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Tomi Juselius

Effect of Diesel Fuel Composition on Sealing


Materials

Metropolia University of Applied Sciences

Bachelor of Engineering

Automotive Engineering

Thesis

March 3, 2018
Acknowledgements

I would like to express my sincere gratitude to Neste Corporation, for giving me the op-
portunity to participate in this project and to write my Bachelor’s thesis in their facilities.
This project was an extremely fruitful continuation to my summer trainee period, and a
finalizer to my studies at Helsinki Metropolia University of Applied Sciences.

As this is my opportunity to express my gratitude to the people who have helped me to


succeed in this project, I would like to show my highest of thankfulness’s to my instructor
Mr. Kalle Lehto, Researcher, for valuable guidance and expertise in the field, to the de-
partment staff of the engine laboratory in the research and development unit, for making
the working conditions filled with a welcoming and a helpful atmosphere, and to my in-
structor Mr. Heikki Parviainen, Senior Lecturer at Helsinki Metropolia University of Ap-
plied Sciences, for all the help I needed. Special thanks also go to Trelleborg Sealing
Solutions Finland Oy and Trelleborg Sealing Solutions Germany GmbH, for providing me
with the materials tested during the experimental phases of this thesis, and to Mr. Janne
Autio, who through our friendship and his occupation, without hesitation, assisted me in
the experimental arrangements of this thesis.

I also thank my parents for the unceasing encouragement and support to succeed in my
studies by providing me with the necessities, so I could pursue my dreams and goals
with full efficiency.

Done at Porvoo, 3 March 2018,

Tomi Juselius
Abstract

Author Tomi Juselius


Title Effect of Diesel Fuel Composition on Sealing Materials

Number of Pages 102 pages + 3 appendices


Date March 3, 2018

Degree Bachelor of Engineering

Degree Programme Automotive Engineering

Professional Major Automotive Electronics Engineering

Kalle Lehto, Researcher, Neste Corporation


Instructors
Heikki Parviainen, Senior Lecturer, Helsinki Metropolia Univer-
sity of Applied Sciences

Through several already concluded tests it is known that fuel compositions have an effect
on how sealing materials react when exposed, but the results are not always easy to under-
stand or comparable.

This thesis provides Neste Corporation with research material on the effects of fuel compo-
sition on sealing materials at the research and development unit. The tests included in this
thesis were carried out in the engine laboratory of the research and development unit in
Kilpilahti, Porvoo.

In this thesis fuels and sealing materials, and their compatibility, especially in automotive
fuel systems, are studied. In the experimental part, sealing materials were tested by two
different standards, ASTM D471 and ASTM D395, which define the tests that simulate the
underlying conditions during vehicle usage such as temperature and mechanical compres-
sion.

Materials which are not fully compatible with fuels were also chosen to undergo the tests.
Experimenting these materials is important because it eases the visualization of extreme
reactions, which then helps to understand the results.

After the tests were successfully carried out, the differences between sealing materials could
be seen. Results pointed, that materials such as fluorocarbon and nitrile rubbers, which are
widely used in automotive fuel systems, showed minimal alteration. Instead, materials, such
as butyl and ethylene propylene diene rubbers, which are not knowingly used in applications
with imminent fuel contact, showed extreme reactions, which would be fatal for the designed
functionality of automotive fuel system applications.

Keywords sealant, fuel composition, experimental setup


Tiivistelmä

Tekijä(t) Tomi Juselius


Otsikko Dieselpolttoainekoostumuksen vaikutus tiivistemateriaaleihin

Sivumäärä 102 sivua + 3 liitettä


Päivämäärä 3.3.2018

Tutkinto Insinööri (AMK)

Koulutusohjelma Ajoneuvotekniikka

Suuntautumisvaihtoehto Autosähkötekniikka

Tutkija Kalle Lehto, Neste Oyj


Ohjaaja(t)
Lehtori Heikki Parviainen, Metropolia Ammattikorkeakoulu Oy

Useiden jo suoritettujen testien kautta tiedetään, että polttoainekoostumuksilla on vaikutus


siihen, kuinka tiivistemateriaalit reagoivat altistuttuaan, mutta tutkimustulokset eivät ole aina
helposti ymmärrettäviä tai vertailukelpoisia.

Tässä insinöörityössä laadittiin Neste Oyj:lle tutkimus polttoainekoostumuksien vaikutuk-


sista tiivistemateriaaleihin. Insinöörityöhön sisältyvät testit suoritettiin tutkimus- ja kehitys-
osaston moottorilaboratoriossa Porvoon Kilpilahdessa.

Insinöörityössä tarkastellaan polttoaineita ja tiivistemateriaaleja sekä niiden yhteensopi-


vuuksia erityisesti ajoneuvojen polttoainejärjestelmissä. Kokeellisessa osuudessa tiiviste-
materiaaleja koestettiin kahden eri standardin, ASTM D471 sekä ASTM D395, määrittämillä
testeillä, joissa simuloidaan ajoneuvokäytön aikaisia olosuhteita kuten lämpötilaa ja mekaa-
nista puristusta.

Kokeisiin valikoitiin myös materiaaleja, jotka eivät täysin sovellu yhteiskäyttöön polttoainei-
den kanssa. Näiden materiaalien kokeilu on tärkeää, koska silloin voidaan visualisoida ää-
rimmäiset reaktiot, joiden kautta tulosten ymmärtäminen helpottuu.

Kokeiden suorittamisen jälkeen voitiin havaita tiivistemateriaalien väliset erot. Tulokset


osoittivat, että materiaalit kuten fluori- ja nitriilikumit, joita laajalti käytetään ajoneuvojen polt-
toainejärjestelmissä, suoriutuivat testeistä minimaalisin vaihteluin. Sen sijaan materiaalit ku-
ten butyyli- ja eteeni-propeenikumit, joita ei tietoisesti käytetä sovelluksissa, joissa on välitön
polttoainekontakti, reagoivat erittäin voimakkaasti, mikä olisi kohtalokasta ajoneuvojen polt-
toainejärjestelmäsovellusten suunnitellulle toiminnalle.

Avainsanat tiiviste, polttoainekoostumus, koejärjestely


Contents

List of Abbreviations

1 Introduction 1

2 Use of Sealants 2

2.1 Automotive Applications 3


2.2 Adverse Effects of Fuel Composition 4

3 Presentation of the Experiments 7

3.1 Materials 7
3.1.1 Elastomers 7
3.1.2 Thermoplastics 13
3.2 Fuels 14
3.2.1 Petroleum Products 16
3.2.2 Biofuels 17
3.2.3 Blends 20
3.3 Test Standards 21
3.3.1 ASTM D471 21
3.3.2 ASTM D395 24

4 Experiments 31

4.1 Immersion Tests with Fluctuating Use of Diesel Fuels 31


4.1.1 Reports 38
4.2 Residual Compression 41
4.2.1 Report 44

5 Results 45

5.1 Fluctuating Immersions in Diesel Fuels 46


5.1.1 Petroleum Diesel → HVO → Petroleum Diesel 46
5.1.2 HVO → Petroleum Diesel → HVO 60
5.1.3 FAME → Petroleum Diesel → HVO 74
5.2 Residual Compressions 88

6 Summary of the Results 98


7 Conclusions 99

References 100

Appendices

Appendix 1. Technical Drawing of the Compression Set

Appendix 2. Result Lists for Fluctuating Immersions in Petroleum Diesel, FAME and HVO

Appendix 3. Result List for the Compression Set Tests


List of Abbreviations

AEM Ethylene acrylate rubber.

AFV Alternative-Fuel Vehicle. AFV is a vehicle equipped with an internal com-


bustion engine that operates with any other fuel than conventional fuels,
e.g. gasoline or diesel. An example would be a vehicle capable of running
only with fuel with high ethanol content

ASTM American Society for Testing and Materials. ASTM is an international


standardization organization

AU Polyester urethane.

EPDM Ethylene propylene diene rubber.

FFV Flex-Fuel Vehicle. FFV is a vehicle equipped with an internal combustion


engine that can operate with more than one fuel, which usually is gasoline
with or without any content of ethanol

FAME Fatty Acid Methyl Ester. FAME, also known as biodiesel, is a type of fuel
produced from animal fats or vegetable oils through a process known as
esterification

FKM Fluorocarbon rubber.

FVMQ Fluorosilicone rubber.

HNBR Hydrogenated acrylonitrile-butadiene rubber.

HVO Hydrotreated Vegetable Oil. HVO is fuel produced from animal fats or veg-
etable oils through a process of hydrotreating

IIR Butyl rubber.

NBR Acrylonitrile-butadiene rubber (nitrile rubber).


OEM Original Equipment Manufacturer. Manufacturer which manufactures the
original parts or equipment of a certain product

Ppm Parts per million. Ppm is a percent- and permille-like relative unit that indi-
cates how many parts of a million something is

PTFE Polytetrafluoroethylene.

R&D Research & Development. R&D refers to innovative activities in developing


new or improving existing services and products

VMQ Silicone rubber.


1

1 Introduction

The vast amount of different types and mixtures of petroleum and biofuels set high de-
mands for sealant manufacturers to find solutions that can withstand the effects of differ-
ent fuel compositions. Excellent chemical resistances are crucial for the required func-
tionality of sealants. There is not one sealant material that meets the requirements of all
applications in the automotive industry, and therefore, multiple solutions must be availa-
ble for a variety of needs. Even though researches and tests are carried out to find the
best sealant material that suits most automotive applications – the product development
does not stop.

In this thesis, several different types of OEM sealant materials used by the automotive
industry, especially in the automotive fuel systems, were tested and compared. The seal-
ants were experimented and differentiated by properties on how the different fuel com-
positions affected them. Sealants tested were made from elastomeric materials, except
for PTFE which is a thermoplastic polymer. These materials can be found in vehicle
applications all around the world.

This thesis was assigned by Neste Corporation as a research project at the engine la-
boratory located in Kilpilahti, Porvoo. Neste Corporation is a Finnish refining and mar-
keting company of high quality fuels, lubricants and chemicals, a pioneer in sustainable
development and a global market leader of renewable diesel [1]. Neste invests highly in
R&D in the field of renewable fuels which requires active suitability testing with current
technologies and materials – for example sealants, which this thesis investigates.

The tests were conducted by designing an experimental setup for the safe immersion of
sealant materials in fuels. A key factor during the tests was to simulate the conditions
such as temperature and mechanical pressure in which the sealants are used in vehicles
to get genuine results. During and after these test cycles analyzing, reporting and creat-
ing visual data for further use played a major role for the commissioner of this thesis,
Neste Corporation.

This thesis is divided into parts where theory leads to practice. First the background of
the thesis is explained; after that the experiments are conducted and the results are
analyzed.
2

2 Use of Sealants

Sealants are used to develop a static seal between two separate members of a mechan-
ical assembly and to maintain that seal under operating conditions, which may differ be-
cause of changes in pressure, temperature or a variety of chemical exposures. If two
surfaces could be connected perfectly, and if it was possible to maintain the intimate
contact under extreme conditions, a sealant would not be needed. However, since this
is not possible, sealants must be used because of the following reasons:

▪ size of the edges that require sealing in the application,

▪ difficulties in manufacturing a connecting surface so smooth that it would not re-


quire sealing,

▪ corrosion, erosion and other materialistic wear and tear on the surface of the
edges,

▪ the amount of sealable connections in a typical mechanical application.

