Journal of Hazardous Materials 411 (2021) 125045

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Journal of Hazardous Materials

journal homepage: www.elsevier.com/locate/jhazmat

An alternative method to assess permeation through disposable gloves

Matteo Creta a, Luke D. Savory b, Radu-Corneliu Duca a, c, Wai Kei Chu a, Katrien Poels a,
Jin Pan d, Jiamin Zheng d, Lode Godderis a, e, Mike Draper b, Jeroen A.J. Vanoirbeek a, *
a
Environment and Health, University of Leuven (KU Leuven), Leuven, Belgium
b
Ansell (U.K.) Limited, Willerby, Hull, United Kingdom
c
Unit Environmental Hygiene and Human Biological Monitoring, Department of Health Protection, National Health Laboratory (LNS), Luxembourg
d
Ansell Xiamen Limited, No 39 East 2nd Haijing Road, Haicang, Xiamen 361026, China
e
Idewe, External Service for Prevention and Protection at Work, Heverlee, Belgium

A R T I C L E I N F O A B S T R A C T

Editor: Dr. R. Teresa Previously, we have demonstrated the capability of activated charcoal cloth (ACC) to assess dermal exposure to
VOCs. Here we investigated whether ACC patches can be used as an under-glove indicator to evaluate the ingress
Keywords: of toluene through disposable gloves in a controlled environment, and compared these results to the amount of
Toluene toluene ingress determined from the standardized test methods for determining chemical permeation through
Activated charcoal patch
PPE. In a test chamber, with plugs for air sampling, five to six ACC patches were placed on a mannequin hand
Organic vapor monitor
underneath disposable gloves (latex, nitrile, neoprene, polymer laminate). Three work-exposure scenarios were
Gloves
Personal protective equipment (PPE) simulated to assess toluene ingress through the different gloves: vapor exposure; spray exposure, and immersion.
Permeation The standard permeation test, using a diffusion cell, was carried with glove material of the palm, with continuous
contact conditions. In all of ACC test, the order of toluene ingress was latex > neoprene > nitrile > Barrier, but
for the standardized testing, the order of the neoprene and nitrile was reversed, and nitrile had higher levels of
toluene ingress. These results show the need to think beyond standard testing techniques for occupational
exposure to hazardous substances, and the added value of “application style” testing.

1. Introduction
Occupational skin exposure to hazardous chemicals increased
significantly in the last decades (EUROSTAT, 2010a, 2010b; Home | U.
S.). According to classic prevention hierarchy, a stepwise strategy needs
to be implemented to reduce (dermal) exposure at the workplace,
comprising the substitution of chemicals used with less toxic options, the
re-design of the work process or the closure and isolation of the
contamination source (Safety and Health Topics | Dermal Exposure).
However, if the implementation of engineering and administrative
measures cannot sufficiently control dermal exposure to chemicals, the
use of personal protective equipment (PPE) remains the “last solution”
(Evans et al., 2001). PPE is designed to create a barrier to isolate the skin
of the worker from possible contact with hazardous substances. PPE
ranges in complexity and comprises chemical protective clothing for
different parts of the body (i.e. gloves, boots, coveralls, aprons, jackets,
full body suits) as well as skin protective products such as barrier creams
(Coletta, 1984). Protective gloves certainly represent the most used and
the most effective protection to prevent contact of chemicals with the
hands (Evans et al., 2001; Creely and Cherrie, 2001; European solvents
industry group, 2011).
In Europe, chemical protective gloves must meet the requirements of
European standard EN ISO 374-1:2016, that evaluates gloves for, three
important parameters for chemical protection: penetration (flow of a
chemical through pinholes or other imperfections of the protective
glove); degradation (a deleterious change of material); and permeation
(the process by which a chemical diffuses through the material at mo­
lecular level). Penetration is assessed by filling a statistical sample of
gloves per batch with water based solution and checking for leaks or
drops (Liwkowicz and Kowalska, 2000); degradation is tested by
comparing the force required to push a standard stylus through a sample
of the glove material before and after exposure to the challenge chemical
(International Organization for Standardization., 2019); glove perme­
ation testing is described in the norm EN 16523-1:2015. It is based on a
diffusion cell experiment (European Commission, 2017), which was first
described in the American standard, ASTM F739. The diffusion cell

* Correspondence to: KU Leuven, Department of Public Health and Primary Care, Centre for Environment and Health, O&N1, Herestraat 49 box 706, 3000 Leuven,
Belgium.
E-mail address: jeroen.vanoirbeek@kuleuven.be (J.A.J. Vanoirbeek).

https://doi.org/10.1016/j.jhazmat.2021.125045
Received 12 November 2020; Received in revised form 24 December 2020; Accepted 2 January 2021
Available online 6 January 2021
0304-3894/© 2021 The Author(s). Published by Elsevier B.V. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/).
M. Creta et al.
comprises a donor and a receptor chamber; in between the two cham­
bers the glove material, generally a circle with exposure area of approx.
