Analytical techniques for successful cosmetic compact manufacture By Tim Freeman, Freeman Technology Formulating and manufacturing cosmetic

compacts to deliver market-leading performance characteristics requires a high degree of powder processing expertise. This paper considers the measurement of some of the most appropriate properties of both the formulation and the finished product. Many cosmetics are produced as compacts that, when packaged, are convenient to use and aesthetically pleasing to the consumer. Formulated to give the desired performance in terms of finished effect and ease of application, these discs of compressed powder are typically blends of emollients, preservatives, pigments, fillers and binders. While end-use performance targets tend to be the main drivers in formulation, successful and cost-effective production demands the development of a blend that processes well. Over the long term, the value of a robust manufacturing solution lies in the delivery of consistent product at high throughput and for the least cost. Assessing the processibility of a cosmetic blend is potentially a complex task since an array of different factors affect its behavior. This makes it important to examine a wide variety of parameters in order to achieve the best possible understanding of the formulation and its behavior when subjected to real manufacturing conditions. Instruments such as the FT4 Powder Rheometer from Freeman Technology combine dynamic, bulk and shear property measurement and are therefore well suited to this type of application. For the cosmetics industry, for example, the ability of the FT4 to assess compact hardness and pay-off further extends the usefulness of the system. Compact manufacture The first step in manufacturing a cosmetic compact is to blend the dry raw ingredients to acceptable homogeneity and consistency. Adding binder ensures that the powder exiting the blender is cohesive enough to form a stable, uniform compact but remains sufficiently freeflowing to process well in subsequent manufacturing steps. A cone blender, often incorporating a supplementary chopper, is a frequent choice for this application; however controlling the process to get the stickiness of the exiting material just right is not easy. At this preliminary stage it is also important to appreciate that many cosmetic ingredients, such as talc or titanium dioxide for example, are available from multiple suppliers. It is therefore essential to develop specifications that quantify these raw material properties in ways that relate to their performance during manufacture. It is not uncommon for a switch in supplier to result in issues with product quality or production, even though the specification of the new material is ostensibly the same as that of the previous one. Even within suppliers, batch to batch variation can lead to variability. Developing better, more differentiating specifications overcomes these problems. Filling the compacts is the next stage in the manufacturing process. Here, the aim is to ensure a consistent fill and to avoid segregation or separation of the powder blend. At this point relatively free-flowing materials are advantageous and help to avoid frequent stoppages and incomplete filling. However, if they are insufficiently cohesive, segregation and poor compact strength become more likely, compromising product quality. The final production step is compression of the powder. Compaction to a stable product of consistent bulk density is essential because the mass of the final product, although the basis for sale, is not directly controlled during manufacture. Compacting a known volume of powder to a consistent bulk density gives a reproducible mass. Properties of the finished compact, such as hardness and strength, are central, directly affecting consumer response, and form the basis of QC testing.

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Characterizing cosmetic powders Cosmetic ingredients are often specified simply in terms of composition and particle size. These properties are of course important. For example, the particle size of titanium dioxide, which is often used as a pigment or to give opacity, directly influences its optical properties and consequently its performance in the compact. However, the preceding analysis of the steps involved in compact manufacture suggests that other information is necessary to predict in-process performance. The ease with which the raw materials and the blend flow is crucial, as is the formulations response to compaction. Defining specifications for these materials in terms of more appropriate powder parameters can therefore pay dividends. By measuring a powder in motion powder rheometers give a direct indication of flowability, a dynamic material property. With these instruments the axial and rotational forces acting on a blade as it agitates a powder bed are precisely and accurately measured to yield values of flow energy. Well-defined sample preparation techniques, in combination with automated testing methodologies confer a high degree of reproducibility making this analysis sensitive and differentiating. Furthermore, powders can be tested in a compacted, conditioned, aerated, or even fluidized state to fully capture their response to air, a defining characteristic. Combining dynamic analysis with shear and bulk property measurement builds a valuable toolkit for cosmetic powder characterization. Shear analysis is a well-established way of quantifying the cohesivity of different materials (the tendency of the particles to stick to each other) and is especially relevant for more cohesive materials. Bulk properties on the other hand, such as permeability, compressibility and bulk density, help to rationalize observed behavior and provide basic information for process design. The FT4 Powder Rheometer incorporates bulk, shear and dynamic testing methodologies and for cosmetic applications combines them with hardness and pay-off test protocols. Hardness testing across the surface of the compact is a common way of testing the uniformity and success of the filling and compaction process and the integrity of the final product. Pay-off is also a routine test, involving wiping an applicator across the surface of a compact and measuring the amount of powder removed. Traditionally this test is completed by a QA technician and therefore is subject to inter-operator variability. Automation of applied force and shear rate, coupled with more precise mass measurement, gives much more reliable data. The following studies demonstrate the relevance of these testing methodologies at various stages of compact manufacture. All the data referenced were measured using the FT4. Case study: Controlling the blending process Developing a suitable formulation and blending it to a desirable endpoint is the most challenging aspect of compact manufacture. Usually, manipulating binder addition (both amount and rate), processing time and impeller speed delivers a blend with properties that translate into a high quality, stable, uniform compact. However, since this material is not the final product it can be difficult to recognize when an optimal point has been reached. Producing a compact is the only way to truly assess the blends suitability but this means a lengthy iterative development cycle. Examining an easily measured variable can circumvent this. Figure 1 shows basic flow energy [1], a dynamic powder property, changing as binder is added during a blending process.

