ANALYTICAL METHOD - SPECIFICATION
PREPARED BY
ANALYTICAL SCIENCES LABORATORY
EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
600 BILLINGSPORT ROAD, PAULSBORO, NEW JERSEY 08066
MOISTURE IN LUBRICATING OILS
1. Introduction
1.1 This revision changes the lower detection
limit, based on data from an evaluation comparing
the crackle method versus the azeotropic Karl
Fischer method, as well as editorial changes.
2. Scope
2.1 This method is used to qualitatively detect
moisture in new and used lubricating oils. The
detectability limit is based on the individual
sample's characteristics (new or used oil, high or
lowly additized and low or high viscosity oil, etc.) as
well as laboratory background noise and lighting.
Experience has shown typical detectability limits
around 0.05 wt % are achievable with lower
detection limits possible under very good
conditions. Gasoline dilution in used automotive
engine oils may sometimes interfere. If quantifiable
data at low concentrations of water is required then
a Karl Fischer titration method (e.g. AM-S 738)
must be performed.
3. Referenced Documents
3.1 "Evaluation of Crackle Test," Reference
No. 2005AN203, Janet L. Lane.
3.2 AM-S 738, “Water in Gear and
Lubricating Oils (Distillation-Electrometric Titration
Method)."
4. Summary of Method
4.1 A small portion of sample is poured onto a
hot plate. Water is present if the sample spatters,
makes a crackling sound, or if a cloud of tiny
bubbles appears in the pool of oil.
5. Apparatus
5.1 Hot Plate, maintained at 200 ± 15°C
(NOTE 1).
NOTE 1: Most electric hot plates of the three-heat
type will give a temperature of approximately
200°C. If the temperature is lower than that
specified, test sensitivity is reduced.
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EXXONMOBIL RESEARCH AND ENGINEERING COMPANY
ALL RIGHTS RESERVED
AM-S 449-09
August 2009
5.2 Temperature-sensing device - capable of
accurately monitoring the temperature of the hot
plate within the limits specified in 5.1.
5.3 Aluminum Block- required if the
temperature-sensing device used to monitor the
temperature of the hot plate is a thermometer. A
solid piece of metal approximately one inch in
diameter and one inch in height has been found
suitable to use. Drill a hole into the block large
enough to insert the bulb of the thermometer. The
thermometer shall be properly supported and held
vertically in place, such as with the use of a clamp.
6. Safety
6.1 This standard may involve hazardous
materials, operations, and equipment. This
standard does not purport to address all of the
safety concerns associated with its use. It is the
responsibility of whoever uses this standard to
consult and establish appropriate safety and
health practices and to determine the applicability
of regulatory limitations prior to use.
6.2 Handle all reagents and samples with
appropriate caution. Obtain and read MSDS for all
substances and follow all instructions for handling,
cleanup, and personal protection. If in doubt about
the composition of a given sample, consult the
requestor for additional information.
6.3 This method involves hot surfaces and hot
oils with the potential for oil spattering and burns to
the skin. Follow all instructions for handling, cleanup,
and personal protection to avoid injury. (NOTE 2)
NOTE 2: Gloves designed to provide thermal
protection at the test temperature of interest, along
with a wiping towel of heavy cloth, such as terry cloth,
has been found suitable to prevent burns to the
hands when wiping clean or removing the pool of oil
from the hot plate. In addition to wearing safety
glasses, the use of a clear protective shield placed
around the hot plate can prevent oil spatter from
contacting an individual, while still allowing visual
observation of the sample as part of the analysis.
7. Procedure
7.1 Turn on the hot plate. If necessary (see 5.3),
place the aluminum block on the hot plate and insert
1
AM-S 449-09
August 2009

the properly supported thermometer in the hole, (Distillation-Electrometric Titration Method” are
otherwise place or support the temperature-sensing presented in Table 1.
device on the hot plate surface. Allow sufficient time
for the hot plate to reach and maintain the test 10. Document History
temperature of interest. Check the temperature of the
hot plate before proceeding. It shall be within 200 ± February 1959 First issued.
15°C. October 1980 Change temperature from
Fahrenheit to Celsius
7.2 Wipe the hot plate clean of all dust and oil January 1985 Insertion of precautionary
film with a wiping towel made of heavy cloth such statements for handling
as terry cloth (NOTE 2). Shake the sample well hazardous materials.
and withdraw approximately 1 mL of oil with a
medicine dropper. Place 1 drop of the oil onto the January 2004 Revision of requirements for a
plate by squeezing the rubber bulb of the dropper temperature-sensing device
(NOTES 3 and 4). Listen for a crackling sound and the insertion of
and watch for spattering or the appearance of precautionary statements for
small bubbles of steam. performing the analysis, as
well as editorial changes.
NOTE 3: The sample size can be increased if August 2009 Revision changes the lower
continuous testing is not being conducted. detection limit, based on data
However, too large a sample will cool the hot plate from an evaluation comparing
and reduce test sensitivity. the crackle method versus the
azeotropic Karl Fischer
NOTE 4: Some laboratories perform the test in a method, as well as editorial
hood with the exhaust turned off during the changes.
performance of the test to better hear any crackling.

7.3 After a test is completed, remove the pool

of oil with a heavy wiping towel. Allow any
remaining oil film to evaporate completely before
placing the next sample on the hot plate.
8. Reporting
8.1 Report water present in the sample if a
crackling sound is heard, the oil spatters, or a cloud
of tiny steam bubbles is seen in the pool of oil.
9. Precision and Bias
9.1 Precision - Since the result of this test is
a subjective or qualitative judgement, no
statement is made regarding precision.
DISCLAIMER
The method, and information upon which it is
based, is believed by ExxonMobil to reflect sound
scientific analytical techniques; however,
ExxonMobil does not represent that the analytical
method is error free. ExxonMobil makes no
representations, warranties, or guarantees, with
respect to its use. ExxonMobil shall have no
responsibility hereunder to (the other party) or to
(such party's) employees for any injury or harm,
for loss of profits, consequential or indirect
damages resulting from use of such information,
or for liabilities relating to negligent acts or
omissions by ExxonMobil's employees.

9.2 Bias - No statement is made regarding

the bias of this test method.

9.3 Data comparing this test method to AM-

S 738, “Water in Gear and Lubricating Oils

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ALL RIGHTS RESERVED
 AM-S 449-09
August 2009

Table 1. Results of Crackle Test versus Karl Fischer Test

Water Testing - Karl Fischer vs. Crackle

KF, ppm Crackle
Sample ID Description water* Result
04-61158 DTE 832 23 no
05-11336 Rarus - GP2 67 no
05-21609 Used oil 103 no
04-12983 Mobilgear 626 107 no
04-14365 Mobilgear 600 115 no
05-18550 Fuel oil 276 no
05-10427 Lube oil 325 no
05-10019 Heavy fuel oil 450 unsure
05-09239 #6 Fuel oil 679 yes
04-70576 #6 Fuel oil 1300 yes
04-14365** Mobilgear 600** 1500 yes
04-12983** Mobilgear 626** 2000 yes
04-50850 Mobilguard 570 2800 yes
00-28815 SAP 007 3400 yes
05-28888 Used oil 8500 yes
05-08896 Fuel oil 18400 yes

* Repeatability is approximately 10% of value

** Original sample spiked with water

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ALL RIGHTS RESERVED