Technical Manual Section - 03b

BCIS-03B REV.
BCI Battery
Technical DEC02
Manual
Issued 1992-03
Current Revision: 2002-12
BCI RECOMMENDED MATERIALS SPECIFICATIONS

BATTERY SEPARATOR TEST METHODS
TABLE OF CONTENTS
1. Standard Test Method for Overall Thickness of Battery Separator........................................... 3

2. Standard Test Method for Overall Thickness of Battery Separator Including Attached Retainer
Mat ............................................................................................................................................ 5
3. Standard Test Method for Backweb Thickness of Battery Separator ....................................... 7
4. Standard Test Method to Determine Squareness of Battery Separator ................................... 9
5. Standard Procedure to Determine Height and Width of Battery Separators........................... 11
6. Standard Test Method to Determine the Skew of Roll Stock Battery Separator Material....... 14
7. Standard Test Method to Determine Volume Porosity and Moisture Content of Battery
Separators ............................................................................................................................... 16
8. Standard Test Method for Pore Size Characteristics by the Mercury Intrusion Method for
Microporous Separators .......................................................................................................... 18
9. Standard Procedure for Dimensional Stability of Separators in Group Formation Dry and Wet
Charge Batteries...................................................................................................................... 21
10. Standard Procedure for Dimensional Stability of Separators to Air Drying............................. 23
11. Standard Test Method for Elongation and Tensile Strength of Microporous Polyethylene
Battery Separator .................................................................................................................... 25
12. Standard Test Method for Taber Stiffness of Leaf Separators................................................ 29
13. Standard Test Method to Determine Pin Puncture Resistance of Battery Separator Using a
Manual Chatillon Tester........................................................................................................... 32
14. Standard Test Method to Determine Puncture Resistance of Battery Separators Using a
Tensile (Instron®) Machine .....................................................................................................35
15. Test VIII - Wetting Properties Procedure VIIIA - Acid Floatation Method ............................... 37
16. Test VIII - Wetting Properties Procedure VIIIB - Acid Drop Absorption Method ..................... 39
17. Test VIII - Re-Wetting Properties Procedure VIIIC - Dry Charge Process Simulation ............ 41
18. Standard Test Method for Determining the Electrical Resistance of Battery Separator Using a
PalicoMeasuring System.......................................................................................................... 43
19. Standard Procedure for Separator Degradation Testing......................................................... 51
20. Standard Test Method for Acid Extraction by Acid Reflux Procedure A-1 .............................. 52
21. Standard Test Method for Hot Acid Soak Procedure A-2 ....................................................... 54
22. Standard Test Method for Metal Analysis by Inductively Coupled Plasma Emission (ICP)
Procedure C-2 ......................................................................................................................... 56
23. Standard Test Method for Atomic Absorption Spectrophotometer (AA) Procedure C-1......... 63
24. Standard Test Method for Total Organic Carbon (TOC) Procedure D-1 ................................ 64
25. Standard Method for Chloride Analysis in Sulfuric Acid by Atomic Absorption
Spectrophotometer (AAS) ....................................................................................................... 67
BCIS-03B Rev. DEC02
26. Standard Test Method to Determine Chlorides in Sulfuric Acid by Turbidimetry .................... 71
27. Standard Procedure to Determine Chlorides by Ion Specific Electrode ................................. 74
28. Standard Test Method to Determine Pin Puncture Resistance of Battery Separator Using a
Motorized Chatillon Tester....................................................................................................... 78
29. Standard Test Method to Determine Resistance of Battery Separators to Oxidative
Degradation Using Hydrogen Peroxide in Sulfuric Acid as Oxidizing Medium ....................... 80
30. Standard Test Method to Determine Resistance of Battery Separators to Hold Sulfuric Acid 85
31. Standard Test Method to Determine Resistance of Battery Separators to Oxidative
Degradation Using Potassium Dichromate in Sulfuric Acid as Oxidizing Medium.................. 89
32. Standard Test Method to Determine Reistance of Battery Separators to Oxidative
Degradation Using Simulated Electrochemical Cell Environment as Oxidizing Medium ........ 95
33. Standard Test Method to Determine Elemental Chlorine in Sulfuric Acid Solutions by
Inductively Coupled Argon Plasma Optical Emission Spectroscopy (ICP/OES) .................. 100
34. Standard Test Method to Determine Chlorides by Potentiometric Chloride Determination in
Aqueous Extracts .................................................................................................................. 104
2
BCIS-03B Rev. DEC02
1. STANDARD TEST METHOD FOR OVERALL THICKNESS OF BATTERY SEPARATOR
1.1. SCOPE
1.1.1. This procedure provides a method of measuring the overall thickness of a battery separator
using three different pressures depending on the application and type of separator.