20 cm2 (2 in. diameter) cut from the palm, is placed. After filling the
donor chamber with the challenge chemical, the quantity of permeant
passing through to the receptor chamber is regularly measured using
appropriate means, to determine the permeation rate through the ma­
terial (Anna et al., 1998). The permeation test results in parameters such
as the normalized breakthrough time (NBT), defined as the time needed
to reach a permeation rate of typically 1 µg cm− 2 min− 1 (for the majority
of the standards), and the steady state permeation rate (SSPR), which is
the permeation rate at the point at which it does not vary with time (the
time leading up to this is known as the “lag time”). Aside from EN
16523-1:2015, similar methods are used worldwide to test the chemical
resistance of gloves and other chemical PPE, such as ASTM F739-12ε1
and ASTM D6978-05, or ISO 6529:2013 (Organisation internationale de
normalisation, 2013). The methods described in these norms are the
most used, standardized and validated techniques to measure chemical
permeation through PPE materials, yet they also possess some limita­
tions: 1/ Differences in parameters of the aforementioned methods, such
as the diameter of the permeation cell challenge area and the flow rate
and type of collection medium, could lead to different value NBTs and
SSPRs (Xu and Que Hee, 2006, 2008; Que Hee and Zainal, 2010; Chao
et al., 2003; Banaee and Hee, 2019; Mäkelä et al., 2003); 2/ these
methods typically use only continuous contact of the selected chemicals
(liquid or gas), while specific exposure scenarios and real-life protection
effectiveness cannot be assessed (American Society of Testing and Ma­
terials (ASTM); Baker, 1994 Oct; Wang et al., 2006); 3/ only a small
swatch of the PPE material is tested, so flexure or abrasion of the ma­
terial in real life situations cannot be assessed, and 4/ although there are
some tests carried out on both commercial and lab created mixtures
(Zainal et al., 2006; Zainal and Que Hee, 2005; Phalen et al., 2003; Chao
et al., 2008), such mixture testing is non-standardized and mis­
conceptions in the testing of mixtures are very apparent in the industry.
A different approach to evaluate chemical permeation, such as an
indicator underneath the protective clothing, could be considered. Such
an indicator would then be analyzed with specific analytical techniques
(Creely and Cherrie, 2001; Boeniger and Klingner, 2002). We already
demonstrated that activated charcoal cloth (ACC) could potentially be a
good absorptive material to serve as a dermal indicator for volatile
organic compounds (VOCs) (Perkins and Vescial, 1997; Perkins and
Rainey, 1997; Creta et al., 2017, 2018).
Here, we aimed to develop an alternative method to assess ingress for
specific exposure scenarios, using the ACC patches. We selected vapor
exposure, spray exposure and immersion exposure, and tested the
patches with a selection of common glove materials found in occupa­
tional settings: natural rubber latex, neoprene, nitrile and polymer-
laminate gloves (Barrier®). The results from these tests were then
compared with the results obtained from the standardized diffusion cell
testing as detailed in EN 16523-1:2015.
2. Materials and methods
2.1. Chemicals
For the application test experiments, Highest purity toluene (≥
99,5%) was purchased from Acros Organics (Thermo Fisher Scientific,
Waltham, MA, USA), carbon disulfide (CS2), used for the sample prep­
aration, and a 250 mL flask-type sprayer were purchased from Sigma-
Aldrich (Saint Louis, MO, USA).
For the standardized permeation testing, Toluene (≥ 99.5%) from
Xilong Scientific Co., Ltd, was used.
2.2. Gloves
Four disposable gloves types have been tested for toluene ingress in
this study: natural rubber latex (TouchNTuff® 69-210), nitrile
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Journal of Hazardous Materials 411 (2021) 125045
(TouchNTuff® 92-600), neoprene (Microflex® 73-847), polymer-
laminate (02-100, referred to herein as Barrier®), all supplied by
Ansell (U.K.) Ltd (Hull HU10 6FE, U.K.). The specifications of the gloves
for chemical permeation, based on the norm EN 374-1:2016, are given in
Table 1.
From here on in, when referring collectively to the experiments
carried out using the ACC patches the term “application tests” will be
used, and the testing performed according to EN 16523-1:2015 will be
referred to as “standardized permeation testing”.
2.3. Exposure box and measurement set-up (application tests)
The experiments were performed in an acrylic glove box workstation
GB-2202-P-D (length: 950 mm; depth: 540 mm; height: 650 mm;
weight: 21 kg; tot. volume: 300 L) (Mbraun, Garching bei München,
Germany). The activated charcoal cloth (ACC) patches used, were Per­
mea-Tec™ solvent indicator and activated charcoal tubes (ACT) were
CSC tube, 100/50 mg sections, 20/40 mesh, both purchased from SKC
Inc. (PA, USA). Gilian LFS-113 low flow sampler pumps, for active air
monitoring were used. An automatic shaker (Heidolph) was used during
the sample preparations. A plastic mannequin hand (provided by Ansell
(U.K.) Ltd.) was placed inside the acrylic box. To measure the air con­
centration of toluene, using the Gilair pump and the charcoal tubes,
three sampling openings are present on the rear of the acrylic box (as
shown in Fig. 1). The side opening is used as the connection for the
sprayer flask. The acrylic box used was completely closed during the
experiments, and it was placed under a cabinet hood to minimize the
exposure to the operator.
2.4. Exposure scenarios
To evaluate the extent of toluene permeation through the disposable
gloves, different exposure scenarios were tested: 1/ vapor exposure, 2/
spray exposure and 3/ immersion exposure. In all scenarios tested, sol­
vent free medical tape was used to fix the gloves on the mannequin
hand, providing an appropriate seal. Admittedly, we cannot assure
whether this closure system is hermetic.
2.4.1. Vapor exposure
To assess the permeation of toluene vapor, five ACC patches were
stuck on the mannequin hand (Fig. 2a): four ACC patches were placed
directly on the hand (palm, thumb, middle finger and back), then the
glove was put on the hand, and one more patch was placed on the
outside (attached on top of the glove). This external ACC patch will
allow to evaluate the percentage of permeation through the glove, by
dividing the internal toluene concentration with the external
concentration.
In the vapor exposure test, 99.5% grade toluene (0.1 mL) was
pipetted into a petri dish and the dish placed in the middle of the box in
proximity to the mannequin hand (Fig. 2b). Three separate vapor
exposure experiments were performed for each glove type.
The vapor concentration of toluene in the chamber was measured
using active monitors (CSC tube, 100/50 mg sections, 20/40 mesh; SKC
226-01): two ACTs were placed in the top corners of the chamber, and
one tube was placed in the middle via the openings in the back of the box
(see Fig. 1). The flow rate of the active monitors was set at 100 mL/min.
