Measurement of Silicone Deposited on Hair

by Various Analytical Methods

Poster presented at the 19th IFSCC Congress, Sydney

22 - 25 October 1996

A. De Smedt, I. Van Reeth, S. Marchioretto, Dow Corning SA, Brussels, Belgium

D.A. Glover, Dow Corning Corp. Midland, Michigan
J. Naud, University of Louvain, Louvain-La-Neuve, Belgium
 Measurement of Silicone Deposited on Hair
by Various Analytical Methods

A. De Smedt, I. Van Reeth, S. Marchioretto, Dow Corning SA, Brussels, Belgium

D. A. Glover, Dow Corning Corp. Midland, Michigan
J. Naud, University of Louvain, Louvain-La-Neuve, Belgium

Abstract
Silicones, commonly used as conditioning agents in 2-in-1 shampoos, are already effective at very
low levels. To date, no single analytical method has been identified as ideal for quantifying these
deposits on hair.
Methods currently described in the literature are Fourier transform infrared DRIFT
spectroscopy (FT-IR DRIFT) and atomic absorption (AA). However, both methods have
limitations. The FT-IR detection limit is quite high, and the accuracy of AA measurements is
strongly influenced by the efficacy of the extraction step.
A broad literature search has been carried out in order to cross-fertilise with different areas of
analytical chemistry and possibly generate new ideas about screening tests for small amounts of
silicone deposited on hair. The current study describes an evaluation of new methods which
complement each other very well.
l An innovative X-ray fluorescence (XRF) method that characterises bulk hair. XRF methods

already have been described in the literature as means of analysing trace elements such as
copper, cobalt, or nickel within the hair shaft, Prior to this study, these methods had not
been used to document the presence of conditioning agents including silicone. Moreover,
the sample preparation proposed in this study includes a pyrolysis step at 700°C, ensuring
homogeneity of the analysed sample.
l A wettability measurement method that characterises single hair fibre surface by assessing its

hydrophilicity or hydrophobicity.

Introduction
Knowing the amount of conditioning agents deposited on hair surface by shampoos or
conditioners is vitally important for cosmetic chemists. It allows them to study the absorptivity of
polymers/surfactants on the hair surface, to correlate absorptivity with sensory properties, and
also to greatly facilitate claim substantiation (European Cosmetic Directive 6th Amendment).
However, as the levels of conditioning agents are usually very low, accurate data are very difficult to
get.
Silicones possess a range of unique properties like lubricity, low solubility parameter, low
intermolecular forces, water insolubility, and a very low surface tension, such that they spread
easily on most surfaces to give a uniform, smooth, hydrophobic film (Todd and Hayes, 1971;
Starch, 1984). This explains why silicones have been used for years as superior conditioning
agents, even at very low deposition levels (e.g., Bergman and Bess, 1991). The following benefits
are well described in the literature:
l Silicones replace the conditioning benefits of the sebum which is being removed from the
hair during shampooing, with no oily feel.
l Silicones provide a smooth, silky and not tacky feel, and excellent detangling and
compatibility performance (e.g., Yahagi, 1992). They are also gloss enhancers.
l Silicones reduce the damage associated with oxidative treatments such as straightening or
permanent waving (Berthiaume et al., 1994, 1995).
l Silicones also help the spreading of other active ingredients (Alexander, 1992), ensuring a
better film homogeneity, and may retard the rate of sebum spreading (Bogardus et al.,
1985).
Silicone polymers especially effective in conditioning shampoos are high molecular weight
dimethicones, dimethicone copolyols, and amodimethicones.
Measurement of Silicone Deposited on Hair

Because silicones are very commonly used ingredients in conditioning shampoos, many studies
have been carried out in an attempt to quantify silicone deposition on hair. Atomic absorption
(AA), and to a lesser extent Fourier transform infrared DRIFT spectroscopy (FT-IR DRIFT), are
very popular and in many cases, the best option. However, the FT-IR DRIFT detection limit is
quite high, and AA is not really suitable for the analysis of organofunctional or crosslinked
polymers, due to the lack of efficiency of the extraction method.

Literature Search Summary

A broad literature search has been carried out in order to cross-fertilise with different areas of
analytical chemistry and possibly generate new ideas about screening tests of small amounts of
silicone deposited on hair. Information on analytical methods was gathered from the following
areas:
l Characterisation of uncoated hair
l Characterisation of conditioning agents other than silicone deposited on hair
l Characterisation of silicone deposited on substrates other than hair
l Characterisation of silicone deposited on hair
The analytical methods used to characterise hair composition can be divided into two
categories, depending on the kind of information generated:
l Surface and near-surface methods analyse only an extremely small portion of a hair fibre at
a time (maximum 1 square micron, depending on the method).
l Bulk methods provide an average value of the analysed species for the hair tress, which is
more representative of the real value of the whole scalp.
The aim was to select one idea for bulk analysis, one for sample preparation, and one for
surface analysis.