1.1.2. This procedure should not be used for separators with a retainer mat or with recombinant
battery separator mat (RBSM).
1.2. SIGNIFICANCE AND USE
1.2.1. Accurate measurement and control of overall thickness of battery separators are essential to
ensure correct assembly, and acceptable performance and life characteristics of the battery.
1.2.2. The variety of separators and their end uses requires that three methods of measurement are
available.
1.2.3. Ribbed, corrugated, or embossed separators intended for SLI and most stationary
applications are tested at 2.1 kPa (0.3 psi). See section 1.3.1.
1.2.4. Separators intended for motive power and heavy duty stationary applications are generally
thicker and stiffer. They are best measured at a higher pressure. See Subsections 1.3.2 and
1.3.3.
1.3. APPARATUS
1.3.1. TYPE A - A gauge equipped with a 50 mm (2 in), diameter upper contact foot that exerts a
pressure of 2.1 kPa (0.3 psi) on the full area of the anvil. The anvil to be equal to or larger
than the upper contact foot. Dial graduation of the gauge is either 0.01 mm or 0.0001 in.
Examples are Ames's Dial Micrometer Model 262 with base Model #16, and Emveco's
Microgauge Model 200A or equivalent.
1.3.2. TYPE B - A gauge equipped with a 76 mm x 76 mm (3 in x 3 in) upper contact foot that exerts
a pressure of 6.9 kPa (1.0 psi) on the full area of the anvil. Dial graduation of the gauge is
either 0.01 mm or 0.0001 in. e.g. Amerace gauge, figure 1, or equivalent.
1.3.3. TYPE C - A gauge equipped with a 76 mm x 76 mm (3 in x 3 in) upper contact foot that
exerts a pressure of 3.45 kPa (0.5 psi) on the full area of the anvil. This gauge is equivalent
to TYPE B except that the loading is only at 3.45 kPa.
1.4. CALIBRATION
1.4.1. Make sure that the lower anvil and upper contact foot are clean, and operating smoothly
without binding. Check to ensure that the anvil is parallel with the contact foot, making
uniform contact when they are closed. This is done by using a gauge block and checking the
reading obtained at a minimum of three spots.
1.4.2. Check micrometer accuracy using certified gauge blocks. Be sure the dial micrometer is
zeroed when anvil and foot are in contact without the sample. To adjust the gauge, check the
manufacture’s instructions.
3
BCIS-03B Rev. DEC02
1.5. PROCEDURE
1.5.1. Raise the foot and insert the separator sample, major rib-side up on the anvil.
1.5.2. Gently lower the contact foot until it contacts the ribs. The upper foot should not extend
beyond the last rib of the separator by more than 6 mm (0.24 in). Do not allow the foot to free
fall or be spring driven onto the separator. Take a minimum of three (3) readings.
1.5.3. Measure the separator at each side and in the center. Read the thickness to the nearest
limiting decimal point of the gauge. Record all numbers and location of measurements.
