, Dr. Sandri worked at the European Institute of Oncology (IEO) in Milan and at Oxford University Hospitals NHS Foundation Trust, Oxford, UK.",coeditorOneBiosketch:null,coeditorTwoBiosketch:null,coeditorThreeBiosketch:null,coeditorFourBiosketch:null,coeditorFiveBiosketch:null,editors:[{id:"50811",title:"Dr.",name:"Alberto",middleName:null,surname:"Sandri",slug:"alberto-sandri",fullName:"Alberto Sandri",profilePictureURL:"https://mts.intechopen.com/storage/users/50811/images/system/50811.jpg",biography:"Thoracic Surgery Unit, Department of Oncology, San Luigi Gonzaga Hospital, Torino, Italy\nDr. Alberto Sandri is a Thoracic Surgeon at San Luigi Gonzaga Hospital, Orbassano, Torino, Italy since 2018 where he is in charge of Minimally Invasive Thoracic Surgery (uVATS).\nHe qualified in Medicine from the University of Torino in 2010. He completed his speciality in thoracic surgery at the AUO Città della Scienza e della Salute in Torino in 2016 with first class honours. During his fourth year of speciality Dr. Sandri completed a fellowship in minimally invasive thoracic surgery at St. James's University Teaching Hospital in Leeds, UK with a significant focus in minimally invasive thoracic surgery. In the years following his speciality, Dr. Sandri worked at the European Instituite of Oncology (IEO) in Milan and at Oxford University Hospitals NHS Foundation Trust, Oxford, UK.\nSince September 2018 Dr. Sandri is a consultant thoracic surgeon at San Luigi Gonzaga Hospital in Orbassano Torino, His main fields of interests are Minimally Invasive Thoracic Surgery; Uniportal VATS Lobectomy and Segmentectomy; Thoracic Oncology; Mediastinal tumours and VATS thymectomy for Myasthenia Gravis.\nHe has published more than 50 scientific articles, is author and co-author in 10+ book chapters and made many national and international presentations.\n\nhttps://orcid.org/0000-0001-6421-2270",institutionString:"Ospedale San Luigi Gonzaga",position:null,outsideEditionCount:0,totalCites:0,totalAuthoredChapters:"2",totalChapterViews:"0",totalEditedBooks:"0",institution:{name:"Ospedale San Luigi Gonzaga",institutionURL:null,country:{name:"Italy"}}}],coeditorOne:null,coeditorTwo:null,coeditorThree:null,coeditorFour:null,coeditorFive:null,topics:[{id:"16",title:"Medicine",slug:"medicine"}],chapters:null,productType:{id:"1",title:"Edited Volume",chapterContentType:"chapter",authoredCaption:"Edited by"},personalPublishingAssistant:{id:"280415",firstName:"Josip",lastName:"Knapic",middleName:null,title:"Mr.",imageUrl:"https://mts.intechopen.com/storage/users/280415/images/8050_n.jpg",email:"josip@intechopen.com",biography:"As an Author Service Manager my responsibilities include monitoring and facilitating all publishing activities for authors and editors. From chapter submission and review, to approval and revision, copy-editing and design, until final publication, I work closely with authors and editors to ensure a simple and easy publishing process. I maintain constant and effective communication with authors, editors and reviewers, which allows for a level of personal support that enables contributors to fully commit and concentrate on the chapters they are writing, editing, or reviewing. I assist authors in the preparation of their full chapter submissions and track important deadlines and ensure they are met. I help to coordinate internal processes such as linguistic review, and monitor the technical aspects of the process. As an ASM I am also involved in the acquisition of editors. Whether that be identifying an exceptional author and proposing an editorship collaboration, or contacting researchers who would like the opportunity to work with IntechOpen, I establish and help manage author and editor acquisition and contact."}},relatedBooks:[{type:"book",id:"6550",title:"Cohort Studies in Health Sciences",subtitle:null,isOpenForSubmission:!1,hash:"01df5aba4fff1a84b37a2fdafa809660",slug:"cohort-studies-in-health-sciences",bookSignature:"R. Mauricio Barría",coverURL:"https://cdn.intechopen.com/books/images_new/6550.jpg",editedByType:"Edited by",editors:[{id:"88861",title:"Dr.",name:"R. Mauricio",surname:"Barría",slug:"r.-mauricio-barria",fullName:"R. 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Because of these excellent properties, UHMWPE has been widely used in many applications including mining, transportation, military industries, biomedical engineering, sports and livelihood projects [3, 4, 5, 6].
\nUHMWPE is a special kind polyethylene. Except it, the polyethylene family also includes linear low density polyethylene (LLDPE), low density polyethylene (LDPE), high density polyethylene (HDPE) and cross-linked polyethylene (XLPE) [7, 8, 9]. These polyethylenes are synthesized with ethylene as monomers. By using different catalysts and synthetic process conditions, a variety of polyethylene with different structures, density and properties can be synthesized, such as LLDPE, LDPE and HDPE. In addition, cross-linked polyethylene can be obtained by the crosslinking reaction during or after the synthesis reaction process. UHMWPE is an unbranched linear polyethylene and can be synthesized with Ziegler-Natta or metallocene catalyst under the low-pressure polymerization process conditions [10, 11]. UHMWPE has extremely high molecular weight of up to several millions g/mol, which is several times larger than HDPE with a molecular weight of 200,000 g/mol. Actually, the precise molecular weight of UHMWPE is too high to be measured directly by conventional means, and it must be inferred by its intrinsic viscosity as an alternative approach.
