BCIS-03A REV.

BCI Battery
Technical FEB02
Manual

Issued 1993-05
Current Revision: 2002-02

RECOMMENDED BATTERY MATERIALS SPECIFICATIONS

VALVE REGULATED RECOMBINANT BATTERIES

TABLE OF CONTENTS

1. Organizations for Referenced Test Methods ...................................................................................... 2

2. Suppliers of Testing Equipment and Materials.................................................................................... 3
3. Sampling Procedure for Recombinant Battery Separator Mat............................................................ 7
4. Standard Test Method for Thickness of Recombinant Battery Separator Mat ................................... 9
5. Standard Test Method for Basis Weight (Grammage) of Recombinant Battery Separator Mat ....... 14
6. Standard Test Method for Volume Porosity of Recombinant Battery Separator Mats...................... 18
7. Test for Pore Size by the First Bubble Method Of Recombinant Battery Separator Mat.................. 20
8. Test for Pore Size by the Liquid Porosimetry Method of Recombinant Battery Separator Mat........ 23
9. Test for Pore Size by the Mercury Intrusion Method of Recombinant Battery Separator Mat.......... 28
10. Test Method for Surface Area of Recombinant Battery Separator Mat ............................................ 31
11. Test Method for Determining Percent Moisture Content of Recombinant Battery Separator Mat.... 34
12. Test Method For Percent Ignition Weight Loss of Recombinant Battery Separator Mat .................. 36
13. Test Method for Tensile Strength and Elongation of Recombinant Battery Separator Mat.............. 39
14. Acid Wetting and Wicking of Recombinant Battery Separator Mat................................................... 45
15. Test Method for Determining the Compressibility of Recombinant Battery Separator Mat .............. 46
16. Test for Determining Acid Weight Loss of Recombinant Battery Separator Mat (Reflux Method) ... 48
17. Extractable Metallic Impurities of Recombinant Battery Separator Mat............................................ 51
18. Extractable Chloride of Recombinant Battery Separator Mat ........................................................... 57
19. Test Method for Electrochemical Compatibility of Recombinant Battery Separator Mat .................. 58
20. Total Organic Carbon For Recombinant Battery Separator Mat....................................................... 71
21. Identification of Organic Impurities In Recombinant Battery Separator Mat ..................................... 72
22. Electrical Resistance of Recombinant Battery Separator Mat .......................................................... 77
23. Conversion Factors for SI Units ........................................................................................................ 78
 BCIS-03a Rev. Feb02

1. ORGANIZATIONS FOR REFERENCED TEST METHODS

Referenced Test Method Procurement Addresses

1.1. American National Standard Institute, Inc. (ANSI)

1430 Broadway
New York, NY 10018 USA
Tel: 212-260-5400

1.2. ASTM
1916 Race Street
Philadelphia, PA 19103 USA
Tel: 212-260-5400

1.3. British Standard Institution

2 Park Street
London W1A 2BS, England
Tel: 266933 BSI LON G

1.4. Technical Association of Pulp and Paper Industries (TAPPI)

PO Box 105113
Atlanta, GA 30348-5113 USA
Tel: 800-333-8686 (USA)
Tel: 800-446-9431 (Canada)
Tel: 404-446-1400
Fax: 404-446-6947

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2. SUPPLIERS OF TESTING EQUIPMENT AND MATERIALS

2.1. Summary

The following list of manufacturers and suppliers of testing materials, instruments and
machines is published by BCI solely for the convenience of its members. BCI has made no
investigation of its own with respect to the listed company compliance, however, and makes
no certification, representation or warranty, express or implied, with respect to such
compliance nor with respect to the quality of performance of such materials, instruments or
machines. Publication of this list or any reference to it in BCI Test Methods shall not be
construed to be any such certification, representation or warranty. Any purchaser or user of
such material equipment or machinery desiring any certification or warranty with respect
thereto must negotiate the same directly with the manufacturer or supplier from whom he
makes such purchases.

This equipment supplier listing is not intended to be inclusive, only a reference point, any
manufacturer or supplier wishing to have his name included in this list should direct a request
to BCI Headquarters.

2.2. General Supplies

2.2.1. Cole-Parmer Instrument Company

Vernon Hills, IL 60061
Tel: 800-323-4340
Fax: 847-247-2929

2.2.2. Fisher Scientific

711 Forbes Avenue
Pittsburgh, PA 15219

2.2.3. Nalge Company

Rochester, NY 14602-0365
Tel: 716-586-8800

2.2.4. Omega Engineering, Inc.

PO Box 4047
Stamford, CT 06907

2.2.5. SGA Scientific Inc.

735 Broad Street
Bloomfield, NJ 07003
Tel: 800-245-2300

2.2.6. Thomas Scientific

99 High Hill Road
PO Box 99
Snedesboro, NJ 08085-0099
Tel: 800-345-2100

2.2.7. VWR Scientific Products

1310 Goshen Pkwy.
West Chester, PA 19380
Tel: 610-431-1700

2.2.8. EG&G, Princeton Applied Research

PO Box 2565

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 BCIS-03a Rev. Feb02

Princeton, NJ 05840
Tel: 609-452-2111

2.3. Surface Area (1) and Porosity (2)

2.3.1. Coulter Electronics, Ltd. (2)

Northwell Drive
Luton, Beds LU3 3RH England
Tel: (0582) 582442

590 West 20 Street

Hialeah, FL 33010
Tel: 305-885-0131
Tel: 800-653-4306

2.3.2. Micromeritics Instruments (1) (2)

One Micromeritics Drive
Norcross, GA 30093
Tel: 770-662-3633

2.3.3. Quantachrome Corporation (1) (2)

1900 Corporate Drive
Boynton Beach, FL 33426

2.3.4. PMI (Porous Material, Inc.) (2)

83 Brown Road
Ithaca, NY 14850
Tel: 607-257-5544
Tel: 800-332-1764

2.4. Atomic Absorption

2.4.1. Spectro Analytical Institute

160 Authority Drive
Fitchburg, MA 01420
Tel:

2.4.2. Spectra Instrumentation

11850 Industrial Court
Auburn, CA 95603
Tel: 916-823-1638

2.4.3. Buck Scientific, Inc.

58 Fort Point Street
East Norwalk, CT 06855-1097
203-853-9444

2.4.4. Cathodeon, Ltd.

Nuffield Road
Cambridge, England CB4 1TW
Tel: 1-022-346-0100

2.4.5. Fisons Instruments, Inc.

24911 Avenue Sanford
Valencia, CA 91356
Tel: 800-551-8741

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2.4.6. Leeman Labs, Inc.

600 Suffolk Street
Lowell, MA 01854
Tel: 508-454-4442

2.4.7. The Perkin-Elmer Corp.

Norwalk, CT 06859-0177
Tel: 800-762-4000

2.4.8. Phillips Export B.V.

Lelyweg 1
Almelo, Netherlands 7602EA
Tel: 1054-903-9440

2.4.9. Preiser Scientific, Inc.

94 Oliver Street
St. Albans, WV 24177
Tel: 800-624-8285

2.4.10. Spectro Products, Inc.

385 State Street
North Haven, CT 06473
Tel: 203-281-0122

2.4.11. Biomed Instruments, Inc.

1020 S. Raymond Ave., No. B
Fullerton, CA 92631
Tel: 714-870-0290

2.4.12. Stackpole/Ultra Carbon

PO Box X924
Baycity, MI 48707
Tel: 517-894-2911

2.4.13. Thermo Jerrell Ash Corp.

Forge Pkwy.
Franklin, MA 02038
Tel: 800-225-4087

2.4.14. Varian Instrument Group

220 Humboldt Court
Sunnyvale, CA 94089
Tel: 800-231-8134

2.4.15. VWR Scientific Products

1310 Goshen Pkwy
West Cjester. {A 19380
Tel: 215-891-2782

2.5. Thickness (1) and Tensile (2)

2.5.1. Customer Scientific Instruments, Inc. (1)

13 Wing Drive
Kearny, NJ 07927
Tel: 201-538-8500

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2.5.2. EMUECO Inc. (1)

PO Box 16
Newberg, OR 97132
Tel: 503-538-8616

2.5.3. Huygen Instruments Assoc. (1)

8782 Gull Road
Richland, MI 49083
Tel: 816-629-5824

2.5.4. Instron Corporation (2)

2500 Washington Street
Canton, MA 02021

2.5.5. H.E. Messmer, Ltd.

144 C Off Road
London N1 1NS England
Tel: 01-607-2416/7

2.5.6. Testing Machines Inc. (1) (2)

400 Boyview Avenue
Amityville, NY 11701
Tel: 516-842-5400

2.5.7. Thwing-Albert Instrument Co. (1) (2)

10960 Dutton Road
Philadelphia, PA 19154
Tel: 215-637-0100

2.5.8. Tinius Olsen Testing Machine Co. (2)

Easton Road
Willow Grove, PA 19090-0429
Tel: 215-675-7100

2.5.9. B.C. Ames Co. (1)

131 Lexington Street
Waltam, MA 02254-0070
Tel: 617-893-0095

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 BCIS-03a Rev. Feb02

3. SAMPLING PROCEDURE FOR RECOMBINANT BATTERY SEPARATOR MAT

3.1. Scope

3.1.1. This method summarizes sampling requirements for recombinant battery separator mat
(RBSM) and outlines the sample size needed for each BCI RBSM Test Method.

3.1.2. Prior to purchase, there should be agreement between supplier and purchaser on details of
the sampling and acceptance procedure as well as on the required physical and chemical
properties, dimensional tolerance, etc., and the test methods to be employed to determine
frequency (and/or need) of testing.

3.2. Reference Documents

3.2.1. BCI’s RBSM Test Methods, BCIS-03a

3.2.2. TAPPI’s T 400 – Sampling and accepting a single lot of paper, paperboard, fiberboard, or
related product.

3.2.3. ASTM’s – D585 – Sampling and accepting a single lot of paper, paperboard, fiberboard, or
related products.

3.3. Terminology

3.3.1. LOT – a quantity of RBSM of a single grade, making (manufacture run), grammage, and
thickness about which it is desired to make a judgement (usually as to conformance to
specification) by examining or testing a small fraction called the sample.

3.3.2. SAMPLE – a specified number of test units selected according to a prescribed procedure to
represent a lot. Each test method should be reviewed for any special procedures.

3.3.3. TEST UNIT – an area of RBSM sufficient to obtain a single adequate set of test result for all
the properties to be measured.

3.3.4. SPECIMEN – a test unit, or a portion of a test unit, upon which (for a specified property) a
single test determination is to be made.

3.3.5. TEST DETERMINATION – the process of carrying out the series of operations specified in
the test method whereby one or more readings (observations) are made on a test specimen
and the observations combined to obtain the value of a property of the test specimen, or the
value obtained by the process.

3.3.6. TEST RESULT – the value obtained for one test unit of the sample by carrying out the
complete protocol of the test method, the value being (as specified in the test method) either
a single test determination or specified combination of a number of determinations.

3.3.7. ROLL – A coil of RBSM of continuous length.

3.3.8. QUALIFICATION

3.3.8.1. RBSM test which are done for initial acceptance of vendor’s material.

3.3.8.2. An agreement between user and supplier on subsequent testing frequency.

3.4. Procedure

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 BCIS-03a Rev. Feb02

3.4.1. RBSM generally is a very delicate product. Any rough handling or misuse of the test
specimen may result in test results, which are not representative of the material.

3.4.2. RBSM may have specific aging characteristics. These aging characteristics may have no
effect on the RBSM performance inside a battery but will result in different results of physical
properties such as tensile and elongation. This aging effect is believed to be accelerated by
hot and humid conditions.

3.4.3. If a lot number or roll identification system is needed then reference should be made to either
TAPPI’s T400 or ASTM’s D-585 for guidance.

3.4.4. Table No. 1 should be referenced for a summary of test specimens needed and the size of
each specimen.

Table No. 1

Sample Size Frequency Comments

Test Method Needed (Per Lot)
Thickness 1000 cm2 1 per roll Thickness should be checked right after
sampling.
Grammage 1000 cm2 1 per roll Moisture must be subtracted.
Volume Porosity 1000 cm2 Qualification Use thickness and grammage results.
Pore Size 300 cm2 Qualification RBSM, which has been densified, will give
smaller pore size values.
Surface Area 10 g. Qualification Sample size depends of sample surface area
and may vary depending on whether the test
specimen is taken from the wire of felt side of
the RBSM.
Moisture Content 10 g. 1 per roll
Ignition Loss 6 g. Qualification
Tensile and 25 x 150 mm Qualification Tensile is extremely sensitive to handling.
Elongation 3 – strips Sufficient sample should be obtained to cut
strips without any damage.
Compression 1000 cm2 Qualification
Acid Weight Loss 1 g. Qualification
Extractable Metal 5 g. Qualification
Analysis
Extractable No Method Qualification
Chlorine Analysis
Electrochemical 8 x 10 cm Qualification
Compatibility
Organic Impurities Variable Qualification
Organic Variable When Required
Identification
Notes: Remove the outer two wraps before sampling.

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 BCIS-03a Rev. Feb02

4. STANDARD TEST METHOD FOR THICKNESS OF RECOMBINANT BATTERY

SEPARATOR MAT

4.1. Scope

4.1.1. This method covers the determination of the thickness of recombinant battery separator mat
(RBSM) which is used in a recombinant lead acid cell. This method is to be used, except as
otherwise required by materials specification.

4.1.2. This method covers RBSM from 0.127 mm (0.005 in) to 3.048 mm (0.125 in).

4.1.3. This method covers measurement of RBSM using a pressure of 10 kPa (1.5 psi) and a 29
mm (1.14 in) presser foot.

4.2. Referenced Documents

4.2.1. ASTM Standards

4.2.1.1. ASTM D-374 Standard Test Method for Thickness of Solid Electrical Insulation.

4.2.1.2. ASTM D-645 Standard Test Method for Thickness of Paper and Paperboard. ISO No. 534.

4.2.2. TAPPI Standards

T 411 Thickness (Caliper) of Paper and Paperboard.

4.3. Significance

Thickness and its consistency is an important property of RBSM. RBSM is used at various
thicknesses and degrees of compression. The thickness of RBSM allows for the proper
selection of the mat for a given cell construction and the electrical characteristics desired.

4.4. Description of Terms

4.4.1. RECOMBINANT BATTERY SEPARATOR MAT (RBSM) – Any material intended for use as a
separator between the cathode and anode plates in a VRLA battery.

4.4.2. THICKNESS – The perpendicular distance between the two principal surfaces of a material,
as determined by the prescribed procedure.

4.5. Apparatus

4.5.1. Method A – Manually-Operated Dead Weight Type Thickness Gauge

4.5.1.1. The gauge shall be a dead-weight type having a presser foot and a lower anvil parallel to
within 0.002 mm (0.0001 in). The presser foot shall move on an axis perpendicular to the
anvil face.

4.5.1.2. The diameter of the presser foot and anvil shall measure 29 mm (1.14 in). The presser foot
shall apply pressure of 10 ± 0.6 kPa (1.5 psi) on the specimen.

4.5.1.3. If a dial gauge is used, the dial spindle shall be vertical. The dial shall be at least 50 mm (2
in) in diameter and shall be continuously graduated to read directly to 0.002 mm (0.0001 in).
If necessary, it will be equipped with a revolution counter recording the number of complete
revolutions of the large hand. The dial indicator shall be essentially friction free.

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 BCIS-03a Rev. Feb02

4.5.1.4. The indicator shall give readings repeatable to 0.001 mm (0.00004 in) at a zero setting or on
a steel gauge block.

4.5.1.5. The frame of the indicator shall be of such rigidity that a load of 13 N applied on the dial
housing, out of contact with either the weight or the presser foot spindle, will produce a
deflection of the frame not greater than the smallest division on the indicator.

4.5.2. Method B – Motor-Operated Dead Weight Gauge:

4.5.2.1. Except as additionally defined in this Subsection, the instrument shall meet the requirements
of 4.5.1.1.

4.5.2.2. The dead weight dial spindle shall be raised and lowered by a constant-speed motor through
a mechanical linkage such that the rate of descent (for a specified range of distance between
the presser foot and the anvil) and the dwell time on the specimen are within the limits
specified for the material being measured. Downward force on the presser foot shall be only
that of gravity on the weighted spindle with no addition from the lifting-lowering mechanism.

4.6. Calibration

(General Considerations for Care, Use and Calibration of Thickness Measuring Apparatus)

4.6.1. Surfaces of Micrometer Apparatus

4.6.1.1. Cleaning Surfaces of Micrometers – Before and during instrument calibration and thickness
measurements, the micrometer surface shall be maintained in a clean condition. Cleaning
can be accomplished by pulling through a sheet of smooth paper.

Warning
When using a motorized micrometer, caution should be exercised in pulling a sheet of RBSM
through the anvil while in motion, since this may negatively effect the life of the instrument.

4.6.1.2. Parallelism of Surfaces of Micrometers:

4.6.1.2.1. A hardened calibrated gauge or a calibrated tread measuring cylinder of suitable dimensions
to fit conveniently between the presser foot and the anvil of the thickness gauge shall be
measured at several locations. Note the maximum variations of readings.

4.6.1.2.2. In calibrating the gauge, it is important that the gauge block or cylinder is inserted only under
the edge of the pressure foot.

4.6.1.3. Flatness of Surfaces of Micrometers:

4.6.1.3.1. The anvil and spindle surfaces of the micrometer shall be flat to within 0.0013 mm (0.00005
in). The flatness may be determined by use of an optical flat.

