E. T. Contis et al.

(Editors)
Food Flavors: Formation, Analysis and Packaging Influences
© 1998 Elsevier Science B.V. All rights reserved 753

Identification of the source of an off-odor in premiums intended

for use with dry mix beverages
Dimitrios Apostolopoulos

Kraft Foods, Technical Center, Packaging Research and Technology, 801 Waukegan Road,
Glenview, IL 60025, USA

Abstract
Premiums intended to be inserted inside packaged dry mix beverages were tested for
off-odor. Headspace gas chromatography/mass spectrometry was used in combination with
an odor test to identify the volatiles in the premiums and also evaluate the odor barrier
characteristics of the overwrap film. Data obtained from the headspace analysis of unwrapped
premiums showed extraordinarily high amounts of chemicals with the major residual
component being identified as cyclohexanone. Toluene, 2-methyl heptane, and 3-methyl
hexane were the next sizable components.
The source of those residual chemicals was considered to be solvents used with either
the resin or the paint employed in the manufacturing and painting of the premiums.
Odor testing of unwrapped premiums demonstrated a very strong, "solvent-like",
objectionable odor. Residual cyclohexanone in overwrapped premiums was found to be about
16 times less than in the unwrapped premiums. Furthermore, the overwrapped premiums
exhibited no off-odor. This clearly suggested that the solvent barrier provided by the plastic
film used for overwrapping of the premiums was sufficient to prevent any residual solvent
contamination of the dry mix beverages.
It is apparent, however, that an unsealed premium overwrap or a premium with a
punctured overwrap film would allow significant amounts of residual cyclohexanone and other
residual solvents to transfer into the packaged contents and cause a severe off-odor problem.
For that reason, it was recommended that those premiums should not be used with packaged
dry mix beverages.

1. INTRODUCTION

A common promotional tool is the insertion of a premium inside a food package. The
volafiles in these inserts, if not controlled, can impart an undesirable flavor to packaged foods.
Common practice is the use of an overwrap film to prevent direct contact and contamination
of the product (1).
The present study was undertaken with the objecfive to identify any product quality
issues associated with the insertion of premiums inside packaged dry mix beverages. More
specifically, i) identify any volatiles of the premiums that could potentially impart an off-odor
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to the dry mix beverages,

ii) quantify the odor impact of such volatiles upon their potential transfer into the
product, and
iii) determine whether the barrier provided by the premium overwrap film was
sufficient to prevent transferring of the premium volatiles into the packaged
contents.

2. MATERIALS AND METHODS

2.1 Premiums
The premium samples under evaluation were molded polyethylene bodies shaped as
potato men and women, which were painted and sealed in a nylon overwrap film.

2.2 Identification of Residual Species Present in Premiums by Using Headspace

Gas Chromatography/Mass Spectrometry
The identification of residual species present in the premiums under evaluation was performed
in accordance with the ASTM F 151-86 method, modified as described below. Two
over wrapped or two unwrapped premiums were placed into half-quart Mason jars. The jars
were fitted and sealed with teflon-lined lids, equipped with sampling ports. Mason jars
containing the premium specimens were placed inside a mechanically convected oven and
heated at 110°C for 90 minutes, to ensure vaporization of the premium residuals into the
headspace of the Mason jars.
Using a preheated gas-tight syringe to avoid condensation of the volatiles, headspace
aliquots of ImL were withdrawn from the Mason jars and injected into a gas
chromatograph/mass spectrometer (GC/MS), equipped with a CP-Sil 8 CB chromatographic
column operated at 20°C for 2 minutes and then increased at 10°C/min to 250°C.
The compounds present in the injected aliquots were separated resulting in GC/MS
scans with tentative mass spectral identification presented in Figures 1, 2, and 3.

I i ° r 99a i»

Figure 1: GC/MS profile of residual compounds for overwrapped premiums

 755

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371 I Mrs 1244 1356 H5S ISS-I

Figure 2: GC/MS profile of residual compounds for unwrapped premiums

Overwrapped Premiums

Figure 3: GC/MS profile of residual compounds for overwrapped versus unwrapped premiums

2.3 Odor Test

The odor test was performed as described below. Three overwrapped or unwrapped
premiums were placed in thoroughly cleaned one quart Mason jars, sealed with aluminum foil
lined lids and heated at 49°C for 1 hour. Blanks (empty jars) were prepared and carried
through the entire odor test to assure against any extraneous odors resulting from the jars or
the screw caps.
The Mason jars containing the premium specimens, as well as the blanks, were cooled
to room temperature and then presented to an experienced panel for odor evaluation. The
panel was composed of four people. All the panel menbers were familiar with the odor of
solvents commonly used by the packaging industry.
Odor evaluation entailed removing the screw caps of the Mason jars, opening a hole
through the aluminum foil to allow sniffing of the headspace and determinating the odor given-
off by the premiums.
756

The odor evaluation panel was asked to briefly describe the type of odor present, rate
the odor intensity on a 0-10 scale, and also indicate whether the odor was objectionable or not.

3. RESULTS AND DISCUSSION

As indicated by the GC/MS profiles presented in Figures 1 and 2, both the

overwrapped and unwrapped premiums exhibited a rather large number of residual
compounds. The most abundant of all the residual compounds identified was cyclohexanone,
followed in concentration by toluene, 2-methyl heptane, and 3-methyl hexane.
The source of such residual chemicals was considered to be either the polyethylene
resin or the paint used with the premiums.
A comparison of the GC/MS profiles of the overwrapped and unwrapped premiums
showed that the amount of cyclohexanone given-off by the unwrapped premiums was about 16
times more than the amount of cyclohexanone displayed by the overwrapped premiums (See
Figure 3).
This clearly suggested that the plastic film used for overwrapping of the premiums
possessed very good solvent barrier characteristics and provided sufficient protection against
any odor transfer under this test procedure.
The conclusion above was also supported by the results of the odor test.
Overwrapped premiums exhibited essentially no odor at all, unlike their unwrapped
counterparts which exhibited a very strong solvent-like, objectionable odor, as shown by the
table below.

Table 1
Results of Odor Test for Premiums
Type of Premium Type of Odor Odor Intensity on a 0-10 Scale*

Overwrapped None 0

Unwrapped Very strong, 9

solvent-like,
objectionable

* Where: 0 corresponds to essentially no odor and 8-10 to excessive odor, usually

characterized as objectionable

Based on the data generated, it can be stated that the overwrapped premiums inserted
in the package were expected to contribute no odor to the dry mix beverage.
However, the same data suggests that an occasionally unsealed or punctured overwrap
could allow significant amounts of residual cyclohexanone, as well as other odorous residual
compounds to transfer very easily into the packaged contents and cause a severe off-odor
problem. For that reason, it was recommended that those premiums not be used in dry mix
beverage packages.
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4. REFERENCES

1. M.G. Heydanek, Jr., G. Woolford, and L.C. Baugh, J. Food Sci., 44 (1979) 850

2. ASTM Designation: F151-86. Standard test method for residual solvents in flexible barrier
materials, (1986) 812-816.