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float glass process - an overview | sciencedirect topics

The mathematical description for producing nonequilibrium thickness in the float glass process is complex and the numerical solutions are produced using computer calculations (Narayanaswami 1977, 1981).

The float glass process, which was originally developed by Pilkington Brothers in 1959 (Haldimann et al., 2008), is the most common manufacturing process of flat glass sheets. More than 8085% of the global production of float glass is used in the construction industry (Glass for Europe, 2015a). In the float glass process, the ingredients (silica, lime, soda, etc.) are first blended with cullet (recycled broken glass) and then heated in a furnace to around 1600C to form molten glass. The molten glass is then fed onto the top of a molten tin bath. A flat glass ribbon of uniform thickness is produced by flowing molten glass on the tin bath under controlled heating. At the end of the tin bath, the glass is slowly cooled down, and is then fed into the annealing lehr for further controlled gradual cooling down. The thickness of the glass ribbon is controlled by changing the speed at which the glass ribbon moves into the annealing lehr. Typically, glass is cut to large sheets of 3m6m. Flat glass sheets of thickness 222mm are commercially produced from this process. Usually, glass of thickness up to 12mm is available in the market, and much thicker glass may be available on request. A schematic diagram of the production process of float glass is shown in Fig. 5.2.

Once manufactured float glass, which is also known as annealed glass, is sometimes processed further to produce tempered glass and/or laminated glass. Tempered glass is also known as toughened glass and is stronger than float glass. The laminated glass has enhanced postbreakage performances, safety on impact, improved fire resistance and special properties such as noise control. Details of the manufacturing methods and the mechanical characteristics of tempered and laminated glass are discussed in Section 5.9.

The float glass process was invented in the 1950s in response to a pressing need for an economical method to create flat glass for automotive as well as architectural applications. Existing flat glass production methods created glass with irregular surfaces; extensive grinding and polishing was needed for many applications. The float glass process involves floating a glass ribbon on a bath of molten tin and creates a smooth surface naturally. Floating is possible because the density of a typical soda-lime-silica glass (~2.3g/cm3) is much less than that of tin (~6.5g/cm3) at the process temperature. After cooling and annealing, glass sheets with uniform thicknesses in the ~125mm range and flat surfaces are produced. The float glass process is used to produce virtually all window glass as well as mirrors and other items that originate from flat glass. Since float glass is ordinarily soda-lime-silica, the reference temperatures and behavior of this glass are used in the discussion below.

Figure 3.48 shows the basic layout of the float glass line. The glass furnace is a horizontal type, as described above. For a float line, the glass furnace is typically on the order of ~150ft long by 30ft wide and holds around 1200 tons of glass. To achieve good chemical homogeneity, the glass is heated to ~15501600C in the furnace, but is then brought to about 11001200C in the forehearth. From there, the glass flows through a channel over a refractory lipstone or spout onto the tin bath. As it flows, the glass has a temperature of about 1050C and viscosity of about 1000Pas. A device, called a tweel, meters the flow of the molten glass.

There are two basic designs for the float portion of the line. In the original Pilkington design (Figure 3.49a), the channel between the forehearth and the tin bath is fairly narrow (~1m). The glass flows over the lipstone, which is not in contact with the tin bath. As the glass flows onto the tin bath, it spreads unconstrained over the surface and progresses down the tin bath. By downstream processes, the glass ribbons width and thickness are controlled. In the Pittsburgh Plate Glass (PPG) design (Figure 3.49b), the channel is as wide as the ribbon and the glass flows over a lipstone, which is in contact with the tin bath. Various methods are used to regulate the glass thickness and the production rate, as described below.

Tin is an ideal bath material because it has the right set of physical properties. Tin melts at 232C, has relatively low volatility, and does not boil until over 2000C. Molten tin is denser than molten glass and is not miscible or reactive with molten glass. The gas atmosphere is controlled so that tin does not oxidize at a fast rate. Any oxide that does form is collected in a dross container on the bath.

Regulating the flow of the glass is important at this stage, both from the entry point and the lateral flow. The glass flow onto the tin bath is regulated by a gate, called a tweel, which is located in the canal between the forehearth and spout. The glass flows down the spout or lipstone onto the tin surface. There is some pressure driving this flow through the gap of the tweel. See Example 3.14. As the glass flows onto the tin bath, the thickness of the glass sheet depends on how that flow is controlled laterally and along the length of the bath. The first step to understanding thickness control is to examine the equilibrium thickness.

A float glass plant produces 500 tons of soda-lime-silica glass a day. The design includes a 1m wide channel between the glass tank and the tin bath. (a) At what position should the tweel be set above the lipstone given that the glass melt height on the upstream side of the tweel is 15cm. (b) Find the average velocity of the flowing glass and comment on the likelihood that the flow is laminar.

a.The production rate should be converted to m3/s for easy comparison. The float glass plant runs continuously. The soda-lime-silica glass melt has a density of ~2.3g/cm3.500 tons/day5.25kg/s0.00229m3/sFigure E3.14. The pressure on the upstream side of the tweel is higher than on the downstream side due to the bath height. The pressure at a depth of 13.5cm (midway in the channel) isP=Patm+gh=Patm+(2300kg/m3)(9.8m/s2)(0.135m)=Patm+3043PaHence the pressure difference with the downstream side, which is at atmospheric pressure is 3043Pa. The volumetric flow rate beneath the tweel is therefore:Qv=H3WP12L=H3(1m)(3043Pa)12(1000Pas)(0.02m)=0.00229m3/sH=5.65cmb.The average velocity is the volumetric flow rate divided by the cross-sectional area over which flow is taking place. In this calculation, we use the volumetric flow rate from the production.v=QvWH=0.00229m3/s(1m)(0.0565m)=0.041m/s

The pressure on the upstream side of the tweel is higher than on the downstream side due to the bath height. The pressure at a depth of 13.5cm (midway in the channel) isP=Patm+gh=Patm+(2300kg/m3)(9.8m/s2)(0.135m)=Patm+3043Pa

Hence the pressure difference with the downstream side, which is at atmospheric pressure is 3043Pa. The volumetric flow rate beneath the tweel is therefore:Qv=H3WP12L=H3(1m)(3043Pa)12(1000Pas)(0.02m)=0.00229m3/sH=5.65cm

Molten glass simply poured atop molten tin adopts an equilibrium thickness that is determined by a balance of gravity and surface tension. Consider a large pool of glass on tin, such that the effects of the curvature where the glass and tin meet can be ignored. Surface tension forces exert a net force on the glass inward toward the center of the glass pool, because the sum of the interfacial tension of the glass-tin interface (~0.5mN/m) and the surface tension of the glass or glass-vapor interfacial tension (~0.35mN/m), which both act inward, is greater than the surface tension of the tin (~0.5mN/m), which acts outward. Gravity, however, results in a net force on the glass outward.

In the Figure 3.50, heq is the equilibrium film thickness; h1 and h2 are the positions of the glass surface and the interface between the glass and tin relative to the tin surface. These relative positions can be found, given that the pressure in the glass at the interface must be equal to the pressure in the tin bath at the same position.

The gravitational force per unit length is found by integrating the hydrostatic pressure (gh) with respect to position. The glass pushes outward over the entire cross-section of the glass sheet from its surface to a depth of heq, while the tin bath resists from its surface to a depth h2.

Substitution of typical values results in the 7mm equilibrium thickness. While this thickness is a useful benchmark, in practice the thickness of the glass is not determined by equilibrium, as described below.

As the floating glass ribbon traverses down the length of the tin bath, its properties change dramatically. The glass enters as a viscous liquid and exits virtually a solid at a temperature very close to its glass transition temperature. The details of how the temperature changes and the viscosity builds are complicated. On one side, the free surface of the glass is exposed the atmosphere; heat can leave this surface by radiation or convection. Cooling and heating apparatuses are stationed above the glass ribbon down the length of the bath to allow adjustment of the ribbon temperature. On the other side, the glass is in contact with the tin bath, which can absorb some of the heat and transport it away from the ribbon. The tin bath is in constant motion due to the moving glass above it as well as the thermal convection currents. Unfortunately, no simple approximations can be made to make the modeling of the heat transfer.

The thickness of the float glass sheet is adjusted by controlling flow onto the tin bath as well as by tension exerted along the length of the bath by rollers in the annealing lehr and sometimes by rollers in the bath unit itself. In the Pilkington design, the melt enters the bath and spreads out laterally to a thickness near the equilibrium value. If a sheet thicker than the equilibrium is required, then this spreading is constrained with physical barriers. If a sheet thinner than equilibrium is needed. then the glass ribbon is pulled in tension by rollers. In the PPG design, thickness is regulated by the tweel position and by tension from rollers in the lehr. The thermal profile allows the thinning deformation to take place effectively. A short distance away from the entry point, the temperature of the ribbon drops and the viscosity rises. Overhead coolers help this process. The glass viscosity is high enough so that knurled rollers contact the glass ribbon and pull it forward (and in some operations, laterally as well). Heaters are placed shortly downstream of these edge rollers to raise the temperature of the ribbon and create a deformable zone. This zone is followed by coolers that again lower the temperature and raise the viscosity. At exit from the lehr, the ribbon is virtually solid. The main deformation is due to the rollers in the lehr, which pull on the glass ribbon from the lehr to the edge rollers; extension takes place in the deformation zone. Example 3.15 considers the exit velocity of glass from the process.

