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Agr’s Advanced Thin-wall Measurement for PET Bottles Helps Producers Get One Step Closer to Meeting Sustainability Goals

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Home New Lightweight option for the Process Pilot® blowmolder management system affords the production of even lighter, more sustainable PET bottles With increasing focus on sustainability in packaging, Agr’s new Lightweight option for the Process Pilot® blowmolder management system gives brand owners and bottle manufactures another tool to meet this complex and growing challenge. The Process Pilot system, with the Lightweight option provides assurance that the limited material available for producing a light weight PET bottle is distributed exactly where it needs to be, and at the appropriate thickness, to ensure proper performance. There are many facets to this issue and improving the sustainability footprint of a product or brand can be a complex undertaking. Most avenues to sustainability are not under the direct control of the bottle manufacturer or brand owner. One option that is within their control however, is the reduction and optimization of the amount of resin that is used to manufacture the bottles. Resin (or weight) reduction per bottle does not need to be excessive to have an impact with regards to sustainability and financial benefits particularly when factoring in the quantity of bottles produced over a given period of time. Over the years, many PET bottle manufacturers have made great progress reducing excess material and moving towards lighter, more sustainable bottles. However, as weights continue to be reduced, the role of process variation and its effect on material distribution increasingly becomes a factor in the success of the weight-reduction program. Agr’s Process Pilot blowmolder management system was developed to address this issue and offers manufacturers a valuable tool to use in their weight reduction efforts. The Process Pilot system, with Agr Pilot Profiler® measurement technology installed inside the blowmolder, provides a means for manufacturers to accurately measure material distribution on every bottle (to 0.05mm), in real time, and proactively adjust the blowmolder to maintain proper distribution, countering the effect of process variation. In the push for more sustainable bottles, weights are being reduced even further and, with that, the sidewall thickness of the bottle. In order to process these bottles effectively and control the material distribution, additional measurement accuracy is required. The new Lightweight option, incorporated into the Pilot Profiler measurement component, offered with the Process Pilot system was developed to address this need for even greater measurement accuracy and control on very light bottles. With this option, a level of control is now available with the Process Pilot system that extends the measurement range to 0.025mm, with an accuracy of +0.01mm for PET bottle sidewall material. This added functionality delivers greater distribution control on bottles with very thin sidewalls or at specific locations on other types of bottles where precise material management is critical to meet performance and quality requirements. This capability removes one of the barriers to producing usable, lighter and more sustainable bottles. Agr’s Process Pilot automated blowmolder control systems are operating on over 400 PET bottle production lines. They have proven to be a vital tool in the production of light weight bottles while improving overall bottle performance and quality. The Process Pilot system is unique in that it manages the blowmolder based on direct bottle measurements, on every bottle produced. By controlling the blowmolder based on direct feedback from bottle measurements rather than just blowmolder performance indicators, the Agr system can ensure that the final product has the desired quality and performance attributes in spite of environmental, blowmolder or material variations that can occur during the production process. Now with the Lightweight option, the process can be controlled for even the lightest bottles. The option is currently available on all new production Process Pilot systems. To achieve these capabilities on existing systems, Agr also offers an upgrade package that can be easily installed in the field.

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Real World Pressure Testing of PET Containers

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Home PURPOSE Proper pressure testing of PET containers is an essential part of a smooth filling process and favourable downstream performance of carbonated soft drinks (CSD) and other pressure products. Whether we realize it or not, all PET containers used for pressure products are being pressure tested, both as they are filled in high-speed counter-pressure filling machines and in the distribution channels as they experience varying ambient temperature conditions. Relying on the filling equipment and downstream events of a container’s life cycle to verify container performance can be very costly and have undesirable implications on brand confidence. For this reason, state-of-the-art container manufacturers have adopted pressure testing protocols that simulate all of the conditions experienced by the container during the filling process and beyond. This paper will discuss the pressurized environments that a PET carbonated beverage is subjected to and the test methods used to ensure that commercial quality containers are produced. CONTAINER FILLING The typical filling process for a PET carbonated beverage container uses a counter-pressure technique. When the empty container is presented to the filling station, it is sealed and quickly charged with CO2. The CO2 located above the carbonated product in a holding bowl as well as in the container are pressurized higher than the desired product carbonation level to prevent the dissolved CO2 in the product from coming out of solution during filling. Typical counter pressures range from 60–100 psi for cold or ambient filling conditions. Gravity is used to transfer the carbonated product from the bowl into the container, and after the filling process is complete, pressure is relieved from the container. A schematic of this technique can be seen in Figure 1.0. INITIAL PRESSURIZATION Of particular note in the filling process is the speed of initial pressurization of the PET container, by far the most important step as it relates to the ongoing performance of the container. The initial pressurization found in normal filling machines occurs in approximately 500 milliseconds, as the ambient air in the container is replaced with CO2. BRITTLE FAILURES This rapid, non-linear pressurization in PET containers can trigger brittle failures, especially in the base. Excess amorphous material that remains in the base of the container after the blowing process creates a region, with high concentrations of stress, between the oriented and amorphous material. The material in this region is brittle and can fracture easily when the container is pressurized. Many of these early failures occur well below the pressure level used in the counter-pressure filling process. Conversely, pressure testing containers with slow initial pressurization characteristics is not sufficient to identify when the blowing process is making containers that will not survive this first step of the filling process (figure 2.0). VOLUME EXPANSION A container that survives the initial rapid pressurization still may not provide acceptable performance. After the counter-pressure has been applied, the container is subjected to a pressure hold for approximately 13 seconds (figure 3.0). Understanding volume expansion behaviour of the container during this hold time provides an important data point about how the container will react throughout the commercial life cycle. A container with a weak overall structure or lower levels of material orientation may expand beyond acceptable levels, causing thinning of the wall thickness, faster loss of carbonation and a higher risk for side wall failures. To ensure that the filled container will ultimately perform for the consumer, a quality pressure testing method must include the pressure hold at a value that simulates the real-world experience of the bottle. PROCESSING HISTORY ON INHERENT MATERIAL PROPERTIES The ultimate material properties of a finished PET container are the cumulative result of multiple factors including the time and temperature profiles for heating the preform, along with the stretching and blowing profiles in the formation of the container itself. A change in any of these variables will affect many factors, including the pressure at which the container will experience an unrecoverable yield or deformation. The natural frequency and potential impact of these processing changes drive the need to regularly pressure test containers to determine how a given production run will perform under filling and down-stream conditions. PRESSURE TESTING For over 25 years, PET containers have been pressure tested with the intent of understanding how well a container will perform under real-world filling, storage, transportation, shelf-life and consumer-use conditions. When PET, as a material, is tested using a tensile tester, a stretching force is applied to determine the amount of force required to reach the yield point (where material is permanently deformed) and is continued until failure (point where the material stops stretching and breaks). With a container, this can be equated to the application of internal pressure expanding the container volume and stretching the material to the point where the PET yields, and then a continuation of pressurization to container failure (burst). Yield and burst are the two key material failure modes experienced by a PET bottle. This simple ramp approach is acceptable for use only after the 13 second hold spoken of earlier. To simulate actual conditions, a complex test is warranted that subjects the container to the same abrupt, non-linear pressure dynamic (counter-pressures) seen in the filling process, then held at actual filling pressures for the appropriate filling time, and then subjected to a continuously increasing pressure ramp to identify the container yield point and ultimate failure. Testing PET containers in this manner provides the manufacturer with the information required to understand how the containers will perform in the filling operation and throughout the commercial life cycle. An example of a testing system that provides the capabilities to simulate the complex pressure profile of the filling operation is the Agr PPT3000TM. The PPT3000 accurately represents the counter-pressure filling simulation by providing a precise pressure profile that simulates a true filling environment. This pressure profile has been dubbed the “Fill Ramp”, where the container is subjected to an abrupt, ~500 millisecond non-linear pressurization, up to the test pressure hold level (60–100psi). It is held at that test pressure for 13 seconds,