1.6. REPORT
1.6.1. Report all readings of overall thickness per customer/ vendor requirements.
1.6.2. Report apparatus type used.
4
BCIS-03B Rev. DEC02
2. STANDARD TEST METHOD FOR OVERALL THICKNESS OF BATTERY SEPARATOR

INCLUDING ATTACHED RETAINER MAT
2.1. SCOPE
2.1.1. This procedure provides a method of measuring the overall thickness of a battery separator
with attached retainer mat. The retainer mat is usually a glass mat.
2.2.1. Some batteries use separators with a retainer mat attached, usually to their major ribbed
side. The purpose of the retainer mat, positioned facing against the positive plate in the
battery, is to reduce shedding of positive active material during the service of a battery.
2.2.2. Unlike most rigid battery separators, the retainer mat is compressible under low pressure
similar to Recombinant Battery Separator Mat (RBSM). The measured thickness of a
retainer mat or a separator with a retainer mat attached depends on the pressure applied by
the thickness gauge. Therefore, the accuracy and value obtained for thickness of a separator
with a retainer mat attached depends on the pressure applied by the thickness gauge.
2.2.3. The ideal pressure of the thickness gauge may be the one that will simulate the pressure the
element exerts on the glass mat in the cell. Since the pressure varies depending on the
intended battery design, the purpose of this procedure is to provide a standard method that
should be universally acceptable for most battery assemblies and designs.
2.2.4. The compressibility of a retainer mat attached to a separator varies depending on the
configuration and area of separator ribs against which a glass mat is compressed. The
measured thickness of a separator / retainer mat assembly may not necessarily be the same
as the sum of individually measured thickness of a separator and a retainer mat.
2.2.5. With this method one may specify the thickness of a separator / retainer mat assembly,
specify the thickness of a retainer mat, or thickness of a separator to which retainer mat will
be attached.
2.3. APPARATUS
2.3.1. A precision deadweight micrometer with a 50 mm (2 in) diameter upper contact foot
and anvil, exerting a pressure of 3.0 kPa (0.435 psi). Two models are TMI’s
No. 553M and Ames No. 24, or comparable gauge with 3.0 kPa spring tension with
suitable loads and anvil sizes. Dial graduation of the gauges is either 0.01 mm or
0.0001 in.
2.4. CALIBRATION
2.4.1. Make sure that the lower anvil and upper contact foot are clean and operating
smoothly without binding. Check to ensure that the anvil is parallel with the contact
foot making uniform contact when they are closed.
2.4.2. Check the accuracy of the micrometer using certified gauge blocks. Make sure that the dial
micrometer is zeroed when the anvil and the foot are in contact without the sample. To adjust
the gauge, check the manufacturer’s instructions.
2.4.3. The load applied to the anvil should be checked with a load cell or other suitable force
measurement device.
2.5. PROCEDURE
5
BCIS-03B Rev. DEC02
2.5.1. Raise the contact foot and insert the retainer mat or separator / retainer mat or assembly,
retainer mat side up on the anvil.
2.5.2. Gently lower the contact foot until it contacts the sample. The upper contact foot should not
extend beyond the last rib of the separator by more than 6 mm (0.24in). Do not allow the foot
to free-fall or be spring driven onto the sample backweb. Take a minimum of three (3)
readings. Measure the separator at each side and in the center.
2.5.3. Record all readings and locations measured.
2.6. REPORT
2.6.1. Report all readings and overall thickness per customer/vendor requirements.
2.6.2. Report the gauge, anvil size, loading of the gauge and what was measured.
6
BCIS-03B Rev. DEC02
3. STANDARD TEST METHOD FOR BACKWEB THICKNESS OF BATTERY SEPARATOR
3.1. SCOPE
3.1.1. This procedure describes the general method for measuring backweb thickness between
major ribs of various battery separators.
3.2.1. Accurate measurement and control of backweb are essential to ensure performance and life
characteristics of the battery.