A sealant provides a seal by utilizing external forces that compress the sealant material
between the connecting surfaces. The connection of the surfaces would be imperfect
without a sealant, and because of that, for a functioning sealant closure, three major
aspects must be considered for a sufficient seal to be achieved.

▪ enough force must be applied to the connection so that the sealant between it
squeezes into the surface structures and seals the connection,

▪ force must be sufficient, but not excessive, so that the sealant can maintain its
capabilities under operating conditions,

▪ sealant material must be chosen correctly for the desired application so that it
can withstand the effects, such as temperature in its whole range, pressure ex-
erted to the connection and exposure to the present chemicals. [2, p. 4.]
3

2.1 Automotive Applications

In automotive applications, sealants are used for blocking the passage of oils, fuels and
other liquids of chemical nature through the surface, joints or openings in the engine
compartment, fuel systems and other mechanical applications which require sealing.

Varying temperatures, pressures and chemical exposures, particularly in applications in


the engine compartment of a vehicle, set high requirements for the durability, perfor-
mance and resistivity of the sealants. A sealant that meets these requirements, should
also be lightweight, efficient and recyclable to lower the overall costs. [3, p. 3; 4.]

Especially in fuel systems, different fuel compositions can cause insidious effects and
serious damage to sealants. This requires high amounts of suitability research to find the
correct material because of the large selection of fuel types and blends available on the
market.

There are many affected components (figure 1) in a typical vehicle and all of these re-
quire a variety of sealants to function as designed. Components and the sealants af-
fected by fuel can be listed in the following order from the filling station to combustion in
cylinders:

▪ fuel filler and cap,

▪ fuel tank,

▪ fuel filters and fuel valves,

▪ fuel pumps,

▪ fuel lines,

▪ fuel line connectors,

▪ fuel rails,

▪ regulators and dampers,

▪ fuel injectors.
4

Figure 1. Affected components in fuel systems [4].

As the demand for better technologies increases in the automotive industry, the sealant
solutions must keep up with it. Constant testing and development of new materials and
products is required to meet the ever-changing needs. [3, p. 3.]

2.2 Adverse Effects of Fuel Composition

Fuels are known to influence certain types of elastomers, natural rubbers and plastics
used as sealants in automotive fuel systems [5, p. 26; 6, p. 121; 7; 8, p. 103]. Common
ways for the damage to occur is during longer periods of fuel storage. Fuels being vul-
nerable to oxygen causes fuels to oxidize and to form hydroperoxides and carboxylic
acids, which then causes damage to the immersed sealants. Oxidizing of fuels is more
of a problem with biofuels (especially FAME) than with fuels derived from petroleum. [9,
p. 25–26, 49.]

Variations in temperature and contamination of the fuel are known to accelerate the ad-
verse effects of chemical degradation. For example, FAME with even the smallest per-
centage of water can have a significant effect on the adverse reaction. [4.]
5

There are many alternatives on how sealant materials react when exposed to a chemical
for which it does not have good resistance to. Usually, the negative reactions have harm-
ful effects related to functionality, such as swelling (figure 2), which may cause the ma-
terial to soften, which can then lead to loss of sealing force and cause possible leaks
from the system. Other possible disadvantages are hardening and shrinkage of the ma-
terial, which usually leads to the material drying and losing its elasticity which then leads
to an eventual failure. [6, p. 121; 7.]

Figure 2. Example of volumetric swell on an elastomeric O-ring before and after immersion to
an inappropriate chemical [10, p. 33].

The degradation is not always as obvious as in figures 2, 3, 4 and 5, so other means of


damage identification must be conducted. There are various standardized tests to find
out the changes in the properties of elastomers.

Figure 3. Visible chemical degradation on an elastomeric O-ring [10, p. 34].


6

Adverse effects, visible and nonvisible, caused by chemical degradation, even by the
slightest margin, are irreversible, and therefore, it is important to perform a full environ-
mental check on the material selection [10, p. 34].

Figure 4. Visible chemical degradation on an elastomeric O-ring [10, p. 34].

Structural changes in elastomers posed by chemical degradation may promote the dam-
age caused by compression (figure 5), in applications where the sealant is exposed to
constant or momentary mechanical pressure. This effect, however, is usually quite rare
because of the high elastic properties of elastomeric substances. [10, p. 34.]

Figure 5. Fracturing of an elastomeric O-ring caused by over-compression [10, p. 34].


7

3 Presentation of the Experiments

The features of various fuels are known to have an influence of different results on seal-
ing materials when they are in direct contact for longer periods of time. These tests are
conducted extensively and the results are somewhat publicly released but the data avail-
able is not always clearly understandable or comparable.

The experiments in this thesis were carried out to provide Neste Corporation with test
results of the effects of fuel composition on sealing materials executed in their own facil-
ities. Experiments are divided into two major parts; one part being the standardized tests
ASTM D471 and ASTM D395 to sealant materials, and the other part being the analysis
of each material’s success and comparison of all the results.

3.1 Materials

Sealants are in most cases made from substances of rubber, known as elastomers,
which are sometimes combined with a strengthening part such as carbon, graphite, metal
or thermoplastics, such as PTFE [3, p. 7, 13; 2, p.15].

3.1.1 Elastomers

Elastomers are based on polymers which have the property of elasticity. Elastomers are
made up of long chains of carbon, hydrogen and oxygen atoms, which are cross-linked
with the neighboring chains. These cross-linking bonds pull the elastomer back in to
shape when the force causing the deforming is removed.

Elastomers are by far one of the most versatile engineering materials available. The ex-
traordinary property of being able to deform and recover under load makes them very
different from plastics and metals.

Though unique properties such as elasticity and resiliency apply to almost all variations
of elastomers, research on choosing the most suitable material for the desired applica-
tion must be conducted. Exposures to harsh chemicals, temperature extremes and
changes in pressure can exclude some materials for the intended application because
of complete incompatibility. [10, p. 4–5.]
8

The elastomeric materials for the tests were received from Trelleborg Sealing Solutions
Germany GmbH (table 1).

Table 1. List of elastomers received from Trelleborg Sealing Solutions Germany GmbH.

Material Category Supplier


AEM, ethylene acrylate rubber Elastomer Trelleborg Sealing Solutions Germany GmbH
EPDM, ethylene propylene
Elastomer Trelleborg Sealing Solutions Germany GmbH
diene rubber
FKM, fluorocarbon rubber Elastomer Trelleborg Sealing Solutions Germany GmbH
FKM, fluorocarbon rubber with
Elastomer Trelleborg Sealing Solutions Germany GmbH
higher fluorine content
FVMQ, fluorosilicone rubber Elastomer Trelleborg Sealing Solutions Germany GmbH
HNBR, hydrogenated acryloni-
Elastomer Trelleborg Sealing Solutions Germany GmbH
trile-butadiene rubber
IIR, butyl rubber Elastomer Trelleborg Sealing Solutions Germany GmbH
NBR, acrylonitrile-butadiene
Elastomer Trelleborg Sealing Solutions Germany GmbH
rubber (nitrile rubber)
AU, polyester urethane Elastomer Trelleborg Sealing Solutions Germany GmbH
VMQ, silicone rubber Elastomer Trelleborg Sealing Solutions Germany GmbH

Materials for the tests were chosen with anticipation of the fact that some might not be
suitable for applications with a possibility of fuel exposure. It is of high importance to
conduct tests also to these materials, so the results are much easier to compare, visual-
ize and understand.

Received materials were not directly mentioned by the material. Trelleborg Sealing So-
lutions uses their own codes to recognize the materials. Some of the materials are even
dyed to specific colors for easier identification. Material codes and colors can be identi-
fied as seen in table 2.

Table 2. Trelleborg Sealing Solutions material codes and colors.

Material Material code Colour


AEM, ethylene acrylate rubber ACT70 Black
EPDM, ethylene propylene
E7T70 Black
diene rubber
FKM, fluorocarbon rubber V7T30 Black
FKM, fluorocarbon rubber with
VCT7B Green
higher fluorine content
FVMQ, fluorosilicone rubber FCT30 Yellow
HNBR, hydrogenated acryloni-
H7T32 Black
trile-butadiene rubber
IIR, butyl rubber I7I03 Black
NBR, acrylonitrile-butadiene
N7T30 Black
rubber (nitrile rubber)
AU, polyester urethane Z20 Turquoise
VMQ, silicone rubber S7T30 Red
9

AEM, Ethylene Acrylate Rubber

Typical applications for AEM are all kinds of static seals in vicinity of oils as they occur
in gearboxes, oil pumps, cam covers and other similar applications. Operating tempera-
tures for AEM materials range from –40 °C to +160 °C and momentarily up to +190 °C.

AEM has excellent resistances to most oils and greases (even with aggressive addi-
tives), heat and ozone. It also shows good properties in colder climates. Special formu-
lations of AEM can be manufactured to have an increased resistance to chemicals. [11.]

EPDM, Ethylene Propylene Diene Rubber

Applications where glycol based brake fluids and hot water are used, are often sealed
using EPDM sealants. Temperature range for EPDM material operation is from –45 °C
to +150 °C and for a short period of time up to +175 °C. EPDM sealants vulcanized with
sulfur have a lowered temperature operation area of –45 °C to +130 °C (momentarily up
to +150 °C.)

EPDM sealants have good resistances to heat, ozone and aging. A high level of elastic-
ity, good behavior in lower temperatures as well as good insulation are also some of the
properties of EPDM. [12, p. 6.]

FKM, Fluorocarbon Rubber

FKM material is particularly known for its non-flammability, low gas permeability and ex-
cellent resistances to ozone, weathering and aging. Temperature range for FKM material
begin from –20 °C to +200 °C and +230 °C for a limited amount of time. Special formu-
lations of FKM material can function in temperatures as low as –35 °C. Common uses of
FKM materials are applications where direct contact with mineral based oil or grease is
certain at higher temperatures. [12, p. 7.]

Different structure and fluorine content can greatly influence the chemical resistance of
FKM [4.] For this reason, two types of FKM were received for the tests; one with so-
called standard properties and the second one with higher fluorine content, which in-
creases its resistance to chemicals.
10

FVMQ, Fluorosilicone Rubber

Good heat resistance, very good flexibility in low temperatures, good electrical properties
and excellent resistances to weather, ozone and UV rays are some of the features of
FVMQ materials. Compared to a standard silicone material, FVMQ has better chemical
resistance especially to hydrocarbons, aromatic mineral oils, fuels and low molecular
aromatic hydrocarbons such as benzene and toluene.

Temperature range for FVMQ materials range from –50 °C to +175 °C and temporarily
up to +200 °C. [12, p. 7.]

HNBR, Hydrogenated Acrylonitrile-Butadiene Rubber

HNBR material is made from NBR butadiene groups via selective hydrogenation. HNBR
material properties are dependent on the ACN (acrylonitrile) content, ranging from 18 %
to 50 %, as well as the materials degree of saturation. Operating temperatures for HNBR
material range between –30 °C to +140 °C with time limited extensions of up to +160 °C.
Special types of HNBR can be used in temperatures as low as –40 °C.