Analysis of uncoated hair

Analysing bulk and surface composition of human hair is rather difficult due to their fibre
characteristic and natural heterogeneity. However, analysis of hair composition has generated a
great deal of interest from many disciplines, including environmental, epidemiological, and
forensic sciences. This interest has arisen primarily as a result of the following.
l The trace element levels in hair are considered as a possible quantitative indicator for their

levels in other parts of the body and for exposure of the person to various environmental
sources.
l Hair is easy to sample and handle, compared to human tissues.
During the last two decades, several hundred papers and books have been published
concerning hair composition analysis.
Analytical methods
The most commonly used analytical methods for hair composition analysis include the following
(Table 1):
l Surface/single fiber analysis: scanning electron microprobe (SEM/EDX), electron
spectroscopy for chemical analysis (ESCA), secondary ion mass spectroscopy (SIMS), atomic
force microscopy (AFM), particle-induced X-ray emission (PIXE), and Fourier-transform
infrared spectroscopy (FT-IR).
l Bulk analysis: atomic absorption spectrometry (AA) and X-ray fluorescence (XRF). Some
work has also been initiated with neutron activation analysis (NAA).
l Ion chromatography (IC).
Hair sample preparation for bulk analysis
For bulk analysis of major elements or polymers, hair tresses do not require special sample
preparation. However, for bulk analysis of trace elements or polymers, the hair tresses need a
sample preparation step in order to ensure their homogeneity and to increase their trace
elements concentration. Several sample preparations are described in the literature (Table 2),
including: cryogenic grinding, pyrolysis, mineralisation by dry ashing, and solvent extraction.
 A. De Smedt et al.

Table 1. Analysis Methods.

Hair Coated With Silicone Coated

Analytical Organic Conditioning Substrates Other
Method Uncoated Hair Agents Than Hair Silicone Coated Hair
Surface Analysis
SEM (EDX) Bottoms et al., 1972 Goddard and Schadt, Bergman and Bees 1991
Kanetake et al., 1992 1988 Sejpka, 1993
Swift, 1991 Schmidt and Berthiaume et al., 1994,
Goddard, 1994 1995
Yahagi, 1992
ESCA Robbins et al., 1984 Goddard and Schadt, Smarajit, 1995
1988 Wendel and DiSapio,
Goddard and Harris, 1983
1987 (Berthiaume et al., 1994,
1995)
(Klimisch, 1991)
Pavlichko et al., 1994
Schmidt and
Goddard, 1994
Cipriano et al., 1994
FT-IR DRIFT Joy and Lewis, 1991 Klimish and Klimisch et al., 1987
Jurdana et al., 1994 Chandra, 1986, Bergman and Bees, 1991
(skin)
SIMS Braida et al., 1994
TOF-SIMS Berthiaume et al., 1995
PIXE Cortes Toro et al., 1993
Wu et al., 1993
Wettability Braida et al., 1994 Watanabe and Yahagi,
Kamath et al., 1984, 1995
1984,1985,1985,
1987

Bulk Analysis
AA Cortes Toro et al., 1993 Bergman and Bees, 1991
Folin et al., 1991 Gooch and Kohl, 1988
Berthiaume et al., 1995
GC-MS Solka and Kocis, 1994
NAA Cortes Toro et al., 1993
XRF Havranek et al., 1989 Helliwell, 1994 (skin)
Torok et al., 1984 paper
Eltayeb and Van
Grieken, 1989
Volkov et al., 1994
Qi et al., 1986
Cortes Toro et al., 1993
Folin et al., 1991
Ion chroma- Sturaro et al., 1993
tography
Measurement of Silicone Deposited on Hair

Table 2. Sample Preparation For Bulk Hair Analysis.

Hair Coated With Silicone Coated

Analytical Organic Substrates Other Silicone Coated
Method Uncoated Hair Conditioning Agents Than Hair Hair
No-sample pre- Qi et al., 1986
treatment Torok et al., 1984
Cryogenic Qi et al., 1986 Klimisch et al.,
grinding 1987
Pyrolysis Havranek et al., 1989 Solka and Kocis, 1994
Volkov et al., 1994
Mineralisation by Sturaro et al., 1993 Homer et al.,
dry ashing Eltayeb and van 1960 (meat)
Grieken, 1989
Solvent Grooch and Kohl, 1988 Holt, 1991 Klimisch, 1991
extraction

Analysis of conditioning agents other than silicones deposited on hair

Surface analytical methods used to determine non-silicone conditioning agents on hair are SEM,
ESCA, AFM, and SIMS (Tables 1 and 2). Radiochemical labelling has also been tried. Qualitative
and indirect assessment via wettability measurements or dye absorption have also been very useful
to characterise conditioned hair.

