Dropping Point Application

Dropping Point of Lubricating Grease

Definition
The dropping point of a lubricating grease is the specific temperature at which a sample becomes fluid to
form a drop that falls from a standardized dropping
point cup with dimensions conforming to the dimensions specified in ASTM D556-87. The dropping point
cup can be made of chromium plated brass (included
in DP accessory box) or Aluminium (optional accessory).

Standardized dropping point cups

Reference Method
The IP396 standard describes a method for the determination of the dropping point of lubricating grease
with an automatic dropping point apparatus. The apparatus is not explicitely specified but the instrumental features such as maximum temperature, temperature resolution, heating rate and the automated
workflow description is given.
Scope
The dropping point of lubricants is an important test
method for lubricating greases in order to assess the
quality of these materials. Dropping point ranges from
80 C to 300 C can be adjusted depending on the
type of the lubricant (base oil and additive) and the
thickener, the respective proportions and the interactions between the lubricant and thickener. Dropping
point levels of lubricating greases depend mostly on
the thickener type, but could also vary considerably
due to variations in raw materials and manufacturing process and thus could be used as a quality
control standard. The dropping point establishes the
maximum usable temperature of the grease, which is
typically set from 50 C to 100 C below the experimentally determined dropping point. Dropping point
can be used to identify whether the correct grease
was supplied or is in use and to determine whether
used grease can be still used for the intended purpose. The IP396 method assists the identification of a
grease type and to establish and maintain standards
for quality control.

Instrument/Accessories
Excellence Dropping Point System DP70 or
DP90
DP accessory box
Calibration and Adjustment
In order to test the instrument's performance, a temperature calibration shall be performed monthly. The
calibration shall preferentially be performed with reference substances that have a known thermodynamic melting point. Benzoic acid (mp thermodynamic 122.4 0.2C), which is included in the DP
accessory box, is usually sufficient to perform this
check. If available, a reference substance with a
lower melting point such as Benzophenone (47.8
0.2C) or Vanillin (81.5 0.2C) can be used as alternative or in addition. In order to perform the test
there are ready-to-use Mettler-Toledo methods available in the DP70 or DP90. If the results do not meet
the acceptance criteria, the instrument needs to be
adjusted.
Sample preparation
Required items:
DP sample preparation tool
DP dropping point cups (chromium-plated brass
or Aluminium)
Cup lid
Glass collector
Sample carrier with holder
Metal rod for grease removal from cup
Spatula
Procedure
Make sure that the sample cups are clean and free
from any residual fat or oil by using toluene and
ultrasonic irradiation.
Pack the grease sample into the cup with the spatula until it is completely filled. Remove any excess
with the spatula.
Penetrate the metal rod into the grease sample
from the smaller opening at the bottom to the top
in such a manner that it makes contact at both the
upper and lower cup peripheries.
Maintain the contact and move the cup downwards
in a precession-like movement in order to remove a
conical section of the grease.

Dropping Point of Lubricant Grease

Clean the outer surface of the sample with a tissue

that was soaked in Toluene.

Method parameters

The grease removal yields a smooth film of reproducible thickness inside the cup. Since the heat transfer is
dependent on the mass of the sample, it shall be reduced to a reasonable minimum in order to ensure efficient and thorough heat transfer.
Measurement process
The IP396 standard requires an automatic dual heat ramp
workflow for the measurement of the dropping point of lubricating grease. The METTLER TOLEDO M005 method
template allows exact adaptation to the IP396 workflow:
Heat the DP furnace to an initial temperature (T(init))
that is 10 C above the ambient temperature by press
ing Start.
Once the initial temperature is reached place the
sample into the furnace and press Start again.
Heat the samples to the start temperature (T(Start))
with an initial heating rate of 10 C/min. The start
temperature depends on the expected dropping point of
the grease:

Greases with DP <= 200 C:

T(Start) = (Expected DP [C] 20 C)

Greases with DP >200:

T(Start) = 200 C
Once the start temperature T(start) is reached the second heating ramp of 1 C/min shall be started without
time delay (Waiting time = 0 s) and without manual
intervention.
The dropping point shall be detected and recorded automatically and then the furnace shall be cooled to the
initial temperature.

Mettler-Toledo AG, Analytical

CH-8603 Schwerzenbach, Schweiz
Telefon
+41-44-806 77 11
Fax
+41-44-806 72 60
Internet
www.mt.com

Subject to technical changes

11/2013 Mettler-Toledo AG
(electronic publication only)
Marketing Melting and Dropping Point Excellence MTANA

Temperature segments
Initial temperature
Initial heating rate
Start temperature:
Waiting time:
Heating rate:
End temperature:
t(iso):

30 C
10 C/min
150 C
0s
1 C/min
180.0 C
0s

Evaluation
Operation mode:
Set manually:
Temperature correction:
Brightness:
Result round-off:
Calibration substance:

Dropping point
No
No
50%
0.1
No

Termination and end behaviour

Stop at event:
Yes
Stop condition:
Left & right sample
End bahaviour:
Remove temperature: 30 C
Lubricant
grease
Brand

Number
of samples

DP [C]

STD
[C]

IP396 max.
repeatability
[C]

Shell

195.4

0.38

4.6

Shell

149.1

0.14

2.7

Shell

147.2

0.19

2.6

Shell

194.7

0.35

4.6

Shell

180.5

0.39

3.9

Shell

223.4

0.83

6.1

Klber

12

283.6

2.3

10.6

Lubrizol

205.7

0.21

5.1

Lubrizol

230.0

0.35

6.4

The measurement repeatability of all measurements expressed as the standard deviation (STD) is much better
than the maximum repeatabilty permitted by the IP396
which is calculated with the following formula:
r = 1.214 x 10-4 (X2 + 7000) (X = average of two results)

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