3.2.2. The true backweb excludes the height of the mini-ribs. However, for separators that have
mini-ribs on either side of the backweb, those ribs may be included in the backweb reading.
If mini-ribs are included in the backweb thickness, then this fact should be noted.
3.2.3. The wide variations in separator materials (degrees of web compressibility, rib pitch,
composition, etc.) dictate the use of different micrometer types (see Apparatus).
3.3. APPARATUS
3.3.1. The gauge with a circular upper contact foot of 9.5mm (0.374 in.) in diameter that exerts a
pressure of 2.1 kPa (0.3 psi) on the sample. Gauge graduation must have at least 0.01mm
(for metric) or 0.001 in. (for English) resolution.
3.3.2. Fibrous separators that are compressible, such as paper and non-wovens made from such
material as cellulose, glass fiber and synthetic wood pulp and that have rib pitch values of
10mm (0.4 in.) or more, should be measured with this gauge.
3.3.3. This method should not be used for recombinant battery separator mat (RBSM).
3.3.4. A gauge with a suitable contact foot and load so that pressure is exerted on the separator to
equal 110 kPa ± 20 kPa (16 psi ± 2.9 psi). The gauge graduation must have at least
0.001mm (for metric) or 0.0001 in. (for English) resolution.
3.3.5. Non-fibrous, non-compressible separators, such as polyethylene, PVC, microporous rubber

and other non-fibrous type separators should use this type of gauge.
3.4. TERMINOLOGY
3.4.1. MINI-RIBS - Another name for smaller ribs located either on the seal shoulder or on either
side of the backweb, between or opposite the major ribs.
3.4.2. NEGATIVE'S MINI-RIBS - Separators that have mini-ribs on the backside. This is the side
that normally faces the negative plate.
3.4.3. SHOULDER - This is the margin between either side edge of the separator and the adjacent
major rib.
3.4.4. SHOULDER MINI-RIBS - The ribs in the area of the shoulders.
3.4.5. MAJOR RIBS - The ribs that normally face the positive plate. These ribs are normally the
tallest ribs.
3.5. CALIBRATION
7
BCIS-03B Rev. DEC02
3.5.1. Make sure that the lower anvil and upper contact foot are clean and operating smoothly
without binding. Check to ensure that the anvil is parallel with the contact foot, making
uniform contact when they are closed. This is done by using a gauge block and checking the
reading obtained at a minimum of three spots.
3.5.2. Check micrometer accuracy using certified gauge blocks. Be sure the dial micrometer is
zeroed when anvil and foot are in contact without a sample. To adjust gauge, check
manufacturer's instructions.
3.6. PROCEDURE
3.6.1. Raise the foot and insert the separator sample, rib-side up on the base plate.
3.6.2. Center the measurement foot between ribs.
3.6.3. Gently lower the contact foot down between the ribs until it contacts the backweb area. Do
not allow the foot to free fall, be spring driven onto the separator, or impinge on the radius
base corner of the rib.
3.6.4. Measure the backweb thickness of the separator at each side and in the center. Read the
thickness to the nearest limiting decimal point of the gauge.
3.7. REPORT
3.7.1. Report all readings per customers / vendor requirements.
3.7.2. Fibrous - nearest 0.1mm or 0.001 in.
3.7.3. Non-Fibrous - nearest 0.01mm or 0.0001 in.
3.7.4. The presence of mini-ribs that are included in the backweb thickness.
3.7.5. The gauge used and the loading of this gauge.
8
BCIS-03B Rev. DEC02
4. STANDARD TEST METHOD TO DETERMINE SQUARENESS OF BATTERY SEPARATOR
4.1. SCOPE
4.1.1. This procedure provides a method of measuring the squareness of sheet or leaf battery
separator.
4.2.1. A sheet or leaf separator which is not square will result in difficulty during the battery
assembly process and risk premature battery failure.