\nIn general, molecular weight of polymer has significant effects on its condensed structure, chemical performance, mechanical properties and processability. It is obvious that the excellent characteristics of UHMWPE are largely benefited from its extremely high molecular weight. The acceptable reasons are related to the enhanced intermolecular interactions and intensive chain entanglements. With increasing molecular weight, van der Waals force between macromolecules would be strengthened, and the ultra-long molecule chains of UHMWPE are prone to become entangled and to form intensive physical entanglements [12, 13]. These factors synthetically result in the significant improvement of mechanical strength, abrasion resistance, chemical stability, and so on.
\nEven if the ultra-high molecular weight has brought superior performances for UHMWPE, the extremely high molecular weight also brings great challenges for its processing and forming such as poor dissolution, extremely high melt viscosity and poor melt flowability [14, 15, 16]. The long chain movement of UHMWPE can be restricted by the strong constraint effect due to the enhanced intermolecular interactions and dense physical entanglements, resulting in improving the solvent resistance and solution or melt viscosity. This result is not a good thing for processing and forming of UHMWPE, including solution method and melting method.
\nFor most thermoplastic polymers, there are a variety of processing and moulding methods, such as extrusion, injection, compression and casting. By these processing technologies, raw materials can be fabricated into polymer products with given profiles and appropriate properties such as large products with sufficient strength or micro/nano parts with high precision. However, it is very difficult to process nascent UHMWPE via conventional batch processing methods. UHMWPE extrusion products (pipes, sheets and bars) only can be extruded by large trust extruder with special screw structures, simultaneously adding a large amount of organic compounds as lubricants. According to the literature, even with improved upgrade screw extruder, it is almost impossible to extrude UHMWPE without any processing aids. The most straightforward reason is the extremely high melt viscosity and low melt flowability [16, 17, 18, 19]. It is also very difficult to carry out injection moulding due to the poor fluidity of UHMWPE. Even though Huang et al. [20, 21] have obtained injection parts of UHMWPE blend containing 90 wt% commercial UHMWPE and 10 wt% ultra-low molecular weight polyethylene(ULMWPE), with a modified injection moulding technique named as oscillation shear injection moulding, pure UHMWPE parts with profiled surfaces still cannot manufactured directly by injection moulding. Thus, multistep processing method is usually used to prepare UHMWPE parts with complex profiles. For instance, in order to manufacture artificial knee joints, nascent UHMWPE powder particles must first be moulded into primary products with square or cylindrical profiles by compression moulding or plunger extrusion, and then artificial knee joints were fabricated by turning from primary products [1].
\nAs a matter of fact, the problem of UHMWPE processing is always a worldwide challenge for material engineers and researchers from past to present. The efficient and easier processing solutions for UHMWPE could not be put forward over the past few decades. It is still a main constraint for promoting the development and application of UHMWPE at present. Actually, UHMWPE extrusion processing technique is the most likely to first achieve industrial production. The objective of this chapter is to review the progress of extrusion processing technique for UHMWPE, as a basis for understanding the processing principles and methods for such thermoplastic polymer with ultra-high molecular weight.
\nAs previously described, UHMWPE is synthesized with ethylene as monomers and has same repeat units as other common polyethylene. The single molecular chains of UHMWPE can consist of as many as hundreds of thousands repeat units. Because of the internal energy, the molecular chain could become mobile at elevated temperatures. Considering the ultra-long length and movement, a single molecular chain of UHMWPE is like a moving string over a kilometre long and tends to be tangled gradually.
\nAs the temperature decreases, the molecular chain has a trend to rotate around the C-C bonds and create chain folds, reaching a new energy equilibrium state at a lower temperature. When cooled below the melt temperature of polymer, the activity of molecular chain is reduced, and the folded chains begin to form crystalline lamellae, which is the local ordered sheet-like regions. These lamellae gradually grow and accumulate in order to form crystalline regions of polymers. It is well known that there is almost no complete crystallization for polymer. In other words, there are always disordered regions in polymer, namely amorphous regions. Although the molecular chain of polyethylene is regular and flexible, not all segments of polyethylene chain can arrange into the ordered regions to form lamellae and crystalline regions. The lamellae are embedded within amorphous regions and may communicate with surrounding lamellae by tie molecules. Kurtz [1] has clearly observed the crystalline morphology of UHMWPE by using transmission electron microscopy (TEM), showing the composite nature of UHMWPE as an interconnected network of amorphous and crystalline regions. It can be clearly seen that UHMWPE is a typical semi-crystalline polymer as ordinary polyethylene.
\nDespite the close crystallinity, the morphology of nascent UHMWPE powder particles is quite different from that of HDPE. Obviously, from scanning electron microscope (SEM) images as shown in Figure 1, the individual nascent powder particle of UHMWPE is composed of several secondary particles. There are many orientation fibres as connections between secondary particles. Compared with other dense parts in the individual particle, the orientation fibres are loose. These fibres as weak sections in powder particles may be first melted when the temperature rises to the melting point.
\nThe morphologies of polyethylene with different molecular weight (a) HDPE with molecular weight of 600,000 g/mol, 10,000× magnification; (b) UHMWPE with molecular weight of 2,000,000 g/mol, 5000× magnification.
The values of crystallinity degree and melting point of nascent UHMWPE with different molecular weight are listed as Table 1. Apparently, the crystallinity degree and melting point have a rising trend with increasing molecular weight. However, the values of crystallinity degree and melting point from the second scanning curves are all lower than that from the first scanning. The possible reason is that the crystallinity degree of polymer depends upon various factors, including molecular weight, processing conditions and environmental conditions (such as loading, flow field, ultrasonic, and so on) [22, 23, 24, 25]. It is helpful to understand the melting mechanisms and melt flow process by realizing the melting process and crystallization process.