At the start of the experiment, the operator opened the vial and pipetted
the toluene in the petri dish to let it evaporate. After 30 min of exposure,
all liquid toluene was evaporated, the hand was removed from the box
and the gloves and ACC patches were removed being careful to avoid
cross contamination. All four glove types; latex, neoprene, nitrile and
Barrier®.
2.4.2. Spray exposure
For the spray exposure test, an Aldrich® flask-type sprayer of 250 mL
connected with an air pump was used to generate a spray of pure toluene
M. Creta et al.
Table 1
Classification of tested gloves, based on the norm EN 374-1:2016.
EN 374-1:2016 classified chemical resistant gloves in the following type:
Type A: Protective glove with permeation resistance of at least 30 min each for at least 6 test chemicals;
Type B: Protective glove with permeation resistance of at least 30 min each for at least 3 test chemicals; Type C: Protective glove with permeation resistance of at least
10 min for at least 1 test chemical;
a
A: methanol; B: acetone; C: acetonitrile; E: carbon disulfide; F: toluene; G: diethylamine; H: tetrahydrofuran; I: ethyl acetate; M: nitric acid 65%; J: n-Heptane; K:
sodium hydroxide 40%; P: hydrogen peroxide 30%; S: hydrofluoric acid 40%; T: formaldehyde 37%.
(Fig. 2d). The spray rate was 0.89 mL/s. The flask was placed on the left
side of the box connected to an airflow pump through the opening at the
left side (Fig. 1). For this experiment, six ACC patches were placed on the
mannequin hand (Fig. 2c), underneath the gloves.
The hand was placed on the right side of the chamber, 40 cm from
the sprayer with the palm of the hand facing the spray and fingers
pointing upwards. We have performed five spray exposure scenarios,
with increasing total spray time (5, 10, 20 and 40 s), number of sprays
applied (single, 2 and 4 sprays), spray interval and total exposure time of
the gloves. The details are summarized in Table 2.
Immediately after the exposure, the gloves were gently removed and
ACC patches detached from the hand were analysed as described in
sample preparation. Experiments were performed three times per each
glove type. We did not assess the toluene vapor concentration generated
by the spray. Also, we did not place an external ACC patch on the gloves
because it would reach the saturation level (200 mg/patch).
2.4.3. Immersion exposure
In the immersion exposure test, six ACC patches were placed on the
mannequin hand, identical to the spray exposure scenario (Fig. 2c).
Toluene (1.5 L) was poured in a 2 L glass beaker (Fig. 2e). The gloves
were placed on the hand, on top of the dermal monitors, fixed on the
wrist with medical tape and immersed for 10 min. After the exposure,
the hand was taken out and the excess toluene was removed using a
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Journal of Hazardous Materials 411 (2021) 125045
Fig. 1. Schematic representation on the acrylic glove box
workstation GB-2202-P-D. Three openings on the rear of
the box, with appropriate connections allow air sampling
using low flow air pumps, with activated charcoal tubes.
The opening at the side of the box was used to connect a
spray flask. The openings at the front side of the box are
used to set-up the mannequin hand with the gloves. These
openings are closed during the exposure time. The ACC
patches were placed on the mannequin hand.
gentle air stream, to avoid post-exposure patch contamination. After
removing the glove, the six ACC patches were detached from the hand
and analysed as describe in the sample preparation chapter. For all glove
types, experiments were performed in triplicate. We did not assess the
toluene vapor concentration in the box. In addition, we did not place an
external ACC patch on the gloves because it would certainly reach the
saturation level (200 mg/patch).
2.5. Sample analysis
After each experiment, the ACC patches were analysed using the GC-
FID method as described previously Creta et al. (2017). Briefly the ACC
was removed from the patch and placed into a vial containing 2.0 mL of
CS2 to extract toluene. After 30 min of shaking, the solution was ana­
lysed by gas chromatography (GC) with flame ionization detection
(FID). Toluene was identified based on its unique retention time.
Quantification was based on a specific relative response factor for
toluene, which is a unique parameter, determined and updated on a
regular basis by validated laboratory tests.
For the vapor exposure test, activated charcoal tubes were used to
evaluate the air concentration of toluene. ACTs were analysed based on
the method of Sekkal et al. (2012), with minor modifications as
described in Creta et al. (2018). Briefly, the two sections of the tubes
were individually extracted using 1 mL of CS2. Samples were shaken for
M. Creta et al. Journal of Hazardous Materials 411 (2021) 125045

Fig. 2. (a) Location of the activated charcoal

patches on mannequin hand to perform the
vapor exposure test. Four patches were
attached on the hand, the glove was worn over
the patches, and one ACC patch was placed
externally on the glove. (b) Experimental
setting of the vapor exposure test: the hand was
placed horizontally in proximity to the Petri
dish where 0.1 mL of toluene was applied. (c)
Activated charcoal patches placed on manne­
quin hand to perform the spray and the im­
mersion exposure test. Five patches were
attached on the hand and the glove was worn
on top of the patches. (d) Experimental setting
of the spray exposure test: the hand was placed
vertically (finger pointed on top), 40 cm from
the sprayer. (e) Experimental setting of the
immersion exposure test: the hand with ACC
patches placed underneath the glove was placed
vertically (fingers pointed downwards) and
immersed in 1.5 L of toluene for 10 min. Med­
ical tape was used to fix the gloves on the wrist.

30 min on an automatic shaker and analysed using the same GC-FID

Table 2 method used for ACC patches.
Spray time and exposure time of the different experiments performed to test
permeability of latex, neoprene, nitrile and Barrier® gloves.
