Fuel Test Astm d396
Fuel Test Astm d396
Fuel Test Astm d396
I Disclaimer
This manual was prepared as an account of work sponsored by the National Oilheat Research
Alliance (NORA). Neither NORA, the United States Government nor any agency thereof, nor
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w n o w OILHEATRESEARCH ALLIANCE
@ 2004 All Rights Reserved
National Oilheat Research Alliance
Alexandria, VA 22314
I www.nora-oilheat.org
2 THE NORA FUEL QUALITY MANUAL
A GUIDE TO FUEL PERFORMANCE
TABLE OF CONTENTS
1. Introduction ..................................................................................................................................... 5
2 . Overview of Heating Oil ................................................................................................................. 6
3 . Purchasing Fuels.............................................................................................................................. 8
Specifications ............................................................................................................................................ 8
What to buy ............................................................................................................................................... 8
4 . Understanding Fuel Properties...................................................................................................... 10
Fuel Properties and PerFormance............................................................................................................ 10
How Properties are Defined .................................................................................................................... 11
Fuel Stability ............................................................................................................................................ 13
Cold Flow Properties of Heating Oil ....................................................................................................... 14
Using Additives for Improved Storage and Handling ............................................................................. 17
Blending with Kerosene .......................................................................................................................... 17
How t o Evaluate Cold-flow Additives ..................................................................................................... 19
Cost of Fuel Additive Treatment vs . Kerosene Blending ........................................................................ 20
5 . Common Fuel Problems................................................................................................................ 22
Fuel Cleanliness ...................................................................................................................................... 22
Water ....................................................................................................................................................... 22
Products of Fuel Degradation ................................................................................................................. 25
Microbial Contamination ......................................................................................................................... 27
6 . How to Diagnose Fuel Problems................................................................................................... 30
Clear and Bright Test .............................................................................................................................. 31
Fuel Sampling ......................................................................................................................................... 35
How to Sample Incoming Fuels from Barge ........................................................................................... 36
Specification Testing and Labs ................................................................................................................ 37
How to Sample Bulk Storage Tanks ........................................................................................................ 38
How to Sample Transport Trucks ............................................................................................................. 40
How to Sample Home Tanks ................................................................................................................... 41
Testing for Microbial contamination ....................................................................................................... 42
7 . Assessing Problem Home Tanks .................................................................................................... 45
Water and Sludge Accumulation ............................................................................................................. 45
Fuels Degrading in Storage .................................................................................................................... 47
Tank Bottom Samples (BS&w) ................................................................................................................ 48
What t o Do if the Fuel is Deficient .......................................................................................................... 49
8 . How to Prevent Fuel Problems ...................................................................................................... 50
Monitoring Home Tanks .......................................................................................................................... 50
How to Store Fuel Oil .............................................................................................................................. 51
Tank Considerations ................................................................................................................................ 51
Piping Considerations ............................................................................................................................. 51
9 . About Fuel Oil Additives ............................................................................................................... 52
Types of Additives and How t o Test ....................................................................................................... 52
Antioxidants/ Metal Deactivators............................................................................................................ 54
Dispersmts .............................................................................................................................................. 55
Corrosion Inhibitors ................................................................................................................................. 55
Biocides ................................................................................................................................................... 55
Cold Flow Improvers ............................................................................................................................... 57
Appendices ....................................................................................................................................... 58
List of Commercial Petroleum Test Labs
List of Petroleum Testing Equipment Suppliers
I.
Introduction
Heating oil, as its name implies, is intended for end use heating consumption as its primary
application. But its identity in reference name and actual chemical properties may vary based on a
number of factors.
By name, heating oil is sometimes referred to as gas oil, diesel, No. 2 distillate (middle
distillate), or light heating oil. Kerosene, also used as a burner fuel, is a No. 1 distillate.
Due t o the higher heat content and competitive price in most markets, No. 2 heating oil
is primarily used in modern, pressure-atomized burners. Using No. 1 oil for heating has the
advantages of better cold-flow properties, lower emissions, and better storage properties. Because
it is not nearly as abundant in supply, it is often markedly more expensive than No. 2 heating oil.
Given the advanced, low-firing rate burners in use today, the objective is for the fuel to be
compatible and achieve combustion performance a t the highest achievable efficiency of the
heating systems - with minimal service requirements.
Among the Oil heat industry's top priorities are improving reliability and reducing service costs
associated with fuel performance. Poor fuel quality, fuel degradation, and contamination can
cause burner shut-downs resulting in "no-heat" calls. Many of these unscheduled service calls are
preventable with routine inspection of the fuel and the tank.
This manual focuses on No. 2 heating oil - its performance, properties, sampling and testing.
Its purpose is to provide the marketer, service manager and technician with the proper guidelines
for inspecting the product, maintaining good fuel quality, and the best practices for proper storage.
Up-to-date information is also provided on commercially available fuel additives, their appropriate
use and limitations.
h Gasoline
Distillation Kerosene, No. 1 Heating Oil
Diesel, No. 2 Heating Oil
Lubricating Oil
I I
Residual Oil
Coker
treater
-'
-
Straight Run, 12.4%
2.000 DDm s
SULFUR
-- " . "_.