Find the velocity of float glass as it exits the tin bath on a line that produces 500tons of soda-lime-silica glass a day. The flat glass produced has a thickness and width of 3mm and 4m, respectively, at room temperature. At exit, the glass is at about 600C. Assume that the average thermal expansion coefficient over the range from room temperature to 9106 C1.

As shown in Example 3.14, 500tons a day corresponds to a volumetric flow rate of 0.00229m3/s. To find the exit velocity, we need to divide this volumetric flow rate by the cross-sectional area of the glass sheet at this point in the process.

Modern flat glass for architectural applications is commonly manufactured by the float glass process, or less frequently using the older sheet process, or the rolled process. It is a sodalimesilica glass with a typical raw material composition (by weight) of silica sand (72%), soda ash (13%), limestone (10%), and dolomite (4%). Coloured glasses are produced by additions of small amounts of colouring agents such as iron (green), nickel (brown) or cobalt (blue).

Microscopical examination of glass can provide much useful information. It affords a quick means of identification of glass type through measurement of the refractive index. Glass comprises amorphous silica that appears isotropic under the optical microscope. Although relatively uniform in composition it may contain impurities and imperfections, of which the frequency, size, and sources may be determined.

Imperfections include bubbles (or seeds) that may have a number of possible sources, the most common being gas evolved during firing. Bubbles may contain crystalline materials formed during cooling of the glass that may provide clues to the origin of the bubbles. Cords are linear features within the glass that may result either from imperfectly homogenized raw materials, dissolved refractories or devitrified material. Figure 360 shows the appearance of sodalimesilica glass that exhibits bubbles and cords. Stones are solid crystalline substances occurring in glass that are regarded as defects. They are usually derived either from the batch material, refractories, or devitrification. Figure 361 shows the appearance of sodalimesilica glass that contains a devitrification stone. These may develop as the result of incomplete mixing of the molten glass constituents and/or too low a firing temperature. The stone shown in Figure 361 contains an aggregation of tridymite crystals (see 362).

In 1959, Sir Alastair Pilkington announced the development of the float glass process for making flat glass that fundamentally changed the way in which high-quality flat glass was made (Pilkington). Float glass combines many key qualities that allow its use in such a wide range of applications. These include:

As a result of these properties float glass is widely used today in many segments of our lives for high-quality windows and mirrors in residential, architectural, commercial, and automotive applications.

Since the 1980s research has allowed us to add a range of extra functionality to float glass. In particular technology has been developed that allows coatings to be put onto the glass either as the float glass is manufactured or in a batch process. As a result, a range of added functions are now available such as:

low-emissivity coatings that allow heat into a room, but when this is reradiated from black bodies within the room at longer wavelengths the coatings are designed to keep this energy within the room, thus reducing heating bills;

For many years, however, the glass industry has been trying to solve a problem which affects almost every building in the world. How do you maintain the fundamental characteristics of glass, such as optical clarity and external esthetics without constant and costly maintenance? Whether the building is for commercial or residential use, the one constant requirement is for regular cleaning to be undertaken to ensure the glass maintains its optimum appearance.

The challenge for the glass industry is increased as a result of architects finding ever more resourceful and novel uses for glass. The use of glass in atria and overhead glazing can sometimes result in complex areas, which can make maintenance more difficult.

In addition to the esthetic issues it is a well-known phenomenon that if glass is not cleaned regularly then over a period of time the glass can weather, which makes it almost impossible to restore its esthetic properties. In extreme circumstances this can lead to the glass needing replacement.

The process of cleaning windows can also lead to safety and environmental issues. Window cleaning generally involves the use of portable ladders for cleaning windows on ground, first, and second floors. Figures for accidents reported to the Health and Safety Executive (HSE) and local authorities reveal that unfortunately between two and seven window cleaners have been killed every year in Great Britain and around 2030 suffer major injuries due to falls involving ladders. From an environmental aspect window cleaning can involve the use of harsh chemicals. These are often washed off during the cleaning process and can ultimately lead to ground contamination.

Recently, self-cleaning coatings have been developed, which are designed to reduce the amount of maintenance required by working with the forces of nature to clean dirt from the glass. These coatings are based on a well-known metal oxide called titanium dioxide, which is regularly used in paints, toothpaste, and sunscreens.

The most common transparent substrate to be used is glass. The cheapest glasssoda-lime glass or windowpane glassis suitable. It exhibits, if made by the float-glass process, a very flat surface well suited to thin-film deposition. It is limited in processing temperature at 520C, or somewhat higher if suitably suspended. It is sufficiently cheap (<$10/m2), and can be bought cut and edge treated in virtually unlimited quantities. It is indeed used by the three production facilities that have recently become operative.

If higher temperature (which may lead to better quality films) is desired, the second option is borosilicate glass, which can be heated to temperatures above 600C without softening. The higher cost of this material presently prevents its industrial use. Research groups have made cells of up to 16.2% efficiency on such glass.

The material. Soda-lime glass is the glass of windows, bottles, and lightbulbs, used in vast quantities, the most common of them all. The name suggests its composition: 1317% NaO (the soda), 510% CaO (the lime), and 7075% SiO2 (the glass). It has a low melting point, is easy to blow and mold, and is cheap. It is optically clear unless impure, when it is typically green or brown. Windows today have to be flat and that was notuntil 1950easy to do; now the float-glass process, solidifying glass on a bed of liquid tin, makes plate glass cheaply and quickly.

In Chapter 7, I gave a summary account of optical glasses in general and also of the specific kind that is used to make optical waveguides, or fibres, for long-distance communication. Oxide glasses, of course, are used for many other applications as well (Boyd and Thompson 1980), and the world glass industry has kept itself on its toes by many innovations, with respect to processing and to applications, such as coated glasses for keeping rooms cool by reflecting part of the solar spectrum. Another familiar example is Pilkington's float-glass process, a British method of making glass sheet for windows and mirrors without grinding and polishing: molten glass is floated on a still bed of molten tin, and slowly cooled a process that sounds simple (it was in fact conceived by Alastair Pilkington while he was helping his wife with the washing-up) but in fact required years of painstaking development to ensure high uniformity and smoothness of the sheet.

The key innovations in turning optical waveguides (fibres) into a successful commercial product were made by R.D. Maurer in the research laboratories of the Corning Glass Company in New York State. This company was also responsible for introducing another family of products, crystalline ceramics made from glass precursors glass-ceramics. The story of this development carries many lessons for the student of MSE: It shows the importance of a resolute product champion who will spend years, not only in developing an innovation but also in forcing it through against inertia and scepticism. It also shows the vital necessity of painstaking perfecting of the process, as with float-glass. Finally, and perhaps most important, it shows the value of a carefully nurtured research community that fosters revealed talent and protects it against impatience and short-termism from other parts of the commercial enterprise. The laboratory of Corning Glass, like those of GE, Du Pont or Kodak, is an example of a long-established commercial research and development laboratory that has amply won its spurs and cannot thus be abruptly closed to improve the current year's profits.

The factors that favour successful industrial innovation have been memorably analysed by a team at the Science Policy Research Unit at Sussex University, in England (Rothwell et al. 1974). In this project (named SAPPHO) 43 pairs of attempted similar innovations one successful in each pair, one a commercial failure were critically compared, in order to derive valid generalisations. One conclusion was: The responsible individuals (i.e., technical innovator, business innovator, chief executive, and especially product champion) in the successful attempts are usually more senior and have greater authority than their counterparts who fail.

The prime technical innovator and product champion for glass-ceramics was a physical chemist, S. Donald Stookey (b. 1915; Figure 9.14), who joined the Corning Laboratory in 1940 after a chemical doctorate at MIT. He has given an account of his scientific career in an autobiography (Stookey 1985). His first assigned task was to study photosensitive glasses of several kinds, including gold-bearing ruby glass, a material known since the early 17th century. Certain forms of this glass contain gold in solution, in a colourless ionised form, but can be made deeply colored by exposure to ultraviolet light. For this to be possible, it is necessary to include in the glass composition a sensitizer that will absorb ultraviolet light efficiently and use the energy to reduce gold ions to neutral metal atoms. Stookey found cerium oxide to do that job, and created a photosensitive glass that could be colored blue, purple or ruby, according to the size of the colloidal gold crystals precipitated in the glass. Next, he had the idea of using the process he had discovered to create gold particles that would, in turn, act as heterogeneous nuclei to crystallise other species in a suitable glass composition, and found that either a lithium silicate glass or a sodium silicate glass would serve, subject to rather complex heat-treatment schedules (once to create nuclei, a second treatment to make them grow). In the second glass type, sodium fluoride crystallites were nucleated and the material became, what had long been sought at Corning, a light-nucleated opal glass, opaque where it had been illuminated, transparent elsewhere. This was trade-named FOTALITE and after a considerable period of internal debate in the company, in which Stookey took a full part, it began to be used for lighting fittings. (In the glass industry, scaling-up to make industrial products, even on an experimental basis, is extremely expensive, and much persuasion of decision-makers is needed to undertake this.) Patents began to flow in 1950.