2.6. Statistical Analysis – application testing
Total Number of Spray Total Abbreviation
spray time sprays interval exposure time
The data is presented as the mean and standard deviation and was
5s Single spray At time 0 10 min 5 s/10 min
analyzed using one-way ANOVA test, followed by a Tukey post hoc test
10 s Single spray At time 0 10 min 10 s/10 min
10 s Single spray At time 0 40 min 10 s/40 min (Graphpad 8.3.0, Graphpad Software Inc, San Diego, USA). A level of
20 s 2 spray 10 s 1st spray at 40 min 20 s/40 min p < 0.05 was considered to be significant (* p < 0.05, ** p < 0.01 and
each time 0 *** p < 0.001). When the concentration measurements on the ACC
2nd spray patches were below the limit of quantification (LOQ), 0.9 µg/patch, a
after 10 min
40 s 4 spray 10 s 1st spray at 40 min 40 s/40 min
value corresponding to ½ LOQ was used. When all concentrations in an
each time 0 experimental set-up are below the LOQ, the data is presented as zero.
2nd spray
after 10 min
2.7. Standardized permeation testing
3rd spray after
20 min
4th spray after The standardized permeation (EN 16523-1:2015) set-up used a
30 min diffusion cell based off the designs as described in ASTM F739. The
All experiments have been performed in triplicate. The spray rate was 0.89 mL/ collection medium was nitrogen, which was flowing at a flow rate of
min. Five different spray regimes were assessed, each time in triplicate, for each 100 mL/min through the collection side of the cell. The nitrogen flows
glove type. through an automated valve system, which is connected to a Shimadzu
GC 2014 with an FID detector. An empty copper tube was used, in placed
of a packed column, as no separation was needed for this experiment,

4
M. Creta et al.
and this allows for faster sample throughput and higher resolution on
the time axis (x-axis). The permeation cells were placed in a water bath
that was kept at 23 ◦ C.
2.8. Statistical Analysis – standardized permeation
The data is presented as the mean and standard deviation, and each
experiment was carried out in triplicate. The method described in the
UKAS document, M3003 – The Expression of Uncertainty and Confi­
dence in Measurement (Edition 4), was used to estimate experimental
uncertainty. Based on this, the permeation rate uncertainty was calcu­
lated to be 2.5% with an expanded uncertainty, taking into account
k = 2, of 5.0%.
3. Results
3.1. Vapor exposure
The permeation of toluene through the gloves in the vapor exposure
scenario is shown in Fig. 3. In the experiments with latex gloves, the
mean air concentrations of toluene generated in the acrylic box was
63.0 ± 12.5 mg/m3. Under the latex gloves, toluene was found on all
ACC patches, ranging from 23.1 ± 10.3 to 35.4 ± 8.8 µg/patch. A con­
centration of 222.3 ± 45.1 µg/patch was found on the external ACC
patch.
Despite similar air concentration of toluene in the box
(68.6 ± 7.0 mg/m3), the concentration found on the ACC patches worn
under the neoprene gloves were ten-fold lower than for the latex gloves
(Fig. 3), ranging from 0.6 ± 0.2 to 3.9 ± 5.0 µg/patch. The concentra­
tion of toluene on the external patch was 230.9 ± 28.6 µg/patch. The
mean air concentrations of toluene generated in the experiment with the
nitrile gloves were 65.9 ± 19.6 mg/m3. We only found toluene above
the LOQ (0.9 µg/patch) on one patch of the middle finger. The con­
centration of toluene on the external patch was 223.0 ± 18.6 µg/patch.
The mean air concentration of toluene generated in the experiments
with Barrier® gloves was 61.2 ± 16.3 mg/m3. Underneath the Barrier®
gloves, we could not find any toluene on the patches. The concentration
of toluene on the external patch was 222.0 ± 32.80 µg/patch.
The ACC patch placed externally on the gloves allowed us to calcu­
late the percentage of permeation. For latex gloves, 15.9%, 15.5%,
10.4% and 16.4% permeation were found for the palm, thumb, middle
finger and back respectively. For neoprene gloves, a permeation of 1.1%,
Fig. 3. Results of toluene vapor permeation through latex, neoprene, nitrile, and Barrier® gloves assessed using ACC patches. Results represent the Mean ± SD of
three independent experiments. The gloves were exposed for 30 min to toluene vapor. LOQ for toluene on ACC patches is 0.9 µg/patch.
5
Journal of Hazardous Materials 411 (2021) 125045
1.7%, 0.3% and 1.5% was found for the palm, thumb, middle finger and
back respectively. For nitrile gloves, only the middle finger showed any
permeation, which was found to be 0.6%.
3.2. Spray exposure
The full results of the spray exposure scenario are shown in Table S1
(supplemental materials). Since we have tested several spray exposure
scenarios (Table 2), we have summarized the data in Fig. 4, showing an
average permeation concentration per spray scenario and per glove per
patch underneath the gloves (three replicates for each experiment).
While the concentrations of toluene on the patches of vapor exposure
were in the µg per patch range, with the spray exposure, we found
concentrations in the mg per patch range.
Spraying the latex gloves for 5 s with toluene and leaving them
exposed for 10 min (5 s/10 min), resulted in an average of
10.30 ± 1.58 mg/patch (mean concentration for ACC patches on palm,
thumb, finger 2, 3, 4 and back ± SD) (Fig. 4). Spraying the latex gloves
for 10 s/10 min and 10 s/40 min, we did not observe a statistically
significant higher concentration of toluene on the ACC patches. When
the latex gloves were sprayed 4 times for 20 s and left for 40 min, a
significantly higher permeation was found, compared to the 5 s, one-
time spray left for 10 min. For the 40 s/40 min exposure scenario, we
did not find a statistical difference with the 5 s/10 min scenario.