Straight Run, 51.8%
-
5,000 ppm S 500 ppm
-" HYDROTREATER (0.05 wt%)
i FCC Stock, 22.5%
15,000pprnS 1 -
A major difference between diesel fuel used for vehicles (on-road or highway) and heating oil
is its sulfur content. Highway diesel, defined as low-sulfur, must presently have a sulfur content a t
or below 0.05 wt % (500 parts per million, stated as 500 ppm). Beginning in 2006, the diesel fuel's
sulfur content will be reduced to "ultra-low sulfur" level, such that it will be at a maximum of 0.001 5
wt% or 15 ppm. This is being mandated by the U.S.Environmental Protection Agency (EPA) to
reduce pollutant emissions from vehicles. Regulation of diesel for off-road vehicle use will follow;
sulfur limits are being promulgated as this piece is being written. As sulfur content of diesel fuel is
reduced to much lower levels as compared with heating oil, the amount of hydrocracked stock that
can be blended into diesel fuel becomes more limited.
The EPA does not regulate heating oil used for residential appliances. It may be purchased
as No. 2 (0.5 wt% sulfur max / 5000 ppm), or No. 2 Low Sulfur (0.05 wt% max/ 500 ppm)f though
recent experience shows that most residential heating oil consumed today falls below 2500 ppm.
State and local environmental regulations often limit the maximum sulfur content allowable in
burner fuels.
References:
[ 1] http://science. howstuffworks.com/oiI-refin ing4. htm
This website offers additional information on the subject of oil refining and other reference
sources such as American Petroleum Institute, Institute of Petroleum, Chevron Learning Center.
[2] Sutterfield, F. D., Olsen, D. K., "Technologies fgr Meeting Low-Sulfur Fuel Specifications
in the United States, p. 41 1, Proceedings of the 7 International Conference on Stability and
Handling of Liquid Fuels, January 2001.
A Note on Units:
To convert from weight percent (wt%) to parts per million (ppm), multiply by 10,000
Example: 0.05 wt% Sulfur = 500 ppm Sulfur
A GUIDE TO FUEL PERFORMANCE 7
3. Purchasing Fuels
Specifications
The terms "heating oil" and "diesel fuel" describe the fuels that are used for home heating.
They are very similar, although diesel is often cited when referring t o vehicle fuels and heating oil
when talking about burner fuels. In the U.S. Grade No. 2-D is the most common diesel fuel for
trucks, with Grade No. 1-D and Grade No. 4-D also commercially available. The primary difference
in the specifications is that diesel fuel has a cetane and a sulfur limit. Cetane is an important
component for diesel engines and affects how smoothly the fuel burns, however, it is not relevant
for burner fuels.
Burner fuels include No. 1 (kerosene), No. 2, and No. 6. These grade designations are
established by the American Society for Testing and Materials (ASTM). The grades are numbered in
order of increasing density and visc.osity, with No. 1 the lightest and No. 6 the heaviest.
Fuel specifications and associated test methods are established by committees. They are
developed by consensus among refiners, equipment manufacturers, and users in order t o ensure
that the fuel provides satisfactory performance and reliable operation. The ASTM Committee D-2
(Petroleum Products and Lubricants) is responsible for diesel and burner fuel specifications, ASTM
D 975 and ASTM 0-396 respectively. Refer t o Table 1 for their properties.
In these specifications, there are requirements or limits for the values of fuel properties.
Standard test methods that are used to measure the values of the properties are also listed. These
properties and methods are described in Chapter 4.
What to buy
When purchasing bulk fuels it is always recommended that you ask for the specifications. Look
t o see that its properties are suitable for their intended use. For example, if you purchase low-sulfur
heating oil, be sure that the specifications show the sulfur content is less than 0.05 percent by
weight (wt%).
If you buy heating oil in the summer for use later during the heating season be sure t o review
the cloud and pour points of the fuel (Chapter 4 discusses these cold-flow properties in detail). In
locations where the winter is very cold or there are occasional cold snaps, certain fuels may not be
suitable for use as they could gel. Considerations must then be taken to either blend with cold-flow
additives or kerosene as appropriate to counter gelling problems before they occur.
Some heating oil retailers periodically sample to verify the specifications of the fuel. Others
rely on the sampling and testing of their suppliers. Chapter 6 explains how t o sample fuels being
received by barge or transporter trucks a t the bulk terminals, or those fuels picked u p b y the
delivery trucks a t the rack. The sample of the fuel taken should represent an entire load or batch of
fuel. A commercial lab specializing in petroleum testing will be needed t o analyze the properties
listed in Table 1 using the standard test methods. This is called "specifications testing" and it may
take about a week for the lab to report the results. You need not test for all the properties every
time. Randomly test the incoming fuels as a means of quality control.
A commercial lab specializing in petroleum testing will be required to analyze the properties
listed in Table 1 using the standard test methods. You need not test for all the properties every
time. You should determine how often you test based on the cost of testing and the reliability
of your supplier. A list of commercial test labs can be found in the Appendix. Chapter 3 explains
further what the properties mean.
D 130
Note 1. By federal regulation, these grades of heating oil and diesel sold for tax-exempt
purposes are required t o contain the red dye solvent (ref 40 CFR Part 80 and 26 CFR Part 48).
Note 2. Applies t o No. 2 low sulfur diesel.
Fuel Stability
The stability of heating oil depends a great deal on the crude oil sources from which it was
derived, severity of processing, use of additives and any additional refinery treatment. Different
refineries may produce distillate fuels that vary in composition and stability properties. Normally
produced fuels have adequate stability properties to withstand normal storage and use. However,
fuels that are stored for prolonged periods or subjected t o high temperatures may form excessive
amounts of sediment and gums that can overload filters or plug nozzles. It is therefore necessary t o
consider a fuel's storage and thermal stability.