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Bringing Shelf-life Testing to the Production Line

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Home As soon as the bottle is filled and capped, the countdown begins. Single layer PET bottles, though they appear to be impermeable, are slightly porous, and over time CO2 escapes and/or O2 permeates through the material. How fast this process happens determines the “shelf-life”. In today’s fast-paced environment, it can take less than an hour from preform to case packer. Products show up on the grocer’s shelf within a few short days. Bottles that under perform with regards to shelf-life can affect a consumer’s experience, impact future sales and ultimately damage the brand image. With the trend for bottle self-manufacture by brand owners and increased emphasis on light weighting, bottle shelf-life properties are increasingly impacted by the production process. Faster production processes with lighter bottles dictate a new approach towards shelf-life management. One such approach is the M-RULE® container performance model for analyzing shelf-life in PET beverage bottles. The M-RULE model is notable because of the speed of the tests, and the reproducibility of the result, all at a significantly lower cost than traditional methods. Are all PET Bottles of the Same Design Alike? When a bottle is designed, considerable effort is put into optimizing the mechanical and aesthetic properties of the container. For a given bottle design, the shelf-life is primarily determined by the surface area and effective thickness of the package sidewall, which in turn determines the weight of that package. Because cost is a key objective, the package weight is usually the minimum needed to achieve the targeted shelf-life. In theory, if you get everything right and every bottle is produced by a uniform process, then every bottle should exhibit the same shelf-life properties. In reality, this is not the case. Variations that affect the bottle blowing process continually occur. Differences in preform moisture content and temperature, material properties, blow molder anomalies, plant environmental changes, operator experience… to name a few, all impact material distribution and affect sidewall thickness, the property that is so crucial to shelf-life performance. Why is this so critical now? In the past, variations in the blowing process were masked by heavy sidewalls and extra material. Bottles were over-engineered, and their shelf-life exceeded the minimum targets. As a result, minor variations in material distribution had no impact on product quality. Light weight bottles are the game changer. The processing window on a light weight bottle is very narrow, and the target shelf-life is achieved only in bottles with optimal material distribution. Minor deviations in material distribution and wall thickness that normally would have little impact in the past, now can result in significant production that does not meet shelf-life specifications. With the reality of variability in the process inputs, the only way to ensure consistency in shelf-life is to tightly control, monitor and continually adjust the blowing process. And, by pro-actively managing variations in material distribution and thickness, shelf-life performance can be managed as part of this process. However, even with the various process monitoring techniques in practice today, shelf-life is one aspect that is not typically incorporated into the routine process monitoring and response programs. This is because, until recently, monitoring shelf-life properties on the production floor has not been a simple matter. Traditional shelf-life testing methods can take as long as 8–24 weeks, hardly practical when timely and accurate data is necessary to make process related decisions. Furthermore, these tests require intensive laboratory preparation prior to testing, continual monitoring and attention during the test, and have limitations that can result in testing inaccuracies. Variations in bottle to bottle dosing, fill level, temperature control of the testing environment and so forth affect test results, making it difficult to predict shelf-life with confidence using these methods. “There are a lot of things you can do to compromise a CO2 test…. It is sometimes like throwing dice” claims a bottle development engineer at a major beverage producer. An Alternative to Traditional Shelf-life Testing using the M-Rule Model Container Science Inc, Atlanta GA, offers a very tangible solution to the shelf-life dilemma with its M-RULE container performance model for analyzing shelf-life in PET beverage bottles. Commercially available since 2002, the model has been validated repeatedly by brand owners, converters and technology developers. This model overcomes the variability of traditional testing by providing a means to evaluate bottles using standardized data, testing and environmental conditions, resulting in a very repeatable method. And, with results available within seconds, it overcomes the critical issue of timeliness. The M-RULE container performance model for beverages is a web based predictive tool. It operates by integrating the fundamentals of permeation with critically evaluated physical data for the materials in a given package (bottle and closure) and other pertinent data affecting the permeability of a container, such as temperature and pressure. The M-RULE model takes into account a host of parameters and bottle attributes as part of the shelf-life determination, such as surface area, material distribution (wall thickness), base design, filling conditions, storage and distribution conditions, etc. The impact of material properties such as construction of the sidewall, resin, orientation of the material, crystallinity, the modulus of the resin and scavenging activity can also be tested. The model simultaneously predicts CO2, O2, N2, and H2O permeation based on first-principles calculation of the diffusion and solubility of these gasses, along with the impact of stress, temperature, crystallinity and modulus on these parameters. For this reason, the model can accurately predict bottle performance under a wide range of conditions. Package-specific performance is determined by applying bottle parameters such as surface area, weight, base design, finish, volume and filling conditions. All calculations include the impact of the closure on package performance. Below are three examples of the model’s predictive capability vs. two different traditional test methods. When specific bottle/package details are entered into the model, a very accurate determination of shelf-life can be made. This is accomplished without the influence of many of the issues that compromise the results of traditional tests such as: Precision of initial test carbonation Test control parameters and precision over the