Toluene was found to pass through neoprene gloves with a mean con­
centration of 6.19 ± 4.35 mg/patch (mean concentrations of all patches
on the entire hand), in the 5 s/10 min spray scenario. Increasing the
spray time and exposure time to 10 s/10 min, 10 s/40 min and 20 s/
40 min did not change the level of ingress observed. However, when
applying the 40 s/40 min spray scenario, the toluene concentration on
ACC patches was significantly higher, as compared to the 5 s/10 min
scenario. Overall, a lower permeation was observed for nitrile gloves
exposed to toluene spray (Fig. 4). In the 5 s/10 min scenario, a limited
concentration of toluene was found to pass through nitrile gloves
(0.33 ± 0.29 mg/patch). While the 10 s/10 min and the 10 s/40 min
spray scenarios were not statistically different from the 5 s/10 min
scenario, the 20 s/40 min and 40 s/40 min spray scenarios did show
statistically higher concentrations of toluene on the patches. The poly­
mer laminated gloves were the most resistant to toluene ingress (Fig. 4),
showing an average concentration of 0.0297 ± 0.018 mg/patch for the
lowest spray exposure (5 s/10 min). A significantly higher permeation
was only found in the 40 s/40 min spray scenario, compared to the 5 s/
M. Creta et al.
10 min spray scenario.
3.3. Immersion exposure
The results of toluene permeation for immersion exposure are sum­
marized in Fig. 5. After immersion in pure toluene for 10 min, the latex
gloves show an ingress of toluene, ranging from 20.04 to 28.98 mg/
patch. In particular the amount of toluene detected on finger 4 was
higher compared to the patch on the back (p < 0.0001), palm
(p < 0.001) and thumb (p < 0.01). Neoprene gloves immersed in pure
toluene show a similar ingress compared with latex gloves; this ranged
from 21.05 ± 0.93 mg/patch, measured on the ACC patch placed on the
back of the hand, to 25.46 ± 0.99 mg/patch found on finger 4. For this
glove type, no difference in permeation was found for the different lo­
cations of the patches. The nitrile glove showed similar concentrations
of toluene ingress on all patches, ranging from 10.84 to 14.05 mg/patch,
independent of their position on the hand. Concentrations were slightly
lower than those found on latex and neoprene gloves. The Barrier®
gloves were the most resistant glove type showing toluene concentration
on the ACC patches in the µg range (from 3.1 to 13.2 µg/patch). No
statistically significant differences were found for the different ACC
patches underneath the Barrier® gloves.
Fig. 5. Results of toluene permeation through the four types of gloves for the immersion exposure test. The results represent the Mean ± SD of three independent
experiments. All the results are expressed in mg/patch except for Barrier® that are expressed in µg/patch. The gloves were immersed for 10 min in toluene.
**p < 0.01, ***p < 0.001, ****p < 0.0001 compared to finger 4 of latex gloves. LOQ for toluene on ACC patches is 0.9 µg/patch.
6
Journal of Hazardous Materials 411 (2021) 125045
Fig. 4. Results of toluene permeation after spray exposure
through latex, neoprene, nitrile and Barrier® gloves. 5 s/
10 min: one spray of 5 s, 10 min exposure; 10 s/10 min: one
spray of 10 s, 10 min exposure; 10 s/40 min: one spray of 10 s,
40 min exposure; 20 s/40 min: two sprays of 10 s, 40 min
exposure; 40 s/40 min: four sprays of 10 s, 40 min exposure.
Results represent the average toluene concentration found on
six ACC patches (palm, thumb, finger 2, 3, 4 and back) and are
expressed as the mean ± SD of three independent experiments.
**p < 0.01, ***p < 0.001 compared to the lowest exposure
scenario (5 s/10 min) for each glove type. LOQ for toluene on
ACC patches is 0.9 µg/patch.
3.4. Standardized permeation testing
The results of the standardized permeation testing can be seen in
Fig. 6. The permeation of the toluene through the latex gloves rises
immediately (between the first two data points at 0 and 2 min) up to a
steady state permeation rate (SSPR) of 463 ± 11 μg cm− 2 min− 1. There
is a slight undulating pattern upon reaching steady state, the reasons for
which can be numerous, but it is not within the scope of this paper to
discuss. It is not an uncommon phenomenon to see such non-Fickian
effects in permeation through polymers (Wadhawan et al., 2020). The
permeation of toluene through the neoprene glove also rises immedi­
ately up to a SSPR of 359 ± 7 μg cm− 2 min− 1. The permeation of toluene
through the nitrile glove rises over the course of 10–15 min up to a SSPR
of 409 ± 17 μg cm− 2 min− 1, hence the lag time for permeation of
toluene through this nitrile glove is approximately 15 min. The vari­
ability between runs for the nitrile glove (as detailed by the error bars)
indicates the slightly erratic nature of the permeation rate during the
first few minutes, which is highly sample-dependent. The permeation
rate of toluene through the barrier glove is reported as 0 μg cm− 2 min− 2
on the graph, as nothing was detected throughout the experiment. The
detection limit for this experiment was 0.005 μg cm− 2 min− 1.
M. Creta et al.
4. Discussion
In this study, we show the ability of the ACC patch to detect chemical
ingress through different types of gloves, with detection ranging from µg
to mg quantities of toluene per patch and that this ingress is heavily
depending on the glove type and the type of exposure. Currently, the
choice of gloves is most commonly based on the physicochemical
properties of the chemicals that are used and on the permeation resis­
tance (as normalized breakthrough time) of chemicals through the
selected gloves, as determined by the norm EN 16523-1:2015.
Previous studies showed that ACC patches have good absorbing
properties towards volatile organic compounds (VOC) and are poten­
tially good dermal exposure indicators (Vermeulen et al., 2006; van
Wendel de Joode et al., 2005; Cohen and Popendorf, 1989; Phanprasit
et al., 2019). This sampling methodology was already used to evaluate
the chemical resistance of chemical protective clothing (CPC) by placing
the ACC patches under the gloves and quantifying the permeation of
VOCs (Boeniger and Klingner, 2002; Perkins and Vescial, 1997). Here,
we used ACC patches to assess toluene ingress through disposable gloves
in relevant occupational exposure scenarios, which we controlled in a
lab environment. The selection of the exposure scenarios was based on
different tasks that often occur in occupational settings. With the vapor
exposure scenario, we intended to mimic a situation with ongoing open
process, but no direct contact to the chemical. The spray exposure sce­
nario mimics tasks where aerosols are created (e.g. spray paint) and the
immersion scenario is the most extreme scenario, simulating possible
high chemical exposure tasks. The selection of the gloves was based on
common materials for gloves used in a range of occupational settings.