4.3. APPARATUS
4.3.1. Square rule or squareness set-up plate which consists of a flat surfaced plate with locating
bars positioned at right angle ( the vertical and horizontal members).
4.3.2. Steel rule graduated in a 0.5 mm or 1/64 in. increments.
4.4. TERMINOLOGY
4.4.1. The squareness of a separator is a linear measure of the deviation from exact squareness
that two adjacent sides exhibit. If those two sides form an exact 90 degree angle, the
squareness value is zero.
4.5. PROCEDURE
4.5.1. Place the separator to be checked on working surface of the apparatus of choice with "higher
rib side" up.
4.5.2. Place the side edge of separator against vertical member of the apparatus. The side edge is
that parallel to the ribs.
4.5.3. Gently slide the separator toward the horizontal member until the end edge of the separator
or some portion of the end edge of the separator, first makes contact with horizontal member,
all the while keeping the side edge of separator against vertical member.
4.5.4. Using the steel rule measure the squareness of the separator as the furthest distance (widest
edge) between side edge and the end edge of the separator. Record squareness to the
nearest 0.5 mm or 1/64 in.
4.5.5. Repeat above procedure after rotating separator 180 degrees.
4.5.6. Steps 4.5.1 to 4.5.5 yields a squareness value for the end of the separator (Width) and is
called end squareness. By performing steps 4.5.1 to 4.5.5 with the separator rotated 90
degrees so that the end edge is placed against the vertical member and the side edge
contacts the horizontal member, the squareness value for the side of the separator (height or
length) can be determined. This value is called side squareness and may be of greater
significance where especially long separators are used (e.g., industrial cells).
4.6. REPORT
4.6.1. Report side squareness in mm (in).
4.6.2. Record width and height of the separator in mm (in).
9
BCIS-03B Rev. DEC02
4.6.3. The value can also be reported as mm/ mm of width for end squareness or mm/mm of height
for side squareness.
10
BCIS-03B Rev. DEC02
5. STANDARD PROCEDURE TO DETERMINE HEIGHT AND WIDTH OF BATTERY

SEPARATORS
5.1. SCOPE
5.1.1. This procedure includes two methods for measuring height (length) and width of battery
separators.
5.1.2. Method A uses a graduated measuring device, such as a rule or a square.
5.1.3. Method B uses a higher resolution digital micrometer system. As compared to Method A,
Method B is commonly used to measure the width of roll stock separator materials.
5.2.1. Accurately controlled separator dimensions are vital for the correct assembly and proper
performance of batteries. Method A is sufficiently accurate to insure a good fit and proper
function of the separator in a battery, especially those employing leaf or sheet separators.
Method A uses a ruler or a square to measure the height or width to the nearest 0.50 mm
(0.02 in).
5.2.2. The requirements of assembly procedures employing roll stock for enveloping or sleeving
demand more accurate measurement, because of the complexity of those processes. For
those purposes Method B is used. The measuring equipment required for this degree of
precision utilizes a digital micrometer, that provides measurements to the nearest 0.01 mm
(0.0004 in).
5.3. APPARATUS
5.3.1. Method A - Traceable metal scale or square, accurate to 0.50 mm or 1/64 in.
5.3.2. Method B - Traceable digital micrometer assembly similar to drawing Number IIA-1.
Instrument should have an accuracy of a minimum of 0.01 mm (0.0004 in), e.g., Mitutoyo
350-712 or equivalent.
11
BCIS-03B Rev. DEC02
Number 11A-1
5.4. TERMINOLOGY
5.4.1. Height - The dimension of the edge that is parallel to a vertical rib. Height is also called
length. The edge in question is referred to as the end of the separator.
5.4.2. Width - The dimension that is perpendicular to a vertical rib. This edge is referred to as the
side of the separator.
5.5. PROCEDURE
5.5.1. Method A.
5.5.1.1. Using either the traceable scale or square, carefully place measuring unit against the side
edge (height) and end edge (width) and read the scale.