HNBR materials show good mechanical properties and functions well with mineral oils
and greases. [12, p. 7.]

IIR, Butyl Rubber

IIR has a very low permeability for gas and moisture. On top of that, the material shows
good resistance to many organic and inorganic chemicals, ozone, weathering and aging.
The electrical insulating properties of IIR are also excellent.

Range of temperature where IIR materials function, ranges from –40 °C to +110 °C and
momentarily up to +120 °C. [12, p. 7.]
11

NBR, Acrylonitrile-Butadiene Rubber (Nitrile Rubber)

NBR material properties are highly dependent on the ACN content ranging from 18 % to
50 %. Suitable formulations of NBR have good mechanical properties and they work well
with mineral based oils and greases.

Temperature range for NBR starts from –30 °C to +100 °C (momentarily up to +120 °C.)
Specially formulated NBR can be used in temperatures as low as –60 °C. [12, p. 7.]

AU, Polyester Urethane/EU, Polyether Urethane

In general polyurethanes are an exceptionally complex group of elastomeric materials.


Typically, polyurethanes are individually designed for the intended purpose of applica-
tion, and because of this it is hard to unify any of its unique properties.

Temperature range for polyurethanes starts from –50 °C to +110 °C, with feasibility to
go even higher. [12, p. 7.]

In automotive fuel systems, the chosen polyurethane should be polyester because it is


more resistant to oils, fuels, fuel vapors and solvents. [13.]

VMQ, Silicone Rubber

VMQ has excellent heat resistance, cold flexibility and dielectric properties as well as
good resistance to weather, ozone and UV rays. Special formulations of VMQ work well
with aliphatic engine and gear oils, high temperature water and high-molecular chlorin-
ated hydrocarbons.

Operating temperature for VMQ materials is between –50 °C to +175 °C, and for a short
period up to +230 °C. [12, p. 7.]
12

Operating temperature ranges of different elastomers are shown in the figure (figure 6)
in a more comparable and reader-friendly manner.

Temperature Ranges of Received Elastomers

AEM

EPDM

FKM

FVMQ

HNBR

IIR

NBR

AU/EU

VMQ

-70 -20 +30 +80 +130 +180 +230 +280 +330


Temperature (°C)

Operating temperature range


Temperatures achievable only for a limited amount of time or with special materials

Figure 6. Temperature ranges of different elastomers used in automotive applications.


13

3.1.2 Thermoplastics

A thermoplastic polymer consists of long, unlinked polymer molecules generally with a


high molecular weight. Thermoplastics form a crystalline structure under cooler temper-
atures, resulting in a smooth surface and significant structural strength. As the tempera-
ture rises, thermoplastics gradually soften and gain some elastic properties until they
eventually melt.

Seals fabricated or strengthened with thermoplastics are used in applications where


sealing materials such as elastomers fail to meet the required temperature range, chem-
ical resistance or friction and wear requirements. Strengthening sealants means cover-
ing it with the thermoplastic to give it some of the extraordinary properties (figure 7).

Figure 7. PTFE strengthened elastomer O-ring and gasket.

PTFE, Polytetrafluoroethylene

Pure PTFE is a white waxy solid which has remarkable properties because of its unique
molecular structure. PTFE has a wide temperature range of –270 °C to +260 °C with a
melting point of +342 °C, excellent resistivity for degradation and heat-aging, and shows
no alteration in physical properties during temperature cycling. It has one of the lowest
friction coefficients in solid materials and exceptional dry running ability because of its
self-lubricating capabilities. PTFE also precludes reactions, for example decompression
under pressure and swelling when exposed to chemicals with virtually all industrial ap-
plications – even at elevated conditions. [14, p. 7.]

In automotive applications, PTFE has emerged as one of the most common type of ther-
moplastic polymer for sealants.
14

PTFE materials for the tests were received from Trelleborg Sealing Solutions Finland Oy
(table 3).

Table 3. List of compounded PTFEs received from Trelleborg Sealing Solutions Finland Oy.

Material Category Supplier


Virgin PTFE compounded
Thermoplastic Trelleborg Sealing Solutions Finland Oy
with Turcon® additive
Virgin PTFE compounded
Thermoplastic Trelleborg Sealing Solutions Finland Oy
with carbon and graphite

Thermoplastic materials which were obtained from Trelleborg Sealing Solutions Finland
Oy, were not pure PTFE because of their availability and rather infrequent usage due to
their softness.

As the received elastomers, PTFE materials also have their own codes and colors with
which they are identified from. Material codes and colors can be seen in table 4.

Table 4. Trelleborg Sealing Solutions material codes and colors.

Material Material code Colour


Virgin PTFE compounded
T51 Turquoise
with Turcon® additive
Virgin PTFE compounded
T05 Black
with carbon and graphite

The compounded materials which were received are commonly used in automotive ap-
plications [15].

3.2 Fuels

The reason why some fuels cause vigorous reactions and others do not, is because fuels
differ from each other in many ways. The main differences are the base material which
they are processed from, renewability, processing method, chemical composition and
the characteristics of performance. [5; 6.]

This chapter comprehensively investigates fuels and their differences from a general
point of view. During the execution of the tests in chapter 4, the fuels used are presented
more specifically.
15

Concepts

Flash point is the lowest temperature where vapors of the material will ignite, when given
an ignition source.

Cetane rating is a diesel fuel rating or a number which indicates the time between the
start of the injection and the first identifiable pressure increase during combustion. Higher
cetane rating refers to a shorter ignition delay, or in other words, how easily the fuel can
be ignited. Good cetane number is required for a diesel to properly start and warm-up
with an even combustion in low temperatures. [6, p. 119; 16, p. 83.) In Europe, diesel is
required by the standard EN 590 to have a cetane rating of at least 51 [17, p. 17].

Pour point is the temperature below which the liquid comes semi-solid and loses its flow-
ing characteristics [6, p. 119; 16, p. 83]. Pour point, however, is not regulated in Europe
[18].

Cloud point refers to a temperature below that causes the waxes in diesel fuel to form a
cloudy appearance which thickens the oil and clogs filters and injectors. Fuel suppliers
distribute fuels with cloud point for the climate conditions of the area. [6, p. 119; 16, p.
83.)

Sulfur content influences the life cycle of engines. Sulfur in fuel creates sulfuric acid dur-
ing combustion process, which can damage the engine and cause piston ring wear. Reg-
ulations and standards have limited the sulfur content amount to less than 10 ppm be-
cause high sulfur content also contributes to acid rain. [16, p. 83; 17, p. 17.)

Octane rating indicates the level of compression a fuel can withstand before igniting.
Lower octane ratings may lead to engine knock which can be harmful to the engine. [16,
p. 54.]

Reid vapor pressure is the pressure of the vapor above the fuel when the fuel is at 38
°C. High vapor pressure eases the starting of an engine in cold weather since gasoline
will not burn without air. [16, p. 51.]
16

3.2.1 Petroleum Products

Petroleum or crude oil formed from the remains of tiny sea plants and animals that
passed away millions of years ago and sank to the depths of the oceans [6, p. 3.] This
makes petroleum products nonrenewable, because their rate of renewability is not suffi-
cient enough for a sustainable economic extraction in timeframes meaningful to human
[6, p. 41].

Petroleum consists of a complex mixture of various hydrocarbons, mostly of alkenes and


aromatic compounds [6, p. 3].

Diesel

Petroleum diesel, which is simply referred to as diesel, is composed of drastically varying


amounts of saturated and aromatic hydrocarbons [18]. Diesel is sold in various grades
of quality which are characterized by the sulfur and aromatic content, ignition quality
(cetane rating), properties in cold weather, content of pollutants, viscosity, density and
boiling point. Petroleum diesel has a flash point of at least +55 °C which categorizes it
as a combustible liquid. [6, p. 125; 17, p. 17.]

Emission wise, untreated diesel fuel contains a high amount of sulfur and because of
that desulfurization is required, so that the product can meet the standard requirements.
For example, the diesel fuels used in Europe are under the diesel fuel standard EN 590
which requires diesel to have less than 10 ppm of sulfur [5, p. 72; 17, p. 17). Lowering
the sulfur content reduces the lubricity of the fuel which then requires use of lubricating
additives. Good-quality diesel fuel contain additives such as detergents, dispersants, rust
preventatives, and metal deactivators. [6, p. 125; 16, p. 83.] Oxidation inhibitors are
sometimes added as a preservative, but this is not common [18].

Gasoline

Gasoline is motor fuel derived from petroleum with high energy amount and a high oc-
tane number [8, p. 42]. Gasoline consists of hydrocarbons and several additives which
are added to enhance its properties. Since the regulations and standards have declined
the use of lead in gasoline, other components have been introduced to help maintain the
antiknock properties of gasoline. These octane improvers can be grouped into two broad
categories: aromatic hydrocarbons and alcohols such as ethanol. [16, p. 53; 18.]
17

Because of the high octane rating, gasoline cannot be used in diesel engines. High oc-
tane rating means low cetane rating which then means that gasoline would not ignite, or
would ignite at the wrong time. This would cause damage either to the engine or emission
control components.

Gasoline properties and trade policies in Europe are defined in the EN 228 standard [19,
p. 10].

3.2.2 Biofuels

The share of biofuels in automotive industry have come to stay due to the numerous
benefits, such as renewability and cycle of life, reduction of greenhouse emissions, sus-
tainability, regional development, reduction of rural poverty and to increase fuel security.
[6, p. 17; 18.]

Biofuels are derived from various sources of renewable material such as carbohydrates
which includes grains and sugars, animal fats, vegetable oils and biomasses including
wood, stalk and grasses. [6, p. 16.]

Currently, there are three types of liquid biofuels as alternative or replacement for petro-
leum products: FAME and HVO for petroleum diesel, and ethanol for gasoline. Main dif-
ferences between biofuels and petroleum fuels is the oxygen content, except for HVO
which because of other similarities to petroleum diesel does not contain any oxygen [5,
p. 3, 38; 18]. FAME and ethanol have a 10 to 45 % weight content of oxygen, whereas
petroleum fuels have essentially none, making the chemical properties very different
from the properties of petroleum. [6, p. 17.]

Biodiesel

Biodiesel is a renewable fuel for diesel engines that is comprised of mono-alkyl esters of
long-chain fatty acids processed from animal fats or vegetable oils [6, p. 102]. Biodiesel,
also known as FAME, has to meet the requirement standard EN 14214 which validates
biodiesel manufactured through esterification chemistry, when used as a blending com-
ponent [5, p. 3, 9; 6, p. 117].
18

FAME differs from petroleum diesel in many ways. Advantages are higher flash point of
+150 °C which makes biodiesel nonflammable and nonexplosive. This leads to safety
benefits in situations of an accident. FAME is also biodegradable, nontoxic and it con-
tains virtually no sulfur which significantly reduces toxins and some emissions when
burned as a fuel. [6, p. 102].

Disadvantages of biodiesel are that it produces less power and torque because of a 5 to
10 % less energy content which then leads to higher fuel consumption [6, p. 121]. Higher
viscosity, higher cloud and pour point, and higher emissions of nitrogen oxides are also
downsides of biodiesel. Precautions for cold climate use should also be considered be-
cause FAME tends to gel earlier than petroleum diesel upon cooling. [6, p. 102.]