A byproduct of these studies in heterogeneous nucleation was Stookey's discovery in 1959 of photochromic glass, material which will reversibly darken and lighten according as light is falling on it or not; the secret was a reversible formation of copper crystallites, the first reversible reaction known in a glass. This product is extensively used for sunglasses.

Stookey recounts how in 1948, the research director asked his staff to try and find a way of machining immensely complex patterns of holes in thin glass sheets a million holes in single plate were mentioned, with color television screens in mind. Stookey had an idea: he experimented with three different photosensitive glasses he had found, exposed plates to light through a patterned mask, crystallised them, and then exposed them to various familiar glass solvents. His lithium silicate glass came up trumps: all the crystallized regions dissolved completely, the unaltered glass was resistant. Photochemically machinable glass, trademarked FOTOFORM, had been invented (Stookey 1953). Figure 9.15 shows examples of objects made with this material; no other way of shaping glass in this way exists. Stookey says of this product: (It) has taken almost 30 years to become a big business in its own right; it is now used in complexly shaped structures for electronics, communications, and other industries (computers, electronic displays, electronic printers, even as decorative collectibles). Its invention also became a key event in the continuing discovery of new glass technology, proving that photochemical reactions, which precipitate mere traces (less than 100 parts per million) of gold or silver, can nucleate crystallization, which results in major changes in the chemical behavior of the glass.

In the late 1950s, a classic instance happened of accident favouring the prepared mind. Stookey was engaged in systematic etch rate studies and planned to heat-treat a specimen of FOTOFORM at 600C. The temperature controller malfunctioned and when he returned to the furnace, he found it had reached 900C. He knew the glass would melt below 700C, but instead of finding a pool of liquid glass, he found an opaque, undeformed solid plate. He lifted it out, dropped it unintentionally on a tiled floor, and the piece bounced with a clang, unbroken. He realised that the chemically machined material could be given a further heat-treatment to turn it into a strong ceramic. This became FOTOCERAM (Stookey 1961). The sequence of treatments is as follows: heating to 600C produces lithium metasilicate nucleated by silver particles, and this is differentially soluble in a liquid reagent; then, in a second treatment at 800900C, lithium disilicate and quartz are formed in the residual glass to produce a strong ceramic.

This was the starting-point for the creation of a great variety of bulk glass-ceramics, many of them by Corning, including materials for radomes (transparent to radio waves and resistant to rain erosion) and later, cookware that exploits the properties of certain crystal phases which have very small thermal expansion coefficients. Of course many other scientists, such as George Beall, were also involved in the development. Another variant is a surface coating for car windscreens that contains minute crystallites of such phases; it is applied above the softening temperature so that, on cooling, the surface is left under compression, thereby preventing Griffith cracks from initiating fracture; because the crystallites are much smaller than light wavelengths, the coating is highly transparent. As Stookey remarks in his book, glass-ceramics are made from perfectly homogeneous glass, yielding perfect reliability and uniformity of all properties after crystallisation; this is their advantage, photomachining apart, over any other ceramic or composite structure.

Stookey's reflection on a lifetime's industrial research is: An industrial researcher must bring together the many strings of a complex problem to bring it to a conclusion, to my mind a more difficult and rewarding task than that of the academic researcher who studies one variable of an artificial system.

In today's ferocious competitive environment, even highly successful materials may have to give way to new, high-technology products. Recently the chief executive of Corning Glass, which rivals Los Alamos for the most PhDs per head in the world (Anon. 2000), found it necessary to sell the consumer goods division which includes some glass-ceramics in order to focus single-mindedly on the manufacture of the world's best glass fibres for optical communications. Corning's share price has not suffered.

From the 1960s onwards, many other researchers, academic as well as industrial, built on Corning's glass-ceramic innovations. The best overview of the whole topic of glass-ceramics is by a British academic, McMillan (1964, 1970). He points out that the great French chemist Raumur discovered glass-ceramics in the middle of the 18th century: He showed that, if glass bottles were packed into a mixture of sand and gypsum and subjected to red heat for several days, they were converted into opaque, porcelain-like objects. However, Raumur could not achieve the close control needed to exploit his discovery, and there was then a gap of 200 years till Stookey and his collaborators took over. McMillan and his colleagues found that P2O5 serves as an excellent nucleating agent and patented this in 1963. Many other studies since then have cast light on heterogeneously catalysed high-temperature chemical reactions and research in this field continues actively. One interesting British attempt some 30 years ago was to turn waste slag from steel-making plant into building blocks (Slagceram), but it was not a commercial success. But at the high-value end of the market, glass-ceramics have been one of the most notable success stories of materials science and engineering.

The simultaneous approach is used mostly in mathematical programming methods, and can overcome the aforementioned issues of the sequential approach. Sequential methods alone cannot simultaneously take into account water and energy interactions with regards to investment cost in equipment, such as heat exchangers and wastewater treatment units. In most of the published articles, the simultaneous approach has been used in solving water network problems.

In the study by Ahmetovi and Kravanja (2014), for heating integration in WN, process-to-process streams were incorporated and a network comprising of nonisothermal water-using and wastewater treatment were considered. Two strategies have been proposed for the heat integration of process-to process streams. One of the strategies was to place the heat exchangers on each process-to-process stream. The other strategy provided the cooling and splitting of hot streams, and the heating and splitting of cold streams. To solve heat integrated WN problems, Ibri etal. (2014b) developed a superstructure method that has multiple splitting and mixing options with direct and indirect heat exchange. Ibri etal. (2014a) extended their earlier studies on heat-integrated water networks (HIWN) to heat-integrated water using and wastewater treatment networks (HIWTN) by including wastewater treatment units into the water networks. In this study, the aim was to determine an optimum network design of HIWTN by using the superstructure model. The presented superstructure model included freshwater heating stages, wastewater cooling stages, process and treatment units, with mixers and splitters. After the NLP/MINLP model is optimized in the first step to minimize the operating cost of the network, a solution is provided for MINLP model in the second step to minimize the total annual cost of the overall network simultaneously. The authors focused on using fixed removal ratio of contaminants for the treatment operations and fixed mass load of the contaminants for the process. Mathematical models including mass transfer models of process and wastewater treatment unit could be added in the proposed model.

While Ahmetovi etal. (2014) experimented with a single-step superstructure-based approach, a two-step strategy was presented by Ibri etal. (2014a) to synthesize HIWN while taking into account wastewater streams and their environmental constraints. Zhou and Li (2015) developed a simultaneous optimization model for nonisothermal WN, with consideration for contaminant concentrations of streams. Ibri etal. (2016) employed a compact/reduced superstructure model for the simultaneous synthesis of nonisothermal WNs and solved the problem in two stages. In addition to these applications, the superstructure has also been applied in different examples for solving single and multiple contaminant problems, including those in water-using and wastewater treatment units. In order to determine the cost of water and wastewater treatment networks, Sujak etal. (2015) developed a model that provides a dynamic cost profile that takes into consideration the required land cost for water reuse. For the simultaneous synthesis of nonisothermal water networks, the superstructure solution strategy presented by Ibri etal. (2016), consists of two steps, initialization and design. In the first step, a combined water network, simultaneous optimization and heat integration model are solved. In the second step, a combined water network and heat exchanger network are developed to minimize the total annual cost of the whole network. Dakwala etal. (2014) developed a water energy network (WEN) to minimize the energy and water consumption used in re-circulating cooling water systems with a cooling tower network and a cooler network in a float glass process. In this study, mathematical programming and graphical techniques were combined to solve the WEN problem. In addition to the studies associated with the design of water network, Npoles-Rivera etal. (2015) considered the seasonal situation of the natural water sources, increase in population, uncertainty in the precipitation regimes in their paper.

Lee etal. (2014) proposed a four stage mathematical model to overcome the deficiencies in the study of water minimization for fixed schedule and cyclic operation batch processes. The developed model has been applied in urban and industrial facilities to minimize water network consists of network inter-connections and storage tank capacity. To design the water-using networks to include two internal water mains for multiple contaminants, Zhao etal. (2014) developed a novel method that depends on concentration potential concepts. According to the design procedure, the first step for the conventional water-using network was developed by the arrangement of the processes in order of the Concentration Potentials of the Demand. Then the processes were divided into three parts, depending on the information from the conventional water network. The first part only used freshwater, the processes in the second part used the first internal water main, and the processes in three parts used the second internal water main. As a final step, the first and second water mains were formed and adjusted by the outlet streams in parts 1 and 2. Yang etal. (2014) solved a multi contaminant (total dissolved solids (TDS), total suspended solids (TSS), and organics) water network problem that covered a set of process units and a set of treatment units, sources, and sinks by using a Lagrangean-based decomposition algorithm. The effectiveness of this algorithm was demonstrated through its implementation in the metal finishing industry and in a petroleum refinery.