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A Journey into the Unknown

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Home Agr helps beverage brand owners manufacturing PET containers In many beverage plants, the decision to self-manufacture PET bottles is a journey not just into the unknown, but the unknown unknown. Agr’s Process Performance Optimization Group (PPOG) consultants help processors navigate this unfamiliar terrain. The new millennium has seen tremendous advances in PET bottle blowing technology, from block or integrated blow-fill machines to the breakthrough Process Pilot automated blowmoulder control system introduced by Agr International. At the same time, there’s been an absence of demand growth for carbonated beverages, a consequence of the increasing consumer appetite for a healthier diet as evidenced by tremendous demand growth for bottled water. Several big-name converters have consolidated, changed focus, or exited the business. Not surprisingly, the industry saw a wave of retirements among plastics engineers. All this was unfolding against the backdrop of mounting environmental concerns that prompted fillers to rethink the need to ship empty bottles hundreds of miles to their plants. The beverage industry responded with a logical solution: bring blowmoulding in-house. The numbers pencil out, and it makes sense from the sustainability perspective. Making bottles on demand at the point of filling also offers the advantages of increased flexibility and closer control. According to Paul DiZinno, Manager of Agr’s Process Performance Optimization Group, brand owners have invested in hundreds of blowmoulding lines over the past decade. The seismic shift to self-manufacturing has spread far beyond the U.S. to beverage operations around the globe. But as one major CSD processor in Germany found out, there’s a lot to learn about the blowmoulding process. Labeller trouble Opening in 2018, the German plant was designed and equipped for efficiency and productivity, with the Agr Process Pilot installed inside the 20-mould KHS blow-fill machine. Prior to installation of Agr’s Process Pilot system, container handling issues were observed on the high-speed line producing 42,000 bph. Sometimes, the bottles seemed to wobble in the labeller, as though they weren’t sitting well in the cup. Further downstream, labels would pop off as the containers were going into pallets. New to blowmoulding, plant personnel didn’t know how to track down the cause of the skewed labels. Nor did they suspect that it was the symptom of a much more significant problem. As a long-term supplier of critical measuring instruments and productivity tools to the plastic packaging industry, Agr was keenly aware of the industry shift to self-manufacturing – and its pitfalls. PET bottle making is extremely sensitive to a host of variables. Dynamics like temperature, humidity, preform composition, machine condition, or even operator skill can impact material distribution, the key factor in bottle performance. Process Pilot takes and analyses real-time measurements of the thickness of the sidewall of every single bottle, then adjusts the blowmoulder control parameters if material distribution starts trending out of spec. The result is an optimised blowing process that ensures consistent container quality and performance. PPOG supplements Agr’s Process Pilot by providing plants with fundamental process knowledge. Brand owners have discovered a shortage of knowledgeable plastics personnel in the job market. The PPOG engineers, veterans with a long history in bottle manufacturing operations, have deep expertise in the blowmoulding process. They also take a holistic view of the vast chain of interrelationships throughout the production cycle. All these elements must be coordinated to achieve sustainable improvements in stability, uniformity, and productivity. Turn down the heat The issue of the wobbling bottles came up when PPOG Process Engineer Consultant Damon Choate was in the German plant for phased commissioning of the Process Pilot. Without on-site equipment to do qualitative bottle testing, Choate sent samples to the Agr service depot in Italy for analysis. There, bottle volume expansion and maximum burst pressure data, provided by Agr’s PPT3000 Packaging Pressure Tester, revealed that the bottles were subject to frequent base stress crack failures. “Half the sample bottles burst in the base just a few seconds into the test,” Choate relates. “The ones that didn’t fail had over 40 per cent volume expansion. The resin wasn’t being distributed properly, which is why the bottles wobbled and didn’t fit in the label cup.” “Agr is well known for our ability to test volume expansion,” DiZinno observes. “We were the first to do the 13-second expansion test. This is the number-one parameter PPOG engineers look at. Even if the weights are exactly centered, we can tell whether the problem resides with the material, the process, or the design.” With the PPT results indicating room for improvement in the process, the engineers reviewed the bottle recipe, or blowmoulder settings. It was clear to them that too many oven lamps were directed to turn on during blowing. The process was running too hot, and the preform temperature was higher than necessary to produce the ideal stretch and orientation of the PET molecules. “In general, when making PET bottles, the colder you can make the process, the better,” explains Choate. “The goal in blowing is to get the very best orientation of the PET, both vertically and horizontally. This gives the best container strength.” It’s true that high heat makes the PET more pliable and easier to stretch, but all stretching is not equal, he points out. Cold forces the molecules to align better vertically and horizontally. Reducing the preform temperature specified in the recipe by a few degrees will produce better overall resin distribution and better strength and rigidity, a critical attribute for shelf life. Gas permeation through the walls and resistance to volume expansion also improve with the proper orientation of molecules in a colder blow. In all, the PPOG engineers reduced the number of lamps that turned on in the oven by 15, from 69 from the original recipe to 54 in the revised one. They also lowered the preform temperature setpoint by four degrees. With these two changes, the bottle volume expansion went down to the most desirable rate of 12 to 13 per cent, from 40 per cent prior to the engagement, “a vast improvement,” DiZinno notes. Additionally,