\nSamples | \nMw (1 × 104 g/mol) | \nTm1 (°C) | \nTm2 (°C) | \nXc1 (%) | \nXc2 (%) | \n
---|---|---|---|---|---|
GHR8110 | \n~60 | \n130.2 | \n128.5 | \n71.1 | \n68.3 | \n
145 M | \n~145 | \n140.7 | \n135.8 | \n65.8 | \n54.8 | \n
M1 | \n150–200 | \n143.6 | \n136.4 | \n69.3 | \n54.0 | \n
M2 | \n250–350 | \n144.2 | \n137.1 | \n83.4 | \n65.2 | \n
M3 | \n~350 | \n144.5 | \n137.0 | \n81.4 | \n61.9 | \n
GUR4120 | \n~500 | \n144.5 | \n136.4 | \n78.5 | \n58.9 | \n
Melting point and crystallinity of various UHMWPE with different molecular weight from DSC curves (1—the first scanning, 2—the second scanning).
Thermal stability of polymer is another important factor, which must be considered in processing. In general, the decomposition temperature of HDPE or LDPE is below 400°C. But the decomposition temperature of UHMWPE usually exceeds 430°C probably because of the strong intermolecular interactions from the extremely high molecular weight. As the heating scanning curve of UHMWPE (GUR4120, Ticona) exhibited in Figure 2, the initial decomposition temperature is up to 450°C and the fastest degradation process occurred at about 480°C. Although it has higher decomposition temperature than other common polyethylene, the processing temperature for UHMWPE cannot be such high. Due to poor thermal conductivity, the accumulation of heat causes too high temperature in partial of polymer melt, and the thermal degradation in the melt state occurs in the processing temperature up to 300°C.
\nThermogravimetric analysis (TGA) for UHMWPE.
It is important to note that the melt flow characteristics of polymer usually determine the processing method and conditions. It also greatly affects the forming process and product quality. For instance, the phenomenon of melt breakup in extrusion is usually related to the critical shear rate, which is an important aspect of flow characteristics of polymer melt.
\nFor UHMWPE, its melting point is about 155°C, and the polymer powder particles can completely fuse into melt as temperature is higher than 200°C. However, the UHMWPE melt is rubberlike and has poor flowability even at the temperature much higher than melting point. Even if the temperature and load, respectively, were up to 250°C and 21.6 kg separately, the melt flow rate of UHMWPE was almost zero. Melt viscosity is an important parameter of melt flow. Actually, it is very difficult to determine directly the precise value for the melt viscosity of UHMWPE. But the trend in change of viscosity can be inferred with molecular weight by the following equations [16].
\nwhere k is a constant and η, Mw, and Mwc represent viscosity, average molecular weight, and critical relative average molecular weight, respectively.
\nGenerally speaking, the molecular weight of UHMWPE should be higher than 1.5 million g/mol. Thus, the molecular weight of UHMWPE is much higher than the critical relative average molecular weight. Therefore, the viscosity can be evaluated by Eq. 2. For instance, the viscosity of UHMWPE with molecular weight of 3 million g/mol is about 2500 times higher than HDPE with molecular weight of 300,000 g/mol. According to the references, the melt viscosity of UHMWPE could be up to 108 Pa·s [26].
\nThe extremely high viscosity would certainly result in the poor melt flowability and processability. For example, even if the nascent UHMWPE powder particles were processed with an internal mixer at 200°C for 20 min, the masterbatch still could not be dispersed evenly in UHMWPE melt. As displayed in Figure 3a, during the whole mixing process, the masterbatch only dispersed in a very narrow range along the rotation direction; however, it almost cannot disperse into the melt far away from the place where masterbatch is placed. Probably because the strong shearing effect along rotation direction makes materials exchanging significantly, and there is no obvious material exchange in the direction perpendicular to the rotation. This clearly demonstrates the limited molecular chain mobility and poor melt flowability of UHMWPE melt.
\nMelting state of UHMWPE processed with an internal mixer.
With the increase of temperature, UHMWPE melt will not enter the viscous flow state but to maintain a transparent rubberlike state. In fact, UHMWPE melt has no viscous flow state like HDPE or LDPE because its theoretical viscous flow temperature is higher than the decomposition temperature. In addition, it is easy to find out from the picture that the UHMWPE melt has ruptured and could not form uniform and continuous melt. The fundamental reason is that UHMWPE melt has a low critical shear rate of 10−3 s−1. Therefore, the UHMWPE melt was easy to break up by strong shear effect with internal mixer. Although there exists a metastability processing window in the temperature range of 154°C and 157°C [27, 28, 29], the nascent UHMWPE cannot be processed by conventional or improved upgrade screw equipment without processing aids. Considered the complicated interfering factors of extremely high melt viscosity, low melt flow rate, low critical shear rate no viscous flow and so on, it is a huge challenge to process UHMWPE continuously and efficiently via screw equipment dominated by shear flow and methods based on viscous flow theory.
\nThe most common methods used to process UHMWPE powder particles into bulk products are compression moulding and ram extrusion [30, 31]. Compression moulding originated in Germany in the 1950s is a discontinuous process based on sintering without limitation of molecular weight and melt viscosity. Ram extrusion was developed by converters in the United States during the 1970s. It was a processing process, which can be considered as a continuous compression and sintering process. Taking into account the intermittent feeding and compaction, ram extrusion in the strict sense was a quasi-continuous process. Nevertheless, it still could consecutively produce sheets, pipes, bars and profiles, even the molecular weight of UHMWPE being up to 10 million g/mol. In contrast with single screw or twin screw extrusion, the ram extrusion only was affected slightly by molecular weight and melt viscosity.
