Thermally Protective Packaging Five Essentials of Gel Refrigerant Design and Specification Anthony Alleva, Manager Technical Services

TCP Reliable, Inc. and Karen K. Greene, CPP Vice President Sales and Technology Life Packaging Technology LLC www.lifepackagingtechnology.com
Introduction: Temperature controlled packaging is used throughout many industries to protect temperature sensitive products. These are products especially sensitive to fluctuations in temperature. The industries utilizing temperature sensitive packaging range from highly engineered biotechnology products to gourmet cakes and fish. Designing temperature sensitive packaging requires a level of analysis as detailed as any other type of shipping package. What are the design requirements of the product/device/item being shipped, where is it going and what are the anticipated hazards that can render your product at the minimum, unfit to eat and at the extreme, a compromised biotechnology product, combination drug/device or pharmaceutical which can no longer guarantee the safety and efficacy of the medical product for the patient. The temperature controlled packaging industry has developed some very effective thermally insulative designs utilizing several forms of insulated containers and refrigerant packs. This report will focus on five essentials of gel refrigerant design and specification vital to optimizing thermal protection for your temperature sensitive product while achieving this in a timely and cost effective manner. The refrigerant pack or gel pack is used to power your insulated shipping container to maintain a thermal environment sufficient to meet the products temperature requirements. A few thermodynamic concepts are involved here: heat transfer, heat absorption and phase change. These principles are some of the components of the zeroth law of thermodynamics, commonly known as thermal equilibrium. That is, all systems attempt to reach a state in which heat energy is equally distributed. If an object with a higher temperature comes in contact with a lower temperature object, it will transfer heat to the lower temperature object.

The objects will approach the same temperature and then maintain a single constant temperature. Therefore, your product is maintained at its stable temperature range by attaining thermal equilibrium with your gel pack for some pre-determined period of time. Water is a common material used in refrigerant packs as it is relatively cheap and ubiquitous. We know that if we use a water-based refrigerant pack that we can begin to achieve cold temperatures by freezing the water based refrigerant pack. Water freezes or goes from a liquid to solid at 0 C / 32 F. The change from a liquid to a solid (change in the state of matter) is called a phase change. Water has a relatively high level of heat capacity as it goes through its freezing and thawing process and can be relied upon to maintain that 0 C temperature for long periods of time. Unfortunately introducing water into a protective shipping package means that the design must also protect the product from the new hazards represented by the water. To decrease the potential of product damage caused by water escaping from a damaged container the common approach is to mix additives with the water to cause gelling or an increase in viscosity. The higher viscosity contents of the refrigerant pack will allow the pack to keep its shape longer and not leak from a damaged container as easily. The fact that water gel will maintain 0 C can also be a problem in that for many temperature sensitive goods they also have a requirement of Do Not Freeze. Protecting them with a refrigerant that by its nature promotes freezing can result in damage to the product material. The two ways in which this is usually accomplished is to design the shipping package to buffer the contents from the gel pack so that there is a resultant temperature offset and the product material stays above 0 C. Another solution is to completely replace the water gel with another material that has a freeze/thaw phase change temperature that matches the products stable temperature range. Design of custom phase change materials is a topic in and of itself and will not be explored in the context of this paper. The focus of this paper is the properties of the more commonly used water based gel pack and the derived benefits to your products thermal protection requirements. These benefits include optimized engineering of your refrigerant packs for the greatest consistency in thermal protection for the maximum time (phase change) period of distribution and shipping, while minimizing development time and total package cost. Several laboratory studies were designed, developed and executed at TCP Reliable, Edison, NJ to illustrate the importance of specific design inputs when designing and specifying a gel refrigerant Essential #1: Geometry, Weight and Thermal Protection

An experiment was conducted to collect temperature mapping data from different size and geometry gel packs during a freeze/thaw cycle for a water filled gel pack. The objective of the study was to illustrate that a frozen gel pack is not a homogeneous temperature block as it moves through a typical freeze/thaw cycle that it might encounter during real world distribution and shipping.