4.6.1.3.2. A flat surface forms straight, parallel, and equidistant fringes.

4.6.1.3.3. A grooved surface forms straight parallel fringes at unequal intervals. The estimated
maximum displacement of any line from its normal position, where all lines would be
equidistant, is a measure of deviation from flatness.

4.6.1.3.4. A symmetrical concave or convex surface forms concentric circular fringes, and their number
is a measure of deviation from flatness.

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 BCIS-03a Rev. Feb02

4.6.1.3.5. An unsymmetrical concave or convex surface forms a series of curved fringes, cutting the
periphery of the micrometer surface. The number of fringes cut by a straight line connecting
the terminals of any fringe is a measure of the deviation from flatness.

4.6.2. Calibration of Micrometers (General Requirements)

4.6.2.1. All micrometers shall be calibrated in a standard laboratory atmosphere maintained at 50%
relative humidity and 23°C (73°F), or some other standard conditions as mutually agreed
upon between the purchaser and seller. To calibrate any thickness-measuring device, it is
necessary to obtain standard gauge blocks or other metallic objects of known thickness. The
accuracy of these blocks shall be ±10% of the smallest scale division of the micrometer dial
or scale. Thus, if an instrument’s smallest scale division is 0.002 mm (0.00001 in.), then the
standard gauge block thickness shall be within ±0.0002mm (0.00001 in.). Calibration
procedures shall be performed at least twice every year, and only after the instrument has
been checked and found to meet the requirements of these procedures.

4.6.2.2. Manual Gauge

Force – The force applied to the presser foot spindle and the weight necessary to move the
pointer upward from the zero position shall not exceed the product of the presser foot area
and the maximum permissible force per unit area. The force applied to the presser foot
spindle and the weight necessary to just prevent movement of the pointer from a higher to a
lower reading shall be greater than the product of the presser foot area and the minimum
permissible force per unit area specified for the pressure exerted on the specimen.

4.6.2.3. Accuracy of Scale Divisions

Set the instrument to zero reading, then measure the thickness of the standard gauge blocks
– block thickness are known to be within 0.0002 mm (0.00001 in). Calibration data shall be
collected from observations made on standard gauge blocks using detailed procedures
specified for making measurements on a specimen. The calibration data shall be utilized to
construct a calibration curve, which shall be used to apply the indicated corrections to
observations made on specimens.

4.6.2.4. Motor – Operated Gauge

The calibration of the motor-operated dead weight gauge shall be performed in the same
manner as described for a manually operated gauge, except that the standard gauge blocks
shall be measured using detailed procedures specified for making measurements on a
specimen.

4.7. Procedure

4.7.1. RBSM will give different thickness measurements based on parameters such as conditioning,
rate of loading, ultimate load, and foot/anvil dimensions. Different conditions will result in
different readings of thickness.

4.7.2. Any thickness testing shall be performed within two days of receipt of a shipment. Testing of
any material shall be done within 2 hours (maximum) from the removal of the samples from a
sealed package.

NOTE: It has been determined that if RBSM conditioned or exposed to a 70% relative
humidity atmosphere, a loss of approximately 5-6 percent of its original thickness could be
realized.

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 BCIS-03a Rev. Feb02

4.7.3. Testing should be conducted in a controlled atmosphere (if possible) of 23°C (73°F) and 50%
RH. See Subsection 4.6.2.1.

4.7.4. Manual Gauge

4.7.4.1. Place the gauge on a clean, solid, level table, free of excess vibration. Clean the contacting
surfaces of the presser foot and anvils. Make the instrument’s zero adjustment. Lift the
presser foot and place the specimen under it. Lower the foot onto the specimen at the
location outside the area to be measured. Then raise the foot slightly, move the specimen to
the measurement position, and reposition the presser foot to obtain a reading from 0.007 mm
(0.0003 in.) to 0.01 mm (0.0004 in) higher than the preceding reading then drop the foot.

4.7.4.2. For each succeeding measurement, raise the presser foot slightly, and move the specimen to
the next measurement position. Again, position the presser foot to obtain a reading from
0.007 mm (.0003 in) to 0.01 mm (0.0004 in) higher than the preceding reading, and drop the
foot.

4.7.4.3. Do not make measurements with the presser foot less than 6 mm (0.23 in) from the edges of
the specimen.

4.7.4.4. Recheck the instrument zero setting after measuring each specimen. A change in the setting
is usually the result of contaminating particles being carried by the specimen to the contacting
surfaces of the presser foot and anvil and necessitates the cleaning of the surfaces (as in
4.5.1.1).

4.7.5. Motor Gauge

4.7.5.1. Place the motor driven gauge on a clean, solid, level table, free to excess vibration. Clean the
contacting surfaces of the presser foot and anvil as in 4.6.1.1, and make the instrument zero
adjustment. With the gauge running, position the specimen for the first measurement while
the presser foot is near its maximum height. Take the reading when the indicator pointer
comes to a rest.

4.7.5.2. For each succeeding measurement, shift the specimen when the pressure foot is near its
maximum height and repeat the above procedure at the next measurement position.

Caution: Never attempt to move the RBSM while the presser foot is in contact with the anvil.
This will rip the RBSM and could damage the gauge.

4.7.5.3. Do not make measurements with the presser foot less than 6 mm (0.23 in) from the edges of
the specimen.

4.7.5.4. After measuring each specimen, readjust the instrument zero and clean the instrument as
necessary.

4.7.6. Take at lest five readings, ten if feasible, spaced to represent the full width of the specimen
(at right angles to the machine orientation of the RBSM). Average the readings.

4.8. Report

If a report is required, results of the thickness determinations shall be recorded on a form that
includes the following:

4.8.1. Identification of the material being reported by type, grade, source, lot number, etc.

4.8.2. Date of testing.

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4.8.3. Identification of the testing laboratory and responsible personnel.

4.8.4. Model of gauge used.

4.8.5. Number of specimens per sample and number of measurement per specimens.

4.8.6. Conditioning procedures used (test ambient temperature and relative humidity) and,

4.8.7. Arithmetic mean, sample standard deviation and the range of all measurements.

4.9. Precision and Bias

4.9.1. Precision

A round robin study on one material by three laboratories has indicated a within laboratory
average coefficient of variation of 1.7 percent and a between laboratory reproducibility of 6.3
percent. (Based on 20 separate measurements and each measurement counted as a result.
An average reading of results will give a lower percent reproducibility).

4.9.2. Bias

No statement on bias can be made due to a lack of a standard reference material.

4.9.3. Results will be effected by the relative humidity of the test conditions and prior handling of the
material, since most RBSM are delicate materials.

4.9.4. Because of the high void volume of RBSM, slight changes in procedure, presser foot
diameter, and load will have large effects on the results of the thickness determinations.

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5. STANDARD TEST METHOD FOR GRAMMAGE (BASIS WEIGHT) OF RECOMBINANT

BATTERY SEPARATOR MAT

5.1. Scope

5.1.1. This test procedure covers the determination of the weight per unit area of recombinant
battery separator mat (RBSM) used in battery applications.

5.1.2. The customary units used by the battery industry for this property are grams per square
meter (g/m2). Other units covered by this method are pounds per 3000 square feet (lb/3000
ft2) and pounds per 1000 square feet (lb/1000 ft2).

5.1.3. Weight per unit area is measured on a moisture-free sample and then corrected for the
moisture content of the test specimen.

5.1.4. This method includes both the measure of a minimum size mat sample and the range of
weights, as determined on smaller portions of this sample.

5.1.5. A rapid determination method is also included, which quickly provides approximate values.

5.2. Referenced Documents

5.2.1. BCI Recombinant Mat Test Method BCIS-03-a 11, Test Method for Determining Percent
Moisture Content of Recombinant Battery Separator Material.

5.2.2. ASTM D646 Grammage of Paper and Paperboard (Weight Per Unit Area).

5.2.3. TAPPI T-410 Grammage of Paper and Paperboard (Weight Per Unit Area).

5.2.4. British Standard BS 3432 Grammage.

5.2.5. International Standards Organization ISO 536.

5.3. Terminology

5.3.1. BASIS WEIGHT – The weight of RBSM material per unit of defined area.

5.3.2. GRAMMAGE – The weight of a RBSM material expressed in grams per square meter.

5.4. Significance and Use

5.4.1. The performance of a recombinant lead-acid battery is dependent upon the mass of mat
between the plates and the applied compression. Therefore, basis weight must be controlled
within reasonably close tolerances.

5.4.2. Per pound, RBSM is one of the most expensive components used in a lead-acid battery.
Since, in general, it is sold by weight but used by area, grammage (basis weight)
measurements are one of the criteria by which a shipment of mat is determined to be
acceptable.

5.5. Apparatus

5.5.1. Cutting Device, such as a “four square” cutter, or other device for ensuring parallelism of the
opposite edges, normally capable of repeatedly cutting out test specimens whose area, in at
least 95 out of 100, falls with ±0.5% of a known area, as determined by this method in 5.6.1.

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5.5.2. Measuring Device capable of measuring the dimensions of the test specimen to an accuracy
of 0.2%.

5.5.3. Electric Drying Oven (non-air recirculating), capable of maintaining a temperature of 150 ±
5°C (302°F ± 9°F).

5.5.4. Weighing Device, readable and accurate to within ±0.25% of applied load, and shielded from
air currents when used, Calibration as determined in 5.6.2.

5.6. Calibration

5.6.1. Checking of Cutting Device

Frequently (5.6.3) check the area cut by using the measuring device (5.5.2) to measure 20
test specimens. The cutting accuracy specified in 5.5.1 is attained when the standard
deviation of individual areas is less than 0.25% of the mean area.

5.6.2. Checking of Weighing Device

5.6.2.1. Check the accuracy of the weighing device (5.6.3) by applying accurately measured masses
with both increasing and decreasing loads. The sheet-weighing device must be accurate to
±0.25% of the applied load (5.5.4).

5.6.2.2. Before each use, frictional effects shall be sufficiently minimal and the zero reading shall be
sufficiently correct to obtain the required weighing accuracy (5.5.4).

5.6.3. Frequency of Checking

The frequency of checking in 5.6.1 and 5.6.2 should be based on experience. A new device
should be checked several times before being put into use. Then, if in continual use, it should
be checked twice daily until stability is established, then weekly, monthly, or less frequently
as indicated by its stability, unless moved or unduly disturbed. Because of wear, the cutting
device may require more frequent checking than the weighing device.

5.7. Sampling

5.7.1. RBSM is usually produced on papermaking equipment as large rolls of 50 inch or greater
width. It is generally converted into narrow rolls, as low as 1 inch wide, for use by battery
manufacturers. Therefore, a minimum sample area rather than exact sample dimensions is
specified.

5.7.2. Each test specimen must be comprised of a minimum area of 1000 cm2 (approximately 150
in2).

5.7.3. A minimum of three specimens shall be sampled from each lot, unless the test is to be
performed on an entire slit roll.

5.7.4. Following the completion of testing in 5.8.1.5, each specimen should be cut into 5 pieces of
approximately equal size for a determination of basis weight uniformity within a test
specimen.

5.8. Procedure

5.8.1. Method A

5.8.1.1. Cut the test specimens as described in 5.7.2 and 5.7.3 using the cutting device (5.5.1).

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 BCIS-03a Rev. Feb02

5.8.1.2. Measure and record the dimensions (centimeters or inches) of each specimen using the
measuring device (5.5.2).

5.8.1.3. Dry the specimens for 1 h at 150°C (302°F) in the electric drying oven (5.5.3). Remove the
specimens from the oven and allow them to cool in a desiccator for 15 minutes.

5.8.1.4. Remove each specimen from the desiccator and quickly weigh it using the weighing device
(5.5.4). Record the weight in grams (or in kg if a full roll).

5.8.1.5. Return each specimen to the desiccator as soon as the weighing is complete.

5.8.2. Method B – Basis Weight Uniformity

5.8.2.1. Remove a test specimen from the desiccator and cut it into five pieces of approximately equal
size using the cutting device (5.5.1).

5.8.2.2. Weigh each piece using the weighing device (5.5.4) and record the weight in grams.

5.8.2.3. Repeat 5.8.2.1 and 5.8.2.2 until all specimens from 5.8.1.1 have been cut and weighed.

5.8.2.4. Measure each small specimen with the measuring device (5.5.2) and record the dimensions
in centimeters (inches).

5.8.3. Method C – Rapid Determination

5.8.3.1. Cut and measure the test specimens as in 5.8.1.2 and 5.8.1.3.

5.8.3.2. Weigh each test specimen using the weighing device (5.5.4) and record the weight in grams.

5.8.3.3. This method is helpful for distinguishing between different grades of RBSM. If accuracy
greater than 2% is needed, the specimen can be dried, cooled and reweighed as in 5.8.1.3
and 5.8.1.4.

5.9. Calculations

5.9.1. Measured and calculated parameters (units):

L - Length (cm, in, ft)

W - Width (cm, in)
A - Area (cm2, m2, in2, ft2)
M - Moisture Content (%) as determined in 5.2.1 or 5.8.3.3
WT - Mass (lb)
OBW - Oven-Dry Basis Weight (g/m2, lb/3000 ft2, lb/1000 ft2)
BW - Basis Weight (same units as OBW)

5.9.2. See Annex (5.12) for a table of unit conversions.

5.9.3. Specimen Area: A = L x W

5.9.4. Oven-Dry basis Weight: OBW = WT/A

5.9.5. Basis Weight: BW = (OBW)/(1 – (M/100))

5.10. Report

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5.10.1. Report the basis weight (grammage) average and range in g/m2 (lb/3000 ft2 or 1000 ft2) to
three significant figures for each test unit, along with the moisture content.

5.10.2. Sample size other than 1000 cm2 (150 in2) should be reported.

5.10.3. Results of basis weight (grammage) uniformity tests should be reported as averages and
standard deviations.

5.11. Precision and Bias

5.11.1. Precision

No statement may be made on the precision of this test method, since round robin testing
among laboratories was not conducted.

5.11.2. Bias

No statement on bias may be made due to the lack of a standard reference material.

5.12. Annex: Conversion Factors (Mandatory Information)

To Convert From To Units Multiply By

Length & Width
cm ft 3.281 x 10-2
ft m 3.048 x 10-1
in m 2.540 x 10-2
m ft 3.281

Area
cm2 ft2 1.076 x 10-3
cm2 m2 1.000 x 10-4
ft2 m2 9.290 x 10-2
in2 ft2 6.944 x 10-3
in2 m2 6.452 x 10-4
m2 ft2 1.076 x 10-1

Mass
g lb 2.205 x 10-3
lb g 4.536 x 10-2
kg g 1.000 x 10-3
kg lb 2.205

Basis Weight
g/m2 lb/1000 ft2 2.048 x 10-1
g/m2 lb/3000 ft2 6.144 x 10-1
lb/1000 ft2 g/m2 4.882
lb/3000 ft2 g/m2 1.627

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6. STANDARD TEST METHOD FOR VOLUME POROSITY OF RECOMBINANT BATTERY

SEPARATOR MATS

6.1. Scope

This method covers the calculation of volume porosity to be used for recombinant battery
separator mat RBSM).

6.2. Referenced Documents

6.2.1. BCI

6.2.1.1. Method II for Standard Test Method for Thickness of Recombinant Battery Separator, BCIS-
03a-4.

6.2.1.2. Method III Standard Test Method for Grammage (Basis Weight) of Recombinant Battery
Separator Material, BCIS-03a-5.

6.3. Terminology

6.3.1. Volume Porosity – the ratio of the total void volume to the total apparent volume, expressed
as a percentage.

6.3.2. Apparent Volume – the volume obtained by multiplying the sample area by the thickness
measured at a specified pressure.

6.3.3. Void Volume – that portion of the apparent volume that is not occupied by the solids used to
make the separator. It is usually determined by subtracting the volume of the solids from the
apparent volume.

6.3.4. Solid Volume – the volume that is calculated from the weights of the separator components
and their densities.

6.3.5. Average Density of Solids = (dry weight of RBSM)/(Total solid volume based on a stated
thickness measurement technique)

(supplied by separator manufacturer in g/cc)

6.4. Significance and Use

The volume porosity of RBSM in the compressed state limits the maximum amount of acid
between the plates.

6.5. Apparatus

Thickness gauge – manually or motor-operated dead weight gauge as described in BCI

Standard Test Method II for Thickness of Recombinant Mat.

6.6. Sampling

Sample size shall be as specified in the BCI’s Standard Test Method II for Thickness of
Recombinant Mat.

6.7. Conditioning

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Conditioning shall be as specified in the BCI Standard Test Method II for Thickness of
Recombinant Battery Separator Mats.

6.8. Procedure

6.8.1. Obtain the average density of solids of the RBSM from the battery separator manufacturer.

6.8.2. Measure the thickness and basis weight of the sample as described in the BCI test methods
BCIS-03a for RBSM.

6.8.3. Calculate the volume porosity using the following formula:

For thickness measured in mm and grammage measured in g/m2

VP (%) = (100((TH x 25.4) – (BW/ADS)))/(TH x 25.4)

Where:
VP (%) = volume porosity expressed as a percentage
TH = sample thickness
BW = basis weight in grams per square meter
ADS = average density of solids

6.9. Reporting

If a report is required, it must include the pressure at which the thickness was measured.

6.10. Bias

No statement of bias can be made because there is no standard reference material.