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Antimicrobial Packaging Technologies and Testing Emphases

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Home The antimicrobial and anticorrosive requirements for food are stricter than those of pharmaceuticals, daily chemistry and electronic products; this is because food is composed of perishable components. The common antimicrobial and anticorrosive method is to add anticorrosive agent into food, yet, the safety of this method is still under dispute. The introduction of antimicrobial package has greatly relieved the dependence on food anticorrosive agent, and has become an effective means to improve food preserving quality and reduce the amount of additives. 1. The Limitations of Anticorrosive Agent The traditional antimicrobial and anticorrosive method for food is to add anticorrosive agent inside it. However, there exist several remarkable issues for this method. Firstly, the addition of anticorrosive agent to food would influence food safety. Though some anticorrosive agent has been applied for years, the potential safety hazard has been exposed with the deep-going researches. For example, benzoic acid, which has been widely applied, has led to the reports of several accumulating toxication. Secondly, from the viewpoint of the customers, though anticorrosive agent has been widely used, the acceptance of food with such elements is inferior to those without them. Thirdly, there would be a period of time, relating to the amount of anticorrosive agent inside, for such agent to release to the food surface and bring the antimicrobial and anticorrosive functions into full play. Therefore, even if the anticorrosive agent is added inside food, there would be a high requirement for the environment. 2. Antimicrobial Package The principle of antimicrobial package is different from anticorrosive agent. The antimicrobial function is realized through adding antimicrobial agents inside or on the surface of the packaging materials. Those antimicrobial agents would scarcely permeate the antimicrobial elements into the food, and thus, the food is safer. In this way, antimicrobial package provides a way for the reduction of anticorrosive agent’s amount. The antimicrobial package can be used individually, or with anticorrosive agent(s). The antimicrobial package is not required to instantly kill hazardous microbes, but required to restrain the growth and reproduction of those microbes in the long term so as to protect the food. To achieve this aim, controlled-release technology should be applied in antimicrobial package designing, so as to release the antimicrobial agent in the proper ‘speed’ that matches with the growth kinetics. Antimicrobial agent is the core of antimicrobial packaging system. Such agent has its specific antimicrobial activity, and the suitable agent should be chosen according to the activity of the target microbe. Antimicrobial chemical elements fit for food packaging include organic acid and salt, sulphurous acid, nitrous acid, antibiotics and ethanol, etc. Those elements are categorized into three states: solid state, solute state and gaseous state. Comparing with solid and solute antimicrobial agents, gaseous antimicrobial agent has remarkable advantages. They can evaporate and permeate into the places where the non-gaseous agents can not reach. Meanwhile, gaseous antimicrobial agent is in the headspace and has no direct contact with food. It’s not easy for such antimicrobial agent to permeate into the food so that the food safety is guaranteed. The inner environment of the package is directly influenced by the antimicrobial materials and their characteristics, and thus, the antimicrobial effects would be influenced. The hydrophilic property of the antimicrobial agent is usually better than the film materials. At the same time, the pores inside the materials would be filled with antimicrobial agents. So, the adding of antimicrobial agent would lead to slight changes to materials’ mechanical and processing properties as tensile strength and burst strength, etc., as well as gas and water vapor permeability, hygroscopic property, oil resistivity and glossiness, etc. The functioning of some antimicrobial agents has close relationship with the characteristics of the packaging materials. For example, utilizing anti-oxidant to create a non-oxygen environment to limit the mildew growth and the subsequent deterioration brings high requirements for the permeability of the packaging materials. When using gaseous antimicrobial agents, the oxygen and water vapor barrier properties of packaging materials, and the permeability of gaseous antimicrobial agent itself against the packaging materials should be considered. For example, ethanol’s permeability against the packaging materials needs to be considered for gaseous ethanol antimicrobial packages, and ethanol permeability test against the packaging materials is a necessity to avoid failure of the antimicrobial packaging system. 3. Permeability Testing Demands for Antimicrobial Packages The influence of antimicrobial agent to materials relates to additive amount and type of the antimicrobial agent. Therefore, a complete and comprehensive performance testing for antimicrobial packaging material is a must, so as to avoid losses caused by the decreasing material strength. As to antimicrobial packages with gaseous antimicrobial agents, the permeability of such agent should be especially noticed. The gas permeability of flammable, explosive or poisonous gases like chlorine dioxide or ozone, etc., can be tested by differential-pressure method, a method for common gas permeability testing. However, such instruments should be customized, and structural adjustment should be made according to characteristics of the corresponding testing gases. Labthink has provided customers with several customized differential-pressure method permeability instruments for specialty gas testing. There have been great differences between the testing methods for organic gases and inorganic gases. Organic vapors, such as ethanol, may lead to swelling of the film, and subsequently, remarkable changes to the permeability. Globally, the research of this field is still at the developing stage. Now, Labthink has newly introduced PERMETM2/410 Organic Gas Transmission Rate Test System, which applies the balancing-method to test the organic gas permeability. This instrument has patent structural design, and is composed of permeability cell, organic gas generating device, timed sampling valve, separation chamber and FID (fire ionized device), etc. It’s easy to control, and it’s the most automatic organic gas permeability testing instruments in the market. Now, Labthink Lab has accomplished organic gas permeability testing against several common flexible packaging films. Those organic gases include ethanol, acetone and toluene, etc. Some of the data can be seen in Chart 1. Chart 1. Ethanol Transmission/Permeability Rate through Common Materials Material Ethanol Transmission /Permeability Rate(g/m2.24h) PC(125um) 0.21