Bioethanol

Ethanol is a renewable fuel for gasoline engines. Majority of the world’s ethanol is pro-
duced from corn, sugarcane and beet molasses [6, p. 17]. Ethanol consists of 52 %
carbon, 13 % hydrogen and 35 % oxygen. It is a colorless and highly flammable liquid
with a boiling point of +78 °C and boiling point of –114 °C [6, p. 73].

When put to comparison with gasoline, ethanol has higher octane rating, broader flam-
mability, higher flame speeds and heats of vaporization. These features allow higher
compression ratio, faster burn time and leaner engine which results in better level of
efficiency. [6, p. 73; 8, p. 101–102.]

Disadvantages when compared to gasoline are lower energy density, corrosiveness and
functionality in cold starts because of its low vapor pressure. As well as gasoline, pure
ethanol is not suitable for diesel engines because of its high-octane and low cetane rat-
ing, and high heat of vaporization that causes problems with self-ignition. [6, p. 73; 8, p.
101–102; 18.]

Exceptions to the compatibility of ethanol in diesel engines are products such as ED95
and RED95. These products are designed for heavy transport usage and they consist of
95 % bioethanol and a small percentage of additives. Additives such as ignition improv-
ers, denaturants, lubricants and anticorrosive additives are added to optimize combus-
tion suitable for operation in modified diesel engines. [18; 20; 21.]
19

HVO

HVO is also a type of renewable diesel which often is falsely considered to be a similar
type of biodiesel as FAME [22]. Unlike FAME, HVO is processed through hydrotreating
chemistry, and therefore, it cannot be recognized by the same EN 14214 standard as
FAME, because of the differences in the processing method and the chemical composi-
tion [5, p. 4, 9].

Though HVO is produced from renewable sources, it still has a lot of similarities as pe-
troleum diesel. Like petroleum diesel, HVO is also fully composed of hydrocarbons [5, p.
6]. HVO is a mixture of straight chain and branched paraffin except for that HVO does
not contain significant amounts of aromatics or naphthene, which are not beneficial for a
clear combustion [5, p. 4]. As the diesel fuel standard EN 590 does not regulate the raw
material used to produce fuels or the processing method, HVO technically meets the
requirements, except for minimum density which is below the lower limit [5, p. 6].

For paraffinic diesel fuels, such as HVO, there is a standard EN 15940. Since paraffinic
content is practically impossible to measure, the fuels meeting the standard are limited
to have basically zero content of aromatics. [5, p. 6.]

Overall, HVO has similar properties as petroleum diesel and does not need any modifi-
cations to the engine. Few advantageous exceptions are very high cetane rating ranging
from 70 to 95, cleaner combustion (figure 8), and therefore, lower emissions because
HVO contains less than 5 ppm of sulfur and no aromatics. [5, p. 4, 7, 17, 47; 22.]
20

Figure 8. Smoke testing of HVO and petroleum diesel from left to right respectively [23].

HVO can be used as it is or mixed with either bio or petroleum diesel [5, p. 24–25].

3.2.3 Blends

The blends of previously mentioned fuels are commonly used, either to increase the
properties of fuel or the usage of renewable sources.

Diesel Blends

Diesels can be blended in many ways. Blends containing petroleum and biodiesel are
known as B5, B7, B20 etc. The amount of blending contents the product may contain is
standardized, for example the diesel fuel standard EN 590 limits the use of FAME to 7
%, but allows blending of HVO without any limit. Diesel fuel blend using the maximum
amount of biodiesel defined in EN 590 standard, would be then known as B7. Other
blends are B10, which meets the EN 16734 standard, and B20, and B30 which are de-
fined by the EN 16709 standard. As in EN 590, the standards EN 16734 and EN 16709
does not regulate the amount of blended HVO. [5, p. 7–9.]

Because of its extraordinary properties HVO can be used to increase the quality of the
base diesel fuel, such as increasing the cetane rating or lowering the emissions by de-
creasing the amount of sulfur and aromatics [5, p. 17–19; 18].
21

E5, E10 and E85

Ethanol can be mixed with gasoline to make blends such as E5, E10 and E85 to increase
the use of renewable fuel sources and at the same time some of gasolines properties
such as octane rating. The contents of ethanol in gasoline are defined in standard EN
228 and the requirements for ethanol when used as a blending component are defined
in the EN 15376 standard. [19, p. 10, 14.]

Blends with lower percentage of ethanol consistency can be used without any engine
modifications, but blends such as E85 will function only in alternative (AFV) or flex-fuel
vehicles (FFV) [6, p. 18; 19, p. 31].

3.3 Test Standards

Standards used are shortly briefed in the following chapters to give basic information of
what to expect from the tests. Requirements could not be followed entirely because of
limitations set by the lack of equipment.

How the standards were implemented in the making of this thesis are explained during
the execution of the experiments in chapter 4.

3.3.1 ASTM D471

This standard covers the procedures to evaluate the abilities of certain rubbers and rub-
ber-like compositions to withstand the effects of liquids unchanged [24, p. 1.] Though
PTFE is not a rubbery substance, same tests will be conducted to it because of its com-
mon usage in similar type of applications as elastomers.

One of the main points in ASTM D471 is to simulate the service conditions in the de-
signed use through controlled accelerated testing [24, p. 3.] Comprehensive amounts of
possible experiments are defined in the standard to find out the variables in sealants
properties after immersion in fuel. These include tests such as elongation, tensile
strength and hardness, but because of inadequate equipment to perform most of the
them, only the following were covered in this thesis [24, p. 1]:
22

change in mass (before and after immersion), which was calculated using the following
equation [24, p. 9]:

(𝑀2 − 𝑀1 )
∆𝑀, % = ∗ 100 (1)
𝑀1

where:

∆M change in mass, %,
M1 initial mass of specimen, g,
M2 mass of specimen after immersion, g,

change in length, width and thickness (before and after immersion), which were calcu-
lated using the following equations [24, p.9]:

(𝐿 − 𝐿0 )
∆𝐿, % = ∗ 100 (2)
𝐿0

where:

∆L change in length, %,
L0 initial length of specimen, mm,
L length of specimen after immersion, mm,

(𝑊 − 𝑊0 )
∆𝑊, % = ∗ 100 (3)
𝑊0

where:

∆W change in width, %,
W0 initial width of specimen, mm,
W width of specimen after immersion, mm,
23

(𝑇 − 𝑇0 )
∆𝑇, % = ∗ 100 (4)
𝑇0

where:

∆T change in thickness, %,
T0 initial thickness of specimen, mm,
T thickness of specimen after immersion, mm,

and visual inspections (before and after immersion), which were executed with the help
of a checklist presented later in chapter 4.1.

Standard defines that the specimens used are to be cut from each material sheet into a
rectangular shape, having dimensions of approximately 25 by 50 by 2.0 mm (figure 9).
Each specimen must be separately weighed to the closest milligram and measured to
be as identical in size as possible. [24, p. 6].

Figure 9. Test specimen proportions.

Materials used to suspend the specimens may not contaminate the test liquid and the
setup must be made so that the specimens are not able to touch each other during the
immersion period [24, p. 6.]
24

In actual product testing procedures, temperatures and immersion periods for the tests
are picked with anticipation of the designed service conditions or by what was agreed
between the customer and supplier. Test temperatures and immersion periods are de-
fined in the standard (table 3 & 4) [24, p. 3–4].

Table 5. Test temperatures [23, p. 3]. Table 6. Immersion periods [24, p. 4].

Test Temperature Immersion Periods


°C h

–75 ± 2 22 ± 0,25 (or 1 %)


–50 ± 2 46 ± 0,25 (or 1 %)
–25 ± 2 70 ± 0,25 (or 1 %)
–10 ± 2 166 ± 0,25 (or 1 %)
0±2 670 ± 0,25 (or 1 %)
+23 ± 2 1006 ± 0,25 (or 1 %)
+50 ± 2 2998 ± 0,25 (or 1 %)
+70 ± 2 4990 ± 0,25 (or 1 %)
+85 ± 2
+100 ± 2
+125 ± 2
+150 ± 2
+175 ± 2
+200 ± 2
+225 ± 2
+250 ± 2

After the immersion period is over, specimens are to be cleaned and lightly blotted dry
of lint and excess material with filter paper. After that they are once again to be weighed,
measured and inspected as before the immersion. [24, p. 6].

When the tests are completed, the results are to be handled as averages before and
after the immersions [24, p. 6.]

3.3.2 ASTM D395

This test method covers the testing of rubber intended for use in applications in which
the rubber will be subjected to compressive stresses in air or in liquid media [25, p. 1.]

This test is intended to measure the ability of rubber compounds to retain elastic proper-
ties after prolonged action of compressive stresses [25, p. 1.] Standardized test method
requires the test specimens to be cut into a cylindrical shape of 29 mm in diameter with
a given thickness of 12.5 mm or 13 mm in diameter with 6 mm in thickness [25, p. 2.]
25

Larger specimen size would have been preferred for easier visualization, but because of
availability of certain material thicknesses, this could not be followed and exceptions
were made in the sizing of the specimen.

The specimens used in this thesis have dimensions of 30 mm in diameter and 6 mm in


thickness (figure 10.) The bigger size required by the standard was imitated to be as
close as possible by using two plied specimens of the same material to make the total
thickness of the specimen to 12 mm.

Figure 10. Test specimen proportions.

Standard allows the use of plied specimens but it is to be noted that the results may vary
from solid blocks, because of the possibility of trapped air between the specimens. Par-
ticular care must be present when assembling the compression set so that the circular
faces of the specimens are parallel. [25, p. 2.]

A compression set is used to compress the specimens down to 9.5 mm in thickness,


using a similar kind of a setup as in figure 11. Compression set used in this thesis is built
in the part 3.3.2.1. Compression process in the standard is suggested to last either 22
or 70 hours in a temperature which can be regulated to be identical for each test [25, p.
6.]
26

Figure 11. Illustration of the compression process [24, p. 5; 25].

Residual compression is measured using a micrometer from the center of the com-
pressed specimen after opening the compression set and allowing the specimen recover
for 30 minutes [25, p. 5; 6.] Figure 12 illustrates the possible effects of prolonged com-
pression.

Figure 12. Effect of low and high residual compression on an elastomer

a) Original unconstrained specimen

b) Original specimen compressed

c) Specimen when compressive force has been removed showing low compression

d) Specimen when compressive force has been removed showing high compression
[10, p. 33.]

Residual compression is expressed as a percentage of the compressed material which


has not recovered after the recovery period. In practice: 0 percent indicates full recovery
and 100 percent indicates no recovery.
27

Residual compression was calculated using the following equation [25, p. 6]:

𝐶 = [(𝑡𝑜 − 𝑡𝑓 )/(𝑡𝑜 − 𝑡𝑠 )] ∗ 100 (5)

where:

C residual compression expressed as percentage,


𝑡𝑜 original thickness of the specimen, mm,
𝑡𝑓 final thickness of the specimen, mm,
𝑡𝑠 spacer bar thickness, mm.

After the results of all the tests have been obtained, comparison can be carried out to
spot the effects of different fuel compositions on the material’s capability to resist residual
compression.