Analysis of silicone deposited on substrates other than hair

Silicones are also applied at very low levels on substrates other than hair. Some of the methods to
characterise the deposit are silicon-specific (e.g., AA, XRF, radiochemistry, colorimetry, SEM);
some are silicone polymer-specific (IR, Raman, NMR, GC-MS, ESCA) (Tables 1 and 2).
When background levels of inorganic silicon are high or variable, a silicone-specific method or
physical separation of the silicone from the matrix prior to quantification (e.g., using solvent
extraction) is generally preferred.
l On skin, silicone has been analysed using FT-IR ATR (attenuated total reflectance)
(Klimisch and Chandra, 1987) or XRF. Helliwell (1994) has described how a tape can be
applied on the treated skin, then removed and analysed for Si by XRF.
l In food containing low natural inorganic Si (like meat), Homer et al. (1960) have
determined total Si down to 3 ppm by decomposing it with H2S04 and HNO3, fusing with
Na2CO3, and testing the Si level via colorimetry.
l On paper, the amount of silicone deposited is determined by an XRF detection of inorganic
silicon.

Analysis of silicone deposited on hair

Several methods and sample preparations listed above have also been used to
qualitatively/quantitatively characterise the silicone deposited on hair (Tables 1 and 2).
Surface analysis
FT-IR DRIFT correlates very well to AA data, but has a higher detection limit. Sample preparation
is usually cryogenic grinding. SEM/EDX and ESCA are also often cited in the literature. TOF-
SIMS and wettability studies have been initiated very recently.
Bulk analysis
By far, the most commonly used method to analyse the amount of silicone deposited on hair is AA
(Tables 1 and 2). This method usually includes an extraction step by a solvent like methyl isobutyl
ketone (Klimish, 1991). Its main advantages are speed and a fairly low detection limit. Its drawback
is poor recovery in solvent extraction, especially for crosslinked and amino-functional polymers.
Sonication or enzymatic breakdown of the hair structure (Grooch and Kohl, 1988) may
improve recovery.
 A. De Smedt et al.

Summary
Both straightforward and very sophisticated methods have been developed to analyse coated and
uncoated hair. The most popular methods for bulk hair analysis are AA and XRF, and for surface
and near-surface analysis, SEM, ESCA, and wettability. Sample pretreatment for bulk analysis for
trace elements usually consists of solvent extraction, pyrolysis, and dry-ashing.
Although extensively and successfully developed for related applications, the following
methods have not been used to characterise silicone on hair, but seem very promising :
l XRF (only used to characterise silicon in bulk hair analysis and silicone polymer on skin and
paper).
l Pyrolysis (only used as a preparation prior to XRF analysis of trace element in hair bulk
analysis and as part of GC/MS analysis of PVP on hair).
l Wettability measurements (used to qualitatively characterise the surface of hair fibres
treated with conditioning agents and surfactants; only Watanabe and Yahagi (1995) applied
them very recently to characterise pure silicone on hair).
The potential use of these methods to characterise low levels of silicone deposited on hair by 2-
in-1 shampoos is explored in the following paragraphs.

A New XRF Method for Bulk Analysis of Silicone on Hair

Sample pre-treatment and preparation
Tresses of virgin brown hair from Hugo Royer in tresses of 2.5 g and 20 cm were washed three
times with a 30% sodium lauryl sulfate solution (Empicol LX28) and successively dipped during
30 sec into chloroform, 30 sec in methanol, and 30 sec in chloroform.
Prior to the XRF analysis, the hair samples were pyrolysed (isothermal run at 200°C during 2
hours in an oven, followed by a dynamic run up to 700°C during 1 h 30 min in a furnace).
Temperature and duration of both pyrolysis steps were optimised via thermogravimetric studies.
The resulting ashes were compressed into a 16 mm pellet and incorporated on top of a 40 mm
pellet made of H3BO3. Both pellets were compressed under 40 tons, using an Autopress T40 from
Graseby Specac.
For this study, ten samples at a time were pre-treated and prepared.

XRF equipment and procedure

The XRF apparatus is a sequential wavelength-dispersive X-ray spectrometer Siemens SRS 3000. It
includes a Rh X-ray tube, a 100 position sample turntable, and a flow counter detector. The
analytical conditions included a PET (Pentaerythrite) analyser crystal and a scanning rate of 2
min/degree. The peak is the Si Kalphal ray, measured at 109.2°C. Backgrounds are measured at
107.3 and 110.8°C.
The data were gathered and treated using Siemens Spectra 3000 software. The neat peak
intensity was considered as directly proportional to the concentration (i.e., no correction was
made) because the hair matrix is made of non-absorbing light elements and the thickness of the
hair ashes is much smaller than 1 mm (Eberhardt, 1989).
Determining the Si content of ten samples takes about 30 minutes.