\nRam extruder consists essentially of a hopper, a feeding chamber with heating device, a horizontal reciprocating ram, a heated forming die, cooling and shaping apparatus. So it is easy to understand the ram extrusion process of feeding, compaction, melting and plasticizing, extruding, cooling, and moulding. UHMWPE powder particles are fed continuously into ram extruder and were heated at elevated temperatures. Within the extruder, the powder particles are consolidated and maintained under pressure by the ram, as well as by the back pressure from UHMWPE melt, which caused by frictional forces of the molten resin against the die wall surface. UHMWPE melt is extruded from heated forming die with specified shape. The thrust force to overcome the huge resistance originated from positive displacement movement of the reciprocating ram.
\nAlthough the ram extruder can manufacture UHMWPE products with good surface quality, the intermittent stamping process caused residual stresses inside the bulk. It is necessary for extrusion products to be annealed at elevated temperatures in order to remove residual stresses. The annealing process can also increase the crystallinity of the components, which is helpful to maintain the excellent mechanical performances of UHMWPE.
\nThere are also some disadvantages for ram extruder to process UHWMPE, such as fluctuations in product quality, longer melt plasticization cycle, slow extrusion rate, and high energy consumption. Extruder with multiple plungers is used to reduce the pulsation frequency [32]. Several rams alternately compact the materials and push them forward. This process shortens the operation time between two compaction actions, making the whole process closer to a continuous process, which is conducive to reducing the fluctuations of processing process and product quality. Certainly, this requires more advanced control technology for the extrusion process.
\nIn fact, regardless of high energy consumption and low processing efficiency, compression and ram extrusion are the most suitable processing methods for thermoplastic polymer with extreme high molecular weight and melt viscosity. However, the cost and diversity of products must be considered in industrial production. Screw extrusion is quite popular with people in all conventional processing methods for UHWMPE because of continuous production process and well-compounded effect. The commonly used screw equipment for UHMWPE are single screw extruder and twin screw extruder.
\nIn 1939, Troester Machinery Company in Germany launched an extruder with length/diameter ratio of 10, marking the development and rise of modern single screw extruder. There are many types of single screw extruders, which are widely used in extrusion processing and moulding of polymers [33, 34, 35].
\nDespite various kinds of single screw extruders, they have similar functions for common thermoplastic polymers. After entering the barrel from the hopper, the material was gradually pushed to the head direction with rotation of the screw. Successively, the material passed through several functional areas of the extruder, including solid conveying section, melting section, and melt conveying section. Loose materials were compacted in solid conveying section and melted before reaching the melt conveying section, then the homogenized melt was squeezed out from heating die. For most thermoplastic polymers, they eventually became viscous fluid in the extrusion process. Various processing rheology theories and extrusion equipment are based on this fact.
\nHowever, many cases are very different for UHMWPE. Since the low friction coefficient of UHMWPE and metal, UHMWPE powder particles in the feeding section are easy to slide with the rotating screw, resulting in the difficulty for powder particles being pushed forward. On the other hand, the melt is like rubber without viscous flow, which means a poor flowability for UHMWPE melt. The extremely high resistance is easily established in compaction section and results in huge backpressure due to the extremely high melt viscosity and poor flowability. Then, the melted resins are easy to wrap in the screw and rotate with the screw, preventing UHMWPE melt to move forward. It can even cause the screw to break if the device is forced to run.
\nObviously, conventional single screw extruder is almost powerless to process UHMWPE. Then, many new dedicated equipment with special internal structures were developed in order to overcome the difficulty of feeding and huge extrusion resistance [36]. For example, special single screw extruder with gradient grooves in the barrel was developed in 1971 to avoid the slippage phenomenon of UHMWPE in extrusion processing by Mitsui Petrochemical Company. Depth and width of grooves are gradually decreasing along the extrusion direction, which is favourable for establishing pressure. The principle of establishing pressure is similar to the advanced extrusion system of Institute of Plastics Processing (IKV) at RWTH Aachen University. The pressure peak of extrusion system usually appears at the end of the solid conveying section. Such extrusion system is good for improvement of the extrusion output and stability. Many other special extruders are developed to solve delivery problems for UHMWPE. However, such extruders only increase the coefficient friction between polymer and barrel and do not change the conveying mechanism, which resulting in the increases of wear of screw and barrel, drive load, and friction heat. Although the energy consumption is increasing, single screw extruder with large thrust screw and special screw structures for enhancing conveying capability is the most practical processing device for UHMWPE at present.
\nAs we know, in extruding process, common thermoplastic polymers successively experience solid state, viscous flow state, and high elastic state from feeding section to heating die. However, UHMWPE only experiences two physical states inside the barrel, namely solid state and high elastic state. The rotating screw consecutively grabbed UHMWPE powder particles from the feed inlet and compact them into block. The block is like a solid plug and conveys spirally forward along the rectangular tunnel by the trust of screw flight. Even the block is completely melted in metering section, it still moves forward as a whole. In other words, the flow mode of UHMWPE is plug flow, and there is almost no material exchange during the extrusion process. Therefore, the melting process of UHMWPE is similar to that of it under the static action by compression loads.
\nPolymer melt can be extruded out the extrusion die and forms continuous extrudates with specified cross-sectional shape as the die. During this process, polymer melt passes through the convergent channel inside extruder head and produces a shear deformation. Within the appropriate extrusion processing window, polymer melt with good flowability will maintain as a continuous melt block after flowing through the convergent channel.
