How To Do Millipore Test

How to do Millipore test?
Ransohoff - Millipore Procedure - YouTube

1. Thoroughly Clean & Dry Equipment. [00:11]
2. Clean & Dry Millipore Pad. [00:48]
3. Desiccator Ensures Proper Pad Humidity. [01:04]
4. Determine Baseline Pad Weight. [01:08]
5. Part Flush Down. [01:24]
6. Pour Collected Contaminants Onto Pad. [01:53]
7. Flush Residual Contaminants From Pan. [02:00]
8. Pad Is Removed For Drying. [02:30]
Gravimetric analysis in fluids requires less skill and equipment than microscopic particle
counting. Once the specification has been established by weight, the gravimetric method
provides a simple, inexpensive and highly reproducible routine control measure. For Particle
Contamination in Petroleum Products (D2274) and Aviation Fuels (D2276) the ASTM
recommends a gravimetric and color rating technique.
Refer to online guide to regulated analytical methods
 Introduction
 Filter Selection
 Sample Preparation for Gravimetric Analysis
 Weighing and Calculation
 Inorganic (Noncombustible) Fraction
Introduction
Gravimetric analysis involves filtering a contaminated sample through a control filter and a
sample filter. In this method, you place two preweighed filters, one on top of the other, in a
single filter holder then filter a sample. Particulate contaminants will be retained entirely by
the top test filter. However, both filters are subjected to identical alterations in tare weight as
a result of moisture loss or gain, sample adsorption or desorption, and other environmental
factors. Any change in weight of the bottom (“control”) filter is then applied as a correction to
the weight of contaminant. The contaminant weight is determined by reweighing the test filter
and subtracting its original tare weight. Results accurate to 0.1 mg are routinely attained
using this method.
Filter Selection
The simplest gravimetric analyses use matched weight cassettes. Each cassette contains
two Merck filters that are matched in tare weight to 0.1 mg. These cassettes are factory-
assembled so that preweighing each membrane in the field before filtering the sample is
unnecessary. After sampling, the weight of the contaminant is determined simply as the
difference in weight between the two membranes.
Matched-weight cellulose filters (type AA), 0.8 µm pore size, are preweighed to within
0.1mg. These are available in 47 mm discs, 50 pairs per package, and in 37 mm matched-
weight cassettes. Call Technical Service for more details, or visit:
 MF-Millipore™ Matched-Weight Membrane Pairs, 0.8 µm, mixed cellulose esters, 47

mm, white
 MF-Millipore™ Matched-Weight Membrane Pairs, 0.45 µm, mixed cellulose esters,
47 mm, white
 MF-Millipore™ Matched-Weight Membrane Pairs, 0.8 µm, mixed cellulose esters
with thick pad, 37 mm, white
Sample Preparation for Gravimetric Analysis

The first three steps may be omitted when testing samples from air and other gases, water
and wholly volatile solvents. All steps must be followed with viscous liquids such as paints,
hydraulic oil, and turbine fuels.
Sample Preparation for Gravimetric Analysis

1. Insert the aerosol adapter into stopper on the vacuum flask.
Placing aerosol adapter into rubber stop
2. Remove plugs from cassette and mount the cassette, filter side
up, on the aerosol adapter.
Cassette containing sample is fitted to L

stopper is fitted into filter flask (inlet pl
3. Apply vacuum and introduce membrane-filtered solvent through
the top opening using a solvent dispenser. Release vacuum.

4. Open the cassette and transfer filters into covered glass petri
dishes.

5. Loosen the lids of the glass petri dishes and place in an oven at
90 °C for 30 minutes.

6. Remove the dishes from the oven. With lids ajar, allow the filter
to cool and equilibrate to ambient conditions for at least 15
minutes. Introducing flushing solvent through to
using solvent filtering dispenser.
Weighing and Calculation

The procedure for calculating the results of your gravimetric analysis samples depends on
the filter method used during sample collection.
Matched-Weight Filters or Matched-Weight Cassettes
1. Reweigh both filters and record the weights.

2. Subtract the weight of the control filter from the weight of the test filter. The test
filter will normally be heavier than the control filter. Negative results should be
recorded as “zero” contamination.
Typical results would be:
Test # 1 2
Final weight of test filter (mg) 49.20 51.30
Final weight of control filter (mg) 48.50 50.70
Results in:
mg/volume filtered 0.70 0.60
Control Filter Method
1. Reweigh the filters and record the final weights.

2. Subtract the initial weight from the final weight of each test filter.

3. Determine the loss or gain in tare weight of the control filter by appropriate
subtraction. A weight increase greater than 0.5 mg in the control filter indicates
inadequate flushing of residual test fluid from the filter. The test should be rerun.