6.11. Derivation of Volume Porosity Formula

Let:
TH = sample thickness
BW = grammage g/m2
ADS = average density of solids

By Definition: Volume Porosity = (Void Volume)/(Apparent Volume)

Assume Sample Area to be 1 Square Meter:

Apparent Volume (cc) = TH (mm) x 1 m2 x (10000 cm2/ m2) x (1 cm/10 mm).

= TH (mm) x 1000

Apparent Volume (cc) = TH (mil) x 1 m2 x 10000 cm2/m2 x 0.00254 cm/1 mil

= TH (mil) x 25.4

Solid Volume = Sample Weight = (Grammage)/ADS

Apparent Volume = 100((TH x 1000 – (BW/ADS))/(TH x 1000)

OR

= 100((TH x 25.4) – (BW/ADS))/(TH x 25.4)

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7. STANDARD TEST METHOD FOR PORE SIZE CHARACTERISTICS BY THE FIRST

BUBBLE METHOD OF RECOMBINANT BATTERY SEPARATOR MAT

7.1. Scope

This procedure covers method of measuring maximum pore diameter of recombinant battery
separator mat (RBSM) through the first bubble point test.

7.2. Reference Documents

7.2.1. ASTM F-316 pore size characteristics of membrane filters by bubble point and mean flow
pore test.

7.2.2. BS 6410 British standard method of test for filter papers.

7.3. Principle of Test Method

The bubble point test is based on the principle that a wetting liquid is held in separator pores
by capillary attraction and surface tension, and the minimum pressure required to force liquid
from these pores is a function of pore diameter. The pressure at which a steady stream of
bubbles appears in this test is the bubble point pressure.

7.4. Apparatus

7.4.1. Sample holder Figure 7.1.

Figure 7.1 – Sample Holder

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7.4.2. Test set-up Figure 7.2.

Figure 7.2 – Test Setup

7.4.3. Pressure gauges.

7.5. Reagents

7.5.1. Reagent grade or high purity liquid of known surface tension.

7.5.1.1. Isopropyl alcohol.

7.5.1.2. Petroleum distillate with surface tension of 30 dynes/cm at 25°C.

7.5.1.3. Mineral oil with surface tension of 34.7 dynes/cm at 25°C.

7.5.1.4. Porofil wetting liquid from Coulter Electronics, Inc.

7.5.2. Clean compressed air.

7.6. Procedure

7.6.1. Thoroughly wet the RBSM sample by immersing it in the liquid.

7.6.2. Place the wet RBSM in the sample holder, close it, and fill the fluid reservoir with liquid.

7.6.3. Apply gas pressure making sure to eliminate liquid back flow. Slowly increase gas pressure.

7.6.4. Record the lowest pressure when a steady stream of bubbles rises from center of liquid
reservoir.

7.7. Calculation

Calculate the maximum pore diameter d in µm from the following equation:

D = Cr/p

R = surface tension, mN/m (dynes/cm)

P = pressure, Pa or cm Hg
C = constant, 2860 when P is in Pa, 2.15 when p is in cm Hg and 0.415 when P is in PSI
units.

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7.8. Report

7.8.1. Record the minimum pressure for gas passage as indicated by continuous bubbles.

7.8.2. Record the maximum pore size calculated, identification of RBSM tested and liquid used.

7.9. Precision and Bias

The precision of this test method has not been determined.

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8. STANDARD TEST METHOD FOR PORE SIZE CHARACTERISTICS BY THE LIQUID

POROSIMETRY METHOD OF RECOMBINANT BATTERY SEPARATOR MAT

8.1. Scope

This procedure covers method of determining pore size distribution of Recombinant Battery
Separator mat (RBSM) using liquid porosimetry.

8.2. Applicable Documents

8.2.1. Coulter Porometer Instruction Manual.

8.2.2. ASTM E-1294 pore size characteristics of membrane filters using automated liquid
porosimeter.

8.2.3. ASTM F-316 pore size characteristics of membrane filters by bubble point and mean flow
pore test.

8.2.4. BS 6410 British standard method of test for filter paper.

8.2.5. PMI Capillary Flow Porometer Instruction Manual.

8.3. Principle of Test Method

8.3.1. RBSM saturated with liquid will allow air to pass when air pressure exceeds the capillary
attraction of the liquid in the pores. Smaller pores will exhibit similar behavior at higher
pressures.

8.3.2. The percentage of flow passing through the pores larger than or equal to the specified size
can be calculated from the pressure-pore size relationship by comparing the gas flow rates of
both wet and dry RBSM at the same pressures.

8.4. Apparatus

8.4.1. Coulter Porometer (Coulter Electronics, Inc., Hialeah, Florida) or equivalent.

8.4.2. Sample holders Figure 8.1.

8.4.3. Pressure gauges.

8.4.4. Rotameters.

8.4.5. Fluid trap.

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8.4.6. Test set up Figure 8.3, Figure 8.4.

Figure 8.4 – Set-up for Two Holders

8.5. Reagents

8.5.1. Reagent grade or high purity liquid of known surface tension such as:

8.5.2. Porofil (Coulter Electronics, Inc.)

8.5.3. Isopropyl alcohol.

8.5.4. Petroleum distillate with surface tension of 30 dynes/cm at 25°C.

8.5.5. Mineral oil with surface tension of 34.7 dynes/cm at 25°C.

8.5.6. Adequate liquid shown on Table 8.1.

Table 8.1
Calculation of Maximum Pore Size from Bubble Point Pressure
(d = Cr/p)
Pressure Units of Bubble Point
Fluid Used cm Hg PSI Pa
Water 155/Bubble Point 30.0/Bubble Point 2.06 x 103/Bubble Point

Petroleum distillate 64.6/Bubble Point 12.5/Bubble Point 8.58 x 104/Bubble Point

Denatured Alcohol 47.75/Bubble Point 9.25/Bubble Point 6.38 x 104/Bubble Point

Mineral oil 74.5/Bubble Point 14.4/Bubble Point 9.92 x 104/Bubble Point

Freon TF™ 37.2/Bubble Point 7.2/Bubble Point 4.95 x 104/Bubble Point

Example – A certain RBSM was observed to have a bubble point of 41.0 psi with petroleum
distillate. Size (µm) = 12.5/41.0 psi. Therefore: maximum pore size = 0.305 µm.

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Note: This table was derived from ASTM F315-86.

8.6. Procedure

8.6.1. Procedure for Coulter Porometer, PMI Porometer or equivalent.

8.6.1.1. Follow porometer operating instructions to prepare the RBSM sample to introduce to the
instrument.

8.6.1.2. Establish procedures for standard sampling to obtain repeatable results.

8.6.2. Procedures for One Holder (Fig. 8.3).

8.6.2.1. Place a dry RBSM sample disk in the sample holder.

8.6.2.2. Close the holder and apply gas pressure in increments.

8.6.2.3. Plot gas flow versus gas pressure over the intended range of use.

8.6.2.4. Reduce gas pressure and remove the RBSM sample from the holder.

8.6.2.5. Completely wet the RBSM in the liquid, replace the wet sample in the holder, checking to see
that a tight seal is made.

8.6.2.6. Increase pressure gradually and record the pressure of the gas flow detected by the capillary
tube tip which is immersed in the test tube half filled with liquid.

8.6.2.7. Change to rotameters and plot the fluid wet sample gas flow versus pressure on the same
coordinates as for the plot made in accordance with 8.6.2.3.

8.6.3. Procedure for Two Holders Figure 8.4.

8.6.3.1. Place a dry RBSM sample in the holder to be used exclusively for dry sample.

8.6.3.2. Wet a RBSM sample of the same type and lot as the sample used in 8.6.3.1 in liquid medium
and place it in a holder to be used exclusively for wet sample.

8.6.3.3. Apply gas pressure to the dry sample and plot gas flow versus gas pressure.

8.6.3.4. Change the two position valve to apply gas pressure to the wet sample holder and record the
first gas flow as detected by the capillary tube as bubble point. Switch to rotameters and plot
fluid wet gas flow versus gas pressure.

8.7. Calculations

8.7.1. Calculations of Mean Flow Pore Size.

8.7.1.1. Record the minimum pressure for gas passage (bubble point pressure). Calculate the
maximum pore size from the equation and correlation data found in Table 8.1.

8.7.1.2. Using the graph from 8.6.3.3 draw the line or curve corresponding to one half the dry gas flow
rate of the RBSM sample. Find the intersection of this (one-half dry-flow) line and the wet flow
line or curve as shown in Figure 8.5. Determine the pressure coordinate of the intersection
and substitute into the pressure-pore size equation. (See Table 8.1 for mineral oil).

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Figure 8.5

8.7.2. Calculation of Pore Size Frequency

8.7.2.1. Select the limits of the pore size range being evaluated. Substitute the limit individually into
the pore size versus pressure equation and obtain their respective pressures. From the test
graph determine the wet and dry flows at the pressure limits (pore size limits of the range) as
shown in Figure 8.6.

Figure 8.6.

8.7.2.2. Substitute the value found in the following equation:

Q = [(wet flowh/dry flowh) – (wet flowl/dry flow l)] x 100

Where:

Q = RBSM flow, %

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 BCIS-03a Rev. Feb02

l = lower pressure limit

h = higher pressure limit

8.7.2.3. Report Q as the percent of the sample flow passing through pores within the range specified.

Example – Determine the percentage of the RBSM flow passing through a pore size range
from 0.8 to 0.2 µm of the RBSM described in Figure 8.6.

Q = [(7 L/min / 21 L/min) – 2 L/min / 15 L/min)] x 100

= [0.333 – 0.167] x 100 = 16.6%

A 16.6 percent of the gas passing through the RBSM described in Figure 8.6 moves through
pores between 0.8 and 0.2 µm.

8.8. Precision and Bias

8.8.1. The precision of this test method has not been determined.

8.8.2. Since the change in pore size per unit change in applied pressure is greatest at large pore
sizes and diminishes hyperbolically, repeatability and reproducibility increase accordingly with
applied pressure.

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9. STANDARD TEST METHOD FOR PORE SIZE CHARACTERISTICS BY THE MERCURY

INTRUSION METHOD OF RECOMBINANT BATTERY SEPARATOR MAT

9.1. Scope

9.1.1. This procedure covers method of characterizing pore structure of recombinant battery
separator mat (RBSM) using mercury intrusion porosimetry.

9.1.2. This test procedure may involve hazardous materials, operations, and equipment. This
procedure does not purport to address all of the safety problems associated with its use. It is
the responsibility of the user of this test method to consult Material Safety Data Sheets
(MSDS) of the materials involved with the test and to establish appropriate safety and health
practices as well as determine the applicability of regulatory limitation prior to use.

9.2. Reference Documents

9.2.1. Instruction Manual, Micromeritics Mercury Intrusion Porosimeter.

9.2.2. Instruction Manual, Quantachrome Mercury Porosimeter.

9.2.3. Instruction Manual, Aminco Mercury Intrusion Porosimeter, Super Pressure Inc.

9.2.4. Instruction Manual, PMI Automated Porosimeter, Porous Materials, Inc.

9.2.4.1.1. ASTM D2873 The Method for Interior Porosity of PVC Resins by Mercury Intrusion
Porosimetry.

9.3. Principle of Test Method

9.3.1. The method of mercury porosimetry is based on the principle that the external pressure
required to force a non-wetting liquid into a pore against the opposing force of the liquid
surface tension depends on the pore size.

9.3.2. Mercury is used as liquid medium since it does not wet most solids and its contact angle with
a variety of solids is in relatively narrow ranges.

9.3.3. Assuming cylindrical pore geometry, the relationship between the applied pressure and the
pore diameter into which mercury will intrude is given by the Washburn equation:

d = 4 Γ cos Θ/ p

Where:
d = pore diameter
p = applied pressure
Γ = surface tension of mercury
COS Θ = contact angle between mercury and pore wall

The pressure required to force mercury into a pore is inversely proportional to the pore
diameter.

9.4. Significance and Use

9.4.1. Mercury porosimetry is a widely accepted technique of characterizing structure of porous

materials.

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9.4.2. The method of test is used to determine properties such as pore diameter, pore size
distribution, and pore volume

9.4.3. A pore size determined by mercury porosimetry should not be taken in a literal sense due to
some assumptions such as cylindrical pores, contact angle and surface tension of mercury
imposed to calculate it. Pore size is a relative term used to simplify discussion when making
comparison between samples of certain material type.

9.5. Precautions

9.5.1. Mercury is poisonous. Prevent accumulation of mercury vapor in workspaces through

provision of proper exhaust system. Avoid contact with skin and internal ingestion. Use
plastic or rubber gloves. Clean up spills immediately with mercury clean-up kits. Keep
containers of mercury closed at all times. When cleaning mercury with mercury cleaning kit
and nitric acid do so under well ventilated hood.

9.5.2. Operation of mercury porosimeter requires high hydraulic pressure. Even though all
porosimeters are equipped with built-in safety features, operator should observe strict safety
precautions described in the operating manual.

9.6. Apparatus

9.6.1. Micromeritics Mercury Porosimeter

e.g. Pore Size 9320 Auto Pore II 9220

9.6.2. Quantachrome Mercury Porosimeter

e.g. Autoscan – 33 or 60 Porosimeter

9.6.3. Aminco Mercury Porosimeter

e.g. Model J5-7125D, 60K, 5-7107

9.6.4. PMI Automated Porosimeter

e.g. Model No. PMI 30K-A-1

9.7. Procedure

9.7.1. Follow the detailed procedure as described in the instruction manual provided with the
instrument.

9.7.2. A sample weight between 0.040 to 0.060 gram weighed to an accuracy of 0.0001 g is
suggested for commonly available microfiber glass RBSM.

9.8. Report

Report the following:

9.8.1. The instrument used.

9.8.2. The weight of the specimen used.

9.8.3. Median pore diameter in µm.

9.8.4. Pore size distribution preferably in the form of a graph showing pore diameter in µm on X-axis
(log scale) and porosity in ml/g on Y-axis.

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9.9. Precision and Bias

The precision of this method has not been determined.

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10. STANDARD TEST METHOD FOR SURFACE AREA OF RECOMBINANT BATTERY

SEPARATOR MAT

10.1. Scope

This test procedure covers the determination of specific surface area of a recombinant
battery separator mat (RBSM) sample utilizing B.E.T. adsorption.

10.2. Referenced Documents

10.2.1. Adsorption, Surface Area and Porosity, 2nd Ed. By Greg and Sing, 1982.

10.2.2. NIST Special publication 260 (Standard Reference Materials Catalog).

10.3. Terminology

10.3.1. SURFACE AREA – The total area of exposed surface of a finely divided solid, power, or
porous material. Typically expressed in m2/g.

10.3.2. WRM – Working Reference Material – a mat material similar to that being analyzed.
Repeated testing of a WRM is useful for checking the daily performance of the instrument
and the uncertainty (precision) of the procedure over long periods of time.

10.3.3. BRUNAUER–EMMETT–TELLER (B.E.T.) – describes a model for multi-layer molecular

adsorption and its relationship to surface area based upon active sites on a sample.

10.4. Significance and Use

The performance of a recombinant lead-acid battery is partially dependent on the surface

area of the mat between the plates and must be controlled within reasonably close
tolerances.

10.5. Apparatus

10.5.1. Surface area analyzer such as “Quantasorb Jr.”.

10.5.2. Drying oven capable of reaching a temperature of 260°C (500°F).

10.5.3. Balance capable of weighing to 0.1 mg.

10.6. Calibration

10.6.1. The balance should be cleaned and checked on a yearly basis. It should be calibrated daily
using weights traceable to the National Institute of Standards of Technology (NIST).

10.6.2. Run a WRM with every batch of samples. Results of the standard should be transferred to
the appropriate control chart. NIST SRM’s are available and can be run occasionally to
check accuracy at various levels.

10.7. Sampling

10.7.1. Cut the RBSM into pieces 2 x 10 mm in size.

10.7.2. Load samples into clean, dry, and previously weighed sample cells. Sample weights should
be recorded on surface area data sheets or in laboratory notebooks.

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10.7.3. Place sample cells in oven, connect in series and run nitrogen through cells at a rate of one
bubble/sec. Krypton can be used in place of nitrogen for most RBSM materials.

If the RBSM is 100% inorganic, heat at 260°C (500°C) for 30 minutes and then overnight at
120°C (248°F). If the RBSM contains organics, then the material must be dried at lower
temperature to avoid damage to the organics. If the RBSM contains organics, dry the material
at 80°C (176°F) for a minimum of 24h.

10.8. Procedure

10.8.1. Turn on the adsorbate and calibration gas toggle switches and then the instrument power. Let
instrument warm up for 15 minutes before using.

10.8.2. Turn off the oven and let the sample cool down. Continue the nitrogen flow until the last
sample has been run.

10.8.3. Transfer a sample cell from the oven to a cell holder assembly and place the assembly into
the instrument. After a steady baseline is obtained, the sample is ready to analysis.

10.8.4. Analyze the sample following the procedure for the appropriate instrument. Single point
measurements are used routinely. Multiple point measurements are not routinely used, but
may be made for increased accuracy. See Annex for a condensed operation procedure for a
“Quantasorb Jr.” instrument.

10.8.5. After all samples have been run, turn off the instrument and then the gas flows. Also turn off
the nitrogen in the drying oven.