As a general rule, regeneration recycling or reuse of industrial wastewater minimizes the freshwater consumption and wastewater generation. To design regeneration recycling water networks, Zhao etal. (2016) developed a method where a linear programming (LP) model and the method of concentration potentials have been combined for water network design. Yan etal. (2016) developed a new method to solve simultaneous HIWNs by using the NLP model which removes the binary variables in the MINLP model. In this method, the stream roles have been identified and the existence of process matches have been improved without discrete variables. The MINLP method has been proposed by Abass and Majozi (2016), for the synthesis of the multimembrane regeneration water network, which includes an electrodialysis membrane and reverse osmos units. This method has provided direct water reuse/recycling and regeneration reuse/recycling.

It is challenging to solve HIWN synthesis problems in large-scale cases due to the nonlinear and nonconvex structure of these problems. To overcome this complication, Hong etal. (2018) offered a novel mathematical programming model with three steps, which optimizes the freshwater consumption and total annual cost. Zhao etal. (2019) developed a design method to deal with the complex structure and high costs of heat-integrated water network problems. The authors determined the concentration order of the water streams in water-using processes by calculating the value of the concentration potential of demands and allocated the sources to the demands through the concept of maximum quasi-allocation amount in the first step. Then, the design of heat exchanger network was performed by adopted a self-heating strategy. The synthesis of HIWNs is performed with nonlinear or linear models. Mostly, the formulation for heat-integrated water regeneration network (HIWRN) synthesis is carried out with a nonlinear mathematical model. Nevertheless, in the study by Kamat etal. (2019), a linear mathematical model was proposed for HIWRNs. This method was based on the transshipment model and included simultaneous and three stage sequential strategies.

To solve the simultaneous integration problems of water and energy networks, Torkfar and Avami (2016) proposed an alternative methodology. The optimum heat transfer coefficients and velocity of flows were calculated, the pressure drop in the heat exchanger and its cost were considered in the proposed methodology. The total annual costs have been minimized by using non-convex MINLP. In addition to other water-energy integration problems, the energy recovery of wastewater was also included in this study.

In water-energy integrated systems, the inclusion of wastewater treatment methods in the water allocation network leads to a more accurate optimization. Tovar-Facio etal. (2016) proposed an approach for oil refineries to minimize the cost of the wastewater system. The approach comprised of reuse, recycle, and other different technologies of wastewater treatment, the performance of these technologies, and characteristics of water streams in process units. In this article, the technological viability of the electrocoagulation method has been examined and optimal results were obtained in two case studies. In another article published by Koster and Kuhnke (2018), an Adaptive Discretization Algorithm was developed to simultaneously optimize the cost of water usage and wastewater treatment systems designs. Computation time of the proposed algorithm can be lengthy. Therefore, the proposed algorithm needs to be developed in order to reach a faster solution.

In this section, sequential and simultaneous approaches that are frequently used in solving WN problems were reviewed. In sequential approach, nonisothermal WN problems are divided into water and heat exchange networks and these networks are solved at different stages. This approach is not preferred for large scale and complex nonisothermal WN problems since optimum balance cannot be achieved at different stages. Therefore, only a few studies using this approach have been identified in the literature. Since water and energy interact with each other in industrial processes, the simultaneous approach that takes this interaction into consideration, has been more thoroughly studied with nonisothermal WN problems. In addition, this section provides detailed information about which kind of mathematical methods have been used in solving WN problems involving different constraints and objective functions.

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glass cullet - an overview | sciencedirect topics

Glass cullet is fed into a ball mill for grinding. Very fine glass powder ranging between 100 and 500 microns is mixed with a foaming agent and heated to the foaming temperature between 700 and 900C. Figure 5.19 shows the process flow diagram from the waste glass cullet to the foam glass manufacture of a typical foam glass product. The following factors affect the properties of foam glass:

Glass cullet from the crushing of post-consumer glass is readily available in urban areas. It can be added in small quantities (probably<20%) into many mixes, but its smooth surface means that it is difficult to achieve a good bond with the surface. Glass dust is a hazardous irritant, so appropriate health and safety precautions must be taken (see Section7.4.3). Residual sugars on glass may also delay hydration of Portland cement and hydraulic binders. Use of intact glass bottles is a relatively easy and effective means of putting light-passages into compacted walls and has attracted several architects although usually in Portland cement concrete rather than in compacted materials (e.g. Hundertwasser see Fig. 7.6).

Glass cullet has been used in different construction applications including cement replacement, aggregate replacement in concrete, road beds, pavement, trench fill, drainage medium, etc.; and in general use applications including abrasives, fluxes/additives, manufacturing of fiberglass insulation and foam insulation. When used as sand replacement, there is some indication that there can be a noticeable reduction in compressive strength (CCAA, 2008). This is, however, not consistently observed (Oliveira et al., 2008; Sangha et al., 2004; Limbachiya, 2009; Taha and Nounu, 2009). The main issue with waste glass sand in concrete is the risk of potential alkali-silica reaction. This risk can be effectively managed using blended cement (Du and Tan, 2013; Topu et al., 2008) containing fly ash and/or ground granulated blast furnace slag.

Scrap tire chips and crumb rubber aggregate have also been used in mortars and concretes. Rubber concrete has been recommended for applications where vibration damping or where resistance to impact or blast or where high plastic energy absorption is required. Concrete with rubber aggregate has also been recommended for applications such as trench filling and pipe bedding, low strength flowable concrete, nailing concrete and stone backing. A summary of properties of concrete containing rubber aggregate can be found in the literature (Siddique, 2008).

Hydrogen chloride quantity captured by sodium of glass cullets at 823K as a function of square root of time is shown in Fig. 1. The amount of hydrogen chloride captured as sodium chloride was proportional to square root of time for most of the region, and thus the neutralization rates were controlled by diffusion. On the other hand partial pressure of hydrogen chloride did not affect the formation of sodium chloride even though its partial pressure increased by four times.

Sodium diffusion coefficients in glass cullets calculated from fitting Eq. (10) with the profiles of sodium were 2.9 3.910-16 m2/s at 823K (see Fig. 1). Comparison of experimental results with predicted results for Na neutralized with HC1 at 823K was fairly consistent and indicated that DNa calculated would well represent the neutralization kinetics.

Due to the non-absorbent nature of the GC, Kou and Poon (2009) made an attempt to investigate the feasibility of using recycled glass in the production of self-compacting concrete (SCC), which could be placed and compacted under its own weight with little or no vibration effort. The experimental results showed that partial replacement of river sand and coarse aggregates by GC increased the slump flow, blocking ratio and air content of the SCC mixes. While the mechanical properties (compressive strength, tensile splitting strength and static modulus of elasticity) of the SCC decreased with increased recycled glass content. However, the increasing content of GC was helpful to increase the resistance to chloride ion penetration and decrease the drying shrinkage of SCC. In terms of ASR tests, the high content of GC in mortar bars caused large expansion due to the ASR of GC; however, the expansion could be effectively suppressed by the incorporation of fly ash in the concrete specimens.

Discarded cathode ray tube (CRT) waste is also a major environmental concern in Hong Kong. Ling and Poon (2012) and Zhao et al. (2013a) recycled the CRT funnel glass as a potential material for the production of heavyweight/high-density concrete. Although the inclusion of recycled CRT glass resulted in reductions in the compressive and splitting tensile strengths, it considerably improved the fresh properties and the drying shrinkage of the concrete. Another issue of concern is that the CRT glass is a hazardous waste due to its high content of lead oxide. Therefore, Ling and Poon (2012) treated the CRT glass with nitric acid to remove lead and the results showed that lead and barium leaching levels of the concrete prepared with treated CRT glass were below permissible limits. This indicates that using treated CRT glass as 100% substitution of fine aggregate for making heavyweight concrete is feasible.

When waste glass is to be used as aggregates in concrete, the resistance to fire is a concern because the glass will melt when exposed to high temperatures. As shown in earlier works (Ling et al., 2012; Ling and Poon, 2013), the replacement of natural aggregates by recycled GC decreased the residual strength of the concrete when the exposure temperature was below 600C; however, after exposure to 800C, the beneficial effect of incorporating GC in concrete on the water sorptivity and elastic modulus were shown, which was related to the transition of RG from solid to liquid at high temperature. The melted GC in the concrete may fill the internal cracks and improve the pore structure and resistance to water penetration in the concrete matrix after re-solidification when the concrete cools down to room temperature (Ling et al., 2012).

Old glass can be sorted by color and sold as glass-cullet, which is recycled into new bottle glass. The grades of glass include clear, green, or brown, often also referred to as flint, emerald, and amber, respectively. A photograph of glass cullet in each of these three grades after size reduction in a granulator is shown in Fig. 14.