\nAs the schematic diagram shown in Figure 4, UHMWPE melt has very low critical shear rate, and the extrusion process will produce significant fluctuations when the shear rate is more than 10−2 s−1. Many facts have shown that pure UHMWPE melt is easy to fracture even the extrusion speed was less than 10 r/min. The possible reason is that UHMWPE melt is fractured by shearing effect from deformation, and the fractured melt could not quickly merge to be continuous melt block again due to the poor molecular mobility of UHMWPE.
\nSchematic diagram of UHMWPE melt flow state during extrusion processing.
Many measures have been taken to prevent the unstable extrusion process and to improve the surface quality of extrudates, for instance, extending the length of the parallel flow path behind the convergent channel, reducing the angle of convergence, and reducing the friction resistance by using lubricants. Nevertheless, UHMWPE productivity and production efficiency have not improved significantly.
\nAccording to the relative rotation of two screws, twin screw extruders can be divided into counter rotating and co-rotating. The extruder of counter rotating has discontinuous channel that the spiral forward channel of screw is blocked by the screw flight of another screw with opposite rotating direction. For solid plug of UHMWPE, the continuous melt will be crushed into pieces by the strong shearing and mixing effect, and these crushed melt cannot quickly re-fuse to be a continuous melt block, causing significant instability extrusion.
\nCompared with counter rotating twin screw extruder, co-rotating twin screw extruder has a continuous channel to connect the feeding section and heating die, possessing good self-cleaning, and forcibly conveying capacity. The solid plug of UHMWPE can be conveyed forward along the continuous channel under positive displacement force. Such kind of extruder can effectively prevent material slippage and blockage.
\nAt present, two types of twin-screw extruder are usually used to extrude UHMWPE in industrial production [20, 37, 38]. However, the difficult realities of low extrusion output, high energy consumption, and large driving load are still troubling people and hindering the development of UHMWPE processing.
\nAs previously summarized, the nascent UHMWPE could be directly processed via compression moulding and ram extrusion. However, in most cases, processing aids should be required for screw extrusion even using an appropriative screw with special structures, and the excellent performances of UHMWPE would be damaged evidently. On the other hand, strong shearing action of screw extruder could make ultra-long molecular chains broken and even cause thermal degradation of UHMWPE.
\nSome new processing technologies are adopted to process UHMWPE in order to improve the extrusion output and reduce damage of material properties such as ultrasonic-assisted extrusion, gas-assisted extrusion, and near melting point extrusion process [39, 40]. Despite some progress, these extrusion processes still cannot extrude nascent UHMWPE without processing aids.
\nWith regard to novel equipment for polymer processing, professor Qu and his research team [41, 42, 43] have independently developed novel extruders without screws such as vane extruder as shown in Figure 5 [42] and eccentric rotor extruder as shown in Figure 6 [43].
\nThe schematic diagram of vane plasticizing and conveying system.
The schematic diagram of the eccentric rotor plasticizing and conveying system.
Compared with screw extruders, the rotor instead of screw was used in novel extruders and the rotor rotated eccentrically. The stator and rotor with special structures constitute continuous spatial path. The space volume between the rotor and stator periodically changes along the stator axial direction, which will make the volume of materials inside the spatial path change periodically along the axial direction, so that the materials were mainly subjected to stretch deformation. Put another way, the main flow field in such novel extruder was dominated by elongational flow field, and the materials were conveyed forward by positive displacement action.
\nThe eccentric rotor extruder has the same basic processing principle as vane extruder. Furthermore, eccentric rotor extruder has streamlined flow path, which is conducive to prevent thermal degradation. Nascent UHMWPE powder particles without any processing aids can be extruded directly by using an eccentric rotor extruder. The mechanical properties of the extrudates have almost been maintained as the unextruded samples. Since the material was conveyed by positive displacement force in the entire extrusion process, the energy consumption and extrusion output of UHMWPE were almost the same as that of HDPE. The melting of UHMWPE inside eccentric rotor extruder is a dynamic melting process because of the periodic variation of spatial path. However, the fluctuation of extrusion caused by the pulsating movement of eccentric rotor is one of the problems to be solved at present. Regardless of the current problems, the novel processing based on positive displacement delivery can significantly improve the production efficiency and quality of nascent UHMWPE.
\nThe ultra-high molecular weight of UHMWPE has led to great difficulty in processing such as poor dissolution, extremely high melt viscosity, and poor melt flowability. The improved screw equipment with special structures can process UHMWPE with molecular weight of up to several hundred g/mol, but such modified upgrade equipment still cannot process the nascent UHMWPE without plasticizer and lubricants. The novel extrusion device of eccentric rotor extruder based on pulsating movement can directly process nascent UHMWPE without using any processing aids. Since the material is conveyed by positive displacement force in the entire extrusion process, the energy consumption and extrusion output of UHMWPE are almost the same as that of HDPE, showing small dependence on molecular weight. The melting process of UHMWPE inside eccentric rotor extruder is a dynamic process because of the periodic variation of spatial path.
\nThe authors are very thankful to the Research Foundation for Talented Scholars Program of Foshan University (GG040946), Functional Polymer Materials Engineering Center Program of Foshan City (2016GA1062), and Engineering Technology Research Center Program of Educational Commission of Guangdong Province (2016GCZX008).