10.9. Calculations

The equation used to calculate the surface area is given below:

S = (1-P/Po) (A/Ac) V c (NAcs • Pa/RT) m2

Where:
P = Partial Pressure of Adsorbate
N = Avogadro’s No = 6.023 x 1023
V c = Volume of Calibration
A = Signal Area
A cs = Cross Section Area of Adsorbate Molecule (for N2 = 16.2*10-10 m2)
T = Temperature of Calibration (Ambient) in degrees Kelvin
Po = Saturated Pressure of Adsorbate
R = Gas Constant = 82.1 cc atm/K Mole
Pa = Ambient Pressure, atm.
A c = Area of Calibration

10.10. Report

Report the surface in m2/g.

10.11. Precision and Bias

10.11.1. Precision

No statement may be made on the precision of this test method, since round robin testing
among laboratories has not been conducted.

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10.11.2. Bias

No statement on bias may be made due to the lack of a standard reference material.

10.12. Annex

10.12.1. Safety

10.12.1.1. Standard good laboratory practices should be employed, consistent with the applicable
Chemical Hygiene Plan.

10.12.1.2. In addition, the analyst should be familiar with the Material Safety Data Sheets (MSDS) for
materials employed in the analysis.

10.12.1.3. The analyst must be familiar with the rules governing the use of liquid nitrogen and
compressed gases.

10.12.2. Condensed Operation Procedure

10.12.2.1. After a stable baseline has been obtained, select an attenuator setting that will give a signal
between 700 and 1200 counts. This will usually be 8 or 16.

10.12.2.2. Depress the “ADS” push button and set the signal meter to zero.

10.12.2.3. Raise the liquid nitrogen bath so that the sample cell is immersed under the coolant.

10.12.2.4. Observe the count rate during the adsorption step and make any adjustments in the
attenuator setting to obtain a count rate of 700 to 1200.

10.12.2.5. When a stable baseline is gain obtained, depress the “DES” button and re-zero the signal
meter and integrator.

10.12.2.6. Lower the Dewar flask and immerse the sample cell in a beaker of room temperature water
until the adsorbate flow meter float returns to its starting position.

10.12.2.7. When the signal meter has returned to zero, record the integrator counts and re-zero.

10.12.2.8. Using a gas-tight syringe, inject a sample of pure nitrogen into the gas =stream. The counts
should be within 10-15% of the desorption counts. At an attenuator setting of 32 (150 ma on
the detector), 1 ml of N2 gas will give approximately 600 counts. Total counts can be adjusted
by changing the volume of N2 injected.

10.12.2.9. Record the total counts and volume injected.

10.12.2.10. Turn the sample isolation valve to “Bypass”, remove the cell holder assembly and insert a
new sample in the holder. Place holder into instrument, turn valve to “cell” and begin again at
Step 1.

10.12.2.11. Weigh the full sample cell. Obtain the weight of the sample by subtracting the weight of the
empty cell. Record the weight on the data sheet.

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11. STANDARD TEST METHOD FOR DETERMINING PERCENT MOISTURE CONTENT OF

RECOMBINANT BATTERY SEPARATOR MAT

11.1. Scope

11.1.1. This test procedure covers the determination of the percent moisture in recombinant battery
separator mat (RBSM).

11.1.2. This procedure covers all grades of RBSM used in various battery applications.

11.2. Reference Documents

11.2.1. British Standards BS 3433.

11.2.2. International Standards Organization ISO 287.

11.2.3. TAPPI T-412 Moisture in Paper and Paperboard.

11.2.4. ASTM D-644 Test Method for Moisture Content of Paper a Paperboard by Oven Drying.

11.3. Terminology

11.3.1. RECOMBINANT BATTERY SEPARATOR MAT (RBSM) – Any material intended for use as a
separator between the plates of opposite polarity in a valve regulated, lead-acid battery.

11.3.2. % MOISTURE CONTENT – The percent weight of RBSM attributable to the pick-up of
moisture.

11.3.3. MOISTURE FREE SPECIMEN – A dried and desiccated specimen of RBSM referred to as
dried RBSM in (11).

11.4. Significance and Use

Per pound, RBSM is one of the most expensive components, used in the lead acid battery.
Since it is sold by weight, the moisture content of the material is of major concern to the
buyer.

11.5. Apparatus

11.5.1. Laboratory balance with a sensitivity of 1 mg.

11.5.2. Drying oven (non-air recirculation), capable of maintaining a temperature of 150°C ± 10°C
(302°F ± 18°F).

11.5.3. Laboratory timer, analog or digital, capable of measuring minutes and seconds.

11.5.4. Clean suitable laboratory weighing dish capable of holding 10 ± 1 g of RBSM.

11.5.5. Desiccator & Desiccant.

11.6. Calibration

Checking of laboratory balance.

11.6.1. Check the accuracy of the laboratory balance frequently by applying accurately measured
masses with both increasing and decreasing loads.

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11.6.2. Before each use, frictional effects shall be sufficiently minimal and the zero reading shall be
sufficiently correct to obtain the required weighing accuracy (11.5.1).

11.7. Sampling

The outer two rounds from each roll of RBSM tested should be removed and discarded, to
avoid sampling an area that might have become contaminated during shipping and handling
before sampling.

A minimum of three random specimens shall be sampled from each lot (11.8.1).

11.8. Procedure

11.8.1. Weigh out three 10 g ± 0.10 g specimens of RBSM into tared laboratory weighing dishes
using a laboratory balance accurate to the nearest mg.

11.8.2. Place the specimens in the drying oven at 150°C ± 10°C for 30 minutes ± 3 minutes.

11.8.3. After drying, place the specimens into the desiccator until cool.

11.8.4. Reweigh the specimens to the nearest 1 mg.

11.8.5. Repeat steps 11.8.2 through 11.8.4 until reproducible results are obtained, while periodically
checking the zero of the balance, between the specimen readings.

11.9. Calculations

% Moisture = (Original RBSM weight – dried RBSM weight) x 100 / Original RBSM weight.

11.10. Report

11.10.1. Percent moisture to the nearest 0.1%.

11.10.2. Percent moisture should be reported as averages, range, and standard deviation.

11.11. Precision and Bias

11.11.1. Precision

A round robin study on one material by six different laboratories indicated a between-
laboratory variance of 0.018%, and within-laboratory variance of 0.0009%.

11.11.2. Bias

No statement on bias can be made due to a lack of a standard reference material.

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12. STANDARD TEST METHOD FOR PERCENT IGNITION WEIGHT LOSS OF

RECOMBINANT BATTERY SEPARATOR MAT

12.1. Scope

12.1.1. This test procedure covers the determination of the percent weight loss on ignition on a
moisture-free specimen of recombinant battery separator mat (RBSM).

12.1.2. This method covers all grades of RBSM used in various battery applications.

12.2. Referenced Documents

12.2.1. TAPPI Standards

12.2.2. British Standards BS 3631 Ashin Paper and Paperboard Product.

12.3. Terminology

12.3.1. RECOMBINANT BATTERY SEPARATOR MAT (RBSM) – any material intended for use as a
separator between the plates of opposite polarity in a valve regulated, lead acid battery.

12.3.2. DRIED RBSM WEIGHT – Moisture free specimen weight, which is subtracted from the
original specimen weight to avoid moisture pick-up effect, when calculating the ignition weight
loss of the RBSM.

12.4. Significance and Use

This method will allow the determination of the percentage of combustible materials added to
the RBSM.

12.5. Apparatus

12.5.1. Laboratory balance with a sensitivity of 1 mg.

12.5.2. Drying oven (non-air recirculating), capable of maintaining a temperature of 150°C ± 10°C
(302°F ± 18°F).

12.5.3. Muffle oven capable of maintaining a temperature of 540°C ± 10°C (1004°F ± 18°F).

12.5.4. Analog or digital laboratory timer capable of measuring minutes and seconds.

12.5.5. Clean silica or platinum crucibles and lids.

12.5.6. Heat resistance gloves and crucible tongs.

12.5.7. Clean scissors or paper cutter (free from rust or other oxidation products of contaminants).

12.5.8. Desiccator and desiccant.

12.6. Calibration

Checking of laboratory balance.

12.6.1. Check the accuracy of the laboratory balance frequently by applying accurately measured
masses with both increasing and decreasing loads.

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12.6.2. Before each use, frictional effects shall be sufficiently minimal and the zero reading shall be
sufficiently correct to obtain the required weighing accuracy (12.5.1).

12.7. Sampling

The outer two rounds from each roll of RBSM tested should be removed and discarded to
avoid sampling an area that might have become contaminated during shipping and handling
before sampling.

A minimum of three random specimens shall be sampled from each lot (12.8.1).

12.8. Procedure

12.8.1. Weigh out three 2.000 g ± 0.001 g specimens of RBSM using an analytical balance. Place
each specimen into a clean pre-weighed silica or platinum crucible.

12.8.2. Place the specimens in the drying oven, to dry for 30 minutes ± 3 minutes.

12.8.3. After drying, place the specimens into a desiccator until cool.

12.8.4. Reweigh the specimens to the nearest 1 mg.

12.8.5. Repeat steps 12.8.3 through 12.8.4 until reproducible results are obtained.

12.8.6. Pre-heat the muffle furnace to 540°C ± 10°C (1004°F ± 18°F).

CAUTION: Severe burns will occur if proper handling of crucibles is not observed.

12.8.7. Using heat resistance gloves and tongs, place the crucibles and specimens into the muffle
furnace for 30 minutes ± 3 minutes. Remove the crucibles and allow them to cool for a
moment on top of a heat resistance surface. After the crucibles are sufficiently cool, transfer
the crucibles into a desiccator until cool.

12.8.8. After the crucibles reach room temperature, reweigh the samples again to the nearest 1 mg.
while periodically checking the zero of the balance between the specimen reading

12.9. Calculations

12.9.1. % Moisture Loss = (Original RBSM weight – dried RBSM weights) x 100 / Original RBSM
Weight

12.9.2. % Ignition Loss = (Dried RBSM weight – Muffled RBSM weights) x 100 / Dried RBSM Weight

12.10. Report

12.10.1. Percent ignition weight loss to the nearest 0.1%.

12.10.2. Results of percent ignition weight loss should be reported as averages, range, and standard
deviation.

12.11. Precision and Bias

12.11.1. Precision

Precision data for the methods described above are not available at this time, since no round
robin testing was attempted.

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12.11.2. Bias

No statement on bias can be made due to a lack of a standard reference material.

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13. STANDARD TEST METHOD FOR TENSILE STRENGTH AND PERCENT ELONGATION
MEASUREMENTS ON RECOMBINANT BATTERY SEPARATOR MAT

13.1. Scope

13.1.1. This test method describes the use of a constant rate of elongation apparatus to determine
the force per unit width required to break a test piece (tensile strength) and the percentage of
elongation at break (stretch); it may also be used to define the energy absorbed per unit area
of the test piece before breaking (tensile energy absorption).

13.1.2. This method is suitable for all types of recombinant battery separator mat (RBSM), either
binder-free or those using organic additives to increase strength, and which have tensile and
elongation values within the limitations of the instruments used. It may be used for
handsheets as well as samples taken from large production rolls.

13.1.3. Tensile strength is commonly reported in pounds per inch or kilonewtons per meter; it may
also be expressed as grams per inch or pounds per square inch.

13.2. Referenced Documents

13.2.1. TAPPI T494 Tensile Breaking Properties of Paper and Paperboard (using a constant-rate-of-
elongation apparatus).

13.2.2. ASTM Standards

13.2.2.1. ASTM D 76. Standard specification for Tensile Testing Machines for Textiles.

13.2.2.2. ASTM D 828. Tensile Breaking Strength for Paper and Paperboard.

13.2.2.3. ASTM D 1682. Standard Test Methods for Breaking Load and Elongation of Textile Fabrics.

13.2.3. British Standard BS 6410. British Standard Methods of Test for Filter Papers; Section Three:
Test Methods for Mechanical Properties.

13.2.4. ISO 1924. Paper and Board, Determination of Tensile Strength.

13.2.5. Japanese Industrial Standard JIS C2202. Glass Mats for Lead Acid Storage Batteries

13.3. Terminology

13.3.1. Tensile Strength – the maximum tensile stress of a test sample prior to rupture during a
tensile test carried out under prescribed conditions. It is reported as the force per unit width of
the test specimen.

13.3.2. Percent Elongation – is the maximum tensile strain developed in the test sample prior to
rupture during a tensile test carried out under prescribed conditions. Percent elongation is
expressed as a percentage representing the ratio of the increase in length of the test sample
to its original length multiplied by one hundred.

13.3.3. Tensile Energy Absorption (TEA) (Optional) – the work done when a test sample is stressed
to rupture under tension during a pull test carried out under prescribed conditions as
measured by the integral of the tensile stress over the range of tensile strain from zero to the
maximum value. TEA is expressed as energy per unit area (test span x width) of the test
specimen.

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13.3.4. Breakpoint – The point of peak force on the strain/stretch curve, beyond which the force
rapidly diminishes as the paper continues to be stretched. See Figure 1.

13.3.5. Tensile Index – the tensile strength in newtons per meter (N/m) divided by grammage, a
measure of strength per unit weight of material.

13.3.6. Constant-Rate-Of-Elongation Tensile Testing Machine (CRE) – a testing machine in which

the rate of increase of the specimen length is uniform with time.

13.3.7. Recombinant Battery Separator Mat – or RBSM refers to any material intended for use as a
separator between the plates of opposite polarity in a valve regulated lead acid battery or cell.

13.3.8. Machine Direction (MD) – refers to the orientation of separator mat on a roll; mat is unrolled
in the machine direction (the direction in which the mat is manufactured).

13.3.9. Cross Direction (CMD or CD) – refers to the taking of a sample perpendicular to the MD; i.e.,
across a roll.

13.4. Significance and Uses

13.4.1. The properties measured in this test are primarily tied to the robustness of RBSM in the
manufacturing environment. Once a cell or battery is assembled, filled and formed, these
mechanical properties lose their significance because of the cell stack rigidity and the wetting
process.

13.4.2. In binder-free separators, tensile and elongation properties can be very sensitive to storage
conditions (temperature, relative humidity) and will usually degrade with time. Fiber
orientation is not completely random, and thus tensile and elongation properties vary for the
machine and cross directions. Relative to other battery materials, these mats are extremely
delicate. Careful handling is mandatory during sample preparation and testing. Typically,
machine direction tensile values are in the range of 0.0875-1.75 kN/m and elongation may
vary from 0.5-10%.

13.4.3. Tensile strength is indicative of the “toughness” of RBSM when they are subjected to direct
tensile stress. The tensile strength value will represent the ability of the material to resist
breaking or tearing during handling and passage through cell assembly machinery.
Generally, tensile strength increases with thickness and grammage, and can vary
substantially for a given thickness and grammage from one manufacturing process to
another.

13.4.4. The percent elongation is indicative of the ability of the paper to bend and conform to a
desired contour. High elongation is indicative of a paper with a lot of “spring” or “stretch”.

13.4.5. Tensile energy absorption is a measure of the ability of a paper to absorb energy and
maintain its physical integrity when subjected to sharp stresses and/or repetitive stressing
and straining.

13.5. Apparatus

13.5.1. Tensile Testing Machine, a constant-rate-of-elongation (CRE) type capable of acting on the
test specimen at a defined rate in order to permit the tensile force at the moment of failure to
be read to an accuracy of 1%. The machine must meet the following requirements.

13.5.1.1. It must have two clamping jaws, each with a line contact for gripping the specimen tightly
without severing it (separator samples are very delicate and thus clamping pressure must be
great enough to prevent slippage but not so great as to cut through the sample). The lines of

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contact must be perpendicular to the direction of pull so that no sideways stress is applied to
the sample.

13.5.1.2. The rate of separation of the jaws shall be 25 mm/min ± 5 mm/min (1.0 in/min ± 0.2 in/min)
and shall be resetable and constant to ± 4%. The clamping jaws shall remain parallel to
within ± 1° for the duration of the test.

13.5.1.3. A load cell should be selected which is suitable for measurements on the RBSM samples,
typically one that is rated at roughly 50 N, 10 lb or 5 kg maximum capacity. Since these are
transducer devices, a load cell must be chosen that is within the range of the separator being
tested. Use of a load cell with a high capacity (e.g. 45 kg) will result in diminished accuracy
for tensile and elongation measurements.

13.5.1.4. The sensitivity setting should also be chosen to be greater than the expected maximum
tensile force for the sample, but not so great as to reduce accuracy.

13.5.1.5. A recorder or indicator should be used that is readable to 0.25% of full scale loading force
and that will maintain a calibration accuracy of ±0.5%. Recorder speed should be such as to
provide a readability and accuracy of ±0.05% elongation.

13.5.1.6. An alignment fixture may be desirable to facilitate centering and aligning the test specimen in
the jaws so that the clamping lines of contact are perpendicular to the line of the applied
force.

13.5.1.7. A planimeter or integrator may also be desirable to measure the area under the load-
elongation curve to determine the TEA value or to compute directly the work to rupture;
accuracy should be ±1%.

13.5.2. Cutting Device, for cutting test pieces of the proper length and width, with straight parallel
sides and a reproducible area.

13.6. Calibration

13.6.1. Tensile Tester/Load Cells. These are extremely complex, delicate pieces of equipment.
Consult the User’s Manual for recommendations on method and periodicity of calibration.

13.6.2. Cutting Device. Frequently check the area cut and parallelism of the sides to monitor the
effect of wear on the cutting device. For tensile and elongation measurements, absolute area
is not as critical as the “squareness”, or parallel opposite sides of the cut samples. However,
it is imperative that the samples be cut without any tearing or stressing which might affect the
tensile/elongation properties.