The fuel's storage stability should be assessed a t the time of manufacture. That is, the fuel
should have some performance criteria in the purchase specification. Test Methods ASTM D 2274
and D 5304 are commonly used accelerated stability tests. It should be noted, however, that
positive results from laboratory tests does not guarantee that there will be no operational problems
in the field due to varying tank conditions and mixing of fuels. Nevertheless, adhering t o some
performance criteria assures some level of protection.
Fuels tend to degrade with time in storage, and its effects are only compounded with added
handling and transport due to the potential for contamination. If you start off with an unstable fuel,
it does not improve.
If the fuel fails a stability test, it does not mean that the fuel cannot be used. It is merely a
warning that the fuel only has a limited shelf life before it forms excessive particulates.
ASTM D 6468
I 90 min(3000F)
1500c
80% reflectance
(optical meter reading)
I I
I
Cloud and Pour Points (CP, PP)
As the fuel is cooled a temperature will be reached a t which the clear fuel begins to cloud. The
cloudiness is caused by the formation of wax (paraffin) crystals in the fuel. The highest temperature
a t which this occurs is referred t o as the cloud point. Below the cloud point these wax crystals
might become large enough t o plug the oil-line filter, pump strainer, and burner nozzle. As the
temperature is lowered further, gelling of the fuel occurs. At or below the pour point temperature
the fuel does not flow.
ASTM D 396 specification for heating oil limits the Pour Point a t a maximum of 21O F (-6 "C).
. Cloud Point:
st
August 1 - March 14
th St
th
Maximum: - 9°C (+I
5°F)
Cloud Point: March 15 -July 31 Maximum: - 7°C (+20"F)
Although ASTM D 396 does not specify a range for cloud point, it is recommended that both
cloud and pour points be established and specified in all purchase specifications based on location.
There is no guarantee that satisfactory operation will be achieved on a broad basis where local
temperatures may be much lower than the above-specified temperatures, and so it is advisable to
use a typical temperature chart as shown in Table 4-2.
Recommendation
No single laboratory test can adequately predict the cold flow performance in all fuels and in
all storage systems. Storing fuel oil indoors, or providing insulation t o storage tanks and piping
minimizes problems associated with poor cold flow operation.
In general, satisfactory operation should be achieved in most cases if the Cloud Point is 6°C
above the 10th percentile minimum ambient temperature for the area in which the fuel will be
used. The 10th percentile temperature means that, on average, the ambient temperature is not
expected t o go below this value more than 3 days for a 30-day period. The temperatures are based
on historical data and depend on the local climate. They are listed on the chart in the following
pages by month and region during the winter.
For example, on Long Island, NY during December, the 10th percentile temperature is -1 4°C.
(See table 4.2 on next page, re: New York, South 42 deg. lat.) Six degrees above that is -8"C, so for
Long Island during December, the practical, maximum cloud point specified should be -8°C (18°F).
Appropriate low temperature properties should be agreed upon between
the fuel supplier and purchaser for the expected ambient temperatures.
See Table 4.2 on the next page.
A Note on Units
To convert from degrees Celsius (C) to degrees Fahrenheit (" F), multiply by 1.8 and add 32.
Examde 1
What is -15 "C?
(-15 x 1.8) + 32 = 5 o r 5 deg. F
-!
-9 16 -13 9 -9 16 -7 19
S. 31' lat. 9 48 2 36 -2 28 -3 27 -1 30 2 36
Utah -2 28 -11 12 -14 7 -18 0 -14 7 -8 18
Vermont -3 27 -8 18 -20 -4 -23 -9 -24 -11 -15 5
-3 27 -9 16 -11 12 -9 16 -4 25
1;:gton E.122'long. -8 18 -11 12 -18 0 -11 12 -8 18
W.122'long. -3 27 -3 27 -7 19 -4 25 -3 27
West Virginia -8 18 -15 5 -16 3 -14 7 -9 16
Wisconsin -3 27 -14 7 -24 -11 -28 -18 -24 -11 -18 0
Wyoming -15 5 -18 0 -26 -15 -19 -2 -16 3
r:
-$ -15
v)
e!
-20
n
$
c
!?ia,
E -30
I-
-25
-35
u pt q
Sample A
I
Samde B I
-40 .I" -. -- ... " ... "
It is important to test your additive against the base fuel you use to find the
most effective additive to depress pour points.
Kerosene
30 vol.% 50 vol.% 70 vol.%
0---
-5 -
d,
-10 -
s
S
0
'5 -15 -
v)
2
g- -20 -
n
rn
Q
5
U
-25 -
! -30 -
Sample B
E
I- -35 -
Example: If the Temperature Depression is -2O"F, with a blend of 50% kerosene, this
means that if the base fuel had an initial pour point of +5"F the blend will now have a
pour point of -15°F. At this point the fuel can't flow.
Kerosene
30 vol.%. 50 vol.%. 70 vol.%.
0-
h
L -5 -
d,
:-10
Y -
S
0
.ijj -15 -
In Sample A Sample B
2
g- -20 -
n
2
S
-25 -
m
Y
-30
I- -35
Note: This chart gives temperature depression, or temperature reduction, for cloud paamit.
This is a comparison of the different blends when compared t o the base fuel (no kerosene).
The following lists some of the more common performance tests used t o evaluate the fuel's
response t o cold-flow additives.
Performance Test Method
Additives should be used only when needed to prevent or solve a problem. When comparing
additives consider the following:
The fuel response t o a given additive must be measured to determine the amount of
additive needed.