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Influence of Plastic Packaging on Safety of Edible Oil

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Home Edible oil is a necessity in daily life, to which frequent food safety problems have occurred in recent years. From the quality of product, packaging safety to the shelf life, wave after wave of safety problems with edible oil were reported and caused the panic of the consumers, who become confused about how to choose among various edible oil products. As a special “additive” for food, packaging has a more or less impact on food safety. This article describes the impact of packaging on the safety of edible oils and how to solve those safety problems and promote the safety of edible oil. Influences of Packaging on the Safety of Edible Oil Plasticizer Plasticizers can be used to increase the softness of materials or to liquefy materials, which are also widely used in the production of plastics, rubber and inks. Phthalates plasticizers are most common plasticizers for plastic food packaging materials. Because they do not form covalent bonds when mixed with plastics, they are likely to leach and volatilize into edible oils. During long-term storage’s contacting with the packaging, the plasticizer in the edible oil continues to accumulate and after the accumulated exceed certain amount in the edible oil, it may affect human health. Moreover, the plasticizer’s harm to the human body is not an acute poisoning reaction, but a similar effect of “environmental hormones” causing the body to secrete disorders, thereby impairing the function of the organism. Such damage is occult. In order to avoid the threat of plasticizers to human health, China has issued corresponding national standards to guide the use of plasticizers. For example, in GB9685-2008, it is clearly stated that DBP and DEHP are only used in packaging for fat-free foods. And with the enhancement of public awareness of food safety and arising of the accidents caused by the plasticizers, plasticizers have become the focus of food packaging, and as a result, PVC materials that use plasticizers are gradually disappearing in the edible oil market. Barrier Property Most consumers know about the influence of plasticizers on the safety of edible oil, which will be taken into consideration by the manufacturers of edible oil when selecting packaging materials. But not many people know how the barrier property of packaging material can influence the safety of edible oil. Edible oil contains a large amount of unsaturated fatty acids, which are likely to be oxidized automatically or by photosensitive reaction and hydrolyzed during the storage process being exposed to oxygen, heat, light, moisture and metal ions, etc., and then begin to decompose to form compounds such as aldehydes, ketones, alcohols, acids, etc., which have a special odor. Oxygen is the main factor that causes deterioration of edible oil. Therefore, antioxidants are usually added to the edible oil to ensure the stability of the oil. In order to reduce or avoid the use of antioxidants, it is required to improve the oxygen barrier property of the packaging material. Barrier property refers to the barrier ability of packaging materials to pass through water vapor, oxygen, and nitrogen, etc. The high-barrier packaging material can prevent the oxygen in the air from permeating through the package, so as to avoid the contact of the edible oil with oxygen and ensure the quality and safety of the edible oil. Seal Performance In addition to carrying edible oil, the packaging also protects the edible oil. If the seal performance of the package is poor, it will not only cause the oil leakage, but also create a passage for the oxygen to enter the package. According to the data, even the edible oil in glass packaging, if the bottle is not sealed after use, the peroxide value of soybean oil can reach more than 9mmol / kg, after 6 months of storage at room temperature, while for peanut oil and sunflower blending oil, this value may reach more than 10mmol/kg after three months of storage, all exceeding the national standard of 6.0mmol/kg or 7.5mmol/kg for edible oil quality standards. If the bottle mouth is resealed after opening, the oxidation rate of the edible oil can be effectively reduced, and the peroxide value of the edible oil can be kept within the required standard range within 12 months. Therefore, the seal performance of the bottle mouth is of great significance to the hygienic safety of edible oil. Measures to take to ensure the safety of edible oil Evaporation Residue Test In addition to plasticizer, stabilizer, diluent and other additives of plastics are also liable to dissolve in oil, which may migrate from the packaging into the edible oil during storage. Evaporation residue is an indicator for detecting the mass of chemicals that may come out when food contact materials are exposed to water, acidic substances, alcohols and oils, etc. in use. The simulant materials are generally distilled water, 4% acetic acid, 20% or 65% ethanol and n-hexane. For edible oil packaging, the simulant can be n-hexane. Today, we have special testing instrument for evaporation residue, which can avoid the manual operation errors. For example, Labthink’s ERT-01 Evaporation Residue Constant Weight Tester is a professional automatic testing instrument for evaporation residue of edible oil packaging. The testing accuracy of this instrument reaches 0.3mg and the test temperature can be controlled with the range of 100~130oC so the weighing process can be performed at high temperature, which minimizes the interference to the testing accuracy in the cooling process. The tests follow the test methods described in GB13113-91: Hygienic Standard for Polyethylene Terephthalate Products Used as Food Containers and Packaging Materials, and GB5009.60-03: Method for analysis of hygienic standard of products of polyethylene, polystyrene and polypropyrene for food packaging. Pour the simulant solution into the sample as required so as to contact with the inside of the sample. After soaking for 2 hours, take 200 ml of the soaked n-hexane and pour it into the test cup. At the same time, add 200 ml of the n-hexane stock solution into the test cup for blank test. Each test cup was

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Development of Integral Package Barrier Property Testing