13.7. Sampling and Sample Preparation

13.7.1. Sampling and sample handling are presented here in the form of an incoming goods test for a
battery manufacturer. Others using this procedure may wish to modify sampling to fit their
different situations. Because of the way most mats are manufactured and their sensitivity to
handling, it should be notes that tensile and elongation results between a mat manufacturer
and the end user may differ somewhat.

13.7.2. Sufficient samples should be taken from a lot of separator to characterize the uniformity of
the lot. Typically, at least one sample from each run and set numbers are included, In
addition tensile and elongation values can vary throughout a given roll of separator. As a
separate, discrete test, through-roll uniformity should be periodically measured for a given
supplier.

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Note: RBSM is extremely fragile and must be handled with great care during sample
extraction and preparation.

13.7.3. Remove at least ten layers of material from the rolls selected, as these outer layers are
susceptible to damage during handling, packaging and shipping.

13.7.4. Remove an approximately one-half meter section from each roll to be tested, identify it and
place it in a sealed bag or tote tray, being careful to prevent folds, creases, contamination or
any stretching or compression. Transfer sample sections to inspection area in tote trays or in
sealed polyethylene bags and in either case carry out measurements within two hours.

13.7.5. Using the cutting device, take one sample from each roll sample, again being very careful not
to damage the paper. Standard sample size is 25 x 150 mm (1” x 6”). The longer dimension
denotes the pulling direction and this is usually the separator paper manufacture machine
direction (MD). If desired and if the rolls are wide enough, cross-direction (CD) samples may
also be taken.

13.8. Procedure

13.8.1. This is a generalized procedure intended to cover the use of any electromechanical CRE
device. Individual instruments may have details omitted here and in any case the User’s
Manual should be consulted and followed.

13.8.2. If possible, prolonged sample storage and/or testing should be carried out in a laboratory with
controlled temperature and humidity levels.

13.8.3. The testing machine shall be calibrated and adjusted according to the User’s Manual. The
appropriate load cell shall be used and calibrated with masses approximating the expected
tensile properties of the mat being tested. Full-scale sensitivity shall likewise be set to give
optimum accuracy for the anticipated tensile measurements.

13.8.4. The 25 mm x 150 mm (1 x 6 in) test strip shall be inserted in the jaws and the clamps set so
that the line contacts are 102 mm ± 4 mm (4.0 in ± 0.2 in) apart. See Subsection 13.12.2 for
comments regarding non-standard specimen sizes and their effected on tensile/elongation
values.

13.8.5. The sample should first be clamped in the upper jaw, and then in the lower jaw after
removing any noticeable slack. Use the clamping pressure found to be satisfactory for the
type of mat being tested. Too high a pressure can cause “jaw edge failure” (rupture at the
clamping point), and too low a pressure can obviously result in test piece slippage. Be careful
not to touch the sample between the clamping points.

13.8.6. As mentioned, set the rate of jaw separation at 25 mm/min ± 5 mm/min (1.0 in/min ± 0.2
in/min). If the time to rupture exceeds 30 seconds, a faster pull speed should be used.

13.8.7. If a recorder is used, chart speed should be set to give a readability equivalent to 0.05%
stretch. Select the full-scale force reading, if possible, so that the breaking force can be read
in the upper three-fourths of the scale. Make preliminary trial tests to determine full-scale
load.

13.8.8. If the test piece breaks within 10 mm (0.4 in) of either jaw, or if there is evidence of slippage
or uneven stretching across the sample width, reject that result, If more than 20% of the test
pieces for a given sampling are rejected, discard all sample readings and inspect the
apparatus for conformance with specifications and/or take whatever steps necessary to
correct the problem.

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13.8.9. Read and record the breaking force to 0.5% of full scale and the elongation at break to the
equivalent of 0.05% stretch. If appropriate, record the integrator reading to determine the
area under the force/elongation curve from zero load to the break point (peak force).

13.9. Calculations

13.9.1. Tensile strength is read directly from the chart by observing the point (breakpoint) at which
the force (curve) decreases rapidly to zero (see Figure 1). Some instruments provide direct
digital readout of tensile and elongation values. Divide the breaking force by the specimen
width to obtain the tensile strength. If measurements are in pounds and inches, multiply by
0.175 to convert to kN/m. Other units such as kg/mm, g/in, psi, etc., will require the
appropriate conversion factors to put them into standard units.

13.9.2. See TAPPI Method T494, Note 9, to calculate the tensile index, if desired.

13.9.3. To calculate the percent elongation from the force/stretch curve shown in Figure 1, measure
the crosshead travel distance to the breakpoint (in meters or inches), divide by the length of
the sample and multiply by 100. Instruments with digital readouts will give results directly.

13.9.4. See TAPPI Method T494, Section 7.4, to calculate the tensile energy absorption, if desired.

13.9.5. For all measurements carried out on a particular lot, set, run or roll, calculate the mean and
standard deviation in the normal manner.

13.10. Report

13.10.1. Values may be reported for tensile and elongation properties in the machine direction (MD) or
cross direction (CD), or both. Generally, MD values are greater than those for the cross
direction.

13.10.2. Test values should be reported to three significant figures.

13.10.3. Tensile strength is to be reported as kN/m or lb/in for the mean, standard deviation and
range.

13.10.4. Elongation values for the mean, standard deviation and range are expressed as percentages.

13.10.5. Tensile energy absorption values, if reported, for the mean, standard deviation and range are
as J/m2 or ft-lb/ft2.

13.10.6. For each of the above, report the number of determinations rejected and the reason(s) for
rejection.

13.10.7. Also report any deviations from the standard test procedure, such as short length or non-
standard width samples, alternate clamping configurations, non-standard pull rate (25
mm/min or 1.0 in/min) or unusual sampling or conditioning procedures.

13.11. Precision and Bias

13.11.1. Precision

13.11.1.1. In order to observe the effects of pull rate and sample preparation upon tensile and
elongation properties, a round-robin study was carried out where standard separator samples
from the same controlled lot were analyzed by eight different laboratories, with ten samples
per grouping. Tensile testers, load cells and sensitivity settings were not standardized.

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13.11.1.2. Within laboratory coefficients of variance were in the range of 4.5-20% for percent elongation
and 3.2 to 8.6% for tensile measurements. Individual laboratory means varied from 0.9-3.3%
for elongation and 1.67-2.26 lb/in for tensile. Qualitatively, this indicates that in-house
previsions are good for these measurements, but lab-to-lab comparisons are not precise,
primarily because of instrument differences.

13.11.2. Bias

13.11.2.1. No statement of bias can be made due to the lack of a standard test material.

13.11.2.2. Binder-free 100% glass separators are largely held together by electrostatic forces and
friction between the interlocked fibers. Because of this, their mechanical properties will
change with time and may be affected by the following factors:

Temperature/relative humidity
Machine tension and drag during conversion
Shipping and handling damage
Sample acquisition and preparation damage
Testing machine instability

13.11.2.3. If none of the above factors are operative, tensile and elongation values may change with
time due to fiber relaxation. Samples should be tested after conversion and within 30 days
wherever possible. Test pieces should be run within two hours after sampling and if longer
times are involved, they should be stored in sealed polyethylene bags.

13.12. Additional Information

13.12.1. In the SI (System International) convention, the units or force and energy are newtons (N)
and joules (J), respectively. Conversion units between SI and English/metric are as follows:

Force: Energy: Tensile Strength: Tensile Energy Absorbtion:

1 lb = 4.448N 1 Nm = 1.000 J 1 lb/in = 0.175 kN/m a ft-lb/ft2 = 14.60 J/m2
1 kg = 9.807 N 1 ft-lb = 1.356 J 1 kg/15mm = 0.654 kN/m
1 m-kg = 9.807 J

Tensile Energy Absorption:

1 ft-lb/ft2 = 14.60 J/m2

13.12.2. Shorter-length test pieces will give higher tensile readings and it becomes progressively more
difficult to determine percent elongation accurately. Varying the width of the test piece has an
indeterminate effect and unless it is necessary, the 25 mm standard width should be adhered
to.

13.12.3. Increasing the pull rate will increase the apparent tensile strength by a small percentage.
Running at pull rates less than the standard 25 mm/min. had no apparent effect as measured
in the round-robin tests; thus it is not recommended, as there is no apparent gain in accuracy.

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14. ACID WETTING AND WICKING OF RECOMBINANT BATTERY SEPARATOR MAT

The Battery Council International Technical Subcommittee on Separators has reached a

consensus concerning the subject method.

Although acid wetting and acid wicking are very critical characteristics of recombinant battery
separator mat (RBSM), no wetting or wicking tests presently in use by the industry properly
simulate the wide range of electrolyte addition techniques or all the in situ conditions that
RBSM are subjected to during battery life.

If an appropriate procedure emerges in the future, the Subcommittee may be reactive to

review such a procedure.

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15. STANDARD TEST METHOD FOR DETERMINING THE COMPRESSIBILITY OF

RECOMBINANT BATTERY SEPARATOR MAT

15.1. Scope

This test procedure covers the determination of the compression characteristics of

recombinant battery separator mat (RBSM) when exposed to different pressures.

15.2. Reference Documents

BCI’s BCIS-03a-4, “Standard Test Method for Thickness of Recombinant Battery Separator
Mat”.

15.3. Terminology

15.3.1. COMPRESSION CURVE – The characteristic curve obtained from plotting the thickness
value obtained with various presser foot loadings. The zero load thickness can be obtained
from this curve, based on an extrapolation of the thickness to zero load.

15.3.2. COMPRESSION – A reduction in thickness of the RBSM due to an applied pressure.

15.4. Significance and Use

15.4.1. RBSM is typically used while under compression. (Generally 20% compression). It is
important to know the pressure required to give the desired compression of RBSM within a
battery.

15.4.2. The compression of an RBSM should be an inherent property of the material and should not
change for the same material.

15.5. Apparatus

15.5.1. A gauge suitable to meet the requirements of BCI’s Test Method for Thickness (BSIS-03a-4),
except that the gauge must be capable of applying different loadings.

15.5.2. A set of analytical weights, suitable for loading the gauge which will be used for this
determination.

15.6. Calibration

Calibrate the gauge using the correct calibration method. Refer to BCI’s Test Method for
Thickness (BSIS-03a-4).

15.7. Sampling

15.7.1. Remove the outer two wraps from the RBSM to be tested. A one meter length of separator
should be sampled for each determination.

15.7.2. A minimum of five random specimens shall be sampled for each material to be tested.

15.8. Procedure

15.8.1. Read the BCI “Standard Test Method for Thickness Determination for RBSM” (Subsection 4).

15.8.2. Obtain the one meter strip of RBSM and measure the thickness at a minimum of seven
different presser foot loadings. A reading for each specimen will consist of the average of

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five individual readings at each pressure which is tested. Each reading should be taken after
30 seconds of compression. Recommended loadings are 5 (0.7), 10 (1.5), 20 (2.9), 30 (4.4),
40 (5.8), 50 (7.3), and 75 (10.9) kPa (psi). When the loadings are increased either a different
spot ca be used or the same spot. The same spot will tend to give a smoother curve.

15.8.3. Record the average thickness, mm (in), from the five specimens tested for each loading and
plot the results [thickness (y-axis) versus loading (x-axis)].

15.9. Report

15.9.1. Material tested, lot number, manufacture and equipment used and whether a different spot
was used for each loading or whether higher loading used the same spot.

15.9.2. The graph produced in 15.8.3.

15.9.3. Using the designed or specified space between the plates of an element inside the battery,
determine the amount of pressure required to compress the RBSM into this space, based on
the graph (Subsection 15.8.3).

15.9.4. Report the kPa selected and the thickness obtained from the graph.

15.10. Precision and Bias

15.10.1. Precision

No study has been conducted nor is one planned for this method. The precision of this
method should follow the precision statement in the BCI’s test method for thickness of RBSM.

15.10.2. Bias

No statement can be made due to a lack of a standard reference material.

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16. STANDARD TEST FOR DETERMINING PERCENT ACID WEIGHT LOSS OF

RECOMBINANT BATTERY SEPARATOR MAT (REFLUX METHOD)

16.1. Scope

16.1.1. This procedure covers the determination of the acid weight loss of recombinant battery
separator mat (RBSM), using a reflux method of testing.

16.1.2. The customary units used by the battery industry for this property are percent acid weight
loss per specimen. Other units covered by this method are specific gravity of acid and weight
of RBSM, expressed in grams per specimen.

16.1.3. This covers all grades of RBSM used in various battery applications. Different surface areas
will influence acid weight loss. (Mats with similar chemical composition, but higher surface
area, will have correspondingly greater solubility – thus greater acid weight loss).

16.2. Referenced Documents

BCI’s BCIS-03a-11, Test Method for Determining Percent Moisture Content of Recombinant
Battery Separator Mat.

16.3. Terminology

16.3.1. RECOMBINANT BATTERY SEPARATOR MAT (RBSM) – Any material intended for use as a
separator between the plates of opposite polarity in a valve-regulated, lead acid battery.

16.3.2. SPECIFIC GRAVITY OF ACID – the density of the acid expressed in g/cc.

16.3.3. CORRECTED SPECIMEN WEIGHT – a dried and desiccated specimen of RBSM prior to the
acid refluxing, referred to in (16.9.2).

16.4. Significance and Use

16.4.1. This test will determine the solubility of the RBSM when subjected to battery strength
electrolyte under reflux conditions.

16.4.2. The filtrate from this test can be used to determine the presence of any caution or anion that
might possibly lower the gassing over-voltage of the battery or promote the growth of lead
dendrite through the RBSM.

16.5. Apparatus

16.5.1. Laboratory balance with a sensitivity of 0.1 mg.

16.5.2. Drying oven (non-air recirculation) capable of maintaining a temperature of 150°C ± 10°C
(302°F ± 18°F).

16.5.3. 250 ml Erlenmeyer Flasks (borosilicate glass) fitted with 24/40 ground glass joints.

16.5.4. Hot plate-magnetic stirrers with Teflon-coated stirring bars.

16.5.5. Reagent grade sulfuric acid diluted to the following density: 1.260 ± 0.002 s.g. at 20°C.

16.5.6. Reflux condensers with PTFE sleeves (no silicone grease) with 24/40 ground glass joints.

16.5.7. Sintered glass crucibles (5µm openings), and 7.5 cm Pyrex watch glasses.

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16.5.8. Side arm vacuum flask fitted to receive the sintered glass crucibles and interface with the
vacuum system.

16.5.9. Desiccator and desiccant.

16.5.10. Clean scissors or paper cutter (free from rust or other oxidation products or contaminants).

16.5.11. Disposable polyethylene gloves.

16.6. Calibration

Checking of laboratory balance.

16.6.1. Check the accuracy of the laboratory balance frequently by applying accurately measured
masses with both increasing and decreasing loads.

16.6.2. Before each use, frictional effects shall be sufficiently minimal and the zero reading shall be
sufficiently correct so as to obtain the required weighing accuracy (16.5.1).

16.7. Sampling

16.7.1. The outer two rounds from each roll of RBSM tested should be removed and discarded, to
avoid sampling an area that might have become contaminated during shipping and handling
before sampling.

16.7.2. A minimum of six random specimens shall be sampled from each lot.

16.8. Procedure

16.8.1. Accurately weigh six 1.00 g ± 0.15 g specimens of RBSM, to the nearest 0.1 mg on watch
glasses.

16.8.2. Place three of the specimens into the drying oven for 30 minutes ± 3 minutes at 150°C ±
10°C (302°C ± 18°F).

16.8.3. Remove the specimens from the drying oven and place in the desiccator for cooling before
weighing to the nearest 0.1 mg, using the laboratory balance.

16.8.4. Place the remaining three 1.00 g specimens of RBSM into the Erlenmeyer Flasks taking care
to avoid loss of material or contamination of the specimen by wearing disposable
polyethylene gloves. Add a stirring bar in each flask and place the flasks on hot plates.

16.8.5. To the three flasks, add 100 ± 1 ml of 1.260 ± 0.002 s.g. (at 20°C (68°F)) reagent grade
sulfuric acid (16.5.5). Connect the reflux condensers. Adjust the temperature and stirrer
speed to obtain a reflux rate of 1 drop per second.

16.8.6. Reflux the samples for three hours.

16.8.7. After cooling, vacuum filter through the tared sintered glass crucibles [save the filtrate for
analysis of impurities (cations or anions)].

16.8.8. Rinse the RBSM with one liter of distilled water.

16.8.9. Dry at 150°C ± 10°C (302°C ± 18°F) for one hour and place in the desiccator until cool.

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16.8.10. Weigh and repeat Steps 16.8.0 through 16.8.10 until a constant weight is obtained.

16.9. Calculations

16.9.1. % Moisture Loss = (original RBSM weight – dried weight) / original RBSM weight x 100

16.9.2. Corrected specimen weight = original RBSM weight x (1 –{avg. % moisture/100}).

16.9.3. % Acid Weight Loss = corrected RBSM weight – final dry RBSM weight / corrected RBSM
weight x 100.

16.10. Report

16.10.1. Report the % acid weight loss to nearest 0.1%.

16.10.2. Results of % acid weight loss uniformity tests should be reported as averages, range, and
standard deviation.

16.11. Precision and Bias

16.11.1. Precision

A round-robin study on one material by six different laboratories indicated a between-

laboratory variance of 0.202% (comparing the average (%) acid weight loss of specimen in
1.260 s.g. acid, under reflux conditions, and an in-laboratory weight loss variance of 0.04%).

16.11.2. Bias

No statement of bias can be made due to a lack of a standard reference material.