\nInsulin is a potent anabolic polypeptide hormone which stimulates the uptake and storage of carbohydrates, fatty acids, and amino acids into glycogen, fat, and protein, respectively [1]. The typical physiological effect of its action is hypoglycemia (reduction in blood glucose). The result of a casual or intentional overdose of insulin is a hypoglycemic coma and in extreme cases even death of the user. Today it is used not only in medicine in the treatment of diabetic patients but also in competitive sport as a common doping agent for body building [2, 3] and for different criminal purposes [4, 5, 6, 7, 8]. Suicides and homicides with insulin maybe are not so common, but are seen in the routine medicolegal and toxicological-clinical practice. The first documented case of murder by insulin is dated to the year 1957 (Kenneth Barlow case) [9]. Vincent Marks in his review has analyzed case histories of 66 people alleged or proven to have been poisoned by insulin (murders, manslaughters, attempted murders, Munchausen-by-proxy cases) [7].
Of course, some insulin overdoses are accidental and associated with incorrect dosage of the drug by the patient [10, 11]. Most of these cases are not clinically serious. It seems, however, that the risk of intentional (suicidal) insulin overdose in patients with diabetes of both types (1 and 2) is underestimated. The population-based study of suicide victims in Northern Finland performed by Löfman et al. revealed that 3.1% of all suicide victims had diabetes (34.6% type 1 and 65.4% type 2) [12]. In victims with type 1 diabetes, insulin as a suicide method covered half of the self-poisoning cases, while the proportion in type 2 diabetes was 13%. It is known that the risk of depression and attempted suicide is higher in patients with chronic diseases, including diabetes, so physicians who treat diabetic patients should evaluate co-occurring depression and substance abuse, both of which are major risk factors of suicide [13, 14].
The aim of the author is to present the current state of basic knowledge about the nonmedical use of insulin, with particular emphasis on the possibility of postmortem diagnosis. The study also highlighted the little known, rare clinical problem of insulin abuse for recreational purposes.
In order to illustrate the abovementioned problems, I present two typical cases from routine medicolegal practice of the Department of Forensic Medicine and Forensic Toxicology in Katowice, School of Medicine in Katowice, Medical University of Silesia, Poland [15, 16].
A 44-year-old nondiabetic man was found dead lying on the bed in his flat. Near the body, an ampoule and almost empty syringe were found and taken for further analysis. Two days earlier, the man had called his wife and said that he is going to commit suicide. The forensic autopsy did not reveal the cause of death. The initial stage of putrefaction, blood fluidity, acute blood stagnation (hyperemia) in the internal organs, and two supravital point wounds on the right thigh, which might have been injection sites, were found. Histopathological findings in the main internal organs were the following: brain, hyperemia with numerous petechiae, and edema; heart, adipositas, medium grade of atherosclerosis of the coronary arteries, and local fragmentation of muscle fibers; and lungs, hyperemia with local hemorrhages into alveoli and edema. Additional histochemical staining (Periodic Acid-Schiff, PAS) disclosed low amounts of glycogen in the liver (Figure 1). The standard toxicological analysis disclosed no evidence of drug abuse or alcohol, so due to the suspicion of suicide by insulin injection, a directed analysis with immunoradiometric assay (IRMA Kit Immunotech), routinely used for the in vitro determination of insulin in human serum and plasma, was conducted. It revealed a high insulin concentration level—24.42 μIU/ml in the vitreous humor (measuring range, 0.5–300 μIU/ml; the norm for serum, <22 μIU/ml)—and the presence of insulin in the material secured at the crime scene (in the syringe, 1853.91 μIU/ml). All these results (information from the prosecutor about the crime scene, results of medicolegal autopsy, results of histopathological and toxicological studies) clinched the thesis of insulin overdose.
Low amounts of glycogen in the liver—50% of control sections taken during autopsy of sudden traumatic death victims.
According to the information of the Prosecutor’s Office, a 63-year-old man was supposed to kill his wife and dog and then commit suicide. Such situation in forensic medicine is called homicide-suicide or dyadic death. In the apartment a farewell letter and empty packages after insulin, NovoMix 30 Penfill (a mixture of fast and long-acting insulin analogue), were revealed (Figure 2). External medicolegal examination and forensic autopsies carried out at the Department of Forensic Medicine and Forensic Toxicology of the Medical University of Silesia in Katowice did not explain the cause of death. However, potential injection sites on the thighs and the shoulder of woman were revealed (Figure 3). Different biological materials for additional tests—biochemical, chemical-toxicological, and histopathological and for forensic genetics—were taken. Due to the inability to quickly determine insulin level in body fluids and the site of injection using the reference chromatographic methods [17, 18, 19, 20], the determination of this hormone was ordered to two clinical diagnostic laboratories (by chemiluminometric and immunoradiometric methods). In addition, C-peptide (short 31-amino-acid polypeptide that connects insulin’s A-chain to its B-chain in the endogenous proinsulin molecule), glycated hemoglobin (HbA1c, a form of hemoglobin that is measured primarily to identify the 2- to 3-month average plasma glucose concentration), glucose, and lactate (it is known that one mole of glucose during the process of glycolysis produces two moles of lactate) were ordered. Incomplete, difficult-to-interpret results were obtained. In addition, a successful attempt of immunohistochemical (IHC) detection of insulin in samples taken from the injection sites was made (Figure 4) [21, 22]. The results of the tests carried out in the abovementioned clinical laboratories confirmed our previous experience with the low usefulness of insulin determinations in the autopsy hemolyzed blood specimens (article in press).
Empty packages after insulin, NovoMix 30 Penfill (a mixture of fast and long-acting insulin analogue), revealed in the apartment of victim. Needles can be analyzed by forensic geneticists for the presence of DNA mixture of the victim and murderer in the case of homicide-suicide death.