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Home In the past, barrier property testing was only for films, which has brought great inconvenience to end package manufacturers and users. Most raw materials they bought could make barrier property testing, but the finished packages, owing to the lack of testing techniques, would bring hidden dangers to end-product quality. The difficulty for testing lies in the varied shapes of packages. However, owing to the promotion of barrier property testing, integral package barrier property testing has made great progress with more kinds of testable packages. This article makes a detailed introduction on the development of integral package barrier property testing and relevant testing cases. 1. Introduction to Integral Package Barrier Property Testing Techniques Keeping certain shapes is the most basic characteristic for packages. Therefore, keeping the package intact is the first thing when testing. Secondly, the seal performance of testing instruments and sampling accessories should be guaranteed. Those two points are difficult to achieve for package testing, compared with film and sheet testing. 1.1 Equal Pressure Method Package Oxygen Transmission Rate Testing Techniques The testing principles of equal pressure method oxygen transmission rate for both films and packages are similar. First, the preconditioned specimen separates the transmission chamber into two separate gas flow systems. Testing gas flows in one side of the package, such as pure oxygen or mixed gas with oxygen; high pure carrier gas flows in the other side. Though the gas pressure of two sides are the same, oxygen sub-pressures are different. Therefore, under the gradient of oxygen concentration, oxygen transmits through package and is carried to the sensor by the carrier gas. The sensor will measure the oxygen quantity in the carrier gas flow precisely, so as to work out the oxygen transmission rate of the tested package. If only specimen preparation issue can be effectively resolved, various packages are testable by this method. Testing subjects can be the integral package or a part of it, including various bottles, the connecting part of bottle cup and bottle body, bottle cup, capsule, blister, tube, injection, IV bags, flexible pipe and various ball-shape packages. Besides, the contents of tested packages can be in or not, so as to provide most reliable data for package evaluation in actual application and quality change of contents. At present, ASTM F 1307 is the only testing standard for equal pressure method, and is applicable for all packages that can produce dry spaces inside. Moreover, equal pressure method oxygen transmission rate testing techniques can also be used under humid circumstances, and can further provide an environment with certain humidity in or out side the package. 1.2 Differential Pressure Method Package Gas Transmission Rate Testing Technique Keeping the package shape intact is the main difficulty for differential pressure method package gas transmission rate testing. Owing to the pressure difference between the inner and outside of the package, the tested specimen might be destroyed by pressure difference without appropriate means to keep its shape, and result in meaningless testing results, or even no testing data. At present, in the field of differential pressure method gas transmission rate testing research, Labthink has made breakthrough. At the same time, Labthink has successfully extended integral package gas transmission rate testing from oxygen alone to many common inorganic gases. However, there are not many kinds of subjects can be tested with this method. 1.3 Weighing Method Package Water Vapor Transmission Rate Testing Technique Weighing method water vapor transmission rate testing is the traditional method for package water vapor transmission rate testing; the relevant testing methods are: GB/T 6981-1986, GB/T 6982-1986 and ASTM D 3079-94. The testing process is as follows: first, put the desiccant (container is permitted) into the specimen, and seal the open place on the package wall. After preheating, put the specimen into the testing chamber with constant humidity and constant temperature for humidity and temperature test. Then, weigh the weight of the specimen at proper intervals according to the water vapor transmission performance of the package. When the transmission reaches stability, calculate the integral package water vapor transmission rate on the added weight of the specimen. However, open a mouth on the package wall is not practical, and it would always lead to operational failure and corresponding failure. Therefore, in the standards for pharmaceutical packaging materials, the desiccant is changed into distilled water or other testing solvents when using this method. Thus, there is no need to open and close the package mouth repeatedly; and the only thing needs to do is to weigh the package at certain intervals. However, the long testing periods and precision limit are the inherent shortcomings of this method. 1.4 Sensor Method Package Water Vapor Transmission Rate Testing Technique Sensor method and different pressure method package water vapor transmission rate testing techniques are similar in the testing principle: separate the transmission cell into two isolated gas flow system by the package, one side of the package flows the carrier gas (dry); and another side is in a relative humidity. Thus, a stable water vapor concentration difference exists between the two sides of the specimen (relative humidity). Under the influence of water vapor concentration difference, water vapor transmits through the package wall and is carried to the sensor. The sensor measures the water vapor content in the carrier gas accurately so as to further calculate water vapor transmission rate of the specimen. This method is applicable for bottles, pouches, capsules, blisters, IV packages, flexible pipes and other forms of packages. Now, the testing accuracy of this method is up to 0.001g/pkg·d; the testing period is only 3 to 4 days; and the testing process is completely automatic. 2. Typical Application Examples Usually, package barrier property testing is for bottles or certain parts of the bottle. However, package is not limited to bottle, pouches, flexible pipe and PVC trays also have broad applications, among which, the testing for pouches and small-sized package (e.g., blister) are more emphasized. 2.1 Pouches The space maintenance of the pouches should be taken care of when using

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Innovation, not just Appearance – Labthink’s 30 Years of Ingenuity Brings C130H Gas Permeability Tester to Market