As a container material, glass has many wonderful properties. It is inert, attractive, formable into complex shapes, and provides excellent gas barrier properties that are especially important to the shelf-life of carbonated beverages such as soda and beer. However, it must be manufactured with thick walls due to its fragility and thus adds substantial weight to the package. Accordingly, glass has lost much of its appeal to the packaging industry and is rapidly being replaced by lighter and more impact-resistant metals and plastic containers. One of the advantages of glass from a production standpoint is the low cost of the raw materials that go into it. However, strangely enough, this materials' cost advantage is actually a disadvantage from a recycling standpoint because the packaging material itself does not have much value after it has been used. This adds to the perception that the material is not very recyclable when in fact it is easily recyclable, but the costs to move the container to the recycling facility are high due to the fact that the shipping costs are high per container and the value per pound once delivered is very low.

Glass recovered from bottle bill or deposit systems is very clean and pure, and highly recyclable. The situation can be quite different for glass recovered from curbside programs, especially commingled collection programs where compaction and processing result in significant breakage and contamination. Contamination is even much worse for glass recovered from mixed waste streams. The greatest problems in recycling MRF and glass recovered from mixed waste processing results from the fact that ceramic materials and refractory glass are often present. Moreover, stones from dirt, which frequently find their way into recycled containers, can also be a problem. These materials do not fuse or melt in the glass furnace batch melting process and produce stones in the glass, which are inclusions or defects causing the glass to break when pressurized with carbonation. As the glass bottles have become thinner to reduce the weight of the container, the impact of these defects has become even more important. Stones can be removed from recycled glass cullet by processing the glass using a method called froth flotation, which is a mineral beneficiation technique utilized in many mining operations, but this further adds to the cost of glass recycling and makes it less financially attractive.

Recycled glass cullet is a low-melting eutectic requiring less energy to melt than the virgin raw materials that go into manufacture of new bottle glass. The value of glass is on the order of $30$50 per short ton, only half that of ferrous metals and one-twentieth that of aluminum. If the end user bottling plant is more than 50100 miles from the recycling center, this entire market value is lost to shipping and handling costs. However, if the alternative disposal site is a waste-to-energy plant, the glass contributes nothing to the combustion process, and adds to the ash disposal costs, which can be significant. So a community, when considering the addition of glass to its recycling program, should not only look at its market value, but also the alternative disposal cost that it will incur for ash disposal if its glass is not recycled.

Some of the specific glass waste materials that have found use as fine aggregate are nonrecyclable clear window glass and fluorescent bulbs with very small amounts of contaminants. Possible applications for such waste-glass concrete are bike paths, footpaths, gutters, and similar nonstructural work.

Field testing has shown that crushed and screened waste glass may be used as a sand substitute in concrete. Nearly all waste glass can be used in concrete applications, including glass unsuitable for uses such as glass bottle recycling.

Glass aggregate in concrete can be problematic because of the alkali silica reaction between the cement paste and the glass aggregate, which over time can lead to weakened concrete and decreased long-term durability. Further research is still needed before glass cullet can be used in structural concrete.

Steel is often damaged by the hot and humid climate in the region. Newly developed glass fiber reinforcing bars could mean an end to corrosion, which is often a problem in reinforced concrete structures; the glass fiber reinforcing bars made by German company Schoeck Bauteile GmbH may mean a longer life span for concrete structures, in addition to lower maintenance costs, which may be required as early as 10years after going into service.

The large fiber content and linear alignment of the fibers are achieved at the pultrusion stage, the manufacturing process that produces continuous lengths of reinforced polymer structural shapes. Helical ribs are also cut into the hardened bars to insure an optimal bond between the rebars and the surrounding concrete.

Recycled polymers have a range of uses from bridges, footpaths, and fences to even flood prevention. It will not chip or splinter and is even vandal-proof, and the environmental benefits are huge. Despite their versatility the manufacturer cannot use polyvinyl chloride or thermo-set plastics such as polyurethane in the production process.

Plastics that are often not usable by most plastic recyclers consequently end up in the waste stream. A vast amount of mixed plastic ends up in landfills. Innovative recycling technology can use plastic waste such that it outperforms the traditional alternatives of wood, steel, and concrete products.

To convert MIBA into a homogeneous glass, the residue has been typically melted at very high temperatures, sometimes using plasma technology (Brereton, 1996), and subsequently quenched (Lam etal., 2010) to induce a very rapid cooling of the material. This process is capable of converting highly heterogeneous MIBA into a homogeneous amorphous black material, with significantly improved leaching behaviour (Andreola etal., 2008; Monteiro etal., 2006) in that harmful elements become bound to the structure (Lam etal., 2010).

Despite demonstrating a high degree of material recovery and reuse, with associated volume reduction and lower landfill costs, the energy-intensive nature and associated costs of this glass production process need to be accounted for in the future development of this treatment procedure (Ecke etal., 2000). Moreover, this treatment allows stabilisation of harmful components, with negligible leachability, and thus the resulting material may be classified as non-hazardous or even as inert. This may prevent extra costs that could have otherwise arisen from additional stabilisation treatments (e.g., with Portland cement) of MIBA (Brereton, 1996). As an emerging technology, it is likely that plasma costs will decrease over time, making this process increasingly competitive relative to other treatment alternatives.

Although the vitrification of MIBA alone in glass manufacturing has been successfully tested, other materials have been incorporated (i.e., glass cullet, fly ash, feldspar) with the objective of balancing the silicon, aluminium and calcium contents in the final glass (Andreola etal., 2008). Soda lime silicate glass cullet decreases the viscosity of the melted materials, owing to the increased Na2O content (Barbieri etal., 2000b), and contributes to the amorphous fraction (Barbieri etal., 2000a). Feldspar enhances the chemical resistance of the produced glass, owing to its high alumina content (Andreola etal., 2008). The high Fe2O3 and ZnO contents of steel fly ash are beneficial in improving the crystallisation tendency and lowering the melting points and melt viscosity of the mixtures, without compromising the chemical characteristics of the resulting glass (Barbieri etal., 2000b). MIFA can also be incorporated and converted to a glass-like substance by melting it at high temperatures (above 1300C) (Siddique, 2010). The heating process is effective at destroying the organic contaminants (i.e., polychlorinated dibenzo-p-dioxins/polychlorinated dibenzofurans; PCDD/Fs) and, at the same time, heavy metals become encapsulated in the silicate matrix or separated by evaporation or differential precipitation.

Results on the physical, mechanical and durability-related properties of MIBA-based glass are presented in Table 7.3. It was found that the density of glass resulting from the vitrification process of MIBA was reasonably consistent (around 2.7g/cm3), considering that it was sourced from several studies from different incineration plants in various countries worldwide. Furthermore, the density values of MIBA-based glass products were comparable to the range of values given for other commercially available glasses of 2.9, 2.5 and 2.2g/cm3 for basalt fused cast, soda lime glass and borosilicate glass, respectively.

The thermal expansion coefficient, measuring the response (expansion and contraction) to temperature change, was higher for vitrified MIBA compared to typical values of commercially available glasses (Table 7.5), though it was close to that of soda lime silicate glass.

Various mechanical characterisation tests of glass from vitrified MIBA have revealed a decline in performance compared to its commercial counterparts (Table 7.6), in terms of fracture toughness (Andreola etal., 2008; Ferraris etal., 2001; Monteiro etal., 2006), flexural strength (Lapa etal., 2006) and direct tensile strength (Scarinci etal., 2000). Compressive strength values of vitrified wastes (mixture of MIBA and MIFA) ranged from around 57 to 70MPa (Li etal., 2003), though they increased with increasing MIBA content and clearly exceeded the reference Taiwan standards minimum compressive strength of 15MPa for recycled materials for use in construction.

For glass fibres produced using MIBA and glass cullet, with MIBA contents varying from 10% to 100%, the results of the tensile strength and modulus of elasticity were on the lower end of the commercial fibres range (Barbieri and Lancellotti, 2004). Further improvements in performance can be achieved using sizing and with the application of a protective polymeric layer (Barbieri and Lancellotti, 2004; Scarinci etal., 2000). The presence of soda lime silicate glass cullet was also beneficial for reasons of improved chemical durability and leaching, apart from slightly enhanced mechanical performance comparable to that of commercial fibres.

In terms of the Vickers hardness of MIBA-based glass, the values obtained (Table 7.7) have been reasonably consistent, varying from 5.5 to 6.2GPa, and are comparable to those of commercial glass systems.

From a durability viewpoint, glass from vitrified MIBA is capable of exhibiting abrasion resistance comparable to that of commercial glassy materials (Andreola etal., 2008), very high resistance to water and low susceptibility to alkali attack (Barbieri etal., 2000b; Monteiro etal., 2006), although lower resistance to acid attack has been observed (Barbieri etal., 2000b).

Municipal waste streams across the world generate millions of tons of glass every year. In the United States, about 12 million of tons of waste glass are generated annually, only 25% of which is recycled. Glass powder is rich in silica, and when activated with alkalis can result in the formation of sodium silicate gel. Preliminary studies have been reported on the alkali activation of glass powder/blast furnace slag, using NaOH and NaOH/Na2CO3 solutions as activating reagents (Torres et al., 2009). According to the test results, the best compressive strength value was 27.7MPa for pastes prepared with 30/70 waste glass/slag and activated with NaOH/Na2CO3. The authors also observed that the increase of the glass waste content promoted a decrease in the mechanical properties of alkali-activated pastes.