In the toluene vapor exposure scenario, the natural rubber latex
gloves were clearly the most susceptible to ingress, followed by
neoprene and nitrile, whereas we did not find any ingress for the Bar­
rier® gloves. In this scenario we also attached a patch on the outside of
the glove, so we can calculate an average percentage of permeation. For
the latex gloves this was 12.8%, as mean for the entire hand. So, after
only half an hour of vapor exposure, ingress through the latex gloves has
already occurred. In an occupational setting, where no direct contact
with a chemical is foreseen, workers will often not wear any gloves at all,
although there is substantial risk for vapor-skin contact. Latex gloves
would provide some limited protection, yet, concentrations could in­
crease rapidly inside the glove, and as a consequence of increased hand
temperature with respect to a typical external environment represen­
tative of approximate laboratory conditions, dermal uptake would also
likely increase (Ramsing and Agner, 1996; Dash et al., 2013). The
average percentage permeation for neoprene gloves was significantly
lower, 2.1% approximately, as the mean for the whole hand. Both other
glove types, nitrile and Barrier®, provided overall an adequate protec­
tion for this specific exposure scenario. As the exposure was limited to a
maximum time of 30 min, further experiments would be required in
7
Journal of Hazardous Materials 411 (2021) 125045
Fig. 6. Results of toluene permeation through the gloves as
determined using the standardized permeation experiment.
The results represent the mean ± SD of three independent
experiments. The three vertical dashed lines indicate the
time-scales of exposure of the gloves to toluene as in the
application tests (vapor: 30 min; spray: 40-min exposure
scenarios; immersion: 10 min). The empty symbols repre­
sent the values of permeation rate before reaching the SSPR
(2 min for latex and neoprene, 14 min for Nitrile,
> 480 min for Barrier).
order to confirm the adequacy of the nitrile and Barrier® gloves ac­
cording to longer exposure scenarios.
In the spray set-up, we selected an occupational work exposure
scenario, where dermal exposure can be substantial when applying
products, such as paint, glue or coatings containing organic solvents. In
this exposure scenario, we measured concentrations in the mg per patch
range, which is a 1000× higher than the vapor exposure. Initially, we
started with the scenario of four times 10 s spray, over a total exposure
time of 40 min. Since we found in the latex, neoprene and the nitrile
gloves, high ingress values, we first decreased the time of spraying to
20 s (2 × 10 s spray) and 10 s (1 × 10 s spray) and we tested this
exposure scenario with a shorter overall time of exposure, being 10 min,
with actual spraying for only one time for 10 and for 5 s. For the latex
gloves, we found toluene ingress to be similar in all spray scenarios; only
exposing the gloves for 20 s and 40 min resulted in a significantly higher
level of ingress. The single patch concentration analysis (Table S1),
showed that the permeation of toluene was constant in all areas of the
front of the glove but lower in the back (p < 0.0001), which is thought to
be because the spray was directed towards the palm (Fig. 2d). A striking
observation in all spray tests was that the latex gloves were degrading
with increasing time of contact with toluene, leading to a larger and
distorted appearance and easier breaking of the gloves. In the neoprene
gloves, we observed similar permeation compared to latex, except when
the spray was applied for 20 s and exposed for 40 min. In this scenario
the toluene permeation was higher for latex than neoprene
(p < 0.0001). Also, the neoprene gloves showed a degradation process,
leading to increasing ingress for the most harsh exposure scenario. The
nitrile gloves were certainly more resistant to ingress than the latex and
the neoprene gloves in all spray scenarios, except for 20 s/40 min,
where neoprene and nitrile experienced similar levels of ingress
(p = 0.07)., For nitrile gloves, a significant increased concentration of
toluene was found only for the exposure 20 s/40 min. In all tests with
the nitrile gloves, the ACC patches placed on different locations show
similar concentrations, however when the spray was applied for 10 s
and nitrile gloves exposed for 40 min, a higher concentration was found
on the palm compared with other patches (p < 0.0001). This could be
explained by the thickness of the glove material, which is thinner on the
palm (0.12 mm) than on the finger (0.16 mm), as specified by the pro­
ducer (Ansell Microguard Ltd.,). Overall, the chemical resistance of
Barrier® gloves to toluene spray was found to yield the best results.
Toluene concentrations on ACC patches were almost a thousand-fold
lower than the other gloves (p < 0.001). In two experiments, we were
able to detect toluene on the ACC patch placed on the back of the glove.
This can be explained by the unstandardized closure system (medical
tape) that might allow some penetration of toluene and we could not
fully discriminate between permeation and penetration (hence ingress is
used throughout to encompass generic passage of toluene through the
gloves).
M. Creta et al.
With the immersion exposure scenario, we aimed to simulate an
extreme exposure where workers, pouring organic solvents or rinsing/
washing devices with organic solvents, may be exposed to high levels of
VOCs by liquid contact (Constable et al., 2007). This scenario could be
considered the most similar to the standardized permeation tests per­
formed according to EN 16523-1:2015, where in this case a part of the
glove is placed in continuous contact with liquid toluene in a diffusion
cell. The latex gloves showed the highest ingress after an immersion for
10 min, together with the neoprene, followed by nitrile and the Barrier®
gloves. The Barrier® glove was the only glove type that showed a
toluene concentration in the range of µg/patch. In fact, the Barrier®
gloves are the only gloves in our set-up that are certified to EN
374-1:2016 Type A, with official certification data for Toluene, with a
NBT of > 480 min (Table 1), as confirmed by our standardized perme­
ation testing within this study. A remarkable finding is that the spray
exposure with the Barrier® gloves gave higher permeation than the
immersion scenario. This is probably due to the set-up of the exposure.