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Home Thirty years to build a brand. Labthink was founded in 1989, and has been deeply engaged in the field of packaging physical performance testing for 30 years. It has made a lot of explorations in improving the inspection level in the industry and promoting the standardization of inspection. On the 30th anniversary, Labthink launched a commemorative innovative product, C130H Gas Permeation Test system, a high precision laboratory testing instrument based on differential pressure method, to help realize gas permeability, solubility coefficient and diffusion of thin films and sheets tests in fields of scientific research and food, pharmaceuticals, packaging materials and many others, efficiently enhance product quality control and new product R&D processes. Mr. Chen Xi, Director of Labthink Global Markets Center, said: “C130H has completely overturned the appearance and structure of Labthink’s barrier instruments in the past 30 years, brought together many key technological innovations in Labthink. We hope that through simple operation, powerful functions and comprehensive customization services, users can complete more test tasks in their working hours and obtain more reliable test results. Test has never been simpler Labthink designed a revolutionary overall structure to simplify operation and improve performance, in order to create a simple, comfortable and intelligent operation process. Based on users’ demand, C130H provides three test modes: intelligent test mode, scientific research test mode and high efficiency mode, to fit users’ needs at different levels. Intelligent test mode – Only a small number of parameters such as test temperature need to be set, one-button operation and automatic stop. Simplified parameter setting process requires less operation and offers more comfortable experience. Scientific research mode – Provides flexible and rich parameters and functional settings, users can “freely design” a variety of testing schemes. High efficiency mode – Set the test time in high efficiency mode, and the instrument will stop automatically in the preset test time. Accurate, stable and outstanding For 30 years, Labthink has been exploring for “extreme test precision”. The newly born C130H, which benefits from the continuous improvement and creative integration of cutting-edge technology, presents excellent data reproducibility and test reliability, and represents a significant progress in the accuracy of current differential pressure gas permeation test. Because of the complex and uncertain factors such as temperature and pressure, the differential pressure gas permeation testing instrument requires extremely stable and precise control technology. To this end, Labthink has made many innovative designs, such as: Using imported sensors with higher accuracy – excellent sensitivity and analysis rate, the ultra-high barrier material with 0.01-0.09 cm3/m2* 24h*0.1 MPa can be accurately measured, showing unprecedented test repeatability. Unique temperature control technique – A unique technology based on thermodynamics and hydromechanics is adopted to make the constant and uniform temperature air flow circulate in test chambers. The temperature fluctuation in the test chambers is controlled below 0.05 after rigorous test verification. Wide range pressure setting – support flexible pressure setting of high pressure chamber in 10KPa~210KPa range, accurate pressure sustaining of system. Full automatic precise pressure compensation technology – during the test process the pressure is compensated automatically for high pressure chamber to achieve constant pressure difference between high and low pressure chamber. The test results show that the pressure change is controlled within 0.2KPa. Test Temperature and Pressure Calibration Port – Provide Fast and Convenient Verification of Temperature and Pressure Accuracy. Real-time display of test curves – including pressure-time curve, transmission rate-time curve, temperature-time curve, to facilitate users to fully grasp the test situation, and temperature and pressure fluctuations. Imported pneumatic control system – upgraded reliability, with ultra-low failure rate and ultra-long service life, excellent air tightness, eliminates unstable factors of manual operation. “C130H shows the proved accuracy and stability in the permeability test of medium and low barrier materials, and its performance in the test of high barrier materials is even more surprising. This innovative gas permeability test scheme provides accurate data for inspectors, helps them to make more intelligent improvements or quality control programs. Focusing on best efficiency Accuracy and efficiency achieve high test throughput and reduce laboratory operating costs. Labthink knows this well. Therefore, in the industrial design of this instrument, “high efficiency” runs through the whole process of optimizing the structure, components and system. The innovative three-chamber design enables the system to measure three or even more sample in one test. Upgraded automation technology and vacuum pumping technology can optimize the efficiency while minimizing the complexity of operation. When using C130H for gas permeability testing, the test time is greatly shortened. “Taking vacuuming time into account, the test of medium and low barrier materials can be completed in 4 hours, and the test time of high barrier materials can be controlled in 8 hours.” Labthink R&D Engineer said. More functions for various user needs Based on technological innovation, Labthink has always been committed to the research and development of personalized customization functions. User needs and suggestions are the core driving force of Labthink’s continuous innovation and the reasons of Labthink‘s industrial foresight. At present, C130H provides users with the following mature technology applications. Beside, Labthink will do its best to meet the specific requirements of users. Hazardous Gas Permeability Testing Technology – Through special customization, to achieve the permeability testing of toxic, harmful, flammable and explosive dangerous gases. Data Curve Fitting in Permeation (DCFP) – Obtain gas permeability, permeability coefficient, diffusion coefficient and solubility coefficient of materials at non-standards temperature in a simple, convenient and economical way. Test Gas Humidification Technology – Supports test gas testing with different humidity, automatic and precise control, without manual intervention. Software System Required by GMP – Customize the Software System that meets the data traceability requirements of GMP in China to meet the needs of the pharmaceutical industry. Data ShieldTM System – secure and reliable data centralized management facilitates convenient connection with information systems, and can be shared by multiple Labthink products. C130H is designed based on GB, ISO, ASTM and other national and international standards. It meets the system requirements of differential pressure test standards, adopts the integration of instrument and software and automatic design. Reliable unattended operation facilitates different levels

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Why the Permeability Rate of a Polymer Material is Dependent Upon a Variety of Factors