Additives are fuel specific (varies with crude type) and may perform well in one fuel and
poorly in another. It is therefore recommended to test several different batches of,fuel.
In order t o make an informed decision, comparison tests should be done where all
conditions are controlled and the only variable is the additive. This requires laboratory
analyses in order to measure effectiveness a t various additive concentrations. The costs can
be compared with the various options to improve cold flow.
0 A comparison of additive response may be made with kerosene blending t o achieve the
same response.
A GUIDE TO FUEL PERFORMANCE 19
Mixing
Additives will not fix the product in tanks that have already formed wax crystals. For a cold-flow
improver t o work it must be mixed thoroughly with the fuel so there must be no undissolved wax
present. It should be added t o a tank before the fuel is put in so that mixing takes place. When
adding a cold-flow improver the fuel must be a t least 5 t o 10°C above its cloud point. Pouring it in
the top of a tank in which the wax has dropped out of the fuel is a waste of time and money. This is
not true for kerosene which can help t o dissolve the wax.
Ap plication
Where there is a potential problem with gelling in fuel lines, such as with outdoor tanks or
exposed piping, the cold-flow additives are effective to prevent fuel delivery problems. It is
important t o know whether these additives are already present in the fuel as received from the
supplier. The first increment of additive is most effective, and if the fuel marketer is planning to use
the same type, additional amounts may produce little or no improvement.
Commercially available cold-flow improvers are often combined with detergents and other
additives sold as fuel conditioners. If such additives are used in bulk tanks the detergent in
the additive can strip rust and dirt from tanks, which may then lead t o reduced filter life. It is
recommended t o remove water and loose dirt from tanks before dosing with the product or check
for detergency effects on a few small tanks.
(2) Determine the kerosene blend ratio needed based on your fuel properties and cold-flow
requirements. (i.e. 50/50, 70/30, etc.)
Let's say that we wish to blend a t a ratio 50/50 to reduce the pour point by up t o -23°F.
(Note: You will need to know the pour point of the fuel you wish t o treat. You can get this
from the specifications provided with the fuel or else send a sample to an analytical lab t o
determine this value.)
Water
Water and dirt can lead t o filter plugging and tank corrosion. The water in the fuel can promote
the growth of bacteria, yeast, and fungi (also known as microbes).
One of the most effective ways t o keep the fuel clean is to minimize the water that accumulates
in the tank. There are several pathways that water can get into the tank:
Broken or loose fittings on the tank;
Moisture from the air can condense on the walls of the tank;
Water in the fuel itself (dissolved and free water);
Rain water or snow entering the tank during fill-up
By far the most common entryway, especially for outdoor tanks, is through the fittings. Finding
the right location and proper installation are the keys t o reducing water accumulation in this way.
Stick the tank with water-indicating paste a t every service interval t o get an estimate of how much
is a t the bottom of the tank. This can quickly tell you if this is the cause for burner shutdowns. You
may need t o stick the tank in more than one location t o assess the problem. For tanks with a top-
feed oil line from the tank it may b e necessary to remove the line and stick the tank from this bung.
In a tank that maybe sloped slightly, you may find that the water has collected a t the intake of the
suction line. Pumping out the tank or replacing it are the only solutions.
Where there are lower humidity levels, generally in the Northeast of the country, this amount of
condensation could take longer to accumulate (i.e. over 2 or 3 summers).
Keeping outdoor tanks full will help to minimize water condensation in tanks.
This is a bottom-draw oil supply from the tank that is intended t o minimize sludge accumulation
within the tank. The water and contaminants however tend to get sucked into the oil lines and
deposit inside the lines. Over time this would prevent oil from getting to the burner.
The next page contains recommendations for clearing clogged lines.
Keep fuel oils stable by keeping the fuels clean and maintaining the tanks:
Ensure that the fuels you are supplying t o your customers are clean and free of water.
Inspect your fuel supply. Check for water and sediment in your bulk storage tanks.
Check the cleanliness of your delivery trucks.
Check home tank bottoms by sticking for water or taking sample.
Pump out tanks that have sludge build-up.
Locate tanks away from direct exposure t o the sun t o minimize high
temperatures and degradation of fuel.
Microbial Contamination
Heavy microbial contamination can lead t o costly service problems and is a concern for the
petroleum industry from crude oil production, through product transfer, storage, and finally
consumer use (Figure 5-6). The potential losses include not only equipment failure and downtime
for repairs, but also customer satisfaction.
Throughout the distribution system there are many possible routes where water can enter
the system and be transported along with the fuel. Microbes may be introduced into fuels as
products cool in refinery tanks. Bacteria and fungi (microbes) carried on dust particles and water
droplets could enter tanks through tank vents. Barges often use sea water as ballast, and this can
contaminate stored product if compartments are not adequately emptied before refilling. Water
can enter tanks through broken fittings and improper installation.
The costs for decontaminating facilities or tank cleaning are high. Prevention of problems
by good housekeeping and regular monitoring is more cost effective than the treatment of
microbial problems after they occur.
Figure 5-5 Blue arrows show sites where water and microbes tend to accumulate.
Pipeline
I
I
(low points
trap water)
a”&
TERMINL 2
-. i.
Refinery Refinery
Product tanks Bulk Consumer
Plant Tank
Loading ,f
Rack
Wherever water tends t o accumulate, even in small amounts, microbes (such as bacteria,
yeast and fungi) can grow. There is often enough water in the bottom of large storage tanks, fuel
tanks on trucks and consumer tanks for some microbial growth to occur. The microbes tend t o be
most active between the water and fuel layers, and also on internal tank and fuel delivery system
surfaces. When the tank contents are disturbed, for example when the tank is refilled, the microbes
become suspended in the bulk fuel where they cause fouling and may be passed on down the
distribution chain to contaminate facilities downstream. In a homeowner’s tank these microbes can
clog fuel lines, filters and nozzles causing burner shutdowns.