In the spray test the mannequin hand was placed vertically with the
fingers pointed upwards (Fig. 2d), and the glove was tight on the bottom
using medical tape; this may allow toluene (vapor) to penetrate around
the wrist area, where it is not hermetically sealed. In the immersion
scenario, the hand was turned upside-down (Fig. 2e), and the toluene
was not agitated, so penetration of vapor via the open side is less likely.
Since we were expecting high levels of ingress, we decided only to
immerse the gloves for 10 min. Yet, for the Barrier® glove, we could
consider longer immersion times to study the kinetics of permeation in
more detail.
The permeation rate of toluene through the latex, nitrile and
neoprene gloves, when using the standardized permeation testing, was
expected to be high. It is interesting to note the difference in lag times for
the three materials, which was between 0 and 2 min for latex and
neoprene, and around 15 min for nitrile. In Fig. 7(a,b), we compared the
permeation rates of the standardized permeation test and the applica­
tion test. Using the surface area of the patch, and the total length of the
experiment as the exposure time, we calculated approximate perme­
ation rates for the vapor, spray (10 s/40 min) and immersion experi­
ments, assuming instantaneous reaching of the SSPR (which we know
not to be true for nitrile). This reveals that for all application test
exposure scenarios, the order of toluene ingress rate is latex > neoprene
> nitrile > barrier®. However, for the standardized permeation exper­
iment, the order of the neoprene and nitrile is switched (latex > nitrile >
neoprene > Barrier®), with the nitrile showing a higher SSPR. The
reason for this switch appears to be due to the lag time of the toluene
Fig. 7. (a) Comparison of the permeation rates of toluene through the four gloves for the different exposure scenarios. For the ‘application test’, the permeation rate
has been calculated dividing the toluene concentration found on the patch with the surface area of the patch (3.6 cm2) and the exposure time. For the ‘Standard (Std)
permeation test’ (EN 16523-1:2015) the permeation rate values represent the SSPR. (b) Permeation rate as calculated for the vapor exposure scenario for the different
gloves types.
8
Journal of Hazardous Materials 411 (2021) 125045
permeation through the nitrile gloves. As shown in Fig. 6, the length of
exposure for the immersion experiments is clearly shorter than the lag
time for the permeation of toluene through nitrile gloves, indicating that
SSPR has not actually been reached, and the permeation rate is actually
slower than that for the neoprene in the early minutes of exposure.
For the spray and vapor exposure scenarios, the total exposure time
is longer than the lag time for the nitrile glove, however, in both cases
the toluene may not have been in direct contact with the glove for the
whole time, so SSPR may still not have been reached. This presents us
with an interesting scenario, whereby data obtained using the tech­
niques detailed in the standards used certify products in order to place
on the market in Europe, indicates in this scenario the nitrile glove to be
a more unfavorable PPE choice than the neoprene glove, but the
application style tests contradicts that conclusion. Whilst SSPR is not
normally reported in the technical literature of gloves (and both gloves
have a NBT of 0 min, which would be reported), this is just one example
of many potential chemical/glove/exposure scenarios where this type of
conclusion could occur. In this case, a factor that is not included in any
standard requirements, the lag time, could actually provide the deciding
factor for PPE selection. The Barrier® glove showed no permeation at
all, which means that we can effectively use this as the control experi­
ment for all the application tests (aside from the fact that Barrier®
material is harder to seal than the softer, more malleable rubber gloves).
A second observation with respect to the comparison between the
standardized permeation and the application testing, is that the im­
mersion experiments showed a higher rate of permeation than the
standardized permeation. Given that both experiments had the same
extent of chemical exposure (full immersive contact), we need to un­
derstand the reason for this discrepancy. There are three possible rea­
sons for this: 1) ingress through penetration around the sealing of the
glove cuff (as discussed below), 2) degradation and subsequent defor­
mation of the glove, leading to higher surface area, but limited move­
ment possible within permeation cell, and 3) surface area of the ACC
patches (being the detection area) not being equal to the test area of
gloves, and picking up vapors that have permeated from a larger surface
area of the glove, whereas in standardized testing the detection area =
the testing area. As for point 1, the results for the application testing for
the Barrier® glove should give us a reasonable understanding of how
effective the sealing technique was (as mentioned above, it can act as a
control due to no permeation from standardized testing. As discussed
above, there is ingress through the barrier glove for both the spray and
immersion testing. Due to the inflexible nature of the barrier glove, it is
harder to seal than the rubber gloves, so it is likely to be a worst case-
M. Creta et al.
scenario as well. Overall, the amount of toluene ingress through the
Barrier glove is significantly lower than the rubber gloves in all exposure
scenarios, with the spray exposure leading to the highest ingress. This
indicates that the most likely reason for lower ingress from the stan­
dardized permeation testing compared to the immersion experiments is
due to points 2 and 3. The only exception for this trend is for nitrile, and
this can again be understood by the effects of the lag times and the
permeation not having reaching steady state in the immersion
experiments.
In all the application test exposure scenarios, medical tape was used
in order to allow a better adherence of the gloves on the mannequin
hand and avoid possible penetration at wrist level. However, we could
not determine whether this closure system was hermetic and if only
permeation through the glove material took place. However, as
mentioned above, we can assume for the Barrier® gloves that all
chemical ingress was due to penetration around the seal, given that the
material offers a full permeation barrier (i.e. no detectable permeation is
observed during a 480 min standardized laboratory permeation test).
For the standardized permeation testing, rubber gaskets were used to
seal the diffusion cells, and a sufficient torque used on the bolts to close
them, so that a hermetic seal was known to have been made.
Overall, the ACC patches are shown to be able to evaluate toluene
ingress for different glove types in different occupational exposure sce­
narios. The different exposure scenarios resulted in a large range of
toluene concentration on ACC patches (from 1.3 µg/patch to 28 mg/
patch) without reaching saturation (200 mg/patch), even in the extreme
exposure scenario with the most poorly performing glove (latex).