Validation of the proposed method

Validation of this method is based on the following requirements:
l During the pyrolysis step, the silicone film deposited on the hair is fully thermally degraded
into silica ash.
l The XRF method analyses silicone and not specifically silicone polymer. The amount of Si
within the hair shaft must be low compared to the amount of silicone deposited on the hair
surface; moreover, the Si content of the hair shaft must be homogeneous within a single
hair lot.
Thermal degradation of the silicone film
Following Lipowitz and Ziemelis (1976) and Larena et al. (1992), silicone species of more than
5 cS undergo a surface oxidation during burning into a white surface silica ash with a gelled
methylsiloxane layer beneath. Subsequently, all silicone will be oxidised into silica, provided
Measurement of Silicone Deposited on Hair

enough oxygen is available during the pyrolysis and the silicone layer present on hair is thin
enough.
Si present within the hair shaft
Although 40 trace elements have been measured in hair, not a lot of data exist concerning Si level.
Wilkinson and Moore (1982, p.410) give a value of 188 ppm for European brown hair.
In order to check the robustness and representativity of this analysis, the level of other trace
elements more commonly reported in the literature, like Fe, Cu, Zn and Pb, has been compared
in Table 3. Considerable variation is observed. Fe and Cu concentrations range between a few
ppm and about 200 ppm. This would suggest that the Si content of hair may also be very variable
and even as low as a few ppm.
XRF analysis of Si carried out in this study on several hair tresses of the same lot has shown a
standard deviation of 10% between the different hair tresses and a Si average value 3 to 5 times
lower than the one found for hair tresses washed with conditioning shampoos containing silicones
(depending on the shampoo formulation).
Table 3. Comparison between Fe, Cu, Zn, and Pb levels (in ppm) in hair.

References Fe Cu Zn Pb
Wilkinson and Moore, 1982 133 64 116 21
Havranek et al., 1989 50-88 4-134 169-220 10-12
Iengar et al., 1978 5-45 11-34 99-450 3-70
Sturaro et al., 1993 - 11-22 189-319 5-9
Torok et al., 1984 65 38 228 9.5
Total range 5-133 4-134 99-450 3-70

Linearity, calibration, and cross correlation with AA

Standards were prepared by dipping several of these tresses into a solution of various amounts of
high molecular weight dimethicone diluted in cyclomethicones (Dow Corning® 345 Fluid and 1401
Fluid). These standards have been analysed by AA following the procedure described in Klimisch
(1991), and by XRF following the method described hereabove. The Si detection results obtained
by the two methods correlated very well. The XRF calibration curve is linear down to 5 ppm.

Wettability Measurements
Sample pre-treatment and preparation
Virgin brown hair from Hugo Royer in tresses of 2.5 g and 20 cm were washed three times with a
30% sodium lauryl sulfate solution (Empicol) and successively dipped during 30 sec into
chloroform, methanol, chloroform.
Because the hair hydrophilicity increases as a function of its distance to the root, hair samples
of 5 mm long were cut at the middle of the tress. Their diameter is measured using a Zeiss optical
microscope.

Equipment and procedure

Wettability measurements were carried out using a Kruss El4 tensiometer. The method consists of
hanging a 5 mm hair sample on a scale and dipping it into water. The wettability of hair fibre is
measured by the instrument as being the difference between its weight in air and its weight at the
contact with water. For each hair tress, thirty samples were analysed, and their wettability values
averaged.

Validation of the proposed method

Three sets of samples were analysed for their wettability in pure water : (1) untreated hair, (2)
silicone-coated hair, and (3) hair washed with shampoos containing silicone. The results show that
the three samples were significantly different from one another at more than 99% confidence.
Untreated hair was less hydrophobic and silicone-coated hair was more hydrophobic.
 A. De Smedt et al.

This method is qualitative; it is sensitive to the presence of silicone on hair, not to the level of
silicone. For example, hair coated with 700 ppm silicone has given exactly the same wettability
value as hair coated with 100 ppm.

Conclusions
This paper outlines two innovative methods to analyse and characterise low levels of silicone
deposited on hair by 2-in-1 shampoos.
l The bulk hair analytical method consists of a pyrolysis step followed by XRF Si detection. Its

main advantages are speed, low detection limit, and accuracy. It seems to be a very
promising screening tool, which could act as a back-up for AA tests.
l The single hair fibre surface analytical method consists of single fibre wettability

measurements. It provides information on the change in hydrophilicity of the shampooed

or silicone-coated hair. The method, still at an initial development stage, is sensitive to the
presence of silicone and not to its concentration level.

Acknowledgement
The authors wish to thank Anne Dupont and Brenda Reimer for their contribution.

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