Numerous supravital point wounds and surrounding bruises on the thighs—potential insulin injection sites.
Positive immunohistochemical (IHC) detection of insulin in the subcutaneous tissue around needle tracts between adipocytes (right) and control section from distant area of the skin with no reaction (left).
A classic postmortem macroscopic examination of the corpses (forensic autopsy) usually does not explain the cause and mechanism of death [23, 24]. Typically a feature of acute cardiorespiratory failure and nonspecific lesions related to the age of victim (e.g., atherosclerotic changes in vessels) can be found. For this reason, additional laboratory tests are necessary in each case. In addition to routinely collected sections from internal organs and body fluids (blood and urine), it is worth to take at least the sample of vitreous humor (VH) and the samples from potential injection sites for both histopathological and directed toxicological analyses.
A detailed histological examination of all internal organs, especially of the pancreas and liver, aiming at detection of insulinoma (tumor of the pancreas that is derived from β cells and secretes insulin) and morphological symptoms of hypoglycemia, respectively, should be always performed by experienced pathologist. The content of glycogen (multibranched polysaccharide of glucose that serves as a form of main energy storage) in the liver may be evaluated by the Periodic Acid-Schiff (PAS) or Best’s Carmine staining. Its low amounts can indirectly confirm insulin overdose, as it was presented in the first case [15]. Another useful option is to perform IHC staining for the presence of insulin at the injection site. It is not necessary to buy special antibodies. These routinely used in clinical histopathology can be successfully used for this purpose, as we demonstrated in the second case [16].
In routine forensic practice, usually antemortem blood samples of the victim, who sometimes is hospitalized before the death, are unavailable for forensic toxicologists, so they can analyze only postmortem biological material taken during autopsy and nonbiological specimens revealed at the crime scene, like syringes, ampoules, vials, or remnants of the infusion solution and tubings [24, 25, 26].
What is important from the medicolegal point of view is that the interpretation of insulin levels in the postmortem biological material is difficult and still in doubt [27, 28, 29, 30, 31]. The number of published papers dealing with this problem is relatively low. The time of survival after insulin injection depends on many different factors: type of insulin (differentiated onset of action and insulin half-life), method of administration (injection or insulin infusion pump), anatomical localization of injection sites on the body (different rate of absorption), etc. [32]. It certainly influences the insulin levels detected in the postmortem biological material. Unfortunately, in the forensic practice, investigators usually do not know that time, because the cadavers not infrequently are found after a long time since death at an advanced stage of late postmortem changes, for example, when the victim lived alone or the killer committed suicide [21].
Additionally, insulin determination in postmortem blood has a low diagnostic and testimonial value, mainly because of ongoing thanatochemical processes of autolysis and putrefaction [8, 24]. The main barrier that prevents receiving correct and trustworthy results of insulin determinations in postmortem blood with radioimmunological methods is the blood hemolysis (rupturing of red blood cells and the release of their contents into surrounding plasma). This fact was confirmed in the literature and by our own studies performed in the Department of Forensic Medicine and Forensic Toxicology in Katowice [32, 33].
Fortunately, insulin crosses the blood-retinal barrier and may be identified in the VH, which is generally very valuable alternative material for many different chemical-toxicological analyses [34, 35]. The advantage of this material is that it is easy to obtain during typical forensic autopsy. Another advantage is anatomical isolation, useful especially in the case of advanced autolytic and putrefactive changes
In 2011 Thevis et al. have published the first successful mass spectrometry-based analysis of postmortem material (VH) related to an insulin poisoning case [17]. The natural levels of insulin in vitreous humor determined by the authors were below the liquid chromatography–tandem mass spectrometry (LC-MS/MS) limit of detection. LC-MS/MS is modern advanced instrumental method widely used in analytical chemistry. This was a significant advance in postmortem biochemistry. Our own experience shows that in cases where suicide by insulin poisoning is suspected, determination of its concentration in the vitreous humor and nonbiological material using the immunoradiometric assay (IRMA) gives the opportunity, similarly as the LC-MS/MS analysis, of objective confirmation of the poisoning, so both methods can be used in forensic practice [32].
In our department, we have analyzed material consisted of 93 samples of vitreous humor taken during forensic autopsies. Analysis revealed that in 86 vitreous humor samples (92.5%), the concentration of insulin, determined with IRMA, was below the limit of detection of this method (below 0.5 μIU/ml). The concentration of insulin in vitreous humor was determined only in seven cases (range of results, 1.42–24.42 μIU/ml). We have described above one of these cases, where insulin was used to commit suicide [15].
The IRMA method is known as sensitive, specific, and relatively cheap in comparison to modern methods, but it requires adequate apparatus for the measurement of radioactivity and some experience in its interpretation. It is worth knowing that the studies on insulin determination using antibody-radiolabeled antigen reaction in the late 1950s were the beginning of a new medical discipline—radioimmunology [36]. Until the introduction of radioimmunoassay (RIA), death caused by insulin overdose was extremely difficult to prove [4]. In turn, the huge advantage of modern chromatographic methods (LC-MS/MS) is the possibility of differentiation between different types of insulins (human or animal insulin and their synthetic derivatives/analogues). In 2015, Palmiere et al. have presented preliminary results of postmortem determination of insulin using chemiluminescence enzyme immunoassay (CLEIA). Their conclusion was that the analysis of vitreous humor with CLEIA may provide suitable data, similar to analysis with LC-MS/MS and immunoradiometric assay, to support the hypothesis of insulin overdose [37].