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The gel packs were placed lying down in an environmental chamber and five thermocouple temperature probes were inserted into them to form a diagonal pattern to measure the thermal penetration across the gel pack. The probes were located at the opposite corners of the gel pack and the center with additional probes located at the intermediate distance between the corner and the center forming a straight line across the entire gel pack. The study summarized below did illustrate that the geometry and mass of the gel pack did not influence this freeze/thaw temperature progression pattern. Each gel showed a progression of the thermal penetration moving from the opposite corner through the intermediate probe to the center probe which consistently showed the longest time to complete its phase change. Looking only at the center probes and comparing the 2lb gel packs that were square vs. rectangular shows that the square gel takes longer to freeze/thaw completely and consequently remains longer at the phase change temperature than the rectangular gel owing to the difference in the distance(gel pack thickness) that the thermal penetration has to cover in order to complete the phase change. The phase change elapsed time difference, illustrated by the mapping across the gel, is significant. This effect of gel package geometry on the phase change time should be considered when designing shipper container packaging around these sorts of refrigerant packs. The following table summarizes the highlights of the study inputs: Gel Pack Size Thermocouple Detail Freeze/Thaw Cycle Time Duration at Phase Change Temp(0 C)

Group A = Geometric Equivalence Square, Mass difference 6 X 61 lb.

8 X 8---2 lb.

Ea. TC probe into the gel pack. 5 locations2 corners, geometric middle, midpoint between middle and corners. Ea. TC probe into the gel pack. 5 locations2 corners, geometric middle, midpoint between middle and corners.

(+) 20 C (-) 20 C. (+) 25 C (-) 25 C.

4.2 hours

5.3 hours

Group B = Mass Equivalence 2.0 lbs., geometric difference 6 X 122 lbs. 8 X 82 lbs.

Ea. TC probe into the gel pack. 5 locations2 corners Ea. TC probe into the gel pack. 5 locations2 corners
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(+) 20 C (-) 20 C. (+) 25 C (-) 25 C.

3.8 hours 5.3 hours

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Essential #2:

Package Design and Freeze/Thaw Time

The selection of an insulative shipper design is a key component of your final temperature controlled package. The answer to your question, how long will my thermal protection last can be answered by selecting the appropriate phase change material (when the gel pack is frozen at what temperature does it remain in a frozen state) and designing/selecting an insulative shipper. Our experiment included the use of an 8 X 8 gel pack (phasing at 0 C), 2.0 lbs. One (1) gel pack was placed into the center of the bottom of the shipper, with thermocouple probe inserted into the geometric center of the gel pack. The shipper designs were at room temperature and then placed into a (-) 20 C chamber, freeze cycle. This was repeated for a total of 3 different shipping configurations and a naked gel as the control: Empty RSC shipper EPS(expanded polystyrene) panels, lining the RSC Vacuum insulated panels lining the RSC Readings were taken from the thermocouples inserted into gel packs, recording the time that the instrumented gel packs took to freeze (phase change) and then come to equilibrium with the environmental chamber (control, ambient thermocouple), (-) 20 C. The following is a summary of the test results: Insulating Shipper Study and Thermal Performance Shipper Design Gel Freeze Thermocouple Time to Time at Phase Pack Cycle cool to 0 Change(Freeze) C 8 X (-) 20 C Probed into Control Gel, 1.5 4 hours 8, 2.0 geometric center hours No Container lb. Unlined RSC, 12 8 X 8 (-) 20 C Probed into 3.6 11 hours X 12 X 12 geometric center hours EPS panel lined 8 X 8 (-) 20 C Probed into 6 hours 19 hours RSC, 12 X 12 X geometric center 12 Vacuum 8 X 8 (-) 20 C Probed into 13 hours 48 hours insulated panel geometric center lined RSC, 12 X 12 X 12 The data very simply illustrates the principle of heat transfer through conduction.