3.3.2.1 Building the Compression Set

Technical drawing (appendix 1) for the compression set was designed with a profes-
sional-grade 2D design program DraftSight developed by Dassault Systèmes.

Requirements for the compression set are defined by the Test Method ASTM D395 [25,
p. 6.]. Main pieces of the construction are the 20 mm thick steel plates, which when
tightened squeeze the rubber specimens placed in between to the 9.5 mm thickness
limited by the spacers. Tightening was done by welding nuts with 130 mm long M20
threaded rods to the base plate, which when assembled allowed tightening as seen in
figure 13.
28

Figure 13. Compression set assembly.

Smooth finish was required on the surfaces which are in direct contact with the speci-
mens [25, p. 5–6.] This was executed with 0.5 mm thick acid-proof metal sheets with the
same shape as the 20 mm plates.

Design was fulfilled into reality by a professional metal worker, who through his occupa-
tion was able to offer laser cutting services. The technology of laser cutting provides
precision, excellent work quality and swiftness beyond human capabilities (figure 14.)
29

Figure 14. Laser cutting parts for the compression set.

Manufacturing the spacers for the compression set required some changes to the first-
hand drawing because of material availability and machining possibilities. Steel plates
were not available in 9.5 mm thickness, so either they had to be milled from 10 mm thick
steel plates or piled up from different thicknesses. The latter proved to be an easier so-
lution, and the spacers were manufactured from two pieces of 4 mm thick steel plates
and one piece of 1.5 mm thick steel plate, to then reach the summarized thickness of 9.5
mm (figure 15). Spacer pieces were slightly welded together for easier usage.
30

Figure 15. Spacer-build using the layering technique to reach the required thickness.

Results of the build came out to be exactly as planned. Figure 16 shows all the pieces
of the set and the set from different angles when it is assembled. The compression cham-
bers where the rubber specimens are placed can be seen in the bottom right corner of
the collage.

Figure 16. Compression set.


31

4 Experiments

The main interest in the tests was in fluctuating immersions and residual compressions
of sealant materials in petroleum diesel, FAME and HVO. The availability of several
grades from which the customer can freely choose when fueling causes unavoidable
mixes, which the sealant must withstand by retaining its properties and the required func-
tionality, so that the sealed application may function as designed.

4.1 Immersion Tests with Fluctuating Use of Diesel Fuels

There are strict requirements for the equipment used in the Test Method ASTM D471,
but because of limitations set by the lack of equipment, standardized test setup require-
ments were not the uppermost concern.

The tests began with the preparation of the specimens. Elastomeric materials from Trel-
leborg Sealing Solutions Germany GmbH (table 1) were received as material sheets with
approximate dimensions of 200 mm by 200 mm by 2.0 mm (figure 17).

Figure 17. Test material sheet of VMQ, silicone rubber (S7T30).


32

Derived from the size of the test sheets, a total of 32 specimen pieces could be cut from
one sheet. Since two sheets were received, a total of 64 material specimens of each
material were available for the tests conducted in this thesis.

PTFE materials from Trelleborg Sealing Solutions Finland Oy (table 2) were received as
approximately 3 mm thick material sheets with uneven dimensions. Regardless of the
uneven size, it was possible to cut the required number of specimens for the tests.

Immersion container was chosen to be a metal container with approximately one-liter


capacity, which when processed as designed in figure 18, allowed the simultaneous im-
mersion of six specimens. The specimens were suspended using stainless steel wiring.
Attaching the specimens on to the lid of the container eased the specimen immersions
tremendously.

Figure 18. Illustration of the immersion container with the specimen setup.
33

The idea of the fluctuating immersion test was to immerse the same specimen alternately
in petroleum diesel, HVO and again in petroleum diesel, and vice versa in HVO, petro-
leum diesel and HVO. One immersion path also included the use of FAME, and the im-
mersions path was carried out as FAME, petroleum diesel and HVO.

The way the immersions were designed to be executed, was to immerse three speci-
mens of each sealant material in to each of the diesels, and after a prearranged period
of one week or 166 hours (table 6), move all the specimens of each material into a con-
tainer designed to hold the same material, but with a different grade of diesel. This was
repeated until the immersions were conducted as follows (figures 19–21):

Week 1. Week 2. Week 3.


Three (3) specimens of Move the specimens Move the once
each material in from petroleum diesel switched specimens
petroleum diesel. to HVO. from HVO back to
petroleum diesel.

Petroleum diesel HVO Petroleum diesel

Figure 19. Immersion path of petroleum diesel → HVO → petroleum diesel.

Week 2. Week 3.
Week 1.
Move the specimens Move the once
Three (3) specimens of
from HVO to petroleum switched specimens
each material in HVO.
diesel. from petroleum diesel
back to HVO.

HVO Petroleum diesel HVO

Figure 20. Immersion path of HVO → petroleum diesel → HVO.


34

Week 2. Week 3.
Week 1.
Move the specimens Move the once
Three (3) specimens of
from FAME to switched specimens
each material in FAME.
petroleum diesel. from petroleum diesel
to HVO.

FAME Petroleum diesel HVO

Figure 21. Immersion path of FAME → petroleum diesel → HVO.

During each transfer, the specimens were measured with a caliper, photographed,
weighed with GWB Mettler AM100 scale and visually inspected for comparison (figure
22).

Figure 22. Inspection station for the weighing and placing of the specimens on to the lid-specimen
contraptions.

The amount of materials and safety regulations prevented the use of individual contain-
ers for each material, so two materials had to be placed in the same container. Materials
were merged in the same container by the presumed reactions, so the possible dissolved
media would not compromise the results of the material which was anticipated to have
better success in the tests. Materials were paired as seen in table 7.
35

Table 7. Material pairings.

Container number Materials


1. AEM, ethylene acrylate rubber FVMQ, fluorosilicone rubber
EPDM, ethylene propylene diene
2. IIR, butyl rubber
rubber
FKM, fluorocarbon rubber with
3. FKM, fluorocarbon rubber
higher fluorine content
NBR, acrylonitrile-butadiene rub- HNBR, hydrogenated acrylonitrile-
4.
ber (nitrile rubber) butadiene rubber
5. AU, polyester urethane VMQ, silicone rubber
Virgin PTFE compounded with Virgin PTFE compounded with car-
6.
Turcon® additive bon and graphite

The metal containers used to immerse the specimens (figure 23) were marked in several
ways to avoid the interference of losing track of which container held which material.

Figure 23. Prepared specimen containers.

During the first phase of the tests, which did not include any use of fuel, a simple marker
was used to mark, and so, recognize the materials in the containers. The materials were
marked with the abbreviations of the material types. The same base material composi-
tions were differentiated with a sequential numbering representing the appearance order
in tables 1 and 3.
36

For the possibility of a fuel spillage soaking the ink or the ink notwithstanding the heat of
the oven in the latter phases, the specimens were also marked with steel wiring and
different sizes and amounts of washers from the steel wire which suspended the speci-
mens.

Due to any process deviation or confusion, the containers were placed inside the oven
according to the immersion paths as follows:

▪ bottom shelf had the immersion path of petroleum diesel → HVO → petroleum
diesel,

▪ middle shelf had the immersion path of HVO → petroleum diesel → HVO,

▪ top shelf had the immersion path of FAME → petroleum diesel → HVO.

Container placements on each of the shelves (figure 24) were done so that each of the
containers had identical amount of space from the inner surfaces of the oven and from
the other containers.

Figure 24. Container placements in the oven.


37

The tests were executed in an oven (figure 25) with a regulated temperature of +50 (± 2)
°C, as defined by the standard in table 3. Increased test temperature imitates the genuine
conditions of vehicle usage, and at the same time, accelerates the possible adverse re-
actions [4].

Figure 25. SalvisLab Thermocenter oven used to heat the specimen containers filled with fuels.

For the specimen inspections and switches, a stand was built for easier processing (fig-
ure 26). The way the stand was utilized, was by placing the lid-specimen contraption on
to it to cool the specimens, and at the same time, free both hands on to inspection of the
specimens.

Figure 26. A stand to hold the lid-specimen contraptions for easier processing.
38

To ease the visual inspections of the specimens an inspection checklist was made to
quicken the recording and to keep the descriptions of the results identical, and therefore,
easier to compare (table 8).

Table 8. Visual inspection checklist for immersed materials.

The possible adverse effects of chemical degradation are listed. Each of them have unique
letter corresponding to the possible effect.
Number placed after the letter implies the level of damage. Scale is from 1 to 5, where 1 is
minor and 5 is high level of damage.
An example on how the checklist works, A2 would indicate medium swelling.

A Specimen has visually swollen compared to the original size.


B Specimen has visually shrunk compared to the original size.
C Specimen has softened compared to the original state.
D Specimen has hardened compared to the original state.
E Visible deformation of the specimen.

Abbreviations of the visual inspection results were then listed, along with the specimen
weights and dimensions, after each immersion period to the result lists (appendix 2).

4.1.1 Reports

As an addition to the results, Test Method ASTM D471 requires that all known infor-
mation of the tested specimens, test conditions, dates, test cycle lengths, equipment
used and any process deviations must be precisely reported.

The tests were carried out during a consecutive period of three weeks. Each of the weeks
were individually reported. The first report included the most comprehensive amount of
the information regarding the specimens, test conditions, dates, test cycle lengths and
equipment used, whereas the reports of the following weeks focused on any possible
process deviations and remarks, since the conditions did not change during the tests,
except for the immersion paths explained in the previous chapter.

Immersions were conducted in accordance with the Test Method D471 to a point which
was doable with the available equipment and safety regulations.
39

Week 1 (Jan 3 – Jan 10, 2018) Report

Descriptions of the samples and their origins (tables 9 & 10):

Table 9. Elastomeric material descriptions.

Elastomers
Supplier Trelleborg Sealing Solutions Germany GmbH
Date of vulcanization 27th of November 2017 (conditions unknown)
Specimens prepared 27th of December 2017

Table 10. PTFE material descriptions.

PTFE
Supplier Trelleborg Sealing Solutions Finland Oy
Date of manufacturing Unknown
Specimens prepared 9th of December 2017

▪ materials were processed and stored in a room temperature of +23 (± 2) °C,

▪ oven mentioned in the previous chapter was used to heat the fuels to a tem-
perature of +50 (± 2) °C,

▪ exposure period was set to be 166 ± 0,25 (or 1 %) hours,

▪ tests began on January 3rd of 2018 at 15:45,

▪ results are shown and deduced in chapters 5 and 6.

As a plausible process deviation, it was noted that the oven used was not able to
perform the whole 166 ± 0,25 (or 1 %) hours test cycle without rebooting it manually.
It was also noted through past experiences that the oven might shut down due to un-
known reasons. The consequences of a premature shutdown were minimized by
checking up on the oven at the beginning, throughout and at the end of each day.

Notes: During the first week, the oven shutdown by itself on three occasions, totaling
about 10 hours of inactive heating. Specimen inspections were started on Jan-
uary 10th of 2018, at 7:14.
40

Week 2 (Jan 10 – Jan 17, 2018) Report

▪ Inspections of the first week’s immersions were done on January 10 th of 2018,


between 7:14 and 15:34.

▪ Specimens were re-immersed in the second fuel grade and the oven was re-
started on January 10th of 2018, at 16:15.