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17. EXTRACTABLE METALLIC IMPURITIES OF RECOMBINANT BATTERY SEPARATOR

MAT

17.1. Scope

17.1.1. This test procedure covers the quantitative determination of metallic impurities which are
extracted from recombinant battery separator mat (RBSM) by sulfuric acid under controlled
conditions.

17.1.2. An extraction procedure and analysis by atomic absorption spectroscopy or Inductively

Coupled Plasma spectroscopy comprises this method. Analysis of the following metals I
described: aluminum, antimony, arsenic, bismuth, cadmium, calcium, chromium, cobalt,
copper, iron, lead, magnesium, manganese, mercury, nickel, platinum, selenium, silver,
strontium, tellurium, tin, titanium and zinc.

17.1.3. Barium is determined by the total dissolution of a RBSM sample in perchloric

acid/hydrofluoric acid mixture, diluted and then analyzed by either atomic absorption
spectroscopy or inductively coupled plasma spectroscopy. The barium in the sulfuric acid
extract is then calculated based on the solubility of the RBSM in sulfuric acid (Subsection
17.11.7). Barium is of a concern mainly to determine microglass chemistry and not
performance within the battery. This should be an acceptance procedure only, based on the
difficulty of this determination.

17.1.4. The customary units used by the battery industry for this property are micrograms of impurity
per gram of RBSM, which has been subjected to extraction or parts per million by weight
(ppm).

17.1.5. A moisture determination is run on a duplicate sample of mat, in order to correct extractable
metallic concentrations to an oven dry mat basis.

17.1.6. This procedure requires using chemicals, equipment and procedures which can be very
dangerous, therefore this procedure should only be practiced by a trained operator who is
knowledgeable of the dangers of handling concentrated acids and of the applicable safety
standards necessary to run this method safely.

17.2. Referenced Documents

17.2.1. BCI Recombinant Mat Test Method I Sampling.

17.2.2. BCI’s BCIS-03a-11, Test Method for Determining Percent Moisture Content of Recombinant
Battery Seaprator Mat.

17.2.3. BCI’s BCIS-03a-16, Test for Determining Acid Weight Loss of Recombinant Battery
Separator Mat (Reflux Method).

17.2.4. ASTM E 885 Analysis of Metals in Refuse-Derived Fuel by Atomic Absorption Spectroscopy.

17.2.5. ASTM D 1193 Specification for Reagent Water.

17.2.6. Perkin-Elmer Corporation Literature L-335B and L-655B.

17.3. Terminology

See ASTM E 885 (2.4) for definition of terms.

17.4. Significance and Use

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17.4.1. Many metallic impurities present in the electrolyte adversely affect the performance of a
recombinant battery due to generation of excess hydrogen at normal charging voltage. The
hydrogen will not recombine, thus causing pressure build up in the battery and lowering the
recombination efficiency of the battery.

17.4.2. Certain metallic impurities are known to cause adverse effects on other components within
the battery (e.g. grid corrosion, paste deterioration).

17.4.3. Short term extraction will be influenced by the surface area of the RBSM. Higher surface area
RBSM of the same chemical composition will give relatively higher impurity test levels.

17.4.4. It should be noted that reported metallic values are based on the total weight of the mat.
Values will therefore be 100 times those detected in the extract for a 1.000 gram RBSM
specimen. Estimates of potential metallic impurities in a battery will depend on the ratio of the
electrolyte to RBSM within the battery.

17.5. Apparatus

17.5.1. Electric drying oven (non-air recirculating), capable of maintaining a temperature eof 150°C ±
10°C (302°F ±18°F). Mechanical convection oven can also be used. Sample upset, due to air
turbulence within oven, must be avoided.

17.5.2. Weighing device, readable and accurate to within ±0.25% of applied load, and shielded from
air currents when in use. Calibration as determined in 17.7.1.

17.5.3. Desiccator and desiccant.

17.5.4. 250 ml borosilicate glass flat-bottom boiling flask (4) with ground glass joint, 24/40.

17.5.5. Reflux condenser (4), Liebig or Fredricks.

17.5.6. Magnetic stirrer hot plate (4).

17.5.7. Filter unit (4) – Malgene, Cat. No. 126-0045 w/0.45 micron membrane or equivalent unit.
Teflon filters can also be used.

17.5.8. 100 ml volumetric flasks.

17.5.9. Pipettes – plastic (various sizes).

17.5.10. Atomic Absorption Spectrometer or ICP Spectrometer.

17.5.11. Perkin-Elmer Kydride Generation Systems 303-0849 or MHS-10 or equivalent hydride

generation system supplied by the AA or ICP manufacturer.

17.5.12. Hollow cathode lamp for each analyte.

17.6. Reagents and Materials

17.6.1. Purity of Reagents – Reagent grade chemicals shall be used in all tests. Unless otherwise
indicated, it is intended that all reagents shall conform to the specification of the Committee
on Analytical Reagents of the American Chemical Society where such specifications are
available. Other grades may be used, provided it is first ascertained that the reagent is of
sufficiently high purity, to permit its use without lessening the accuracy of the determination.

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17.6.2. Purity of Water – Unless otherwise indicated, reference to water shall be understood to mean
18 megaohm reagent water as defined by Type II of ASTM Specification D 1193 (2.5).

17.6.3. Sulfuric Acid – J.T. Baker Trace Metal Analytical Grade or equivalent.

17.6.4. Stock Metal Solutions – J.T. Baker, MCB or equivalent; purchased as 1000 µg/ml standard
solutions.

17.7. Calibration

Weighing Device

Check the accuracy of the weighing device frequently by applying accurately measured
masses with both increasing and decreasing loads. If a sheet weighing device is used, it must
be properly calibrated to the required accuracy (17.5.2).

17.8. Preparation of 1.260 s,g. H2SO4 Blank and Standard Metal Solutions

17.8.1. Blank solution of 1.260 s.g. H2SO4.

17.8.1.1. Caution: Extreme heat is generated when diluting 96% H2SO4.

17.8.1.2. This procedure makes one liter of 1.260 s.g. sulfuric acid blank solution.

17.8.1.3. Into a one-liter volumetric flask, add 500 ml DI water. Place the flask into an ice bath.

17.8.1.4. In a separate beaker, weigh 445 grams of 96% sulfuric acid.

17.8.1.5. Slowly and very cautiously add the sulfuric acid to the iced flask while constantly swirling the
flask. Rinse the beaker several times with DI water and add to the flask.

17.8.1.6. Bring the flask to room temperature, adjust with DI water to the 1000 ml mark.

17.8.2. Standard Metal Solutions

17.8.2.1. Determine the analytical range (analyte concentration) of interest and then select the
necessary analytical technique (instrumentation). Prepare the multi-element metal standard
solution using the same procedure as for making the blank solution, except the metal analyte
spikes should be added before bringing to the 1000 ml mark with DI water. Minimally, a blank
(0) and three standards in the range of quantification should be used, i.e., 1X, 5X, 10X the
detection limit for each element. Since the metal of interest and expected concentration may
vary with the material it is between the vendor and user to determine suitable standards to be
used. Annex A.1 should be referenced before standards are set.

17.8.2.2. The calibration step is a single most important activity. If not done consistently, the ability to
compare results prepared by different analysts or different labs could have significant
variations.

17.9. Sampling

The sampling procedure in BCIS-03a-3 is to be used.

17.10. Procedure

17.10.1. Acid Extraction

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17.10.1.1. Weigh to three decimal places, four 1.000 ±0.05g RBSM samples. Samples should be torn by
hand while using gloves. Scissors should be avoided since the scissors will introduce
additional metal ions.

17.10.1.2. Determine moisture content of two of the samples using BCIS-03a-11, Test Method for
Determining Percent Moisture content of Recombinant Battery Separator Mat.

17.10.1.3. Place each of the remaining two samples in a 250 ml flat bottom boiling flask fitted with a
24/40 ground glass joint. Put a magnetic stirring bar in each flask, add 126 g ± 0.05 g
(approximately 100 ± ml) of 1.260 s.g. sulfuric acid and attach a reflux condenser (do not use
silicone grease). Place each extraction assembly on a hot plate magnetic stirrer. Accuracy
and reproducibility is effected by the precision of the volume of acid introduced to the flask.

17.10.1.4. Prepare two blank, reflux assemblies, as above (17.10.1.3) without RBSM.

17.10.1.5. Adjust the temperature control and stirrer speed to obtain a reflux rate of one drop per
second and maintain these conditions for 3 hours. Assure stirrer is agitating the slurry to
avoid dangerous bumping conditions.

17.10.1.6. After cooling, vacuum-filter the contents of each flask through the filter apparatus (17.5.7).
Transfer the filtrate to a 100 ml volumetric flask.

Note: If insufficient suction is pulled during vacuum filtration, there could be up to 5 grams
residual 1.260 s.g. in the sample. This needs to be rinsed out by first removing original filtrate
container and replacing with a "waste" suction filtration flask. Several 20 ml aliquots of DI H2O
are then applied until separator sample is free of excess 1.260 s.g. H2SO4 . Oven corrosion
damage may result if excess acid is left in the sample when the acid weight loss test is done.
Do not save washed filtrate.

17.10.1.7. Determine the acid weight loss according to BCIS-03a-16, Test for Determining Acid Weight
Loss of Recombinant Battery Separator Mat (Reflux Method).

17.10.2. Atomic Absorption of Inductively Coupled Plasma Emission Analysis of Metal Ions (except
barium).

17.10.2.1. Perform these analyses according to procedure described in ASTM E885 (Subsection 2.4) on
both the extracts of test samples and the blanks. A corrosion-resistant plastic nebulizer is
recommended for aspirating 1.260 s.g. H2SO4 matrix when using Atomic Absorption. It should
be determined whether any viscosity effects are present.

17.10.2.2. The choice of specific elemental analysis technique variations, such as metal hydride
generation, or electro thermal (furnace) atomization should be based on the need for
improved sensitivity and/or freedom from interference. Implementation of such variations
should include evaluation of the limit of quantitation, precision, and freedom from
interference. If required then use the hydride generation system (17.5.11) as described in
Referenced Documents 17.2.6, in the analysis of the following elements: antimony, arsenic,
bismuth, lead, mercury, selenium, tellurium and tin.

Note: The Hydride Standard conditions can be obtained from Perkin Elmer Corporation or
OEM equipment manufacturer.

17.10.3. Barium Analysis of Recombinant Mat.

17.10.3.1. Weigh four, 1.000 g ± .005 g samples of RBSM.

17.10.3.2. Perform a Moisture Content determination on two of the samples according to 17.2.2.

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17.10.3.3. Digest each of the remaining RBSM samples in 5 ml perchloric acid (s.g. 1.54 @ 20°C) and
15 ml hydrofluoric acid (s.g. 1.13 @ 20°C) at a minimum temperature of 260°C (500°F) until
dissolved (approximately 1.5-2 hours is required). Either a platinum crucible or PTFE
container can be used. Two digestions without mat samples are performed to serve as
blanks.

Danger: Both perchloric and hydrofluoric acids are extremely corrosive. Proper
handling equipment and ventilation are required. Perchloric acid can be explosive if
concentrated by evaporation in absorbent materials, concrete, or in contact with
organic matter. Use a perchloric acid approved fume hood (one that has wash-down
capabilities). Check with manufacturers MSDS.

17.10.3.4. Carefully, heat to near dryness, using a magnetic stirrer-hot plate, then dissolve the residue
in 25 ml of diluted hydrochloric acid (1 volume of 1.18 s.g. HC1 to 1 volume of deionized
distilled water).

WARNING: If charring or dryness is obtained, an explosion will occur.

17.10.3.5. After cooling, transfer the residue (dissolved fiber) to a 100 ml volumetric flask while washing
the vessel used to dissolve the residue, with deionized distilled water. Fill to the 100 ml mark.

17.10.3.6. Analyze the sample and blank by atomic absorption spectroscopy using the procedure
described in ASTM E 885 (2.4) or Inductively Coupled Plasma spectroscopy. A procedure in
which the sample is run, with and without a known concentration of added barium, is also
acceptable.

17.11. Calculations

17.11.1. Measured and calculated parameters (units):

M Moisture Content (%) as determined in 17.10.1.2.

WT Mass of Sample (g).
ODWT Oven Dry Mass of Sample (g).
L Acid Weight Loss (%) as determined in 17.10.1.7.
C Analyzed Concentration of Metallic Ion (except barium) in 100 ml volumetric
dilution (µg/ml) as determined according to ASTM E 885 (2.4)
B Analyzed concentration of Barium Ion µg/ml) in 100 ml volumetric dilution from
17.10.3.6.
K Analyzed Concentration of Metallic Ion or Barium Ion in Blank (µg/ml).
V Total Mass of Metal Ion in volumetric dilution (µg).
VBA Total Mass of Barium Ion in volumetric dilution (µg).
I Concentration of Extracted Metallic Impurity (except barium) based on ODWT
(µg/ml by weight).
TBA Total Concentration of Barium (µg/ml by weight) based on ODWT.
BA Extractable Concentration of Barium (ppm by weight) based on ODWT. (Note:
Barium is calculated barium based on total solubility of RBSM in 1.260 s.g. sulfuric
acid. Actual extractable barium may be lower).

17.11.2. ODWT = WT x (1 – (M/100)).

17.11.3. V = (C – K) x 100 (Corrected Blank).

17.11.4. VBA = (B – K) x 100 (Corrected for Blank).

17.11.5. I = V / ODWT.

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17.11.6. TBA = VBA / ODWT.

17.11.7. BA = TBA x L

17.12. Report

17.12.1. Report the average extractable concentration of each element in ppm by weight, based on
oven dry sample mass, to one decimal place.

17.12.2. Elements not detected are reported as concentrations less than the detection limits indicated
in the Annex.

17.13. Precision and Bias

Precision and bias for methods are not available at this time.

17.14. Annex (Mandatory Information)

Limits of detection of extracted metallic impurities based on oven dry RBSM weight (ppm by
weight)

Metallic Impurity Atomic Flame Absorption Hydride AA ICP

Aluminum 80 40
Antimony 100 0.06 12
Arsenic 520 0.04 5
Barium 30 3
Bismuth 30 0.06 25
Cadmium 1 5
Calcium 2 4
Chromium 4 4
Cobalt 10 3
Copper 2 2
Iron 8 6
Lead 12 ** 5
Magnesium 1 0.4
Manganese 2 2
Mercury - 0.005 -
Nickel 14 6
Platinum 70 3
Selenium 30 0.04 50
Silver 2 2
Strontium 4 1
Tellurium 30 0.06 20
Tin 200 0.05 30
Titanium 50 3
Zinc 4 2

** Not Determined.

Note: Expected detection limits for 1:100 dilution. DL = 3 x standard deviation.

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18. EXTRACTABLE CHLORIDE OF RECOMBINANT BATTERY SEPARATOR MAT

The industry at this time is unable to offer a recommendation of any one procedure which it
feels provides suitable accuracy or repeatability. Current industry practice employs several
different procedures for extractable chlorides of recombinant battery separator mat (RBSM)
but round robin studies demonstrated unacceptable results. At such time that an acceptable
procedure will be developed it will be published by BCI.

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19. STANDARD TEST METHOD FOR DETERMINING THE ELECTROCHEMICAL

COMPATIBILITY OF RECOMBINANT BATTERY SEPARATOR MAT

19.1. Scope

19.1.1. This procedure covers method of determining electrochemical compatibility of materials

including recombinant battery separator mat (RBSM) used in lead acid battery.

19.1.2. The procedure involves leaching a sample of material in sulfuric acid and determining its
electrochemical activity by differences between the rotating lead disc electrode current
voltage curves for pure acid and leach solution.

19.1.3. This test procedure may involve hazardous materials. This procedure does not purport to
address all of the safety problems associated with its use. It is the responsibility of the user of
this test method to consult Material Safety Data Sheets (MSDS) of the materials involved with
the test, to establish appropriate safety and health practices and determine the applicability of
regulatory limitation prior to use.

19.2. Reference Documents

19.2.1. AT&T Technology Systems Manufacturing Standard 17000 Section 1241.

19.2.2. Amerace Corporation Procedure No. 4-74 Electrochemical Compatibility of Materials for Lead
Acid Batteries.

19.2.3. Evanite Fiber Corporation Test Method No. ECTM-01 Electrochemical Test Method.

19.2.4. ASTM D1193 Specification for Reagent Water.

Note: Documents 19.2.1, 19.2.2 and 19.2.3 listed above are available through BCI.

19.3. Significance and Use

19.3.1. The cell behavior of a lead acid battery is quite sensitive to small amounts of
electrochemically active substances in cell electrolyte. This phenomenon becomes
particularly critical in float service batteries.

Different additives may reflect totally different electrochemical responses.

19.3.2. This test procedure describes an accelerated test method by which the extraction rate of
contaminants from lead acid battery components into the cell electrolyte is predicated and
electrochemical effect of these contaminants is determined.

19.3.3. This method is a very detailed and complicated test method and for pure separators like
100% microglass RBSM, a simple screening analysis may be more practical.

19.4. Apparatus

19.4.1. Electronic Instrumentation

19.4.1.1. Potentiostat with output capability of ± 5V and ± 1A with the capability of raising or lowering
the voltage of the potentiostat at a rate of 200 mV per minute ± 10mV/minute linear sweep
rate. E.g. EG & G Princeton Applied Research Model 273 or Model 362 with factory
modification for 200 mV/min scanning rate.