Other attempts have been made using glass cullet/clay mixtures (Carvalho et al., 2008). Optimized formulations showed an interesting mechanical strength of 20MPa, after 48h of curing at room temperature. The addition of foundry sand as an aggregate minimized shrinkage upon curing and increased the density of the specimens. In addition, the curing conditions are also decisive in determining the final characteristics of the materials. Curing in room conditions had a beneficial effect on the mechanical strength, contradicting some reported results in the literature. This was probably related to a slower and well-controlled curing process conducted at room temperature.

Idir et al. (2011) and Cyr et al. (2012) have reported the production of geopolymer from cullet glass without any additional mineral admixture. Idir et al. (2011) used glass obtained from glass bottles. The assessed parameters were the fineness of the glass, the geopolymerization temperature (20, 40 and 60C) and the nature and concentration of the activator solution (KOH, NaOH). The results showed that the cullet of soda-glass activated with KOH or NaOH had good mechanical strengths (60MPa for optimal conditions) but high fineness of glass yielded better mechanical performance. In addition, it was not necessary to use high curing temperature (60C) to obtain high performance, although the optimal curing temperature was 40C. KOH was the activating reagent which yielded the highest performance.

Cyr et al. (2012) extended the previous research, and concluded that waterglass was not necessary for the setting of geopolymers, contrarily to metakaolin-based geopolymers. The authors also demonstrated that the durability of glass cullet geopolymers is affected by water conservation, probably due to a lack of aluminum. Optimization was still needed and long-term durability tests should be carried out.

Other glass wastes have been used in geopolymer production. Tashima et al. (2013a) used a waste from glass fiber manufacturing: the vitreous calcium aluminosilicate (VCAS). The authors analyzed the influence of curing time on the microstructure and mechanical strength development of alkali-activated binders based on VCAS (see Figure18.6). Compressive strength values around 77MPa after three days of curing at 65C were obtained. A mathematical model of compressive strength development of mortars was proposed in the range 472h curing time. This mathematical model was:

Figure18.6. Compressive strength development of alkali-activated VCAS mortars. Solid circles are experimental data and solid line is fitting curve according to Eq.(18.1) (from Tashima et al., 2013a, with kind permission from Springer Science and Business Media).

In another paper, Tashima et al. (2012a) activated VCAS using NaOH and KOH solutions. The results showed that the type of cation and the concentration of the activating solution play a key role in determining changes in the microstructure of pastes. VCAS mortars had compressive strength in the range of 2077MPa when cured at 65C for three days, with higher compressive strengths obtained for NaOH compared to KOH-based systems. In addition, alkali-activated mortars based on VCAS cured at room temperature were also evaluated in a third paper (Tashima et al., 2013b). Mortars yielded 78.5 and 89.5MPa compressive strength values after 91 and 360days of curing, respectively. The microstructure of these mortars was amorphous and no crystalline phases were detected by X-ray analysis.

In a recent paper, Redden and Neithalath (2014) used a glass powder that is a by-product of industrial and highway safety glass bead manufacturing with pozzolanic properties (Schwarz and Neithalath, 2008; Schwarz et al., 2008). This is a silica-rich glass powder that can be activated using high concentrations of NaOH and high curing temperatures (50 and 75C) at 48 and 72h. However, high curing temperatures and long-term curing times adversely influenced the strength of glass powder-based binders when higher alkalinity was used in the activation process. In this case, a porous and disconnected microstructure was observed. The lack of hydrolytic stability of sodium silicate gels formed was evident because of the drastic strength loss under moisture curing conditions. Silica depolymerization in sodium silicate gels could explain this strength loss. The doping of this system with Ca and Al, by means of addition of ground granulated blast furnace slag and metakaolin, respectively, allowed a better control of the strength loss under moisture exposure.

Hao et al. (2013) analyzed the effect of solid/liquid ratio (0.41.0) on the properties of geopolymer where part of metakaolin was replaced by solar panel waste glass (040% range) using as activating solutions NaOH/waterglass mixtures. The experimental results indicated that geopolymer containing 10% solar panel waste glass at solid/liquid ratio of 1.0 had higher compressive strength at 1day (57.6MPa) and 7days (64MPa) curing time than geopolymer without solar panel waste glass. The experimental results showed that the degree of the geopolymerization is higher if the solid/liquid ratio is increased. Additionally, as the amount of solar panel waste glass increased, the reaction degree of the geopolymer decreases, resulting in a microstructure with lower density and higher porosity.

Kourti et al. (2010a, 2010b, 2011a, 2011b) have published various papers, where glass produced from DC plasma treatment of air pollution control (APC) residues was used for geopolymer production. APC residues are hazardous wastes produced from cleaning gaseous emissions at energy-from-waste (EfW) facilities processing municipal solid waste (MSW). APC residues have been blended with glass-forming additives and treated using DC plasma technology to produce a high calcium aluminosilicate glass.

Kourti et al. (2010a, 2010b) prepared geopolymers from the glass produced by the DC plasma treatment of APC residues. The effect of activating solutions with NaOH (212m)/sodium silicate (Si/Al 2.6), and with a constant solid/liquid ratio of 3.4 was assessed. The pastes were cured at room temperature. These residues of APC, due to high calcium content, could cause the formation of some amorphous calcium silicate hydrate (C-S-H) gels. Samples prepared with 6m NaOH or above yielded high compressive strengths, ranking between 80 and 110MPa after 28days and 100 and 140MPa after 92days room curing time. Density and water absorption also depended on the sodium hydroxide concentration; high NaOH concentrations increased density and result in a decrease of absorption, which was relatively low (810%).

Kourti et al. (2011a) investigated in depth the properties of geopolymers prepared with this residue, with the same previous optimal conditions (NaOH 6m). They concluded that APC glass geopolymer is a composite consisting of a binder phase and unreacted APC glass particles which act as reinforcement rather than a pure geopolymer. The binder phase was a three-dimensional geopolymeric network that contains C-S-H gel and probably Al modified C-S-H gel. The excellent mechanical properties of APC glass geopolymers (110MPa at 28-day room curing time) can be attributed to these microstructural characteristics. These geopolymers also exhibited high density (2.3g/cm3), low porosity (5.5%) and low water absorption (11%), good resistance to freeze/thaw test (2% of weight loss after 92cycles), low leaching and high acid resistance.

In a subsequent paper, Kourti et al. (2011b) compared the properties of geopolymers from glass derived from DC plasma treatment of APC residues with a geopolymer prepared, in a similar way, from metakaolin or blast furnace slag (BFS). The results showed that APC glass geopolymer exhibited significantly higher compressive strength values than metakaolin or BFS geopolymers.

Waste glass is another waste material that is produced in large quantities and is difficult to eliminate. It is known that most of the waste glass is collected, especially container glasses, remelted, and used to produce new glass. However, not all of the waste glass is suitable for the production of new glass. Therefore, it is necessary to find other applications for this solid waste, especially in the concrete industry.

Waste glass obtained from building demolition and crushed containers has been studied extensively as both a recycled aggregate in concrete and a supplementary cementing material. Kamali and Ghahremaninezhad (2015) pointed out that cementitious materials modified with microscale glass powders demonstrated better mechanical and durability properties at later ages compared with the control of concrete materials. These improvements are probably owing to the microstructure improvement caused by the pozzolanic property of glass powders.

Kou and Poon (2009) evaluated the feasibility of using recycled glass cullet as an aggregate for producing self-compacting concrete. The increased blocking ratio, workability and air content, and decreased compressive strength of concrete with increasing recycled glass content were found. At the same time, the drying shrinkage and chloride ion penetration seemed to decrease. The overall assessments of fresh and hardened properties showed that it is possible to produce self-compacting concrete with recycled glass aggregates. However, some researchers found the problems with using recycled waste glass in cement-based binders, such as the expansion and cracking due to the alkali gel from the reaction between silica in the waste glass and alkali in cement paste (Bazant et al., 2000; Ling and Poon, 2017).

There are few investigations on the use of waste glass in geopolymer base matrices. Tho-in et al. (2018) investigated the effects of 10%40% fly ash replacement by ground container glass and ground fluorescent lamp glass on the properties of geopolymer pastes. The results showed that highly fine glass powder could be used for fly ash replacement to make geopolymer pastes with compressive strengths in the range of 3448MPa. The denseness of microstructures observed using scanning electron microscopy (SEM) and characterized using mercury intrusion porosimetry (MIP) is closely related to the improved compressive strengths. The appropriate replacement levels are 10%20% of ground container glass.

Hajimohammadi et al. (2018a) reported that recycled glass can be easily ground to very fine particles, which can replace fine aggregate in lightweight geopolymer foam concrete. The surface of recycled glass particles reacts with the paste and creates stronger bonds with the geopolymer binder. These unique properties make it a suitable alternative to a fine aggregate in geopolymer foam concrete applications. In addition, Hajimohammadi et al. (2018b) found that fine glass particles help to enhance the geopolymerization reaction. Although the development of organized geopolymer gel structures is delayed, the final geopolymer gel is denser and stronger as shown in Fig. 19.9.