Notes: During the second week, the oven shutdown by itself only on one occasion,
totaling about 5 hours of inactive heating. Specimen inspections were started
on January 17th of 2018, at 7:10.

Week 3 (Jan 17 – Jan 24, 2018) Report

▪ Inspections of the second week’s immersions were done on January 17th of


2018, between 7:10 and 14:05.

▪ Specimens were re-immersed in the third and final fuel grade and the oven
was restarted on January 17th of 2018, at 14:29.

Notes: Specimen inspections were started on January 24 th of 2018, at 7:34.

The tests were finished on January 24th of 2018, at 14:15.


41

4.2 Residual Compression

The residual compression tests were only implemented to elastomeric materials. The
reason for this was because PTFE is not a rubbery substance, and therefore, does not
show an elastic behavior sufficient enough to provide reliable results in this test method.
[4.]

Materials did not need any preparations since they were already processed by the sup-
plier, Trelleborg Sealing Solutions Germany GmbH (figure 27).

Figure 27. Test material buttons of VMQ, silicone rubber (S7T30).

The tests began with the materials being compressed without any effective fuel compo-
nent to find out the material’s own unique resistivity to residual compression (figure 28).
The same oven was used as in the immersion tests (figure 30). Compression time was
set to be 70 hours in a temperature of +50 (± 2) °C.

Figure 28. Specimens placed into the compression set.


42

After the first test cycle was completed, the compression set was taken out of the oven
and allowed to cool. After cooling, the set was opened and the specimens were removed
and allowed to recover for 30 minutes before using a micrometer to measure the final
thicknesses of the specimens, which were then recorded in the result list (appendix 3).

After the test without any effective fuel component, the specimens were once again pre-
pared and placed into the compression set. Then, the set was placed into a slightly larger
container and filled with fuel, so that the specimens were completely submerged (figure
29).

Figure 29. Compression set submerged in petroleum diesel.

When filled, the container was placed into the oven having similar conditions as in the
previous test cycle (figure 30).
43

Figure 30. Compression set in the oven without and with an effective fuel component.

(Immersion containers above the compression set in the right figure were not tested
as a part of this thesis)

After the test involving the use of fuel was completed, most of the fuel was pumped out
to lighten the container. Then it was pulled out and allowed to cool. When the compres-
sion set was cooled, it was then lifted to a dry container to avoid any spillage of fuel and
opened. The specimens were then removed and allowed to recover for 30 minutes. After
the recovery period, the specimens were measured with a micrometer and the results
were then recorded in the result list (appendix 3).

After each test which involved the use of fuel, the compression set was cleaned thor-
oughly to exclude any possibility of specimen contamination in the tests conducted af-
terwards with different fuel compositions.

After the completion of all the test cycles, the results could be processed and calculated
to find out the resistivity for residual compression of the materials in various conditions.
44

4.2.1 Report

Test Method ASTM D395 also required that the tests had to be precisely reported. The
report consisted of information about the tested materials, original dimensions and thick-
nesses of the specimens, time and temperature of the test, whether or not the surfaces
of the specimens were lubricated, final thicknesses of the specimens after removing the
specimens from the set and letting them recover for 30 minutes, and which of the meth-
ods in ASTM D395 was used to test the specimens.

Compression Set Report

▪ Sample descriptions and origins were the same as mentioned in table 9.

▪ Compression set tests were carried out using the test method B of Test Method
D395,

▪ materials were stored in a room temperature of +23 (± 2) °C,

▪ specimen surfaces were not lubricated in any of the test cycles,

▪ the same oven used in the Test Method D471 was used to heat specimens to
a temperature of +50 (± 2) °C,

▪ results are shown and deduced in chapters 5 and 6.

Notes: Test without an effective fuel component was started on January 30 th of 2018,
at 11:47 and finished on February 2nd of 2018, at 11:34.

Test with petroleum diesel was started on February 2 nd of 2018, at 12:59 and
finished on February 5th of 2018, at 11:34.

Test with HVO was started on February 5th of 2018, at 13:15 and finished on
February 8th of 2018, at 11:45.

Test with FAME was started on February 9 th of 2018, at 9:59 and finished on
February 12th of 2018, at 7:54.
45

5 Results

In this chapter, the results of the experiments conducted in the previous chapter are
presented in both visual and graphical form.

From the results and the deductions in the end of each subchapter, it can be seen which
of the materials would function the best in such conditions as simulated in the tests.

The columns in the graphs in the following chapters are colored to represent the effective
diesel fuel composition, as follows:

▪ black stands for petroleum diesel,

▪ red stands for FAME,

▪ green stands for HVO.

In the residual compression tests, the column which represents the test cycle which was
conducted without an effective diesel fuel composition is colored in blue, which stands
for “in air.”
46

5.1 Fluctuating Immersions in Diesel Fuels

The results of the fluctuating immersion tests are reported separately. Each of the test
materials is discussed and reported by the immersion path. Materials are listed in the
appearance order as seen in tables 1 and 3.

5.1.1 Petroleum Diesel → HVO → Petroleum Diesel

This chapter presents the results of the immersion path of petroleum diesel → HVO →
petroleum diesel (figures 31–54).

The photographs of the specimens were taken immediately after thorough examination,
which included weighing of the specimens, measuring of the dimensions of the speci-
mens and visual inspections.

The graphs were created on the basis of the data averages, which were acquired from
the recorded data (appendix 2) using the previously mentioned equations in chapter
3.3.1 (equations 1–4).

Average change in size was calculated from the change in length, width and thickness
of specimen, as it was expected that the size change was equal in each of the dimen-
sions. The measurement accuracy of the caliper and the scale used was calculated to
be approximately ± 2 %.
47

AEM, Ethylene Acrylate Rubber

Figure 31. AEM, ethylene acrylate rubber, in its prepared state and after weekly immersions in
petroleum diesel → HVO → petroleum diesel from left to right respectively.

AEM AEM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
5,05% -0,08% 6,29% 11,95% -1,26% 11,84%

Figure 32. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
48

EPDM, Ethylene Propylene Diene Rubber

Figure 33. EPDM, ethylene propylene diene rubber, in its prepared state and after weekly immer-
sions in petroleum diesel → HVO → petroleum diesel from left to right respectively.

EPDM EPDM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
33,07% 29,45% 33,67% 107,36% 86,69% 106,14%

Figure 34. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
49

FKM, Fluorocarbon Rubber

Figure 35. FKM, fluorocarbon rubber, in its prepared state and after weekly immersions in petro-
leum diesel → HVO → petroleum diesel from left to right respectively.

FKM 1 FKM 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
-1,11% -1,03% 0,14% 0,16% 0,10% 0,31%

Figure 36. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
50

FKM, Fluorocarbon Rubber with Higher Fluorine Content

Figure 37. FKM, fluorocarbon rubber with higher fluorine content, in its prepared state and after
weekly immersions in petroleum diesel → HVO → petroleum diesel from left to right
respectively.

FKM 2 FKM 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
-2,15% -1,98% -1,14% 0,16% 0,10% 0,33%

Figure 38. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
51

FVMQ, Fluorosilicone Rubber

Figure 39. FVMQ, fluorosilicone rubber, in its prepared state and after weekly immersions in pe-
troleum diesel → HVO → petroleum diesel from left to right respectively.

FVMQ FVMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
1,91% 1,33% 2,89% 2,30% 1,44% 2,23%

Figure 40. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
52

HNBR, Hydrogenated Acrylonitrile-Butadiene Rubber

Figure 41. HNBR, hydrogenated acrylonitrile-butadiene rubber, in its prepared state and after
weekly immersions in petroleum diesel → HVO → petroleum diesel from left to right
respectively.

HNBR HNBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
3,36% 0,17% 4,54% 9,68% 1,07% 9,42%

Figure 42. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
53

IIR, Butyl Rubber

Figure 43. IIR, butyl rubber, in its prepared state and after weekly immersions in petroleum diesel
→ HVO → petroleum diesel from left to right respectively.

IIR IIR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
32,30% 29,83% 33,85% 91,51% 76,59% 92,59%

Figure 44. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
54

NBR, Acrylonitrile-Butadiene Rubber (Nitrile Rubber)

Figure 45. NBR, acrylonitrile-butadiene rubber (nitrile rubber), in its prepared state and after
weekly immersions in petroleum diesel → HVO → petroleum diesel from left to right
respectively.

NBR NBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
1,88% -0,85% 2,50% 4,86% -1,38% 4,45%

Figure 46. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
55

AU, Polyester Urethane

Figure 47. AU, polyester urethane, in its prepared state and after weekly immersions in petroleum
diesel → HVO → petroleum diesel from left to right respectively.

AU AU
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
2,03% 0,63% 2,95% 4,49% 1,05% 4,64%

Figure 48. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
56

VMQ, Silicone Rubber

Figure 49. VMQ, silicone rubber, in its prepared state and after weekly immersions in petroleum
diesel → HVO → petroleum diesel from left to right respectively.

VMQ VMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
17,30% 18,32% 19,23% 37,29% 36,54% 38,14%

Figure 50. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
57

Virgin PTFE compounded with Turcon® additive

Figure 51. Virgin PTFE compounded with Turcon® additive in its prepared state and after weekly
immersions in petroleum diesel → HVO → petroleum diesel from left to right respec-
tively.

PTFE 1 PTFE 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
0,39% 0,39% 0,27% 0,19% 0,21% 0,34%

Figure 52. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
58

Virgin PTFE compounded with carbon and graphite

Figure 53. Virgin PTFE compounded with carbon and graphite in its prepared state and after
weekly immersions in petroleum diesel → HVO → petroleum diesel from left to right
respectively.

PTFE 2 PTFE 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
DI HVO DI DI HVO DI
0,29% 0,47% 1,77% 0,45% 0,48% 0,69%

Figure 54. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in petroleum diesel → HVO → petroleum diesel.
59

To summarize the results in the immersion path of petroleum diesel → HVO → petroleum
diesel, the elastomeric materials were ranked by the average magnitude of the reactions
to give an idea of the suitability in conditions as simulated in the test (table 11).

The following results are based only on the results gained from the previously conducted
tests. In actual material selection procedures, many other material properties must be
carefully examined to find the most suitable material for the designed application.

PTFE materials were left outside of the ranking system, because of their unique proper-
ties which are not comparable to elastomers.

Rank Material Effects


FKM 1 showed slight shrinkage in this immersion path. Other than
1. FKM 1
that, the material succeeded with the most minimal alteration.
FKM 2 showed slight shrinkage in this immersion path. Other than
2. FKM 2
that, the material succeeded as well as FKM 1.
NBR showed minimal swelling and increase in weight in this immer-
3. NBR
sion path.
AU showed minimal swelling and increase in weight in this immer-
4. AU
sion path.
FVMQ showed minimal swelling and increase in weight in this im-
5. FVMQ
mersion path.
HNBR showed swelling and medium increase in weight in this im-
6. HNBR
mersion path.
AEM showed swelling and medium increase in weight in this immer-
7. AEM
sion path.
VMQ showed high swelling and increase in weight in this immersion
8. VMQ
path.
IIR showed extremely high swelling and increase in weight in this
9. IIR
immersion path.
EPDM showed extremely high swelling and increase in weight in
10. EPDM
this immersion path.