The relationship between glove permeability and thickness of the
material was not assessed in this study. The disposable gloves tested
showed similar values of thickness: latex and neoprene gloves are
0.10 mm thick on the palm and 0.12 on the fingers; nitrile gloves were
0.12 thick on the palm and 0.16 in the finger regions. Barrier® gloves,
despite showing the best performance, had the thinnest structure, only
0.062 mm for the entire hand, as mentioned on the product data sheet
by Ansell. A clear dependency between glove thickness and permeability
has been already demonstrated for different chemicals, including
toluene, for which an increased thickness determines a reduction in
permeability (Wallemacq et al., 2006; Oriyama et al., 2017; Cheng et al.,
2012). This is further explained when considering the mass transfer
kinetics that take place during these permeation processes. Since in the
case of direct liquid (spray and immersion) or only vapor contact, the
mass of toluene that moves through the gloves is generally dominated
firstly by Fickian diffusion, followed by case-II diffusion, and since both
process are dependent on membrane thickness, an increase in thickness
will certainly result in lower rates of permeation for any single system
(Cheng et al., 2012, 2015; Thomas and Windle, 1982).
For the European legislation, as specified by EN ISO 374-1:2016 for
gloves, the NBT is recorded when the permeation rate reaches
1.0 µg cm− 2 min− 1, independently of the chemical toxicity. The NBT
values are used at the workplace for an initial screening to choose the
most suitable gloves considering the specific chemicals used; however,
once the best glove is selected, the specific tasks performed by the
workers could substantially modify the actual passage of the chemical
through the gloves. To overcome these limitations of the diffusion test,
the use of ACC patches as an under-glove indicator can provide, for
specific workplace exposure scenarios, the real amount of chemical that
crossed the glove barrier. As we have shown in this work, this type of
testing may actually lead to a different glove being chosen than the one
chosen based off the data provided by standardized permeation testing.
Thus, as already demonstrated in Creta et al. (2018), when ACC patches
are applied at the workplace in real exposure scenarios, they could
provide important information on the actual ingress of chemicals
through the PPEs, as related with the task performed by the workers,
together with an accurate evaluation of dermal exposure.
Other studies also evaluated the influence of glove flexure on
permeation (Perkins and Rainey, 1997; Phalen and Hee, 2008; Nalin
9
Journal of Hazardous Materials 411 (2021) 125045
et al., 2020), suggesting that flexure could play a role together with
temperature, thickness variability, and intermittent use (Anna et al.,
1998; Phalen and Hee, 2008; Klingner and Boeniger, 2002). Here, we
could not correct for the influence of flexure and temperature on
chemical permeation. Nevertheless, the temperature in the box was
monitored for all experiments and it was found as 21.1 ± 2.2 ◦ C, while
the temperature for the standardized permeation experiments was
23 ± 1 ◦ C. Another important limitation is that relative humidity also
plays an important role in the absorbing properties of the ACC to VOCs
(INTERNATIONAL STANDARD, 2000). This is particularly true in real
exposure scenarios since the use of protective gloves often results in
higher perspiration of the hands (Branson et al., 1988). In this study, the
influence of the humidity was not tested. In further experimental
set-ups, we will try to monitor humidity underneath the gloves, espe­
cially if measuring more polar VOCs on ACC, such as acetone.
Even if the diffusion cell-based techniques are the current stan­
dardized methods to measure NBT and SSPR, different authors already
highlighted the necessity of performing field monitoring or laboratory
tests that takes into account the entire glove structure and not only the
glove materials (Banaee and Hee, 2019; Klingner and Boeniger, 2002;
Edward et al., 2010) or the application of a conceptual model to help
define the workplace protection factor for gloves (Wang et al., 2006;
Cherrie and Semple, 2004). In our study, besides evaluating the
permeation performance of the gloves, the main goal was to assess the
application of ACC patches as potential indicators for permeation and
penetration through PPE, and compare the results of this to the stan­
dardized permeation methods.
In conclusion, we have shown for the first time that ACC patches
could be useful to quantitatively assess glove permeation in a very se­
lective exposure scenario. This approach has a substantial added value
to the internationally standardized diffusion cell test for permeation
assessment, and it has been shown that results from this method could
actually alter the choice of PPE that may be chosen for specific use-case
scenarios. In future work, we need to extend this approach to test other
PPE such as whole-body coveralls, sleeves, boots, etc., and a bigger se­
lection of hazardous chemicals.
CRediT authorship contribution statement
Matteo Creta: Conceptualization, Methodology, Investigation,
Writing - Original Draft, Review & Editing. Luke D Savory: Conceptu­
alization, Methodology, Writing - Review & Editing. Radu-Corneliu
Duca: Conceptualization, Methodology. Wai Kei Chu: Investigation.
Katrien Poels: Methodology, Validation. Jin Pan: Investigation. Jia­
min Zheng: Investigation. Lode Godderis: Supervision, Writing - Re­
view & Editing. Mike Draper: Supervision, Conceptualization,
Methodology, Writing - Review & Editing. Jeroen A.J. Vanoirbeek:
Supervision, Conceptualization, Methodology, Writing - Review &
Editing.
Declaration of Competing Interest
The authors declare the following financial interests/personal re­
lationships which may be considered as potential competing interests:
The study has been financed by a grant from Ansell (U.K.) Limited (U.K.,
Hull) (R&D2018/1703). The following authors, Luke D Savory, Jin Pan,
Jiamin Zheng and Mike Draper are affiliated with Ansell Limited.
Acknowledgments
This study was supported by a grant from Ansell (U.K.) Limited (U.K.,
Hull) (R&D2018/1703).
Appendix A. Supporting information
Supplementary data associated with this article can be found in the
M. Creta et al.
online version at doi:10.1016/j.jhazmat.2021.125045.
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