It is recommended that fuel supplies be checked for suspended water before being accepted
and transferred into a bulk storage plant. The barge operator should not only sound the tank t o
Figure 5-6 Microbial growth observed in container previously storing fuel oil.
Most bacterial growth takes place a t the boundary between the fuel and water. This usually
occurs a t the tank bottom, although microbes also can stick t o tank walls. They can produce a slimy
layer called a biofilm that adds t o the bottom sludge and sediment. The byproducts of microbial
activity, or wastes, cause the fuel t o degrade and physical damage t o the fuel delivery system.
Under the right conditions, usually hot and humid conditions, their uncontrolled growth leads t o
problems such as filter clogging and fuel lines plugging.
Microbes can cause corrosion of metals including steel, iron, copper, nickel, aluminum, and their
alloys. They can even affect the integrity of nonmetals such as plastics and composites. Microbially
induced corrosion, or MIC, of metals is caused by various direct and indirect mechanisms. The best
known, direct mechanism involves the action of sulfate reducing bacteria (SRB) that grows in water
and sludge in the bottoms of tanks. SRB can cause pitting corrosion in steel tanks. In this process
SRB uses the sulfates found in the fuel t o develop an electrochemical corrosion cell, altering the
condition on the metal surface and enhancing corrosion that would not occur in the absence of
these microbes. This usually occurs along the bottom centerline of the tank where water tends to
accumuIate.
Refer t o Chapter 6 for guidelines on how t o use field test kits to determine microbial
contamination.
Monitoring the fuel is an essential part of maintaining good fuel quality. The following are
guidelines for evaluating and accepting fresh fuels, and monitoring of stored fuels. Stored fuels will
age over time and form sediment that contributes t o sludge a t the bottom of the tank. There are
basically two ways by which fuel quality can degrade: (1) by contaminants introduced during fuel
delivery and storage, and (2) sediment formation from unstable fuels.
The only way to identify if there is a fuel quality problem that could lead t o service problems
downstream is to know the condition of the product. Sampling and analyses should be done to
quality control the fuel oil as it is received from the supplier, while it is stored a t your bulk terminal,
and during transport in the delivery trucks. Once the product is delivered t o the customer and
stored in his tank, all service problems should begin with a diagnosis of the fuel in the home tank,
the condition of storage and fuel delivery system (oil supply lines t o the burner, fuel pump/ strainer,
filter, nozzle).
The types of contamination that could occur during distribution and storage:
Other products - gasoline
Water, dirt (leading t o filter plugging and tank corrosion)
Off-specification fuel (high cloud, pour points)
Trace metals - copper, zinc (accelerates oil degradation)
Microbes/ microbial growth (filter plugging, corrosion of metal tanks)
Contamination with other petroleum products can affect flash point (with gasoline), or viscosity
and boiling range (with heavy oils).
It is important to continuously monitor the condition of the tank so that any accumulation
of water and sediment at the bottom is removed periodically. Inspection and water draining
should be done at least annually. Water promotes corrosion and bacterial growth at the fuel-
water interface.
Method:
Take a sample of the fuel from the tank or truck and fill about 90% of the jar.
Place the bar chart behind the jar. Compare the appearance of the bar chart through the
sample with the standard photos. Look a t the comparison of the lines and how they fade
gradually. Ignore the color differences. However, if the fuel is too heavily dyed or the fuel is
too dark t o allow you t o see through the jar, pour a smaller amount of fuel into the 4 oz.
bottle.
Record the number on the photo that the sample resembles most. This is the rating.
Hold the sample up to the light and check for haze or clarity. Swirl the sample t o produce a
vortex and examine the bottom of the vortex for particles.
Record the following observations:
- Was it clear and bright? Or not?
- Were there particles?
Record the outdoor temperature or the fuel sample temperature if different.
Record your observations if the fuel appears darker than usual.
The fuel should have no water or particles, and this is considered "clean and bright." When
compared t o your observations of typical fuels, the haze rating could give you an indication of an
- unusual batch of contaminated or off-specification fuel.
If a sample is taken when the outdoor temperature is cold, small amounts of wax particles may
settle out and cloud the fuel; this should not be confused with a water haze. These wax crystals
will clog filter systems in your fuel delivery system. Check for the Cloud Point (ASTM D 2500) and
Pour Point (ASTM D 97) temperatures of the fuel. The fuels you store and use should have cloud
and pour points well below the outdoor temperatures in your geographic region. If they are not,
you can expect cold-weather operability problems. Refer to the previous section on Cold Flow
Properties of Heating Oil.
I
I
I 5 I
i 2
. .-... B-'
@
..
SLIGHT HAZE
-ICE
If you see a haze, there is something wrong with the fuel. There is either water in the fuel
or wax settling out of the fuel if the outdoor temperature is below its cloud point.
Sampling Tips
Use clean sampling devices and new sample containers.
Check to make sure how much total volume of sample is needed to conduct all the tests
before a sample is taken. A 1-to-5 gallon total sample size may be necessary, depending on
the number of tests. Determine the appropriate type of sample containers needed.
A 1-gallon epoxy-lined can would be ideal for most tests on bulk samples; a 1-quart plastic
(Nalgene) bottle for bottom samples will do for sediment tests.