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19.4.1.2. X-Y Recorder capable or recording with X axis sensitivity of 200 mV / 25.4 mm and Y axis
sensitivity of 1 mA / 25.4 mm; minimum input impedance to recorder shall be 100 megohms.
e.g. Hewlett-Packard Model 7090A Plotter or Houston Instruments RE-0091.

19.4.1.3. D.C. Power Supply with potential range of at least 0-5 volts DC and current range of at least
0-5 amperes to be used for pre-electrolysis of blank acid.

19.4.2. Cell apparatus

19.4.2.1. Electrode Rotating Motor. A synchronous rotator capable of a constant rotational speed of
600 ± 20 rpm and consisting of a hollow shaft chuck with locking nuts to accommodate
electrodes 6.36 mm in diameter. e.g. Sargent Welch S-76485.

19.4.2.2. Electrolysis Vessel, H Form (Figure 1) equipped with a sealed-in fitted glass disc at the
extreme end of the horizontal section, e.g., Sargent-Welch S-29396 equipped with stopcock
or S-29401 modified to have 50 mm diameter chamber.

19.4.2.3. Reference Electrode, Mercury-Mercurous Sulfate. The glassware for the half-cell reference is
of the hildebrand configuration (Figure 19.1 ) or reference electrode configuration of Evanite
Fiber Corporation.

Figure 19.1 – Electrolytic Cell

19.4.2.4. Counter Electrode. Lead rod approximately 6 mm (15/64 in) in diameter by approximately 130
mm (5 1/8 in) in length (80 mm (3 5/32 in) to be immersed in electrolyte) made from pure lead
of minimum 99.99% purity.

19.4.2.5. Rotating Lead Disc Electrode (Figure 19.2). The lead disc shall be prepared from the same
pure lead as the counter electrode in Paragraph 19.4.2.4, 6.3 mm ± 0.55 mm diameter. The
lead shall be sealed in sufficiently stable and nonleading epoxy such as Ciba Geigy
Corporation’s Araldite 502 and Araldite 951 curing agent.

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Figure 19.2 – Lead Disc Electrode

19.4.3. Other Apparatus

19.4.3.1. Extraction apparatus consisting of a variable transformer with a 380-watt hemispherical

mantle regulated at 71°C (160°F), 1000 ml two-necked round bottom flask, a 300 mm Leibig
condenser with ground glass joints and stoppers.

19.4.3.2. Miniature Machine Lathe capable of machining the face of the rotating disc electrode at 88
degrees to the rotational axis of the electrode.

19.4.3.3. Abrasive paper to be used for sanding rotating disc electrode shall be 600 micron aluminum
oxide sand paper.

19.4.3.4. Hydrometer calibrated at 1.210 s.g. and 20°C (68°F).

19.5. Reagents

19.5.1. Water

The water used for the purposes of this procedure shall meet the requirement of ASTM
D1193 Type II.

19.5.2. Sulfuric Acid

Reagent ACS grade sulfuric acid with specific gravity 1.210 ± .003 at 20°C (68°F) prepared
from deionized water meeting requirements of Paragraph 19.5.1.

19.5.3. Mercury

Instrument grade triple distilled.

CAUTION: Mercury is poisonous. Follow the safety instructions from Material Safety Data

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Sheet of supplier. Prevent accumulation of mercury vapor in work spaces through provision
of proper exhaust system. Avoid contact with skin and internal ingestion. Use plastic or
rubber gloves. Clean up spills immediately with mercury clean-up kits, Keep containers of
mercury closed at all times. When cleaning mercury with mercury cleaning kit and nitric acid
do so under well ventilated hood.

19.5.4. Mercurous Sulfate

Powdered reagent grade.

19.6. Procedure

19.6.1. PRECAUTION: The test described herein is sensitive to trace amounts of electrochemically
active material. Because of this sensitivity the sample handling, preparation, analysis and
storage must be accomplished using techniques which will preclude contamination by foreign
matter.

19.6.2. Sample Leaching

19.6.2.1. Cut an 8 x 10 cm sample of microfiber glass RBSM into suitable sizes allowed to be put into a
1000 ml round bottom flask.

19.6.2.2. Use an extraction apparatus described in Paragraph 19.4.3.1.

19.6.2.3. Leach the sample in 400 ml of pre-electrolyzed 1.210 ± .003 specific gravity sulfuric acid for 1
week at 71°C ± 5°C (160°F ± 9°F). Make certain that samples are fully immersed in acid
throughout the leaching period.

19.6.2.4. Cool the leached sample and transfer the leach liquid to an appropriate size holding flask
which is thoroughly cleaned and rinsed with deionized water.

19.6.3. Electrochemical Compatibility Test

19.6.3.1. Potential Scans – General

19.6.3.1.1. Connect the potentiostat and motor potentiometer as directed in the manufacturer’s operating
manual. The potentiostat controls the potential of the “working” electrode (disc) which may be
either the anode or cathode. The working electrode is used in the electrolytic circuit with two
additional electrodes, known as the “reference” and “counter” electrodes (Figure 1). The
motor potentiometer, which is electrically connected in series to the disc electrode,
superimposes potentials upon this electrode above that available from the potentiostat.
These potentials are programmed to rise cathodically or anodically at the linear rate of 200
mV/min. The scanning rate of 200 mV/min should be calibrated at least once each day prior
to running the first ECC scan.

19.6.3.1.2. With the lead disc electrode rotating at 600 ± 20 rpm, regulate the potentiostat output voltage
to control the potential of the disc to reference electrode at a value of + 0.800 or –0.800V for
anodic and cathodic scans, respectively.

19.6.3.1.3. Set the X-Y recorder with the X axis recording voltage to 200 mV/in (200 mV/25.4mm
sensitivity) and the Y axis recording current to 1 mA/in (1mA/25.4 mm sensitivity). The
potential scans for only one material (acid and leachate) shall be recorded on a sheet of
graph paper.

19.6.3.1.4. Fill the electrolytic cell with pre-electrolyzed 1.210 ± .003 specific gravity sulfuric acid.

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19.6.3.1.5. Set the reference electrode tip approximately 12.7 mm (1/2 in) from the bottom of the lead
disc which is immersed approximately 12.7 mm into the acid electrolyte. Center both
electrodes in the compartment.

19.6.3.1.6. With the disc electrode rotating at 600 rpm, activate the motor potentiometer, starting the
potential sweep at either + or – 0.880V with a linear increase in voltage of 200 mV/minute in
increments of 2 mV to 5 mV.

19.6.3.1.7. A cathodic scan starts at –0.800V. The working electrode voltage is scanned to more
negative values until the cell current attains 3 mA. The potential of the lead electrode at this
current should be approximately –1.80V with visual evidence of hydrogen evolving from the
disc surface. At 3 mA, reverse the sweep direction and return the disc potential to its initial
value of -0.800V. This voltage scan constitutes one cycle, in which the electrode is charged
(PbSO4 → Pb), polarized (H2) and discharged (Pb → PbSO4). See Figure 3.

19.6.3.1.8. An anodic voltage scan starts at + 0.800V. The working electrode voltage is increased to a
cell current of 5 mA which results in a disc voltage (after cycling) of approximately + 1.60V. At
5mA, reverse the sweep direction and return the disc potential to the initial value of + 0.800V.
In this scan the lead disc is charged (PbSO4 → PbO2), polarized (O2), and discharged (PbO2
→ PbSO4). See figure 4. Visual evidence (recorder plot) of PbO2 formation should be seen
on the second cycle.

19.6.3.2. Cathodic Scans

19.6.3.2.1. Prior to the first cycle, the lead disc shall be gently sanded on continuously water wetted 600
micron aluminum oxide abrasive paper until the lead surface appears uniformly abraded. A
small figure eight pattern using minimum pressure is recommended in order to obtain desired
uniformly abraded surface on the working electrode. Care must be taken to maintain a flat
surface of the electrode.

19.6.3.2.2. The voltage current behavior of the disc electrode in acid leach solution is compared to that in
pure sulfuric acid, 1.210 ±.003 s.g.

19.6.3.2.3. Cycle the lead disc electrode in pure sulfuric acid. Record the disc electrode potentials at 2
and 3 mA. Continue cycling until at least 4 cycles and until two successive readings at 2 and
3 mA do not vary by more than 20 mV.

19.6.3.2.4. After each cycle, the scan starting point (0 mA, 800mV shall be offset on the graph paper by
1 mA division. This indexing permits easy identification of the individual scans (see Figure 5).
The 2 mA point of the last standard acid scan must be within the voltage window of 1.650V to
1.850V.

19.6.3.2.5. After reproducible successive voltage readings are obtained, replace the pure acid in the
working disc electrode compartment with leach solution after draining off 80 ± 2% of the pure
acid to a level such that neither the glass frit is exposed nor the electrical continuity is lost,
and run through the voltage sweep. Record the voltages at 2 and 3 mA.

19.6.3.2.6. To determine the electrochemical activity of the leachable components in a material,

calculate the voltage difference between the last pure acid and leach solution at 2 and 3 mA
and report the average as a change in cathodic polarization.

Example (Figure 5).

@2mA @3mA
Pure Acid 1. 1.723 1.751
Pure Acid 2. 1.721 1.748

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Pure Acid 3. 1.718 1.742

Pure Acid 4. 1.715 1.739
Leach 1.711 1.718
Polarization -4 -21

Avg. = -13 mV

19.6.3.2.7. In addition, the cathodic scans in pure acid (see Fig. 3) shall be compared to scans in the
acid leach solution to determine the following:

Figure 19.3 – Cathodic Scan on Disc Electrode

19.6.3.2.7.1. Changes in the current voltage characteristics of the charge (PbSO4 → Pb) and
discharge (Pb → PbSO4) peaks.

19.6.3.2.7.2. Presence of additional peaks which may represent secondary or simultaneous reactions.

19.6.3.3. Anodic Scans

19.6.3.3.1. Prior to the first cycle machine 0.127 mm (0.005 in)off the face of the disc electrode using
lathe and surface the lead disc as in Paragraph 19.6.3.2.1.

19.6.3.3.2. As with the cathodic sweeps the data obtained in acid leach solution is compared to pure
sulfuric acid.

19.6.3.3.3. Cycle the cleaned electrode in pure sulfuric acid until the variation between successive
sweeps is less than 5 mV at 3, 4 and 5 mA. This usually requires a minimum of 5 cycles.

19.6.3.3.4. After reproducible cycles are obtained, stop the scan at d + 0.800V with current still flowing
through the circuit and the disc rotator stopped. Raise the electrolysis cell as high as possible
and drain off 80 ± 2% of the pure acid to a level such that neither the glass frit is exposed nor
electrical continuity is lost. It is important that the disc electrode is always immersed in
electrolyte and that its surface is not disturbed. Refill the working electrode compartment
promptly to the original level with acid leach solution, lower the electrolysis cell to its original
position, and restart the voltage sweep to obtain one cycle in leach solution.

19.6.3.3.5. Determination of electrochemical activity in the O2 evolution region is similar to the cathodic
procedure, with the exception of obtaining potentials in the oxygen evolution region at 3, 4,

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and 5mA. Average the voltage difference and report as the change in anodic polarization.

Example (Figure 19.6)

@3mA @4mA @5mA

Pure Acid 1. 1.658 1.661 1.671
Pure Acid 2. 1.610 1.626 1.638
Pure Acid 3. 1.604 1.621 1.632
Pure Acid 4. 1.603 1.620 1.631
Pure Acid 5. 1.603 1.619 1.631
Pure Acid 6. 1.602 1.619 1.631
Pure Acid 7 1.602 1.619 1.630
Leach 1.601 1.617 1.629
Polarization -1 -2 -1

Avg. = -1mV

19.6.3.3.6. In addition, the anodic scan in pure acid after cycling (see Figure 4) shall be compared to the
scan in the acid leach solution to determine the following:

Figure 19.4 – Anodic Scan

19.6.3.3.6.1. Changes in the current voltage characteristics of the charge (PbSO4 PbO2) – discharge
(PbO2 - PbSO4) peaks.

19.6.3.3.6.2. Presence of additional peaks which may represent secondary or simultaneous reactions.

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Figure 19.5 – Cathodic Scan of Disc Electrode

Figure 19.6 – Anodic Scan of Disc Electrode

19.7. Report

19.7.1. Cathodic Scans. Report values obtained from graph of cathodic scans Figure 5.

19.7.1.1. Cathodic voltage shift (hydrogen). Report average voltage shift between last curve of
standard pure acid and leach acid at 2mA and 3mA as shown in Paragraph 19.6.3.2.6.

19.7.1.2. Cathodic Current charge Peak. Report percent of charge peak current of leach to charge
peak current of standard acid.

Example (Figure 19.5): current, mA (leach / current, mA (standard) x 100

= 0.83 / 0.94 x 100 = 88% charge peak of standard

19.7.1.3. Cathodic Voltage Charge Peak Report voltage charge peak shift between standard acid and
leach acid.

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Example (Figure 19.5): voltage, mV (standard) – voltage, mV (leach)

= (-990 mV) – (-993 mV) = +3 mV shift

19.7.1.4. Cathodic Current discharge Peak Report percent of discharge peak current of leach acid to
that of standard acid.

Example (Figure 19.5): current, mA (leach) / current, mA (standard) x 100

= 1.90/2.40 x 100 = 79% discharge peak of standard

19.7.1.5. Cathodic Voltage Discharge Peak Report voltage discharge peak shift between standard acid
and leach acid.

Example (Figure 19.5): Voltage, mV (standard) – voltage, mV (leach)

= (-898 mV) – (-900 mV) = + 2 mV shift

19.7.2. Anodic Scans – Report values obtained from graph of anodic scans Figure 19.6.

19.7.2.1. Anodic Voltage Shift (Oxygen) Report average voltage shift between last curve of standard
pure acid and leach acid at 3, 4, and 5 mA as shown in Paragraph 19.6.3.3.5.

19.7.2.2. Anodic Current Charge Peak Report percent of charge peak current of leach solution to that
of standard acid.

Example (Figure 19.6): current, mA (leach) / current, mA (standard) x 100

= 0.83 / 0.99 x 100 = 88% charge peak of standard.

19.7.2.3. Anodic Voltage Charge Peak Report voltage charge peak shift between standard acid and
leach acid.

Example (Figure 19.6): Voltage, mV (standard) – voltage mV (leach)

= 1357 mV – 1370 mV = 13 mV shift.

19.7.2.4. Anodic Current discharge Peak Report percent of discharge peak current of leach acid to that
of standard acid.

Example (Figure 19.6): current, mA (leach) / current, mA (standard) x 100

= 5.69 / 5.95 x 100 = 07% discharge peak of standard.

19.7.2.5. Anodic Voltage Discharge Peak Report voltage discharge peak shift between standard acid
and leach acid.

Example (Figure 19.6): voltage, mV (standard) – voltage, mV (leach)

= 1030 mV – 1033 mV = 3 mV shift.

19.8. Precision and Bias

The precision of this test method has not been determined.

19.9. Appendix 1: Pre-Electrolysis of Acid

Preparation of Pure Acid

19.9.1. Prepare eight liters of 1.210 s.g. sulfuric acid from reagent grade concentrated acid and
deionized water.

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19.9.2. Insert two cleaned 13 cm x 15 cm (5 1/8 in x 5 29/32 in) 99.999% lead electrodes with 12.7
mm (1/2 in) grids into the acid. Connect the positive lead from the power supply to the
positive lead electrode and the negative lead to the negative electrode.

19.9.3. Turn on power supply and increase the voltage until there is visible gassing from both
electrodes. Check the current after 1 hour of electrolysis and adjust it to a level of 1.0 to 1.5
amps.

19.9.4. Allow the electrolysis of the acid to continue for 24 hours. Remove the lead electrodes and
turn off the power supply. Allow the acid to outgas for one hour. Then store the acid in glass
bottles.

19.10. Appendix 2

19.10.1. Fabrication of the Rotating disc Electrode

19.10.1.1. In the fabrication of the rotation disc electrode, it is essential that there are no voids in the
lead rod or the epoxy jacket. The lead rod, if cast, must be made in a mold (Figure A) whose
cavity is fed via the bottom of the mold with a 6.3 mm (1/4 in) hole and using lead at a
temperature 550°C (1022°F) tends to form reproducible and uniform castings. Prior to
encapsulation in epoxy, the lead rod is cleaned with 600 micron aluminum oxide wet or dry
abrasive paper. It is preferable to provide a constant washing during the cleaning process to
keep the abrasive paper from clogging with lead.

Figure 19.A – Split Hold for Casting Lead Rod (Aluminum)

19.10.1.2. A concentric holding piece (Figure 19.B) is fitted over one end of the lead rod. The lead rod,
with holding piece, is then mounted in the 12.7 mm (1/2 in) diameter mold (Figure 19.C),
which has been sprayed with Teflon, allowing 3.2 mm of the lead rod to protrude from the end
of the mold.

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Figure 19.B – Concentric Holding Piece (Polyethylene)

Figure 19.C – Split Mold for Casting Epoxy Jacket

19.10.1.3. Epoxy resin (Araldite 502 and Hardener 951) which has been preevacuated to remove all air
bubbles is then carefully poured into the 12.7 mm (1/2 in) mold around the lead rod. It is best
to do this under a vacuum; i.e., in a vacuum desiccator equipped with an addition funnel to
facilitate addition of the epoxy to the mold which is standing upright in the desiccator. When
the mold is filled with epoxy resin, a second concentric holding piece is then pressed over the
end of the protruding lead rod and pushed into the 12.7 mm (1/2 in) diameter cavity. The
resin is allowed to pre-cure for four hours after which time the mold is placed in a 93°C
(200°F) oven for three hours as a final cure. After it has cooled, open the mold and remove
the holding pieces from the ends of the lead rod and cut it into two equal sections using a
saw.