Regardless of the method used in toxicological investigation, an analytically confirmed higher level of insulin in the vitreous humor plays an important and even a decisive role in structuring the final medicolegal opinion about the cause of death. This is the reason why the vitreous humor should be routinely collected and analyzed during forensic autopsy in every case with an “insulin” background [29, 37].
An interesting observation, so far unused in the forensic practice, is an increase in the expression of certain genes stimulated by insulin, especially in hyperinsulinemic conditions. This is a potentially promising area for further research. An example might be the changes of neuropeptide Y (NPY) gene expression and its release during hypoglycemic stress. Han et al. found that subcutaneous insulin injection produced an immediate increase in plasma NPY immunoreactivity and delayed increases in adrenal and neuronal NPY mRNA and adrenal NPY immunoreactivity in rats [38]. They have concluded that these results suggest that NPY may play a role in insulin-induced hypertension. Another example can be increased vascular resistance in the equine digit and overexpression of endothelin-1 (ET-1) in the laminar tissue due to the short-term hyperinsulinemia [39].
An overdose of insulin is a potential life-threatening condition and requires urgent medical attention [40, 41, 42, 43, 44, 45, 46]. The clinical manifestations of hypoglycemia occur when the blood glucose level is less than 2.2–2.8 mmol/l (40–50 mg%). Symptomatology includes two groups of symptoms. The first one is caused by stimulation of the autonomic nervous system and includes profuse sweating, anxiety, tremor, and hunger. The second one is caused by progressive dysfunction of the central nervous system (CNS) due to neuroglycopenia and includes nausea, headache, dizziness, blurred vision, abnormal intellectual processes, behavioral disturbances, and finally loss of consciousness, convulsions, and death.
The most optimal place of the treatment is clinical toxicology ward, but patients who are overdosed with insulin can be also treated in typical intensive care units or in less serious cases—in general internal wards. To differentiate endogenous and exogenous insulin overdose, usually insulin/C-peptide [mol/mol] ratio is used, both in clinical and forensic settings [47]. Physiologically for every molecule of insulin formed, a corresponding molecule of C-peptide is formed. If the above-described ratio is >1, it indicates exogenous origin of insulin (as a result of accident, suicide, or homicide). However, it should be remembered that C-peptide is very unstable in postmortem blood [4].
Treatment of hypoglycemia is initially based on the securing of basic vital functions (breathing and circulation). Subsequently, infusions of glucose solution adjusted to the current blood glucose levels are used. Depending on the clinical situation, other drugs are administered s.c. or i.v. (e.g., glucagon which is a glycogenolysis stimulator), as it was presented in above-cited clinical emergency case reports. In the past such specific methods of treatment and management have been reported as excision of insulin injection site or the use of artificial pancreas [48, 49, 50]. Assessment of patient prognosis relies on clinical findings. According to the results of prospective study of Mégarbane et al., the observed plasma insulin EC50 (the concentration which induces a response halfway between the baseline and maximum after a specified exposure time) is 46 mIU/l [51].
Tsujimoto et al. have described rare case of rapid onset reversible glycogen storage hepatomegaly caused by suicidal administration of a massive dose of long-acting insulin glargine and subsequent supplementation with large doses of glucose in a 41-year-old type-2 diabetic patient [52]. Supravital liver biopsy revealed hepatocytic glycogen deposition with edematous degeneration. PAS staining revealed many PAS-positive granules containing glycogen. The hepatic computed tomography (CT) attenuation was 83.7 Hounsfield units (HU), being markedly higher than the splenic attenuation (49.5 HU), which indicated pathology of the liver. Such situation (initially higher level of hepatocytic glycogen deposition) must be considered not only by clinicians but also by forensic histopathologist during examination of the insulin fatal poisoning victim’s liver.
An interesting, still not fully explained phenomenon, connecting toxicology, diabetology, and psychiatry, is abuse of insulin as a psychoactive substance. Intentional abuse of insulin is quite rare, but not exceptional. Pudlo et al. described an insulin abuser—the 58-year-old patient who injected himself with overdoses of insulin or consumed considerable amounts of pure sugar to increase its dose [53]. No other reason for his insulin abuse was found than pleasure seeking. According to the patient, he felt “pleasure” after insulin. Sheehy has counted 55 cases of patients developing hypoglycemic episodes by intentional insulin injecting [54]. Sometimes people suffering from Munchausen syndrome can also apply themselves an excessive dose of the drug to cause factitious hypoglycemia and get to the hospital [7, 55]. In the case of Munchausen syndrome by proxy (per procuram), the victims may be the relatives, most often children [56].
Despite the often quite clear circumstances of death and a well-established mechanism of action of insulin and its analogues, it is difficult to analytically confirm its excessive exogenous administration in postmortem biological material [8]. There are no uniform standards of conduct in this type of cases, both at the stage of the material sampling and laboratory analysis and in the interpretation of the obtained results.
If insulin overdose is suspected, it is necessary to take the different biological material during autopsy for further testing and to cautiously interpret its results [7]. It seems necessary to immediately develop a unified international standards/algorithm of conduct, similar to those used in clinical medicine, including the determination of insulin level and other parameters of carbohydrate metabolism in the postmortem biological material, taking into account all above-described possibilities and limitations of laboratory analysis [57, 58, 59].
The author would like to thank Marcin Tomsia, MSc, PhD, for his review of the manuscript; Joanna Nowicka, MSc, PhD; and Ewa Czech, MSc, PhD, for their valuable comments during the preparation of previous articles and presentations and Czesław Chowaniec, MD, PhD, and Christian Jabłoński, MD, PhD, for creating optimal conditions for scientific work.
The author has no conflict of interest to declare.
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