Table 11. Suitability rankings of the elastomeric materials in immersion path of petroleum diesel
→ HVO → petroleum diesel.

Judging by the results, FKM 1, FKM 2, NBR, AU and FVMQ would be able to function
properly in conditions which were simulated in this immersion path. HNBR, AEM, VMQ,
IIR and EPDM showed reactions which would not be tolerated in fuel system applica-
tions, and therefore, cannot be recommended for usage in such conditions.
60

5.1.2 HVO → Petroleum Diesel → HVO

This chapter presents the results of the fluctuate immersion path of HVO → petroleum
diesel → HVO (figures 55–78).

The photographs of the specimens were taken immediately after thorough examination,
which included weighing of the specimens, measuring of the dimensions of the speci-
mens and visual inspections.

The graphs were created on the basis of the data averages, which were acquired from
the recorded data (appendix 2) using the previously mentioned equations in chapter
3.3.1 (equations 1–4).

Average change in size was calculated from the change in length, width and thickness
of specimen, as it was expected that the size change was equal in each of the dimen-
sions. The measurement accuracy of the caliper and the scale used was calculated to
be approximately ± 2 %.
61

AEM, Ethylene Acrylate Rubber

Figure 55. AEM, ethylene acrylate rubber, in its prepared state and after weekly immersions in
HVO → petroleum diesel → HVO from left to right respectively.

AEM AEM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
0,33% 5,03% 0,22% -1,39% 10,82% -2,60%

Figure 56. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
62

EPDM, Ethylene Propylene Diene Rubber

Figure 57. EPDM, ethylene propylene diene rubber, in its prepared state and after weekly immer-
sions in HVO → petroleum diesel → HVO from left to right respectively.

EPDM EPDM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
26,78% 29,93% 28,21% 84,79% 104,62% 85,65%

Figure 58. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
63

FKM, Fluorocarbon Rubber

Figure 59. FKM, fluorocarbon rubber, in its prepared state and after weekly immersions in HVO
→ petroleum diesel → HVO from left to right respectively.

FKM 1 FKM 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
-1,43% -1,37% -0,52% 0,07% 0,24% 0,17%

Figure 60. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
64

FKM, Fluorocarbon Rubber with Higher Fluorine Content

Figure 61. FKM, fluorocarbon rubber with higher fluorine content, in its prepared state and after
weekly immersions in HVO → petroleum diesel → HVO from left to right respectively.

FKM 2 FKM 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
0,94% 1,39% 2,06% 0,08% 0,23% 0,20%

Figure 62. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
65

FVMQ, Fluorosilicone Rubber

Figure 63. FVMQ, fluorosilicone rubber, in its prepared state and after weekly immersions in HVO
→ petroleum diesel → HVO from left to right respectively.

FVMQ FVMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
1,76% 2,45% 2,73% 1,34% 2,29% 1,43%

Figure 64. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
66

HNBR, Hydrogenated Acrylonitrile-Butadiene Rubber

Figure 65. HNBR, hydrogenated acrylonitrile-butadiene rubber, in its prepared state and after
weekly immersions in HVO → petroleum diesel → HVO from left to right respectively.

HNBR HNBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
0,82% 4,18% 1,79% -0,18% 9,45% 0,66%

Figure 66. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
67

IIR, Butyl Rubber

Figure 67. IIR, butyl rubber, in its prepared state and after weekly immersions in HVO → petro-
leum diesel → HVO from left to right respectively.

IIR IIR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
27,89% 31,95% 30,65% 71,65% 90,82% 76,20%

Figure 68. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
68

NBR, Acrylonitrile-Butadiene Rubber (Nitrile Rubber)

Figure 69. NBR, acrylonitrile-butadiene rubber (nitrile rubber), in its prepared state and after
weekly immersions in HVO → petroleum diesel → HVO from left to right respectively.

NBR NBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
-1,33% 0,52% -0,73% -1,57% 4,45% -1,80%

Figure 70. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
69

AU, Polyester Urethane

Figure 71. AU, polyester urethane, in its prepared state and after weekly immersions in HVO →
petroleum diesel → HVO from left to right respectively.

AU AU
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
0,71% 2,51% 1,64% 0,61% 4,47% 1,03%

Figure 72. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
70

VMQ, Silicone Rubber

Figure 73. VMQ, silicone rubber, in its prepared state and after weekly immersions in HVO →
petroleum diesel → HVO from left to right respectively.

VMQ VMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
17,53% 17,89% 18,94% 35,25% 38,65% 35,36%

Figure 74. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
71

Virgin PTFE compounded with Turcon® additive

Figure 75. Virgin PTFE compounded with Turcon® additive in its prepared state and after weekly
immersions in HVO → petroleum diesel → HVO from left to right respectively.

PTFE 1 PTFE 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
1,86% 1,31% 0,98% 0,10% 0,16% 0,15%

Figure 76. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
72

Virgin PTFE compounded with carbon and graphite

Figure 77. Virgin PTFE compounded with carbon and graphite in its prepared state and after
weekly immersions in HVO → petroleum diesel → HVO from left to right respectively.

PTFE 2 PTFE 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
HVO DI HVO HVO DI HVO
0,18% 0,37% 0,57% 0,42% 0,59% 0,52%

Figure 78. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in HVO → petroleum diesel → HVO.
73

To summarize the results in the immersion path of HVO → petroleum diesel → HVO, the
elastomeric materials were ranked by the average magnitude of the reactions to give an
idea of the suitability in conditions as simulated in the test (table 12).

The following results are based only on the results gained from the previous test. In
actual material selection procedures, many other material properties must be carefully
examined to find the most suitable material for the designed application.

PTFE materials were left outside of the ranking system, because of their unique proper-
ties which are not comparable to elastomers.

Rank Material Effects


FKM 1 showed slight shrinkage in this immersion path. Other than
1. FKM 1
that, the material succeeded with the most minimal alteration.
FKM 2 showed slight shrinkage in this immersion path. Other than
2. FKM 2
that, the material succeeded as well as FKM 1.
NBR showed minimal swelling and some increase in weight in this
3. NBR
immersion path.
AU showed minimal swelling and increase in weight in this immer-
4. AU
sion path.
FVMQ showed swelling and increase in weight in this immersion
5. FVMQ
path.
AEM showed swelling and medium increase in weight in this immer-
6. AEM
sion path.
HNBR showed swelling and medium increase in weight in this im-
7. HNBR
mersion path.
VMQ showed high swelling and increase in weight in this immersion
8. VMQ
path.
EPDM showed extremely high swelling and increase in weight in
9. EPDM
this immersion path.
IIR showed extremely high swelling and increase in weight in this
10. IIR
immersion path.

Table 12. Suitability rankings of the elastomeric materials in immersion path of HVO → petro-
leum diesel → HVO.

Judging by the results, FKM 1, FKM 2, NBR, AU and FVMQ would be able to function
properly in conditions which were simulated in this immersion path. AEM, HNBR, VMQ,
EPDM and IIR showed reactions which would not be tolerated in fuel system applica-
tions, and therefore, cannot be recommended for usage in such conditions.
74

5.1.3 FAME → Petroleum Diesel → HVO

This chapter presents the results of the fluctuate immersion path of FAME → petroleum
diesel → HVO (figures 79–102).

The photographs of the specimens were taken immediately after thorough examination,
which included weighing of the specimens, measuring of the dimensions of the speci-
mens and visual inspections.

The graphs were created on the basis of the data averages, which were acquired from
the recorded data (appendix 2) using the previously mentioned equations in chapter
3.3.1 (equations 1–4).

Average change in size was calculated from the change in length, width and thickness
of specimen, as it was expected that the size change was equal in each of the dimen-
sions. The measurement accuracy of the caliper and the scale used was calculated to
be approximately ± 2 %.
75

AEM, Ethylene Acrylate Rubber

Figure 79. AEM, ethylene acrylate rubber, in its prepared state and after weekly immersions in
FAME → petroleum diesel → HVO from left to right respectively.

AEM AEM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
22,32% 4,92% -0,06% 62,35% 11,85% -2,16%

Figure 80. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
76

EPDM, Ethylene Propylene Diene Rubber

Figure 81. EPDM, ethylene propylene diene rubber, in its prepared state and after weekly immer-
sions in FAME → petroleum diesel → HVO from left to right respectively.

EPDM EPDM
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
19,85% 32,58% 29,25% 63,10% 105,68% 85,80%

Figure 82. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
77

FKM, Fluorocarbon Rubber

Figure 83. FKM, fluorocarbon rubber, in its prepared state and after weekly immersions in FAME
→ petroleum diesel → HVO from left to right respectively.

FKM 1 FKM 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
-1,86% -1,10% -0,57% 0,35% 0,36% 0,20%

Figure 84. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
78

FKM, Fluorocarbon Rubber with Higher Fluorine Content

Figure 85. FKM, fluorocarbon rubber with higher fluorine content, in its prepared state and after
weekly immersions in FAME → petroleum diesel → HVO from left to right respectively.

FKM 2 FKM 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
1,16% 1,71% 2,35% 0,28% 0,27% 0,22%

Figure 86. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
79

FVMQ, Fluorosilicone Rubber

Figure 87. FVMQ, fluorosilicone rubber, in its prepared state and after weekly immersions in
FAME → petroleum diesel → HVO from left to right respectively.

FVMQ FVMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
0,44% 1,03% 1,60% 2,12% 2,22% 1,34%

Figure 88. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
80

HNBR, Hydrogenated Acrylonitrile-Butadiene Rubber

Figure 89. HNBR, hydrogenated acrylonitrile-butadiene rubber, in its prepared state and after
weekly immersions in FAME → petroleum diesel → HVO from left to right respectively.

HNBR HNBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
10,98% 5,15% 2,13% 25,11% 8,90% 0,02%

Figure 90. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
81

IIR, Butyl Rubber

Figure 91. IIR, butyl rubber, in its prepared state and after weekly immersions in FAME → petro-
leum diesel → HVO from left to right respectively.

IIR IIR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
20,35% 32,45% 30,54% 57,51% 93,50% 77,84%

Figure 92. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
82

NBR, Acrylonitrile-Butadiene Rubber (Nitrile Rubber)

Figure 93. NBR, acrylonitrile-butadiene rubber (nitrile rubber), in its prepared state and after
weekly immersions in FAME → petroleum diesel → HVO from left to right respectively.

NBR NBR
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
6,16% 2,75% 1,02% 13,55% 3,38% -2,79%

Figure 94. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
83

AU, Polyester Urethane

Figure 95. AU, polyester urethane, in its prepared state and after weekly immersions in FAME →
petroleum diesel → HVO from left to right respectively.

AU AU
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
3,31% 2,66% 1,69% 6,62% 4,87% 1,06%

Figure 96. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
84

VMQ, Silicone Rubber

Figure 97. VMQ, silicone rubber, in its prepared state and after weekly immersions in FAME →
petroleum diesel → HVO from left to right respectively.

VMQ VMQ
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
7,06% 17,74% 19,56% 14,41% 37,74% 34,43%

Figure 98. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
85

Virgin PTFE compounded with Turcon® additive

Figure 99. Virgin PTFE compounded with Turcon® additive in its prepared state and after weekly
immersions in FAME → petroleum diesel → HVO from left to right respectively.