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19.10.1.4. Machine the ends of the pieces, make a small shallow hole in one end of each and solder a 2
cm (25/32 in) piece of 0.508 mm (20 mil) platinum wire onto the end. (The hole serves to hold
the Pt wire in position while soldering). Place the rod in the lathe and machine off enough of
the outside area of the Pt wire end so that the lead forms a 3.2 mm (1/8 in) long nub which
makes a snug fit inside a piece of 6 mm (15/64 in) glass tubing.

19.10.1.5. Take a 170 mm long piece of 6 mm (15/64 in) glass tubing, polish the ends, and slide a
concentric holding piece of 80 mm (3 5/32 in) onto one end. Put a dab of epoxy over the lead
protrusion at the base of the platinum wire and fit the long end of the glass tubing over the
platinum wire and lead tip (epoxy should fill 3.2 mm (1/8 in) of the glass tubing). The entire
assembly is mounted in the 12.7 mm (1/2 in)diameter mold which has been sprayed with
Teflon mold release (Figure 4) until the epoxy is cured. The clamping pressure on the mold is
released and the entire assembly is pushed upward in the mold such that the concentric
holding piece is 25.4 mm (1 in) above the top of the mold. The clamping screws are then
retightened. Approximately 2 ml of epoxy is added into the mold and allowed to run down the
sides and the concentric holding piece is pressed into the mold opening. After two hours of
pre-cure at room temperature, the mold is placed in a 93°C oven for three hours, allowed to
cool, and the finished electrode removed.

19.10.1.6. The electrode can then be dressed and filled with mercury to make contact with the platinum
filament of the rotator.

19.10.1.7. Throughout the fabrication of this electrode it must be stressed that the epoxy resin must be
pre-evacuated to remove all entrained air. In general, it can be stated that it is the small
bubbles of entrained air which cause instability and inconsistent scans.

19.10.2. Machining of the Face of the Disc Electrode

19.10.2.1. In the evaluation of electrochemical Compatibility it is critical that the surface of the electrode
is clean; that all traces of previous sample scans are removed, and that the texture of the
surface can be reproduced consistently.

19.10.2.2. To this end, the tool edge (Figure D) must be very sharp. The tool is first ground to the proper
configuration on a medium grit grind wheel. The upper flat surface is then lightly deburred by
rubbing the surface over a piece of 600 micron grit paper which is placed on a flat surface.
Polish the curved surface of the tool by repeatedly rubbing it over the 600 micron paper until
the tool edge is smooth and free of all rough edges. Be careful not to cause the sharp edge to
dig into the grit paper as it will easily dull the tool.

Figure 19.D – Cutting Took (High Speed Tool Steel)

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19.10.2.3. Mount the tool in the tool holder such that the leading edge passes exactly through the
rotational axis of the lathe spindle and approaches the electrode at a 30 to 45 degree angle
(Figure 19.E).

Figure 19.E

19.10.2.4. Adjust the motion of the tool table such that its motion perpendicular to the axis of the spindle
is offset by 2° as per Figure 19.D. This is extremely important since it prevents “smearing” of
the lead surface as the tool edge passes through the rotational axis of the electrode.

19.10.2.5. To obtain a smooth easily reproducible surface the spindle should have a rotational speed of
900 rpm and the feed rate of the tool should be 25.4 mm/min (1.0 in/min). To resurface the
disc electrode position the electrode in the lathe chuck and clamp lightly with the set screw.
With the spindle rotating at 900 rpm bring the tool into contact with the face of the electrode
and then retract the tool with the feed screw. Using the axial screw turn the tool 0.127 mm
(0.005 in) into the electrode and again using the feed screw, pass the tool across the face of
the electrode at a rate of 25.4 mm/min (1.0 in/min). Loosen the set screw and remove the
electrode from the spindle.

19.10.2.6. Always be careful, particularly after polishing, not to touch the face of the electrode against
anything as it may become contaminated.

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20. TOTAL ORGANIC CARBON FOR RECOMBINANT BATTERY SEPARATOR MAT

The industry at this time is unable to offer a recommendation of any one procedure over
another. Current practice employs several different test procedures for Total Organic Carbon
(TOC) of recombinant battery separator mat (RBSM). For those interested in reviewing
examples of test methods for the measurement of TOC in RBSM, several procedures are on
file at BCI.

Additional comments or examples of test methods of TOC may be submitted to BCI for
inclusion to this file.

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21. IDENTIFICATION OF ORGANIC IMPURITIES IN RECOMBINANT BATTERY SEPARATOR

MAT

21.1. Scope

21.1.1. This test procedure covers the qualitative identification of organic impurities in recombinant
battery separator mat (RBSM).

21.1.2. A sample of RBSM is extracted with an organic solvent (e.g. chloroform). After evaporation of
the solvent, an infrared spectrum is run on the residue. The contaminant spectrum is
compared to published reference spectra and/or spectra that have been run on suspected
sources of contamination.

21.1.3. Other spectral techniques, such as ultraviolet, near-infrared, far-infrared and nuclear
magnetic resonance may also be useful. Chromatographic techniques may be useful in
separating mixtures of extracted organic contaminants.

21.2. Referenced Documents

21.2.1. Sadtler Spectra Collections; Sadtler Research Laboratories, Inc.

21.2.2. Infrared Analysis of Polymers, Resinsand Additives – An Atlas – Volumes I & II; Hummel
D.O. and Scholl, F; Wiley Interscience (1969).

21.2.3. Identification and Analysis of Surface-active Agents by Infrared and Chemical Methods;
Hummel, D.; Interscience Publishers (1962).

21.2.4. Identification and Analysis of Plastics; Haslam, J. and Willis, H.A.; Van Nostrand (1965).

21.2.5. An infrared Spectroscopy Atlas for the coating Industry; Federation of Societies for Coatings
Technology (1980).

21.2.6. The Aldrich Library of Infrared Spectra; Pouchert, C. J.; Aldrich Chemical Company.

21.2.7. Perkin-Elmer Infrared Application Studies and Perkin-Elmer Infrared Bulletins; Instrument
Division, Perkin-Elmer Corporation.

21.3. Significance and Use

Some organic impurities in RBSM may adversely affect the performance of RBSM by
oxidation to gaseous products, causing pressure build up in the battery; by oxidation to acetic
acid and other lower organic acids resulting in reaction with the grids and subsequent deposit
of lead during battery cycling; or by direct reaction with gaseous oxygen.

21.4. Apparatus

21.4.1. Infrared or FTIR spectrometer.

21.4.2. Sodium chloride salt plates.

21.4.3. Infrared solvent cell with sodium chloride windows.

21.4.4. Thermostat controlled electric drying oven.

21.4.5. Ventilated fume hood.

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21.4.6. Hot plate-magnetic stirrer.

21.4.7. Erlenmeyer flasks (125 ml and 250 ml), flat bottom, with ground glass joints.

21.4.8. Soxhlet extractor.

21.4.9. Reflux condenser, Liebig or Fredricks.

21.4.10. Magnetic stirring bar.

21.4.11. Funnel.

21.4.12. Filter paper, fast running (Whatman No. 4), fluted.

21.4.13. Boiling stones.

21.4.14. 125 ml Erlenmeyer flask.

21.4.15. 10 ml Erlenmeyer flask.

21.4.16. Watch glass, Pyrex (7 or 8 inch diameter (178 mm or 203 mm)).

21.4.17. Scalpel.

21.4.18. Spatula (small).

21.4.19. Medicine dropper.

21.4.20. Needle probe.

21.4.21. Ringstand and clamps.

21.4.22. Long tweezers.

21.5. Reagents and Materials

21.5.1. Purity of Reagents – The use of spectroanalyzed organic solvents is recommended.

21.5.2. The Choice of extraction solvent(s) is at the discretion of the analyst and will depend on the
chemical nature of the suspected contaminant. Solvents recommended for consideration
include chloroform, carbon tetrachloride, methanol, and acetone and hexane.

21.6. Sampling

21.6.1. Each occurrence of organic impurities in RBSM may differ, thus some judgment must be
used in sampling and sample preparation. Since the weight of impurity compared to the
RBSM is usually quite small, the objective is to extract as much of the impurity as possible.

21.6.2. In cases in which the impurity is present as visual spots or streaks on the surface of the mat,
remove the spots (streaks) with a needle probe, taking a minimum amount of adjoining mat.

21.6.3. For surface coatings or discoloration, remove the contamination along with a thin layer of
RBSM for extraction.

21.6.4. For impurities distributed throughout the thickness of the mat or suspected impurities that are
not visible, a random sample is used in the extraction.

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21.7. Procedure

CAUTION: Due to the presence of potentially toxic solvent fumes, the extraction, filtration,
evaporation and infrared sample preparation steps must be carried out in a properly vented
fume hood.

21.7.1. Boiling Extraction

21.7.1.1. Place the spots or streaks and adjoining mat (21.6.2) in a ground glass-jointed Erlenmeyer
flask (21.4.7) of appropriate size and add a magnetic stirring bar.

21.7.1.2. Fill the flask to approximately 2/3 to 3/4 of its designated volume with extraction solvent
(21.5.2). Attach a condenser (no silicone grease), place the assembly on a hot plate-
magnetic stirrer and clamp it to the ringstand.

21.7.1.3. Heat and stir the solvent-RBSM mixture under vigorous reflux for a minimum of 16 hours,
then remove the hot plate-stirrer and allow the contents of the flask to cool to ambient
temperature.

21.7.2. Soxhlet Extraction

21.7.2.1. For surface coating or uniformly distributed impurities (21.6.3 and 21.6.4) cut the specimen
containing the contamination into rectangular strips of about 6mm (1/4 inch) width and length;
about 6mm (1/4 inch) less than the height of the soxhlet sample compartment.

21.7.2.2. Place the strips in the soxhlet sample compartment using the tweezers (no thimble).

21.7.2.3. Temporarily attach the soxhlet to a ground glass-jointed Erlenmeyer flask (21.4.7). Pour
extraction solvent (21.5.2) through the top opening of the soxhlet until the solvent in the
sample compartment siphons to the flask.

21.7.2.4. When the solvent has stopped dripping, temporarily clamp the soxhlet to the ringstand.
Remove the flask, add additional solvent to a level of about 2/3 the capacity of the flask and
add three boiling stones.

21.7.2.5. Attach the condenser and flask to the soxhlet (no silicone grease), place on the hot plate-
magnetic stirrer and clamp the assembly to the ringstand.

21.7.2.6. Adjust the hot plate setting so that the boiling solvent condenses into the sample
compartment at the rate of about one drop per second and extract for a minimum of 24 hours.
(Note: It may be necessary to wrap insulation around the flask and soxhlet to achieve the
above condensation rate).

21.7.2.7. Remove the hotplate and allow the assembly to cool to ambient temperature.

21.7.3. Filtration and Solvent Evaporation

21.7.3.1. Place the funnel containing a piece of fluted filter paper (21.4.12) into a 125 ml Erlenmeyer
flask.

21.7.3.2. Filter the solvent extract containing the organic impurities into the Erlenmeyer flask. (Note: In
the case of boiling extraction (21.7.1) and possibly soxhlet extraction (21.7.3), the glass fibers
present may clog the pores of the filter paper before its contents have fully drained. When
this occurs, carefully lift the fluted paper from the funnel, place a fresh piece in the funnel and
pour the contents of the plugged paper into the fresh paper. In some instances, this step will
have to be repeated several times.

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21.7.3.3. Remove the funnel, add two boiling stones, place the flask on the hotplate and reduce the
volume of solvent extract to about 25 ml, then allow the flask to cool to ambient temperature.

21.7.3.4. Pour the concentrated extract into the watch glass, place it on the hot plate and evaporate
the remaining solvent. (Note: solvent bumping may be reduced by the addition of a boiling
stone at the start of evaporation. This stone should be removed at about 10-15 ml volume).
When the volume of extract reaches the final 5 ml, hold the watch glass above the hotplate
(use insulated gloves) and swirl slightly.

21.7.3.5. Place the watch glass in a thermostatically controlled oven, set at a temperature of 20°C ±
5°C (36°F ± 9°F) above the boiling point of the extraction solvent, for 20 minutes to remove
any residual solvent. Remove the watch glass from the oven and allow it to cool to ambient
temperature.

21.7.4. Infrared Sample Preparation

21.7.4.1. The sample preparation technique chosen will depend upon the physical nature of the
organic impurity residue on the watch glass. Judgement by the analyst is required. More
than one technique may be applicable in many cases.

21.7.4.2. NaCl Plate Smear – this technique is applicable for semi-solid or liquid residues (e.g. grease).
Remove the residue from the watch glass with a scalpel or spatula. Place on a NaCl plate
and sandwich with a second NaCl plate.

21.7.4.3. Film Cast on NaCl Plate – this technique is applicable for film-forming residues (e.g. polymer
binders or impurities). Scrape the film from the watch glass with a scalpel. Place the scraping
in a 10 ml Erlenmeyer flask and add a minimum amount of solvent to dissolve the residue.
Place a few drops of the impurity solution on a NaCl late and allow the solvent to evaporate,
leaving a film. (Note: Chloroform and carbon tetrachloride are preferred solvents because of
their transparency in most infrared regions).

21.7.4.4. Solvent Cell – This technique is applicable to solid organic impurities, which are not film
forming (e.g. hard polymers). Dissolve the scraped residue in a solvent, fill the infrared
solvent cell with the residue solution and fill the reference cell with pure solvent.

21.7.4.5. KBr Pellet – This technique may be used for preparation of samples not possible by the
methods described in 21.7.4.2, 21.7.4.3, and 21.7.4.4. Spectrum quality is poorer than the
other techniques. Consult infrared spectrometer manufacturers’ instructions.

21.7.5. Running of Infrared Spectra

Follow instructions provided by infrared spectrometer manufacturers.

21.8. Interpretation of Spectra

21.8.1. Observe the position of the major bands of the contaminant spectrum to determine which
organic functional groups are present (e.g. only unsaturated hydrocarbon bands suggests the
presence of some types of grease or a polyolefin; carbonyl and C-O single bond groups
together suggest an acrylic polymer or a phthalate plasticizer).

21.8.2. Based on conclusions drawn in 21.8.1 and from the physical nature of the extracted
contaminant, compare the contaminant spectrum to appropriate classes of reference spectra
(21.2.1 – 21.2.7). It is also very valuable to have infrared spectra for reference of all raw
materials used in the manufacturing of all products made on the same equipment, in addition
to lubricating greases and oils used in the production facility.

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21.9. Report

In cases not restricted by proprietary information limitations, a complete report should include
RBSM sample identification, conclusions as to the identity and/or chemical nature of the
organic impurity, a brief description of techniques used in the analysis, a spectrum (or
spectra) of the impurity and photocopies of reference spectra.

21.10. Precision and Bias

Precision and bias data for the methods described above are not available at this time.

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22. ELECTRICAL RESISTANCE OF RECOMBINANT BATTERY SEPARATOR MAT

The Battery Council International Technical Subcommittee on Separators has reached a

consensus that equipment suitable for measuring the electrical resistance of recombinant
battery separator mat (RBSM) in the partially saturated state does not presently exist.

If such equipment is developed at some future date, the Subcommittee on Separators may
be reactivated to draft an appropriate method.

In the interim, some laboratories have chosen to use BCIS03b-18, Standard Test Method for
Determining the Electrical Resistance of Battery Separator Using a Palico Measuring System
for measurements on RBSM in the flooded state. The use of this test method for RBSM is not
sanctioned.

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23. CONVERSION FACTORS FOR SI UNITS

Value in Trade or Conversion

Quantity or Test Customary Unit x Factor = Value in SI Unit Symbol

Area square inches 6.45 square centimeters cm2

square feet 0.0929 square meter m2
square yards 0.836 square meter m2
acres 0.405 hectares ha

Basis Weight* or lb (17x22-500) 3.760 grams per sq meter g/m2

Substance lb (24x35-500) 1.627 * **

(500 sheet ream) lb (25x38-500) 1.480 * **

or Grammage* when lb (25x40-500) 1.406 * *

expressed in g/m2 pounds per 1000 sq ft 4.882 * **

Caliper mils 0.0254 millimeters mm

Force kilograms 9.81 newtons N

pounds 4.45 newtons N

Length angstroms 0.1 nanometers nm

microns 1 micrometers um
mills 0.0254 millimeters mm
feet 0.305 meters m

Mass tons (2000 lbs) 0.907 metric tons t

pounds 0.454 kilograms kg
ounces (avdmp.) 28.3 grams g

Mass per Unit Volume ounces per gallon 7.49 kg per cubic meter kg/m3
pounds per cubic ft 1.60 kg per cubic meter kg/m3

Stiffness (Taber) gram centimeters 0.0981 millinewton meters mN•m

(taber units)

Tear Strength grams 9.81 millinewtons mN

Tensile Breaking Load pounds per inch 0.175 kilonewtons per meter kN/m
kilograms per 15 mm 0.654 kilonewtons per meter kN/m

Volume, fluid ounces (US Fluid) 29.6 milliliters mL

gallons 3.79 liters L

Volume, Solid cubic inches 16.4 cubic centimeters cm3

cubic feet 0.0283 cubic meters m3
cubic yards 0.765 cubic meters m3

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