Sample containers should be filled t o minimize headspace, but no more than 95% full
t o allow for expansion.
Use the appropriate device for pulling bottom samples. The devices should be cleaned after
each sample has been taken to prevent contaminating each successive sample. A little
rubbing alcohol will do.
Figure 6-4 Drip Sampler Located Between the Manifold and Delivery (Kittiwake)
Needle valve
to control
flow of fuel
into Cubitainer
I450rnrn
:working
:clearance
II +- “Save all”
ondeck
plates
Specification Testinq
Section 3 on purchasing fuels lists the fuel properties and tests that should be done for these
samples. Private testing laboratories that specialize in analyzing petroleum samples can perform
tests for fuel properties specified in ASTM D 396 for burner fuels. ASTM International maintains
a Directory of Testing Labs on-line with full text search for services and locations of testing
laboratories. The information on the types of tests performed, specific tests performed, materials
analyzed, or other services offered has been provided by the laboratories. Refer to this most useful
website,
http://astm.365media.com/astm/la bshndex.html
/
- Hatch
6"
X-----Top
I Sample
X-----Upper Sample Upper Third
.
,,,-Check Valve
Bottle cage to
be used with
Boston Round
Bottle
Zone Samplers made of clear acrylic tube or stainless steel
These bulk samples give valuable information on the general condition of the fuel. A moderate
t o large sample size is required dependant upon the test matrix. Analyses of these samples should
be done when you suspect contamination in the tank, contamination with other products, or cold
flow properties are off-specification.
Samples can be obtained by bottle sampling using a bottle cage with a glass, Boston round
bottle (16 or 32 oz.). Brown glass bottles protect the sample from light, which may affect results.
Zone samplers (shown above) are also simple t o use and versatile for sampling product from
stationary tanks, tank vehicles, and tank ships. This sampler can take all level samples of liquid
products. This type of "fuel thief" is typically 1 in. diameter or larger, and varies in length. A check
valve or a ball valve a t the bottom of the thief remains open as the sampler is lowered. When the
sampler is held stationary near the bottom of the tank, the check valve closes, effectively containing
a column of fuel.
Line Samples
A line sample is another way to sample a tank if accessing the tank interior is difficult. Clean
sample containers can be filled directly from a pipe or spout. For samples taken during loading
(such as into the bulk tank and a t the rack) allow for about 300 gallons of fuel t o be dispensed
before filling sample container. Fill container to within 1/2 inch of the top then cap immediately.
Figure 6-8 Line sample from bulk tank collected in epoxy-lined can.
,
This is preferable to using the water indicating paste on a stick, as a sample can more easily be
inspected visually. Unless there is more than about 1/2-1 ” depth of water, it is hard t o detect it on
the stick. An emulsion a t the bottom (water and sludge mixture) can also displace the water from
the paste, which may appear as spots on the paste. This does not mean there is an insignificant
amount of water, as it does not take much t o cause corrosion or support bacterial and fungal
growth. A sample may give evidence of rust flakes or a slimy type of microbial growth.
Figure 6-11 Bottom sample taken with a Pencil Bomb or Fuel Thief.
Check the level and pitch of the tank. Pull a bottom sample from the low end of the tank if
possible. You may wish to take additional samples near the fuel supply line or from the fill-pipe.
Tanks are sometimes installed with a slight tilt to allow water to collect in one end. Take note that
when a sample is drawn from a port not located at the low end of the tank, sludge or water may not
be detected. For large tanks it is recommended that samples be taken from more than one location
to ensure that water and any contaminants are detected.
Figure 6-12 Obtaining 5cc of bottom sample for microbial field test (left);
injecting sample into aqueous broth for detecting bacterial and fungal growth (right).
Figure 6-13 Example of fuel oil sample in a test vial a t the start of the test.
: Low levels of microbial growth won't affect your fuel delivery system
rowth: If you are getting repeated no-heat calls, burner shutdowns due to filter
and line clogging, then its time for mechanical cleaning and/or chemical treatment, or as a
last resort tank replacement.
References:
1. ASTM D 6469 Standard Guide for Microbial Contamination in Fuels and Fuel Systems
2. ASM (The Materials Information Society) Handbook, Volume 1I , Thomas R. Jack, Biological
Corrosion Failures
-- I _
e Be aware that water can be introduced into tanks from other ways; water can be delivered
along with the fuel if it was already contaminated. Periodically check for water and cleanliness
of the fuels received from your supplier. Sample t o check that your tanker truck and/or bulk
storage tanks are clean and dry.
Sludge is a mixture of water, gum formed from the aging of fuels, rust, and microbes (bacteria
and fungus). Repeat service calls due t o sludge build-up requires special attention. Sampling
the tank bottom using a fuel thief allows you t o assess its condition and how much build-up
there is.
Collect the bottom sample in a clear, glass jar and take note of what it looks like.
Figure 7-2 By the sample drawn above, this tank has a problem with excessive water
accumulation. You can also detect this much water with water-indicating paste on a stick.
Figure 7-3 This sample contains heavy amounts of degraded fuel produc.; and water.
With many years of accumulation, the only effective means of removing sludge is through
mechanical cleaning.
Physical cleaning or replacement of heavily contaminated tanks, and replacement of clogged
fuel supply lines, are the only effective means t o solve these types of service problems.
A floating suction device used on the fuel supply line may help t o reduce the amount of
sediment that gets picked up into the fuel delivery system. When a floating suction is used
it is essential to monitor and remove the water as it accumulates. This should be done t o
prevent internal corrosion of steel tanks and to minimize microbial growth.