4. Apply the control filter weight change as a correction factor to the test result.
Typical results would be:
Test # 1 2 3
Final weight (mg) 49.20 51.30 50.80
Initial weight (mg) 48.00 49.95 49.65
Weight (mg) 1.20 1.35 1.15
Control factor -0.30 -0.30 -0.30
Results in:
mg/volume filtered 0.90 1.05 0.85
Inorganic (Noncombustible) Fraction

The inorganic fraction of the particle weight is easily determined by ashing the filter. This
procedure can be used with filters made of mixed cellulose esters or other ashable material.
1. Clean and ignite a small porcelain crucible.

2. Place in a muffle furnace at 750°C for 20 minutes.

3. Allow the crucible to cool in a desiccator and weigh it to the nearest 0.05 mg.

4. Repeat steps 2 and 3 until the crucible has constant weight.

5. Place the filter containing the contaminant residue in the crucible. Wet it with
ethanol and carefully ignite the filter.

6. Cover the crucible and place it in the muffle furnace at 750°C for 20 minutes.

7. Allow the crucible to cool in a desiccator and reweigh it. As the organic sediment
will have been ignited, the final weight difference represents the inorganic particle
contamination
Particle Identification R
The key to identifying the source of particle contamination is to identify the types of particles
present. Identification almost always reveals the source of the contamination.
Optical Microscopy
The most commonly applied technique in particle identification is optical microscopy. It is
simple to do, inexpensive and, when done with a trained eye, identifies the largest number of
contaminant particles. With experience, a microscopist can recognize a specific particle on
sight. Physical characteristics such as shape, size, color and optical properties are used for
identification.
Supplementary properties include particle hardness (assessed by pushing the microscope

cover slip above the particle with a needle) and magnetism (detected by rotating a small
magnet around the particle and seeing if it behaves like a compass needle).
Often a microscopist can identify minute particles that take major efforts with other analytical
techniques. For example, skin cells, a common contaminant, are easily recognized on sight.
Other methods might show the particles to be complex organic chemicals with traces of
sodium and chloride but still not lead to a useful identification.
To learn more about microscopical particle identification, refer to the Particle Atlas* produced
by McCrone Associates** (* The Particle Atlas by McCrone and Delly published by Ann
Arbor Science Publishers. **McCrone Research Institute, 3620 S. Michigan Avenue,
Chicago, IL 60616.)
Other Methods
If a positive identification is not possible through optical microscopy, other methods used in
particle identification include the electron microprobe or a scanning electron microscope
(SEM) equipped with energy dispersive X-ray analysis (EDXRA). These methods identify the
elements present in a sample. Transmission electron microscopy (TEM) may also identify
very small particles by means of shape and size. In addition, TEM can give selected area
electron diffraction pictures that depend on the particle's crystal structure. By this method,
asbestos fibers such as chrysotile, amosite and crocidolite (blue asbestos) can be
distinguished from each other and from other fibers. X-ray diffraction may also be used to
identify crystal structures and hence chemical compounds. X-ray fluorescence, like EDXRA,
identifies the elements present. Atomic absorption spectroscopy or other spectroscopic
methods are used to determine specific metals, especially hazardous particles in air (e.g.
beryllium or lead). Infrared spectroscopy is useful for identifying organic compounds but,
unlike the methods above, requires a relatively large sample size. When optical microscopy
is inconclusive, you can identify most common contaminants by one of these methods.

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How to do Millipore test?

Ransohoff - Millipore Procedure - YouTube

Refer to online guide to regulated analytical methods

 MF-Millipore™ Matched-Weight Membrane Pairs, 0.8 µm, mixed cellulose esters, 47

Sample Preparation for Gravimetric Analysis

Sample Preparation for Gravimetric Analysis

Placing aerosol adapter into rubber stop

Cassette containing sample is fitted to L

Weighing and Calculation

Matched-Weight Filters or Matched-Weight Cassettes

1. Reweigh both filters and record the weights.

Typical results would be:

Final weight of test filter (mg) 49.20 51.30

Final weight of control filter (mg) 48.50 50.70

mg/volume filtered 0.70 0.60

Control Filter Method

1. Reweigh the filters and record the final weights.

Typical results would be:

Final weight (mg) 49.20 51.30 50.80

Initial weight (mg) 48.00 49.95 49.65

Weight (mg) 1.20 1.35 1.15

Control factor -0.30 -0.30 -0.30

mg/volume filtered 0.90 1.05 0.85

Inorganic (Noncombustible) Fraction

1. Clean and ignite a small porcelain crucible.

Supplementary properties include particle hardness (assessed by pushing the microscope

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