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alexandrian glass confirmed by hafnium isotopes | scientific reports

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Archaeological glass contains information about the movement of goods and ancient economies, yet our understanding of critical aspects of the ancient glass industry is fragmentary. During Roman times, distinct glass types produced in coastal regions of Egypt and the Levant used evaporitic soda (natron) mixed with Nile-derived sands. In the Levant, furnaces for producing colourless Roman glass by addition of manganese have been uncovered, whereas the source of the desirable antimony-decolourised Roman glass remains an enigma. In the Edict of Diocletian, this colourless glass is listed as Alexandrian referring to Egypt, but its origin has been ambiguous. Previous studies have found overlapping strontium and neodymium isotope ratios for Levantine and Egyptian glass. Here, we confirm these findings and show for the first time, based on glasses from the ancient city of Gerasa, that hafnium (Hf) isotopes are different in Egyptian and Levantine natron glasses, and that Sb Roman glass is Egyptian. Our work illustrates the value of Hf isotopes in provenancing archaeological glass. We attribute the striking difference in Hf isotopes of Egyptian versus Levantine glasses to sorting of zircons in Nile sediments during longshore drift and aeolian transport along the south-eastern Mediterranean coast leaving behind a less juvenile fraction.

The Roman glass industry underwent a massive expansion over the first century CE. At its peak it supplied not only tablewares for households across the Empire but also furnished major public buildings with many tonnes of glass for windows and mosaics1,2. The raw glass was made by fusing Egyptian evaporitic soda (natron) and sand to produce large glass slabs in tank furnaces with capacities of 820 tonnes3,4. These were broken up and distributed to glass workshops where the glass was remelted and shaped into objects for use5,6. This division of production continued until at least the ninth century, when a change from a mineral soda flux over to plant ash occurred bringing about the end of the Roman glassmaking tradition7,8.

The technological achievements of the Roman glass industry were precocious and not surpassed until the rise of the European industries in the eighteenth century. In particular, the Romans produced large quantities of an expensive and highly valued glass, described by Pliny9 as colourless or transparent, as closely as possible resembling rock crystal (Fig. 1), where the iron from the sand was oxidised from blue Fe2+ to very pale Fe3+ by the addition of antimony oxide, Sb2O310,11. In the Price Edict of Diocletian, this colourless glass is listed as Alexandrian thereby referring to Egypt12. Despite this, the production site for this so-called Sb Roman glass is unknown but several authors have suggested, on the basis of circumstantial evidence, that it was in Egypt13,14 (see Supplementary Information for details).

Strong evidence that the primary glassmaking factories melting sand and natron to glass were predominantly located along the coast of the eastern Mediterranean is provided by isotopic measurements. Strontium (Sr) isotope compositions for the majority of natron glass groups are close to that of modern seawater, indicating the incorporation of marine shell in the batch and suggesting the use of beach sand as a silica source15,16,17. With regards to neodymium (Nd) isotopes, nearly all natron glass types show a characteristic Nile-related signature reflecting the use of coastal sands along the south-eastern Mediterranean that comprise largely Nile-derived sediments transported here by longshore drift18,19. Hafnium (Hf) isotopes have not previously been applied to man-made archaeological material (see Supplementary Information). Here, we present Sr, Nd and Hf results on natron glass types and show that, unlike the Sr and Nd systems, hafnium isotopes distinguish between natron glass made in Egypt and those made in the Levant, and, in particular, place the production of Sb Roman glass in Egypt.

The modern town of Jerash, located about 50 km from modern Jordan's capital Amman (ancient Philadelphia), is the location of the ancient city of Gerasa, which belonged to the Decapolis, a group of semi-autonomous Greco-Roman city states operating under Roman protection20 (Fig. 2). The city prospered during the first millennium CE until an earthquake in 749 CE led to its demise and abandonment21,22. Samples for this study come from excavations undertaken by the Danish-German Jerash Northwest Quarter Project in highest area within the ancient walled city where our previous elemental and Sr isotope analyses of 25 glass vessel sherds showed a dominance of Apollonia-type glass from the Syro-Palestinian Coast dating to the Byzantine period along with a small early Roman glass assemblage23,24.

Map showing the locations of Gerasa (Jerash), N. Jordan, glass production sites at Apollonia and Jalame in the Levant and Wadi Natrun close to Nile Delta. The Blue Nile and Atbara (south of map) bring minerals to the delta from volcanics to the south in Ethiopia, which controls the Nd isotopic compositions of Nile sands. Hafnium isotopic compositions of Nile sands are instead controlled by zircons presumably dominated by erosion products of the ArabianNubian shield. From the delta, the Nile sands are transported by long-shore and aeolian drift along the south-eastern Mediterranean coast (black arrows). Map created by Lianna Hecht using Lightroom Classic CC/Lightroom 7.0 and Adobe Photoshop CC 2019 (20).

Our screening of a further 160 glass fragments shows the presence of a larger number of previously-established compositional groups: Mn Roman and Levantine-I glass types from Syro-Palestine as well as high TiO2 Egypt-Ib, Egypt-Ic and Foy 2.1 types from Egypt. Two additional identified types, Sb Roman and Sb-Mn Roman glass, cannot be unambiguously attributed to either Syro-Palestine or Egypt. The latter glass type, Sb-Mn Roman glass, shows characteristics of both Roman glass types because it is the result of mixing Sb Roman and Mn Roman type glasses during recycling25. On the basis of our screening, a subset of37 sherds from Gerasa that includes representatives of all identified natron glass types was chosen for Sr, Nd and Hf isotopic analysis.

Dissolution and ion exchange chromatography were performed for 20 mg fresh glass collected from the centre of the vessels to avoid exposed surface contamination. Strontium, neodymium and hafnium isotope analyses were done by Multicollector-ICPMS at AGiR platform using a DSN nebulizer. Hafnium fractions were run in 2% HNO31% HF, mass fractionation corrected for bynormalising to 179Hf/177Hf of 0.7325 and the resultsnormalised to our in-house Ames Hf standard that was adjusted to the low Hf intensity of the glass solutions (down to 20 ppb total Hf). Neodymium and strontium analyses were corrected bynormalisation to 146Nd/144Nd=0.7219 and 86Sr/88Sr=0.1194 and to the JNdi and NBS 987 standards, respectively. Well-characterized glass and basalt standards were processed and run with the samples tocharacterise reproducibility and accuracy. For major and trace elements, 1mmx1mm fresh glass fragments were mounted in epoxy, polished and analysed by electron microprobe and Laser Ablation ICPMS. See Supplementary Information for detailed description of our methods and SI Table S2 for analytical data.

Sr, Nd and Hf isotope compositions of the Gerasa glasses are presented in Fig. 3 as Egyptian groups (panel 1), Levant groups (panel 2) and recycled Roman glass (panel 3). We include Sb Roman glass with the Egyptian glass groups on the basis of our new Hf isotope data (see discussion below). Nd and Hf isotope compositions are reported using the conventional Nd(0) and Hf(0) notations that show part per 10,000 deviations from the present-day chondritic uniform reservoir (CHUR) values26 (see Fig. 3 caption and Supplementary Information for details). The 87Sr/86Sr ratios for all glass types fall within a narrow range (0.70850.7091) close to modern-day seawater27 (Fig. 3a). The only exceptions are Egypt Ib glasses with markedly lower 87Sr/86Sr ratios ( 0.7075). Likewise, Nd(0) values for all glass types overlap within analytical uncertainty (Fig. 3b), while Hf(0) for Egyptian and Levant glasses are clearly distinct with the former below and the latter above 12.2 (grey dotted line in Fig. 3c). The Hf(0) values around 13.9 for Sb Roman glasses place this type with Egyptian products and are indistinguishable from Egypt I andFoy 2.1 glasses. A critical observation from Fig. 3c is that the Hf(0) values observed for Sb-Mn Roman glass encompass the entire Egypt and Levant range (panel 3 in Fig. 3c) as would be expected for mixtures of glass from Egypt (Sb Roman) and the Levant (Mn Roman). Hf isotopes in natron glass of unknown provenance therefore fingerprint whether the glassmaking sands were from Egypt or the Levant, and place Sb Roman glass production in Egypt.