The most important factors affecting storage stability of the fuel are the condition of the tank,
the amount of existing sludge, water or microbial growth.
Most of the incoming heating fuels from major suppliers appear to have acceptable stability.
Pipeline sources of fuel tend t o be more stable; barged fuels tend to be slightly less stable
possibly due to the added handling and transport, longer storage times, and potential
contamination.
Generally, older tanks that have more overall accumulation of sludge show an increased
likelihood of service problems. When replacing a tank, do not transfer old fuel into the new
tank.
Newer tanks with little water or sludge have fewer problems with microbial growth and
provided better fuel storage stability.
High sludge content (measured as Bottoms Sediment and Water or BS&W, of 10% or more)
results in more clogging problems of the fuel line and filter. You can detect large amounts of
contamination at the tank bottom simply by sticking the tank and using water-indicator paste.
If the paste color appears spotty, you likely have a mixture of water and heavy components of
fuel (an emulsion).
Tanks with existing sludge problems do not improve with fuel stabilizing additives. Stabilizers
are typically designed for use with freshly refined, clean fuels t o slow down oxidation and
natural aging of fuels.
Some dispersant-type fuel additives show reduced sludge on filters and may help to maintain
cleaner fuel delivery system (supply line, filter, nozzle).
To minimize fuel degradation during storage, keep outdoor tanks away from direct sun; high
temperatures during the summer can accelerate the fuel aging process. Where possible install
tanks in shaded areas, or on the north side of homes.
SAMPLE 2
SAMPLE 1
The photos above show examples of fuel bottom samples with different layers of contaminants.
The heaviest layers usually consist of sediment and water. The fuel is usually a t the top of the
sample container, below which there exists an emulsion (fuel by-products of ageing and water
mixture). Having some information about the sludge contents allows you t o focus your effort on
how to solve the problem.
In the above samples, Sample 1 shows water and contaminants as related t o fuel-breakdown
(an unstable fuel). A pump-out of the contaminants along with improved practices for minimizing
water build-up would help to improve the cleanliness and stability of the fuel. Sample 2 shows more
evidence of non-fuel contaminants, which indicates that debris may be getting into the tank during
filling.
Fuel is off-specification
Periodically taking a sample of the bulk fuel and testing for its specified properties can give
you an indication of the overall quality of the fuel from your supplier. If there is a problem with a
fresh batch of fuel, then there are two options. The fuel should not be accepted from the supplier
if it is contaminated with water or debris. If there are acceptable ways to bring the fuel back into
specifications then the following methods may be considered.
Dilution and Blending. In some cases, when a fuel is off-specification, dilution with another
batch of fresh fuel can effectively bring the entire batch within acceptable limits. For example,
blending can lower a high cloud point or raise the flash point. Blending should always be done with
small test samples and analyzed before attempting mixing the entire stock.
Fuels that are contaminated with microbes, debris, or water should not be blended.
Contaminants in Tanks
Excessive no-heat calls are likely t o occur with large amounts of sludge in the tank. Field
experience shows that chronic problems occur in tanks having about 1/2” or more water/sludge
using the stick and paste indicator, or about 10% BS&W by analysis. Pumping out these most-
contaminated tanks and clearing out the oil line would eliminate these service calls.
Fuel lines that are piped from the bottom of the tank are more susceptible to line clogging if
there is no fiIter/water separator a t the tank. Where there is no filter a t the tank, any sludge or water
drawn from the tank would become trapped in the lines.
If water is the major constituent, then you will need t o determine where the water is coming
from. There may b e a broken or poorly threaded pipe, loose fill cap, or a crack in the tank. Keep
tanks filled during the summer t o minimize the air space above the fuel. This reduces the amount of
water accumulation in the tank that comes from condensation.
Piping Considerations
Metals such as galvanized steel, zinc, and copper accelerate the breakdown (or oxidation)
of oil. Avoid long routings of copper lines between the tank and burner.
With an outdoor tank all piping should be well insulated from the cold weather. Under
extremely cold conditions, untreated No. 2 oil could gel and lead to burner shutdown.
A floating suction a t the fuel intake may help to reduce the amount of sediment drawn into
the supply line. mprove the cleanliness and stability of the fuel along with improved practices
- corrosion inhibitor
- metal deactivator
- biocide
Multifunctional additives are generally more effective than individual additives in that they can
potentially resolve multiple fuel issues that exist with problem fuels.
Stabilizers cannot reverse the effects of fuel degradation such as color that has changed or
sludge that has been formed. It is important t o recognize their limitations and therefore stabilizers
should be considered only as preventative measures to reduced fuel problems. They are most
appropriately applied with fresh fuels. Additives will not clean tanks that contain existing water and
sludge. In general, fuel supplies that are already clean and stable d o not require additives.
Performance Tests:
1. Accelerated Thermal Stability (ASTM D 6468)
2. Oxidation Stability Accelerated Method (ASTM D 2274)
3. Fuel Storage Stability -1 3 week test, 43 ' C (ASTM D 4625)
Corrosion Inhibitors
Function: Tank surfaces that come in contact with the fuel may rust due t o water that
accumulates or acids that could form in the fuel. Corrosion inhibitors can be used to prevent
the formation of rust.