= kA

T x

qx = conductive heat transfer rate k is the thermal conductivity constant of the insulation A is the total surface area of the insulation
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T is the temperature difference form one side of the insulation to the other x is the thickness of the insulation In practical terms, it provides an illustration of the effect of an insulative shipper design on the thermal performance characteristics of your package design. The conduction effect is the strongest when insulation is involved and the better the insulation, the slower the heat transfer rate. The convection effect, heat transfer that occurs between a surface and a moving fluid when they are at different temperatures, is an additional source of heat transfer and even an unlined RSC mitigates the convection effect. Essential #3: Size and Number of Gel Packs and Their Performance Effect

The question here is how to specify your gel packs relative to total mass of the refrigerant and orientation. The following study was conducted: Refrigerant size and orientation Outcomes Expected thermal mapping, center of refrigerant longest time at phase change temp. Illustrates corners reaching temp equilibrium with chamber fastest. Thermal mapping demonstrated the perimeter is more influenced by heat transfer from the neighboring gel pack and thus heat transfer happens more easily and the overall surface area of the refrigerant has more variability. Thermal mapping demonstrates a performance more like the 8 X 9, (1) - 2 lb. The stacking of the refrigerants minimizes heat transfer during thaw/freeze cycle, thus longer time is spent at the phase change temperature.

Refrigerant Size 8 X 9, (1)2 lb 4 X 9, (2)-1 lb. (2) 4 X 9 1 lb.

Freeze Cycle (+) 20 C to (-) 20 C (+) 20 C to (-) 20 C (+) 20 C to (-) 20 C

The data suggests that a single gel pack is slightly more effective than 2 gel packs of equivalent mass at remaining at the phase change temperature longer. There appears to be greater heat transfer with the 2 side by side units. The possible winner here is a slightly lower cost of purchasing one refrigerant as opposed to two, for the same mass. Essential #4: Gel Structure and Geometric Stability

As mentioned previously, gelling agents are added to water to increase the viscosity and add structure to the gel pack. The feature of structure can also be achieved in several different ways. First, lets focus on the importance of structure or the opposite of free flowing water in a bag. We performed a time lapse photographic study of several different refrigerant designs by placing previously frozen refrigerants on end, at room temperature (20 C) and photographing the thawing process every 30 minutes. The test units were as follows: Melting Photographic Study
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Refriger rant Type an nd Mass 1.0 lb ba ag of water 1.0 lb ba ag of water 3.0 lb ba ag of water 3.0 lb ba ag of water

Structured d or Un-structu ured Un-structur red Structured Un-structur red Structured

Stu udy Observ vations Afte er 5.5 hours s of thawing g, significan nt pooling of o wat ter occurred d. Significa ant loss of shape. s Afte er 5.5 hours s of thawing g, no appre eciable poo oling of water w occur rred. Nearl ly complete e shape ma aintenance. Afte er 5.5 hours s of thawing g, significan nt pooling of o wat ter occurred d. Significa ant loss of shape. s Afte er 5.5 hours s of thawing g, minimal pooling of wat ter occurred d. Minimal loss of sha ape. Slightly bet tter shape retention r than 3.0 lb. un-structure u ed bag g.

M Melting Ph hotographic c Study

1.0 lb. Structured S Ge el--Time 0 Hours Co ompletely Solid

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1.0 lb.S Structured Ge el-Tim me 2.5 Hours Par rtially P Page 6 Melted of 10