5.5.1.2. Report the height and width to the nearest 0.50 mm or 1/64 in. and that method A was used.
Report the results of each separator measured.
5.5.2. Method B.
5.5.2.1. Place the separator rib side up on the work surface of the digital micrometer assembly. The
ribs must be perpendicular to the measuring axis. (The block can be placed atop a light box
to assist in aligning the edges as required below.)
12
BCIS-03B Rev. DEC02
5.5.2.2. Slide the separator towards the fixed guide, until the side edge of the separator engages it
uniformly.
5.5.2.3. Smooth out any undulations and gently hold both edges of the sample in position. Avoid any
excessive tension or stretching of the material.
5.5.2.4. Adjust the micrometer foot to barely contact the opposite side edge of the sample.
5.5.2.5. Report:
5.5.2.5.1. The width of each separator measured to the nearest 0.1 mm.
5.5.2.5.2. The gauge used and that method B was used.
13
BCIS-03B Rev. DEC02
6. STANDARD TEST METHOD TO DETERMINE THE SKEW OF ROLL STOCK BATTERY

SEPARATOR MATERIAL
6.1. SCOPE
6.1.1. This method measures the degree of curvature along a length of battery separator.
6.2.1. Excess skew can impede the smooth flow of separator material through automatic plate
enveloping.
6.2.2. Excess skew can also cause the separator edges to be offset during plate enveloping. The
misaligned edges can reduce seal quality and lead to shorting if plates of opposite polarity
are exposed and make contact.
6.3. APPARATUS
6.3.1. One stainless steel wall-mounted shelf, 200 cm (78.7 in) in length, with straight edge.
Corners must be at right angles. (See Figure 6.1).
Figure 6.1
6.3.2. Two 15 cm (6 in), “Pony” clamps (model #3202), or equivalent, corresponding to a weight of
180 + 20 g (0.397 lb)
6.3.3. A digital caliper or micrometer that will accurately read out to 0.10 mm (0.004 in). A metal
ruler able to accurately measure to 0.50 mm or 1/64 in. is also acceptable.
14
BCIS-03B Rev. DEC02
6.4. SAMPLE PREPARATION
6.4.1. Cut three (3) separator samples, 300 cm (118 in.) in length.
6.5. PROCEDURE
6.5.1. Place the separator sample with the major ribs’ side up and the convex edge facing the wall
side of the shelf. (See Figure 6.1).
6.5.2. Place a weighted clamp on each end of the separator and let hang freely over both ends of
the shelf.
6.5.3. Bring the separator material to each outside corner of the shelf; be sure the material is lying
down flat.
6.5.4. Shift the separator so the greatest deflection is positioned halfway down the length of the
shelf. Leave at least 25 cm (9.8 in) of separator overhanging each edge of the shelf.
6.5.5. Measure the deflection at a point 100 cm (39 in) down the outside length of the shelf or
maximum curvature. (See Figure 6.1).
6.6. REPORT
6.6.1. Report the individual results of three readings to the nearest mm (in).
15
BCIS-03B Rev. DEC02
7. STANDARD TEST METHOD TO DETERMINE VOLUME POROSITY AND MOISTURE

CONTENT OF BATTERY SEPARATORS
7.1. SCOPE
7.1.1. This method measures both the open volume of the separator relative to the total separator
volume and moisture content of the separator.
7.2. SIGNIFICANCE AND USE:
7.2.1. The pore volume is relevant to both the electrical performance of the battery and the volume
of electrolyte displaced by the separators.
7.2.2. This method (Calculations in Subsection 7.6) is not valid for separators that are less dense
than water.
7.2.3. Moisture content of the separator can be an important variable in the manufacturing of the
battery. Moisture content can effect the specific gravity of the sulfuric acid.