Plots illustrating (a) 87Sr/86Sr ratios, (b) Nd(0) and (c) Hf(0) values for glass types from the NW Quarter, Gerasa, N. Jordan. Hf(0) and Nd(0) are calculated using present-day CHUR values of 0.282785 and 0.51263, respectively44. Two sigma analytical precision (2) for 87Sr/86Sr is 0.000018 (SI Table S2), estimated from repeated run of SRM 987 Sr standard (n=44) and is significantly smaller than symbols. 2 for Nd and Hf are0.4 and0.5 units, respectively, estimated from repeat analysis of the JNdi Nd standard (n=37) and AU Ames Hf standard (n=25), except in cases where internal precision for individual samples was higher (SI Table S2). Samples are divided into types from Egypt (Panel 1: Foy 2.1, Egypt Ib and Ic; circle symbols), Levant (Panel 2: Mn Roman, Jalame, Apollonia; tringle symbols) as well as recycled mixtures of Sb Roman and Mn Roman glasses (Panel 3: Sb-Mn Roman glass; diamond symbols). Sb Roman glass is included with the Egyptian types based on the similarity in Hf(0). (a) 87Sr/86Sr ratios for glass types plot close to modern-day seawater (0.7092; black dotted line) except for Egypt Ib-type with markedly lower ratios. (b) Nd(0) values are between 6 and 3 for all groups and largely overlap within uncertainty. (c) Hf(0) values for Egyptian and Levant glasses are distinct with the former below and the latter above 12.2 (grey dotted line). Sb Roman glasses (grey circles in panel 1) have Hf(0)around14 indistinguishable from Egypt I andFoy 2.1 glasses. SbMn Roman glasses (panel 3) have Hf(0) values ranging from 10 to 14 consistent with their interpretation as mixtures of Egyptian and Levant glass types.

To illustrate the underlying processes responsible for the difference in the Hf isotope signatures of Egyptian and Levant glasses, we begin by considering how trace elements, 87Sr/86Sr and Nd(0) compositions of our Egyptian and the Levant type glasses from Gerasa cannot beutilise to unambiguously distinguish sand sources on the coasts of Egypt and Syro-Palestine.

The locations of the raw glass furnaces so far discovered occur mainly on the coastal strip of Syro-Palestine (e.g. Apollonia and Jalame in Fig. 2). Published evidence for primary glass furnaces in Egypt is limited, apart from those close to the ancient soda sources around the Wadi el Natrun, some 50 km northwest of Cairo4 (Fig. 2). Because of this paucity of known Egyptian production sites, and restrictions on the availability of Egyptian cultural material for analysis, attribution of glass types to Egypt is generally inferred from (1) a failure to match the elemental compositions of the well-characterised products of the Palestinian furnaces and (2) the elevated TiO2 concentrations, which are characteristic of the limited data on Egyptian sands as well as of well-provenanced Egyptian glass dating to the Islamic period28,29. However, this approach does not exclude potential sand sources in other areas of the Mediterranean where Nd isotopic compositions and Ti concentrations are broadly consistent with the inferred Egyptian glass compositions19,30. It would also fail for any glass made in Egypt using high quality sands, which had been intentionally selected to be low in iron oxides (and thus unlikely to have elevated TiO2) such as the sands used in the renowned antimony-decolourised glass.

The 87Sr/86Sr ratios just below the value for Holocene seawater observed for the Gerasa glasses conform to previous observations for natron glass and reflect the presence of present-day marine carbonates in the glassmaking recipe16,17,18 (Fig. 3a, SI Fig. S1). Slightly low radiogenic 87Sr/86Sr ratios of 0.7085 for one Mn Roman and one Sb-Mn sample are likely due to minor contamination by strontium from the Mn-ore added to decolourise the glass16,31,32,33 (Fig. 3a). Even lower 87Sr/86Sr ratios around 0.7075 for the Egypt Ib samples can be explained by relative high contributions of strontium from minor minerals in the glassmaking sands due to a low carbonate component in the glasses (as reflected by their low CaO concentrations; SI Table S1). Irrespective of these minor variations, the homogeneous 87Sr/86Sr ratios in glass types from the two regions exclude strontium isotopes as a discriminant between glass from Egypt and the Levant.

Hafnium and neodymium in natron glass are controlled by minerals in the sands used for glass production. A complication in distinguishing sands along the south-eastern Mediterranean coast is their common origin from the Nile Delta. The Nile drains large and widely different terranes producing sediments that accumulate in the Delta and from here are transported due to the Nile littoral cell by longshore drift around the south-eastern Mediterranean and, to a smaller degree, via aeolian transport to the coasts of Sinai and modern-day Israel34,35 (Fig. 2). The two major Nile tributaries, the Blue Nile and Atbara, carry mafic minerals (in particular pyroxene) high in neodymium from Tertiary basalts in the Ethiopian highlands36 (Fig. 2). The result is the slightly negative Nd(0) values observed for Nile delta and coastal sands as well as in Egyptian and Levantine glass14,16,18,19 (Fig. 3b; SI Fig. S1). Slightly higher concentrations of Nd in Egyptian natron glass (811 ppm) versus Levantine glass (58 ppm) indicate the partial loss of these mafic minerals during longshore transport37, while the Nd(0) values remain constant (SI Table S2).

Hafnium in Nile sands and thus natron glass originates from the mineral zircon that traces the detrital quartz component38. The Nile, Sinai and Red Sea follow a collision zone (the northern end of the East African orogeny) that marked the closure of east and west Gondwana and consisted of oceanic island arc volcanics with back-arc sedimentary basins, in some periods mixed with older crustal materials36. Extensive work has shown that zircons and quartz in Nile sands derive from detrital rocks that formed from the breakdown of these collision-zone terranes. The source rocks have been suggested to be the Cambrian-Ordovician sandstone covering much of North Africa35 or the Um Had Conglomerate although the latter is mainly made up of material eroded only from the Arabian-Nubian Shield39 (Fig. 2). As observed for the minerals controlling neodymium, zircon drops out of the sediments during longshore transport34, which is reflected in the Hf concentrations of 24 ppm for the Egyptian natron glass versus below 2 ppm in the Levantine glass from Gerasa (SI Table S2). An important implication of our study is therefore that the longshore transport of the Nile sediments not only leads to lower Hf concentrations in the sediments (and thus glass) along the Levantine coast, but also to changes in the Hf isotope composition. This could be due to (1) the addition of zircons of different compositions delivered by rivers which drain inland Israel or (2) a preferential deposition of larger, non-juvenile zircons during longshore transport. The first possibility can be excluded since the inland lithologies from modern Israel are dominated by carbonates, while siliciclastic sediments of Jordan drain eastwards rather than towards the Mediterranean coast40. Therefore, it appears that there is a progressive change in the Hf isotopic composition of eastern Mediterranean coastal sand due to hydraulic sorting of zircons of different ages and size. Unfortunately, Hf isotope data for bulk sands to confirm this have not been reported from the Nile Delta and Sinai-Israeli coasts. Fieldings et al.41 report values of 15 to 22 (average of 18) for 5 bulk aeolian sands from the Western Desert (WD-C samples in their Fig. 1), which match well the Hf(0) of 16 to 13 observed for Egyptian glass groups but their Nd(0) values and location suggest that they are unlikely to have supplied abundant material to the sands of the eastern Mediterranean coast.

While Hf isotope studies of bulk sands are limited, numerous studies have utilised combined UPb dating and Hf isotopes of the detrital zircon populations in Nile sands from the Egyptian and Israeli coasts to constrain the sediment source(s). These show identical Hf(0) overall systematics with a dominance of 0.561.15 Ga zircons with Hf(0) of+12 to 70 representing a mixture of juvenile and non-juvenile late Mesoproterozoic to Neoproterozoic sources, as well as small populations of ArchaeanPalaeoproterozoic and Palaeozoic zircons35,39,41. However, these studies target cores and only sometimes include analysis of rims from single, often zoned zircon grains39,41,42,43 and cannot be directly related to bulk sand compositions. Thus, analysis of bulk Nilotic sands would be required to evaluate the fractionation mechanism proposed here. For the present, we conclude that natron glass groups reflect the sorting of zircons during the longshore transport of glassmaking sands leading to a change in Hf isotope compositions along the Mediterranean coast. This feature of the coastal sands has enabled us to confirm suspicions that the famous colourless glass of ancient Rome was indeed produced in Egypt despite its low TiO2, Zr and Hf concentrations. The reason for the latter characteristics is most likely that iron-poor sands were targeted for their production and that these sands had zircons that were not yet sorted due to longshore transport (and thus were located in Egypt). Hafnium isotopes are likely to become increasingly important in tracing the products of the early glass industries, not only in Roman empire, but also elsewhere.

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The work was supported by Carlsberg Foundation, the Danish National Research Foundation under Grant DNRF119 (Centre of Excellence for Urban Network Evolutions-UrbNet), the Danish National Research Foundation under Grant 26-123/8 (Niels Bohr Professorship in Geoscience), the Deutsche Forschungsgemeinschaft; Deutscher Palstina-Verein; the EliteForsk initiative of the Danish Ministry of Higher Education and Science, and H. P. Hjerl Hansens Mindefondet for Dansk Palstina-forskning. We thank O. Neill (GeoAnalytical Lab, Washington State University) for performing the EMP analyses, and R. Andreasen and I. Sgaard for assistance during MC-ICPMS analyses and cleanlab processes.

G.H.B. conceived the isotope aspect of the project and conducted the analytical work. G.H.B. and I.F. interpreted the data and drafted the text. C.E.L. contributed to data analysis and interpretation. A.L. and R.R. direct the Danish-German Jerash Northwest Quarter Project and were in charge of the documentation of the samples, gave the overview of all glass samples from the project, initiated the selection of samples and contributed with all work on the archaeological contextualiation of the samples. All authors contributed to drafts of the manuscript and approved the final version.

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