1.0 lb.Struc ctured Gel-Time 5 Hours Fully Melted M

3.0 lb Unstructured d Gel--T Time 0 Hours Completely Solid

3.0 lb. Unstru uctured Gel--Time 2. .5 Hours Partially y Melted

3. .0 lb. Unstructured G Gel--Time 5 Hours Al lmost Fully Melted M

al #4:, conti inued Essentia nificance to o these time e lapse photographs is s the loss of f shape tha at occurs as s the The sign refrigera ant melts, if f not assiste ed by a gell ling agent to increase viscosity or the use of fa rigid bot ttle. The lar rger the gel refrigerant mass, the e greater the e potential to lose symmetry. The los ss of shape creates a non-uniform n m thermal coverage c an nd may negative ely impact the thermal protection of the payload. When n designing g a package e and specifying a ge el pack as the t refrigera ant, whethe er or not you need to have h a gel that t maintain ns its shape e must be considered. c The important thing to t note from m this study y is that whil le the struc ctured and unstructure ed gels com mpared her re are both properly referred to as gel packs p they y each have e very differ rent perform mances from the ctive of geom metric stability. There e are other methods m fo or forcing a water base ed perspec refrigera ant into a re ectangular shape s such h as the rigid bottle but t it must be understood that just by going th hrough its phase p chan nge, water will w end up a different size/con nfiguration, regardless.

Essential #5:

Prototyp ping the Pa ackage

Utilizing thes U se four essentials outlined in this paper, dev velop your design d inpu ut re equirement ts for your temperature e controlled d package design. d

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Plan for thermal and distribution simulation feasibility testing as this is vital to determining if product requirements and thermal protection requirements are being met. o Creating physical samples for testing allow for investigation of the first 4 essentials outlined in this paper. o Rule of Thumb Guidelines for Temperature Controlled Package Design Explore how to specify gel packs and their use in the package in context of these studies. Describe other options available. Cover as much surface area as possible with refrigerant. Use insulation to slow the heat transfer into the package. Buffer your refrigerated product from the frozen gels. Make sure the design is robust enough to survive shock and vibration during shipment. Include enough refrigerant in the package so that it is always undergoing phase change during the shipment. o Specifying a Gel for your Design To ensure best performance the gel should be shaped in a uniform symmetric way, preferably square in shape. Understand that the amount of insulation used in your package directly affects how long it will work. Consider the cost balance between adding more gel and more insulation when trying to improve performance.

Essential #5:, continued When possible use single larger gels instead of many smaller gels. Depending on the size and geometry of your product this will be more or less practical. Remember the importance of the structural properties of the gel material itself. If your package requires gels to stand on end make sure they will maintain their shape. o Other Options Available to Solve these Problems Refrigerant Geometric Stability: Rigid Bottles: The bottle will not change shape but the gel can still flow inside of it and cause voids in your package. Phenol Foam Brick Packs: The performance per pound may not be as high as gel material since the foam does change phase. Gel Blanket: Spreads the refrigerant evenly across the payload trading surface area coverage for pure weight performance. o Other Options Available to Solve these Problems Rigid Bottles The bottle will not change shape but the gel can still flow inside of it and cause temperature voids in your package. Phenol Foam Brick Packs The performance per pound may not be as high as gel material since the foam does change phase.
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Gel Blanket Spreads the refrigerant evenly across the payload trading surface area coverage for pure weight performance. Custom Phase Change Materials The phase change will better match your products stabile range but the material itself is generally much more expensive and depending on the chosen material toxicity issues must be understood and guarded from.

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Summary: It is the intent of this paper to alert packaging engineers of temperature sensitive products that water based gel refrigerants exhibit properties that are unique to the thermodynamic properties of water. For the successful development of a water based gel refrigerant, we have outlined five(5) essentials that will help you achieve success in your temperature controlled package development. It is our goal to highlight performance outcomes of your phasing material so that your thermal protection is not compromised. The five (5) essentials of water based refrigerants: 1. Geometry, Weight, and Thermal PenetrationTemperature distribution across your gel pack 2. Package Design and Freeze/Thaw Time--- The effect of shipper insulation on thermal protection. 3. Size/Number of Gels and Performance---2(1) lb. gel packs vs. 1 (2) lb. gel packs and thermal protection. 4. Gel Structure and Geometric Stability---Physical structural integrity of your gel pack and why it might be important. 5. Prototyping the Package--- Plan for thermal and distribution simulation feasibility testing as this is vital to determining if product requirements and thermal protection requirements are being met.

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