Development of Guidelines for the Formulation of Microbial Resistant Coatings with Optimal Levels of Added Biocide [DEFOG] - Project Updates

Note: The following summaries are provided for dissemination purposes to those who may have an interest in the work but not be directly involved in the projects. They may however contain references to other project reports containing full experimental details, access to which is restricted to Industrial Advisory Group Members.

Overall Summary to the end of the Fourth Quarter, Project DME 4.3

Structural materials are frequently coated with organic surface coatings for aesthetic purposes and to afford protection from degradation in the environment. The organic components of typical surface coatings make them intrinsically susceptible to infestation and spoilage by micro-organisms. In order to provide an acceptable service life, biocidal additives are usually incorporated into the coating formulation but, by their mode of action, such additives are potentially toxic so that their use is subject to increasingly stringent regulation and restriction.

It is suggested that many of the raw materials that are commonly employed in coating formulę have intrinsic microbial effects. Some of the ingredients may support and promote microbial spoilage of coatings while others may be inhibitory in their action. Currently these factors are not usually taken as a primary consideration when designing a coating formulation with antimicrobial protection.

The research contract awarded to the PRA will permit development of screening methods for evaluating the influence of raw materials on microbial activity. A database of the behaviour for individual materials is being compiled. The information will be used for formulation assistance when designing the optimal concentration of biocide additive required for effectiveness. General formulation guidelines are to be developed.

In the first quarter of the Project, procurement of a wide range of raw materials for study had taken place. These had been selected to provide representative samples from each of the generic groups of the formulation ingredients. The materials were catalogued and a list circulated to the members of the Industry Advisory Group (IAG) for comments and advice.

Preliminary studies were carried out to find effective microbial activity screening tests for the individual materials. An important element of the investigation is the quantification of microbial effects for each of the various materials in the presence of other typical formulation components. PRA's initial approaches to activity testing methods were questioned by the IAG who felt the techniques did not adequately take account of the influences from the other components. As a consequence a revised experimental design was sought which would examine the behaviour of each material in association with a selection of other ingredients.

The range of raw materials used in coating formulations is extensive. Restricting the level of each component to that typically used in a coating, while employing simple mixtures, still generates a requirement for a very large number of experiments. Various techniques for handling the scale of the programme have been examined. The team concluded the so termed "Latin Square" experiment design was an efficient and effective means for undertaking the evaluation task.

Work undertaken with a small range of materials in a (4 x 4) Latin Square design, reported in the First Quarterly Report, showed that the method was capable of generating an index value for activity of a material with regard to its effect on growth response for a yeast and for a mould.

To improve the efficiency of the screening programme, larger (9 x 9) Latin Square designs have subsequently been employed. In two series of 9 x 9 Latin Square experiments 51 of the raw materials have been assessed for response to mould and yeast in model combinations comprised from a Resin, a Pigment and an Additive. The results of these experiments were presented in the Second Quarterly Report.

Evaluation of the raw materials will be an ongoing exercise and in the Fourth Quarter Report results for a further 9 x 9 Latin Square are provided, covering in all 75 materials. Statistical methods have been applied in order to link the results derived from the individual Latin Squares experiments. The design for a fourth 9 x 9 screening experiment is introduced.

Within the experimental sets a numerical response rating for each of the tested materials is generated. In most cases a distinction can be drawn for each material, relative to its peers, in terms of its tendency to support or to inhibit micro-organism growth.

When considering any individual rating it must be appreciated that in the simple screening experiments only restricted combinations are being examined and also that, for the Latin square design, interaction effects are not probed.

In the 3rd Quarter, effort had been applied to completing the preliminary screening and to finding the most suitable way to represent the results in the material database. Concerns had been expressed over the possible commercial implication of assigning a specific rank to any raw material (IAG, 1st Meeting Minutes). This is still the subject of much discussion by the IAG members. Categorising the activity of a material towards supporting or inhibiting microbial growth into broad bands, for example, very good, good, neutral or poor could provide an acceptable compromise, but it is difficult to provide agreeable boundaries. The approach currently taken is to report the material rating with a standard error.

It was noted that the level of assessed microbial activity varies with time as well as with the type of organism used in the challenge tests. The importance of the time of assessment and its significance in determining a response index for a material is still receiving consideration.

In response to the IAG's observation that some raw materials may themselves contain undisclosed quantities of biocidal additives, experiments where the test films were leached with water prior to inoculation have been carried out. It is proposed that this treatment should remove a substantial amount of any added biocide. The results of these experiments, which were presented in the Third Quarter Report, do show instances of variation between the leached and non-leached systems.

It is necessary to test the predictive power of the material's activity indices in actual coating formulations. During the 3rd Quarter consideration had been given to this aspect of the project, and formulation proposals were prepared for review by the IAG. Subsequently, a Plackett Burman experimental design was selected to explore the effects of material when combined in a "realistic" paint formulation and in the Fourth Quarter Report results of the laboratory microbial challenge tests on the full formulations are reported.

While in most instances, each formulation ingredient shows an effect which could be predicted from its behaviour in the screening tests, a number of materials show anomalous behaviour, for which explanations must be sought.

The full formulation paints are also undergoing field exposure trials, and two months of assessment are reported. Although only a short exposure period has occurred, the results so far confirm that the component behaviour, predicted from the Latin Squares screening tests, is in general being validated.

With the Fourth Quarter Report a pilot version of the materials' database is being released (on CD-rom), to the IAG members.

Attention is now being turned to the construction of the Formulation Guidelines. With this in mind the Fourth Quarter Report concludes with an outline of the experimental programme which will probe the effects of other relevant factors on microbial behaviour, eg. PVC, biocide concentration and leaching. Also to be examined are the influences of secondary factors such as gloss, surface energy, and water rub resistance.

Dr R Holman
Project Manager

15 November 1999

Note: The Funding Programmes "Degradation of Materials in Aggressive Environments" (DME) and "Materials Degradation in Aggressive Environments" (MDE) form parts of the UK Government's, Department of Industry (DTI) support for manufacturing industries.