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Home The role of your plastic packaging materials is to protect and preserve the quality of your food product from production to end-of-use. In the process of designing your packaging, choosing the right polymer material for your product and package is vital to its success. The barrier properties of your packaging material must be considered, along with the components of your food, the interactions between the material and its environment and its permeability to various gases or vapors. Oxygen transmission rate (OTR), water vapor transmission rate (WVTR) and sometimes carbon dioxide transmission rate (CO2TR) are most common tests for evaluating the permeability of food packaging materials. It is essential to test the material’s transmission rates for each of these gases individually and never assume that your material has the same level of transmission rate for every gas, as Polymer materials behave differently to certain gasses. Likewise, different gasses behave differently to the same material. This article will explain this is in further detail to hopefully help you make the best decisions when selecting new materials for your food or beverage packaging. Oxygen (O2) is abundant in the environment. For most food products, oxygen is destructive and will cause oxidative deterioration of the food and encourage aerobic micro-organism growth. Hence the packaging material should be a good oxygen barrier so that you can meet your desired shelf life (or even improve it) while maintaining the high quality of the food. Moisture ingress or egress is also important factors to many food products due to the fact that the foods physical and chemical deterioration’s are related to the moisture content within the package. Therefore, it is also vital to evaluate the Water vapor transmission rate (WVTR) of the packaging material. CO2 is needed to control aerobic bacteria and mold growth, this is particularly important with food related applications. CO2 is often combined with N2 and used in Modified Atmosphere Packaging (MAP) systems to help avoid food degradation and extend shelf life. It’s also critical to access the CO2 permeability of a bottle used in carbonated drink applications to halt any loss of CO2 while on the shelf, keeping it fully carbonated until consumed. Although it may be difficult to find a mono-layer polymer material that will serve as a good barrier for all these gases remember it is possible and that there is no such thing as the perfect package. You just need to be sure that it can withstand the packaging, handling and shipping process while also maintaining the integrity of the product by properly protecting it from various gases/vapors and environments. This is where testing plays an important role in helping you choosing the right material for your package application. For example, HDPE has the following permeation rates (relative values are shown) to the following gases: HDPE Permeation Rates by Gas Polymer Oxygen Nitrogen Carbon Dioxide HDPE 73 17 580 High Density Polyethylene (HDPE) is a rigid, tough and strong resin of natural milky color. HDPE has very good stress crack resistance as well as high impact and melt strength. HDPE is appropriate for personal care, beverages, food and chemicals. It lends itself particularly well to blow molding. When HDPE is compared with PET, their permeation rates (relative values) to oxygen are also different. Polymer Oxygen HDPE 73 PET 2.3 Note: Data source: Permeability Properties of Plastics and Elastomers, 2nd Edition, L. Massey. Now that we have the basics down let’s dive deeper into what makes a polymer behave so differently to specific gases/vapors. The phenomenon we see here is related to permeation theory, the chemical and physical natures of the polymer and the permeants, as well as the interaction between the polymer and the permeant. Permeation Theory: P = S X D Permeability From permeation theory, we know that P = S x D. It means that permeability (P) is directly related to diffusivity (D) and solubility (S) of a polymer material. Here S is the solubility of a polymer material that related to “like dissolves like”. “Like dissolves like” is an expression used by chemists to remember how chemical substances tend to dissolve in solvents of similar structure. It refers to “polar” and “nonpolar” solvents and solutes. Basic example: Water is polar. Oil is non-polar. Water will not dissolve oil. When talking about gas and polymer, water is polar, so it would dissolve more into polymers that are polar such as PET, Nylon and such. While O2 is non-polar, it would dissolve into non-polar polymers such as PE, PP and most polyolefins. Therefore, usually WVTR is higher for PET, EVOH, Nylon and alike, but OTR will be higher for polyolefins such as PP, PE, etc. On the other hand, D is the diffusivity that is related to the permeant molecule’s size and how fast it moves. Smaller molecules such as Hydrogen and Helium usually move much faster than H2O and O2. Hence, gases with smaller molecules will have higher transmission rate. Permeation Affected by Environment Factors Temperature plays a major role in the permeation rate of a material. The higher the temperature, the higher the permeation. As a Rule of Thumb, every 10°C increase in temperature, the transmission rate doubles, or every 1°C increase, the transmission rate increases 5-7%. The relative humidity (RH) in the environment can impact polymer differently. RH can greatly affect permeation for hydrophilic materials. Proper RH generation and measurement are necessary for accurate permeation results. Permeation Affected by Partial Pressure Differential of Permeant Gas The driving force for permeation is the partial pressure differential of a permeant gas. An example is CO2 permeates out from a bottle of carbonated soft drink after 4atm of CO2 is filled inside the bottle to start with. The permeation is proportional to this driving force. For example, if a film’s OTR is 5 cc/(m^2·day) when the driving force is 21% oxygen (room air), its OTR becomes 23.8 cc/(m^2·day) when the driving force is 100% oxygen. Other Factors There are other factors (Cooksey, K.) would influence the transmission rates for different gases.

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Labthink Introduces Cutting-Edge C406H: A Revolutionary Combination OTR and WVTR Tester

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Home Labthink’s C406H combines OTR and WVTR testing capabilities in a single instrument, we are empowering manufacturers to gain a deeper understanding of their materials’ barrier performance, ultimately enhancing product quality and reliability.” Medford, MA USA, 27th November 2023 – Labthink, a global leader in testing and analysis instrumentation, is proud to announce the launch of its latest innovation, the C406H Combination OTR (Oxygen Transmission Rate) and WVTR (Water Vapor Transmission Rate) Tester. This state-of-the-art testing equipment represents a significant advancement in the field of permeation testing, offering unparalleled accuracy, efficiency, and versatility. The Labthink C406H is designed to meet the evolving needs of industries such as food and beverage packaging, pharmaceuticals, electronics, and materials research. By seamlessly integrating both OTR and WVTR testing capabilities into a single platform, this tester streamlines the permeation testing process, allowing for the measurement of oxygen and water vapor transmission rates within one dual-purpose instrument. This comprehensive approach enables manufacturers to gain a holistic understanding of their materials’ barrier properties, ensuring the production of high-quality and durable products. Key Features of the Labthink C406H Combination Tester : • Dual Testing Capabilities: The C406H allows users to conduct OTR and WVTR tests independently or sequentially, providing flexibility in experimental design and a more comprehensive analysis of barrier performance. • Advanced Sensor Technology: Equipped with cutting-edge sensors, the C406H ensures precise and reliable measurement of transmission rates, even for ultra-thin or highly permeable materials. • User-Friendly Interface: The intuitive and user-friendly interface of the tester simplifies operation and data interpretation, making it accessible to both seasoned professionals and those new to permeation testing. • High Throughput: With its efficient design, the C406H enables high throughput testing, allowing manufacturers to optimize their production processes and bring products to market faster. • Compliance with International Standards: The C406H meets and exceeds international testing standards, ensuring that results are accurate, reproducible, and in compliance with industry regulations. Craig Primiani, Labthink International CEO, stated, “The C406H is a testament to Labthink’s commitment to innovation and excellence. By combining OTR and WVTR testing capabilities in a single instrument, we are empowering manufacturers to gain a deeper understanding of their materials’ barrier performance, ultimately enhancing product quality and reliability.” The Labthink C406H is now available for purchase. For more information, please visit www.flexitest.in

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