Common Names: Anti-rust, Anti-erosion
Performance Tests:
1. Detection of Copper Corrosion by Copper Strip Tarnish Test (ASTM D 130)
2. Steel Corrosion (ASTM D 665)
Possible Side Effects: Some corrosion inhibitors can interact with the fuel and other lubricant
additives to form gums and sludge deposits. Suppliers should be able to demonstrate no-harm
performance (compatibility) when these additives come into contact with the fuel and other
additives.
Biocides
Function: Water accumulation a t the bottom of oil tanks and fuel handling systems is a
common problem throughout the fuel industry. Water in combination with hydrocarbon fuel can
support microbial growth. Certain species of microbes can survive a t the fuel-water interface of
the storage tank where there is no free oxygen. Some bacteria use the oxygen bound in fuel
sulfur compounds, and the hydrocarbon fuel as the nutrition source. By-products of microbial
activity such as hydrogen sulfide and organic acids can lead to storage problems such as ,
corrosion; the sheer amount of cell growth can lead to operational problems.
Microbiological organisms in fuel are commonly classified as bacteria, molds, or yeast. Certain
strains are frequently used to evaluate the effectiveness of additives, such as Pseudomonas
aeruginosa (bacteria), Cladosporium resinae, (mold), and Candida tropicalis (yeast).
A variety of biocides are commercially available to help control microbial contamination in
water. Biocide additives are regulated under the Federal Insecticide, Fungicide and Rodenticide
Act (FIFRA), and the product must be registered with the federal Environmental Protection
Agency (EPA) for specific applications. For example, a biocide that is registered for treating fuel
oil storage tank water bottoms cannot be used for treating gasoline storage tank water bottoms
Check that the product you are using has an EPA registration number, which is usually indicated
Types of Chemicals To Look For: Some common compounds that are approved as fuel-water
biocides include the following [Peyton]: i.
*Actual treat rate and frequency of application depends on the level of contamination and the storage condition
(i.e., fuekwater ratio, turnover of the fuel, etc.). Contact the manufacturer for specific recommendations.
Heavily contaminated systems need to be physically cleaned to remove debris.
Performance Tests:
1. To be effective according to U.S. Military Specifications, MIL-S-53021, the biocide must kill or
inhibit the growth of the three organisms, listed above, based on concentration.
4
2. Common field test kits. Some commercially available ones- Liquid-Cult Fuel Test Kit (MCE
Inc.), EasiCult (Orion Corp.), Hum-Bug Detector Kit (Hammonds Co.)
L
Possible Side Effects: Interaction with other additives, fuel filter plugging due t o mass of
deterio rating m ic robes.
References: Peyton, Kim B., Ondeo/ Nalco Fuel Field Manual, McGraw-Hill Professional
Engineering series, 2002.
56 THE NORA FUEL QUALITY MANUAL
.
Cold Flow Improvers
Function: Flow improvers are designed to lower the cold temperature operability limit of diesel
and heating fuels, and to avoid wax formation in cold weather. Once wax has formed in the
fuel, an additive will not change the waxes already present. Although, if the temperature falls
lower, an additive will interact with, and modify, newly separating waxes.
To dissolve wax, a solvent such as kerosene must b e used. Unfortunately, kerosene cuts can be
expensive and of limited availability, and can reduce heat content.
Commercial cold-flow improvers or pour-point depressants effectively depress pour-point
temperatures. Its effects depend on the characteristics of the fuel as well as on the additive.
Different fuels exhibit different behaviors, even though they are all classified as heating oil.
Some additives are more effective than others a t the same concentrations. Much less chemical
additive is needed to reduce pour point temperature compared to the volume of kerosene
required for the same effect.
Common names: Cold Filter Plugging Point (CFPP) additives, Pour Point Depressants, Low
Temperature Flow Test (LTFT) additives, Nucleators, Wax modifiers, Wax dispersants/ Wax
suspension agents, Cloud Point Depressants
Performance Tests:
1. Pour Point (ASTM D 97) -This test predicts the gel point in the fuel lines and fuel tanks. The
operability limit is always higher than the pour point.
2. Cloud Point (ASTM D 2500) This test indicates the temperature when wax becomes visible
in the fuel. The recommended cloud point temperature depends on the time of year and the
location of operation. These are specified in ASTM D 975.
Possible Side Effects: Adding too much cold-flow improver can thicken the fuel and reduce
CFPP response.
.,
APPENDIX A
SOME COMMERCIAL TESTING LABS FOR PETROLEUM REFINED PRODUCTS,
PETROCHEMICALS, LUBRICANTS
Arizona Florida
Tennessee
Galbraith Laboratories, Inc.
SGS Control Services, Inc.
United Power Services, Inc.
Texas
A 8( B Labs
ANA-LAB Gorp.
Core Laboratories
Dixie Services, Inc.
Harris Testing Laboratories, Inc.
InterCorr International, Inc.
lntertek Testing Services
Lab Consultants and Marine Surveyors, LLC
Perkin Elmer Automotive Research
PoIyhedron Laboratories, Inc.
Saybolt, Inc - Petrochemical Div.
SGS Control Services, Inc.
Southwest Research Institute
SPL, Inc.
Virginia
Hampton Roads Testing Labs, Inc.
Washington
Bio Research Laboratories, Inc.
Wisconsin
Fluid Power Institute
Structu raI Research, Inc.
Thomas A. Edison Technical Center
The above is only a partial listing of what is available under these product headings. To search
for other product he-adings or obtain future updated listings this database can be accessed through
their electronic address:
http://www.thomasregister.com
It should be noted that reference to any specific manufacturer here does not constitute or imply
its endorsement or recommendation. This listing has been published for convenience t o the reader
and was obtained from publicly accessible information.