Document 2248 V1 F2, Language EN V1, Approved 2009-2-12, © 2009 Ashland Inc.

Page 1 (6)

Fitness For Use Guidelines Reference Document

Background Resin manufacturers typically provide an indication of how long they expect resins to remain useable. Frequently this
is meant to limit commercial liabilities and to communicate that resin age can affect a product's performance after a
certain date. This time period is often described as "shelf life" or "commercial warranty". Unfortunately the shelf life
concept carries implications related to the food industry including the concept that disposal after a certain date is
appropriate. Resin consumers often rely on these warranty periods alone without considering all the related factors.
This misunderstanding can lead to increased costs and can even result in production of defective composites. The
purpose of this paper is to address these concerns in terms of a resin's "productive life" and to address ways that
fabricators might determine if a resin can still be used in the production process.

"Fitness for use" is both a practical and a legal term. Ashland customers must determine whether a resin is
appropriate or "fit for use" in their manufacturing process. Legally, Ashland does not warrant that its resins are fit for a
particular purpose or specific process. Fabricators must set their own criteria around suggested tests or other tests
known to them that affect suitability for use. These criteria should be used in shop quality manuals. Resin age should
never be the sole criteria for determining whether resins are appropriate for a particular production process.

The primary reason age alone is inappropriate as a measure of whether a resin is still usable is that storage
temperatures significantly impact product stability and ultimately product performance. Products see varying
storage temperatures throughout the year and depending on the length of the supply chain. For this reason resins
can not be "re-certified" to re-set the supplier's warranty clock. The time / temperature relationship is a reality of
physical chemistry that can not be reversed by a test. Tested and documented fitness for use criteria are the best tool
a fabricator can have to avoid the costs associated with disposal of old resin that may still be viable for production.

Suggested Viability Manufacturer's sales specifications are a good starting point for determining product performance capabilities after it
Tests has been stored for an extended time. Fabricators will most often use broadened versions of these ranges as their
criteria for product viability. The broader ranges allow for higher variability in fabricator labs, testing equipment
differences and natural changes in the resin including possible evaporation of monomers in the resin e.g. styrene. A
sample set of criteria might look like this:

Viscosity Fitness Test Sales Specification Fabricator's Fabricator's Results Adjustment Required Allowed Adjustments
Example Specification

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Fitness For Use Guidelines Reference Document

e.g. 300-500 mPa·s e.g 250-550 mPa·s at Pass/Fail w/Allowed e.g. Allow up to 3%
(cps) at 25°C (77°F) 25°C or Min/Max Time Adjustments? addition of styrene
per Zahn Cup(1)at above manufacturer's
25°C range(2)

(1) This field test is not appropriate for receiving / acceptance specifications. For details related to viscosity
measurements refer to "Viscosity - Quick Reference Guide" from Ashland.
(2) May require %non-volatile test to determine the baseline styrene level and to understand if evaporation is a
contributing phenomena.

Reactivity Fitness Test Sales Specification Fabricator's Fabricator's Results Adjustment Required Allowed Adjustments
Example Specification
e.g. 20-40 Minutes at e.g. 15 - 45 minutes Pass / Fail w/Allowed Customer Defined(3)
25°C (77°F) Adjustments?

(3) e.g. 1-3% MEKP with 0.1-0.5% cobalt 6%, 0-0.4% DMA. For details related to reactivity measurements refer to "Gel
Time - Quick Reference Guide" from Ashland.

The objective of tests like these is to allow for variations in field conditions and product conditions based on
fabricator knowledge regarding variations in resins that can be used to make acceptable parts. The ranges suggested
above are only for illustration and must be individually validated by the fabricator.

Other tests that may be considered include visual inspection of cured samples, cured sample hardness and resin
water content. Simple criteria like these combined with the more common tests noted above can provide validation
for resin fitness for use determinations and also provide diagnostic clues when problems are suspected.

Characteristics of When a vinyl ester or unsaturated polyester resin starts to gel its performance has been compromised. This is true
Compromised whether the product has been catalyzed and starts to gel before wet out and consolidation are complete or if the
Performance same phenomena are evident in the drum. In the case of fabrication the gel time - sometimes called working time -
can be adjusted. Notes about extending the storage time follow this section.