PTFE 1 PTFE 1
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
0,47% 1,06% 0,87% 0,11% 0,10% 0,07%

Figure 100. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
86

Virgin PTFE compounded with carbon and graphite

Figure 101. Virgin PTFE compounded with carbon and graphite in its prepared state and after
weekly immersions in FAME → petroleum diesel → HVO from left to right respec-
tively.

PTFE 2 PTFE 2
Average change in size Average change in weight
120% 120%

100% 100%

80% 80%

60% 60%

40% 40%

20% 20%

0% 0%

-20% -20%
FAME DI HVO FAME DI HVO
0,44% 0,70% 0,99% 0,40% 0,47% 0,79%

Figure 102. Average changes in size and weight of the specimens compared to the original state
after weekly immersions in FAME → petroleum diesel → HVO.
87

To summarize the results in the immersion path of FAME → petroleum diesel → HVO,
the elastomeric materials were ranked by the average magnitude of the reactions to give
an idea of the suitability in conditions as simulated in the test (table 13).

The following results are based only on the results gained from the previous test. In
actual material selection procedures, many other material properties must be carefully
examined to find the most suitable material for the designed application.

PTFE materials were left outside of the ranking system, because of their unique proper-
ties which are not comparable to elastomers.

Rank Material Effects


FKM 1 showed slight shrinkage in this immersion path. Other than
1. FKM 1
that, the material succeeded with the most minimal alteration.
FKM 2 showed slight shrinkage in this immersion path. Other than
2. FKM 2
that, the material succeeded as well as FKM 1.
FVMQ showed minimal swelling and increase in weight in this im-
3. FVMQ
mersion path.
AU showed swelling and medium increase in weight in this immer-
4. AU
sion path.
NBR showed medium swelling and increase in weight in this immer-
5. NBR
sion path.
HNBR showed medium swelling and high increase in weight in this
6. HNBR
immersion path.
VMQ showed high swelling and increase in weight in this immersion
7. VMQ
path.
AEM showed high swelling and extremely high increase in weight in
8. AEM
this immersion path.
IIR showed extremely high swelling and increase in weight in this
9. IIR
immersion path.
EPDM showed extremely high swelling and increase in weight in
10. EPDM
this immersion path.

Table 13. Suitability rankings of the elastomeric materials in immersion path of FAME → HVO
→ petroleum diesel.

Judging by the results, FKM 1, FKM 2, FVMQ and AU would be able to function properly
in conditions which were simulated in this immersion path. NBR showed notable reac-
tions when introduced to FAME, and therefore, cannot be recommended for usage in
such conditions even though the material recovered when exposed to other fuel compo-
sitions. HNBR, VMQ, AEM, IIR and EPDM showed reactions which would not be toler-
ated in fuel system applications, and therefore, cannot be recommended for usage in
such conditions.
88

5.2 Residual Compressions

The results for the residual compressions are individually presented by each of the ma-
terial. Materials are listed in the appearance order as seen in table 1.

The graphs (figures 103–112) were created on the basis of the recorded data (appendix
3), using the previously mentioned equation in chapter 3.3.2 (equation 5). The measure-
ment accuracy of the micrometer used was calculated to be ± 1 %.

AEM, Ethylene Acrylate Rubber

AEM
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
9,83% 13,66% 12,27% 14,38%

Figure 103. Residual compression in AEM when compressed in air, petroleum diesel, FAME and
HVO from left to right respectively.

AEM showed propensity to residual compression, which was increased by an effective


fuel component. Being exposed to HVO showed the highest amount of residual com-
pression followed by petroleum diesel and FAME respectively.
89

EPDM, Ethylene Propylene Diene Rubber

EPDM
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
6,62% 15,02% 11,00% -8,30%

Figure 104. Residual compression in EPDM when compressed in air, petroleum diesel, FAME
and HVO from left to right respectively.

EPDM showed propensity to residual compression, which was affected by an effective


fuel component. Being exposed to petroleum diesel showed the highest amount of re-
sidual compression followed by FAME.

HVO caused the material to swell during the recovery period beyond the thickness of
the untested specimen, and therefore, the residual compression of the material is neg-
ative.
90

FKM, Fluorocarbon Rubber

FKM 1
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
9,84% 17,89% 14,84% 14,35%

Figure 105. Residual compression in FKM 1 when compressed in air, petroleum diesel, FAME
and HVO from left to right respectively.

FKM 1 showed propensity to residual compression, which was increased by an effec-


tive fuel component. Being exposed to petroleum diesel showed the highest amount of
residual compression followed by FAME and HVO respectively.
91

FKM, Fluorocarbon Rubber with Higher Fluorine Content

FKM 2
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
19,60% 19,94% 20,31% 20,57%

Figure 106. Residual compression in FKM 2 when compressed in air, petroleum diesel, FAME
and HVO from left to right respectively.

FKM 2 showed one of the highest propensities to residual compression, but almost
completely negated the effects of any fuel type in the results.
92

FVMQ, Fluorosilicone Rubber

FVMQ
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
5,32% 11,02% 13,37% 12,23%

Figure 107. Residual compression in FVMQ when compressed in air, petroleum diesel, FAME
and HVO from left to right respectively.

FVMQ showed propensity to residual compression, which was increased by an effective


fuel component. Being exposed to FAME showed the highest amount of residual com-
pression followed by HVO and petroleum diesel respectively.
93

HNBR, Hydrogenated Acrylonitrile-Butadiene Rubber

HNBR
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
13,96% 22,15% 19,22% 15,53%

Figure 108. Residual compression in HNBR when compressed in air, petroleum diesel, FAME
and HVO from left to right respectively.

HNBR showed propensity to residual compression, which was increased by an effective


fuel component. Being exposed to petroleum diesel showed the highest amount of re-
sidual compression followed by FAME and HVO respectively.
94

IIR, Butyl Rubber

IIR
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
12,29% 22,17% 17,57% 19,99%

Figure 109. Residual compression in IIR when compressed in air, petroleum diesel, FAME and
HVO from left to right respectively.

IIR showed propensity to residual compression, which was increased by an effective fuel
component. Being exposed to petroleum diesel showed the highest amount of residual
compression followed by HVO and FAME respectively.
95

NBR, Acrylonitrile-Butadiene Rubber (Nitrile Rubber)

NBR
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
5,68% 5,48% 10,21% 6,18%

Figure 110. Residual compression in NBR when compressed in air, petroleum diesel, FAME and
HVO from left to right respectively.

NBR showed propensity to residual compression which was slightly affected by HVO
and petroleum diesel respectively.

As in the immersion test, NBR showed more notable reactions to FAME compared to
any other fuel type.
96

AU, Polyester Urethane

AU
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
14,14% 14,83% 6,92% 13,99%

Figure 111. Residual compression in AU when compressed in air, petroleum diesel, FAME and
HVO from left to right respectively.

AU showed propensity to residual compression which was slightly affected by petroleum


diesel and HVO.

Being exposed to FAME showed the least amount of residual compression.


97

VMQ, Silicone Rubber

VMQ
Residual compression
25,00%

20,00%

15,00%

10,00%

5,00%

0,00%

-5,00%

-10,00%

-15,00%

-20,00%
- DI FAME HVO
8,46% 6,51% 7,36% 6,28%

Figure 112. Residual compression in VMQ when compressed in air, petroleum diesel, FAME and
HVO from left to right respectively.

VMQ showed propensity to residual compression, which was affected by an effective


fuel component. Being exposed to HVO showed the least amount of residual compres-
sion followed by petroleum diesel and FAME respectively.
98

6 Summary of the Results

This chapter summarizes the results gained from the conducted tests, individually subti-
tled by the test method used.

ASTM D471

In the results gained from the immersion tests, it was clearly visible that FKM 1 and FKM
2 transcended the other materials in all of the immersion paths. NBR, AU and FVMQ
overall showed excellent results, but with a few exceptions which would require extra
attention before usage in the designed application.

AEM, HNBR, VMQ, IIR and EPDM showed varying results in all of the immersion paths
from minor to extreme reactions, and therefore, cannot be recommended for usage in
any application with imminent fuel contact.

PTFE materials, as anticipated, were completely inert in all of the immersion paths, ex-
cept for changes which can be explained with the tolerances in the measurement accu-
racies.

ASTM D395

Residual compression tests showed varying results which could not be directly con-
cluded from the immersion tests. Success in this test method would be either minimal
residual compression in the tested conditions, or equal amount of residual compression
regardless of the effective fuel composition.

Almost all of the materials showed fluctuation in the results, which made the interpreting
of the results dependent on the reviewer and the designated application. However, FKM
2 showed the most equal amount of residual compression in all tested conditions, which
points out that the material was not affected by any of the fuel compositions used in the
test. NBR also showed some uniformity in the amount of residual compression in various
conditions with the exception of FAME, as in the immersion test, in which the material
showed considerably higher residual compression than in petroleum diesel or HVO. AU
also succeeded in the tests with uniform results except for FAME, in which the material
showed the least amount of residual compression.
99

7 Conclusions

This thesis investigated the effects of diesel fuel composition on sealing materials. The
increased use of alternative solutions and sources to produce fuels with different com-
positions for vehicles equipped with internal combustion engines demand constant re-
search and development in all applications with even the slightest possibility of fuel con-
tact.

The tests carried out in this thesis covered only a part of what could have been done,
because most of the defined tests would have required specific equipment and machin-
ery, which are limitedly available and are of high cost. The experiments conducted in this
thesis still provided valuable data; though the regulations could not be followed to full
extent even in the tests which were carried out. Therefore, the results are not in complete
accordance with the test methods, and therefore, cannot be used for other than informa-
tional purposes. However, this thesis describes the used testing procedure very precisely
and comprehensively.

As for the results gained, it was clearly visible which of the materials succeeded in the
tests. Success in this kind of tests points out that the material could be safely used as a
sealant in applications with similar conditions as in what was simulated in the experi-
ments. Reactions on each individual material were in most cases as anticipated in com-
prehensive research and information received from trusted sources.

Due to time limitations set by the extent of a Bachelor’s thesis, all the pre-designed tests
could not be conducted. However, this thesis covers all the required information for Test
Methods ASTM D471 and D395, if the need would arise in the future.

As an interesting continuation for the experiments conducted in this thesis, tests with a
wider range of fuel compositions and blends, longer immersion periods and higher tem-
peratures would give new and different kinds of results. Also, simulating the conditions
of vehicle usage even further with fluctuating temperature and using fuels with plausible
contaminations, such as water or foreign chemicals, which could be found in fuel tanks
through condensation or neglectful washing of a vehicle, would be interesting. Other
possible contaminants in fuel are micro-organisms and all kinds of debris. Use of deteri-
orated fuel is also a possible scenario, because of the surprisingly short shelf life of fuel.
[26; 27.]
100

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Appendix 1
1 (1)

Technical Drawing of the Compression Set

Part Amount Material

1. 3 Steel

Acid-proof
2. 4
steel

3. 2 Steel

2.
1.

3.
Appendix 2
1 (3)

Result Lists for Fluctuating Immersions in Petroleum Diesel, FAME and HVO
Appendix 2
2 (3)
Appendix 2
3 (3)
Appendix 3
1 (1)

Result List for the Compression Set Tests

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