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Figure 1: Tracking a blending process with basic flow energy measurements With only small amounts of binder present, the BFE of the mixture remains fairly constant but concentration then reaches a level where the binder has a more marked effect. BFE rises sharply as the mixture transitions to a more agglomerated blend suitable for compact filling. The harder, larger, stiffer particles produced by the blending process have a much higher BFE than the finer cohesive raw ingredients. The sensitivity of BFE measurements to this blend transition indicates this to be useful parameter for identifying the end point of the blending process and establishing optimal operating parameters. BFE is a variable that is independent of the scale at which the blend was made, which means that once established the correlation between BFE and compact quality will remain constant from formulation through to manufacture. In practical terms, the raw BFE data alone narrows the operating range of interest by roughly identifying the conditions that produce a blend suitable for compaction. Producing compacts with a series of blends within this narrowed down region pinpoints a BFE that combines good processibility with high product quality. This correlation can be determined easily at a relatively early stage in the development process but sets an end point specification for the blending process that is independent of scale. From this point on, the blending process and formulation can be optimized independently of the downstream process steps, accelerating and streamlining the progression to efficient production. In addition, over the longer term, operating the process to a BFE endpoint rather than using fixed operating parameters introduces the potential for adaptive control in response to batch-to-batch variability. Batch or supply variability is a frequent problem that will simply translate through to subsequent manufacturing steps if the blending conditions are fixed. Operating to an endpoint specified on the basis of a variable that reliably correlates with compact quality is a more intelligent approach that allows the operator to change control variables to maintain a consistent output, even when feed varies. Case study: Final compact strength and stability Finished product performance targets are ultimately met by ensuring that the developed blend delivers a stable compact of the required hardness. Figure 2 shows three sets of data that illustrate the relevance of shear, hardness and pay-off testing within this context.

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a)

b)

c)

Figure 2: Using (a) shear measurements (b) hardness data and (c) pay-off results to develop and assess the performance of cosmetic compacts

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Measuring the shear properties of the blend enables the prediction of compact stability. Figure 2(a) shows shear data as a function of binder addition, and illustrates an optimal shear strength range for good product quality. The results show that if the blend is too adhesive then it tends to fill the die inconsistently during manufacture, while insufficient shear strength results in a weak, easily broken compact. Hardness testing assesses the uniformity of the compact across its surface by measuring the penetration depth of a short metal probe at a defined force, at various points. The upper trace shown in figure 2(b) indicates poor uniformity with a looser powder bed in certain parts of the compact. The lower plot, in contrast, suggests a more uniform compact with greater overall hardness - a much preferred endpoint. Pay-off tests correspond directly with in-use experience, measuring how much powder is transferred to an applicator drawn across the compact surface. In automated testing, the applicator is circumferentially applied to the surface of the compact as it rotates. Figure 2(c) shows various behaviors ranging from excessive pay-off, where a large amount of material is easily removed, to the opposite situation, where the applicator cannot easily be loaded. The aim is to achieve consistent powder removal at an acceptable rate by tailoring the properties of both the blend and the finished compact, with hardness having a direct impact. In conclusion Sensitive powder characterization techniques, which provide data relevant to both process and product performance, support cosmetic compact manufacturers in their efforts to achieve high product quality at competitive cost. Measuring dynamic, shear and bulk powder properties promotes intelligent tailoring of blending, filling and compaction processes to meet performance targets, as well as the knowledge-based selection of raw materials. Instruments that combine these techniques with QC tests such as hardness and pay-off are a costeffective solution for the industry. Reference [1] J. Cooke and R. Freeman, "The flowability of powders and the effect of flow additives," presented at World Congress on Particle Technology, 2006.

April 2010 Tim Freeman, Director of Operations Freeman Technology www.freemantech.co.uk tim.freeman@freemantech.co.uk

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