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Fitness For Use Guidelines Reference Document

Resin gelation is the first step in the polymer cure process. At this point a significant portion of the resin is forming
macro-molecules and developing a polymer network or structure. This structure can be observed many ways. When
running gel times or fabricating parts the end of the workable time first manifests itself as a string like structure where
the resin snaps instead of flows. This same structure can sometimes be observed when pulling resin from drums that
are starting to gel and are no longer usable (see picture). If this is observed then the resin's performance capability
has been compromised and should not be used.

Gelling Resin Pulled From Drum

Another way to determine if macromolecular structure is being formed is demonstrated in the graphic below. First,
place a resin sample in a test tube, leaving a small amount of air space and then sealing the tube (A) and then invert
the tube. If the rising bubble is symmetrical and smooth (B) then there is no significant structure formed and the
product may be used presuming other necessary performance criteria are met. If the rising bubble is somehow

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Fitness For Use Guidelines Reference Document

irregular (C) and has a tail on the bottom or is channeling and moving forward faster at some places than others
across the diameter of the tube then the product has "structure" and should not be used in production processes.

Bubble Test for Resin Gel

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Fitness For Use Guidelines Reference Document

When a drum of resin nears the end of its "useful life", product at the bottom of the drum may start to gel while
material on the top of the drum still appears fine. For this reason if a problem is suspected the drums of resin should
be inspected all the way to the bottom. The material on the top of the drum may be deemed usable by
predetermined measures but great care should be taken by the fabricator to insure that they separate the good
material from the bad.

Extending a Product's
'Useful Life'
All warranties offered by Ashland on vinyl ester and polyester resins are contingent upon a constant storage
temperature of 25°C (77°F). All things being equal, reducing the storage temperature should extend the useful life of
the product. Anecdotal experience has demonstrated that every 5-7°C (9-12°F) decrease in storage temperature can
double the useful life of the resin. There is a practical limit to this cooling effect because at some point it will be too
difficult to warm the resin. Additionally reduced temperatures can affect the resin's solubility in styrene. As a practical
matter Ashland recommends a minimum storage temperature of 10°C (50°F). Below this level fabricators should
evaluate resin separation and also the effects of the warming process on product stability. Cool storage does not
change the manufacturers warranty period.

Other ways to improve resin stability include adding a small amount of additional inhibitor and in some cases
opening and re-mixing the resin to re-incorporate air. Neither of these practices are without risk and need to be
evaluated on a case by case basis. Too much inhibitor, improper or incomplete mixing, introduction of contaminants
or selecting the wrong inhibitor or inhibitor solvent can make the resin unusable. Mixing air into the resin may help
but it can also cause problems. Incomplete mixing may create a false sense of security. The air source can also
contaminate the resin with water or compressor oils. Consultation with a technical service representative prior to
considering either of these options is recommended. Note that both of these steps can affect the product warranty.

Regardless of the which of these options a fabricator chooses, if the product still meets the fabricator's criteria and the
final articles are fully cured none of these actions will affect the final properties of the tanks, drums, etc.

Conclusion Commercial warranties and product shelf life are complex subjects. The term commercial warranty may be more
appropriate but still must be considered in a broader context including age, storage temperature and other storage
conditions. Age alone is generally not sufficient as a measure of usability or product performance. Instead, various
physical tests ranging from simple visual inspection of the resin to more extensive testing should be used as part of
any usability or performance determination. The fabricator bears the final burden of determining if a resin is
appropriate for use in their application.

The manufacturing, quality control and distribution of products, by Ashland Composite Polymers, comply with one or
more of the following programs or standards: Responsible Care, ISO 14001 and OHSAS 18001.

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Fitness For Use Guidelines Reference Document

Notice All information presented herein is believed to be accurate and reliable, and is solely for the user's consideration,
investigation and verification. The information is not to be taken as an express or implied representation or warranty
for which Ashland assumes legal responsibility. Any warranties, including warranties of merchantability or
non-infringement of intellectual property rights of third parties, are herewith expressly excluded.

Since the user's product formulations, specific use applications and conditions of use are beyond the control of
Ashland, Ashland makes no warranty or representation regarding the results which may be obtained by the user. It
shall be the responsibility of the user to determine the suitability of any of the products mentioned for the user's
specific application.

Ashland requests that the user reads, understands and complies with the information contained herein and the
current Material Safety Data Sheet.

More information Ashland Performance Materials

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* Registered service mark of the American Chemistry Council. ® Registered trademark and ™ trademark of Ashland Inc.