7.3. APPARATUS
7.3.1. Balance, accurate to 0.001 grams, such as a Mettler PM 460 or equivalent.
7.3.2. Density determination kit, per figure No.1, such as Mettler 33360 or equivalent.
7.3.3. Moisture extraction oven, such as Genlab ME/156/HYD or equivalent.
7.3.4. Stainless Steel pan, of sufficient size to hold test specimen and sample holder (See drawing
and Subsection 7.5.4).
7.3.5. Distilled or deionized water
7.3.6. Timer, accurate to + 1 second.
7.3.7. Beakers, 1000 ml and 150 ml.
7.4.1. Cut three separator samples each measuring 40 mm x 70 mm (1.57 in x 2.75 in) (ribs to be
running in the direction of the long dimension).
7.5. PROCEDURE
7.5.1. Weigh and mark each sample accurately to the nearest 0.001 g. Record as W0.
7.5.2. Place the samples in an oven set at 105°C ± 5°C (221°F ± 9°F) until constant weight is
assured (about one hour).
7.5.3. Remove samples from oven and weigh immediately to the nearest 0.001 g. Record as W1.
7.5.4. Secure sample in sample holder, and fully immerse into boiling distilled water for 10-12
minutes, using the stainless steel pan.
7.5.5. Remove sample from the stainless steel pan and immediately remove sample holder.
7.5.6. Place sample into 1000 ml beaker containing distilled water.
16
BCIS-03B Rev. DEC02
7.5.7. Assemble the density determination kit.
7.5.7.1. Place bridge over balance pan.
7.5.7.2. Fill 150 ml beaker with distilled water and place on bridge.
7.5.7.3. Place sample support onto wire frame.
7.5.7.4. Tare the balance to zero.
7.5.8. Remove the sample from distilled water (1000 ml beaker, Subsection 7.5.6). Attach the
sample to the spiral holding device on the sample support.
7.5.9. Ensuring that no air is trapped under the sample, that it is freely suspended (i.e. not touching
the sides of the beaker), and that it is fully immersed, record the weight of the sample
suspended in water. Record as W2. If the sample is not fully immersed add additional water.
7.5.10. Remove the sample from the sample support.
7.5.11. Carefully remove any excess surface water from the sample surface by blotting with paper
towels. Immediately place the sample onto the upper weighing pan of the sample support.
7.5.12. Record the weight of the wet sample in air before any absorbed water evaporates. Record as
W3.
7.6. CALCULATIONS
7.6.1. Porosity is the volume of pores divided by the total external volume of the sample, expressed
as a percentage.
7.6.1.1. Volume of pores = (Wet Weight in air) - ( Dry Weight).
7.6.1.2. Volume of sample = (Wet Weight in air) - (Wet Weight in water).
7.6.1.3. Volume Porosity, % = (W3 - W1) x 100

(W3 - W2)
7.6.1.4. Moisture, % = W0 - W1 x 100

W0
7.6.2. Calculate the percent volume porosity and moisture content for each sample. Report as the
average of three determinations.
7.7. PRECISION AND BIAS
7.7.1. Expected reproducibility is ± 1%.
17
BCIS-03B Rev. DEC02
8. STANDARD TEST METHOD FOR PORE SIZE CHARACTERISTICS BY THE MERCURY

INTRUSION METHOD FOR MICROPOROUS SEPARATORS
8.1. SCOPE
8.1.1. This procedure covers a method of characterizing pore structure of microporous battery
separator using a mercury intrusion porosimeter.
8.1.2. This test procedure does involve hazardous materials ( Mercury and Mercury waste
products). 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, follow the safety requirements as
advised by the equipment manufacturer, and to establish appropriate federal, state and local,
safety and health practices as well as determine the applicability of regulatory limitations prior
to use.
8.2. REFERENCE DOCUMENTS
8.2.1. Instruction Manual, Micromeritics Mercury Intrusion Porosimeter.
8.2.2. Instruction Manual, Quantachrome Mercury Porosimeter.
8.2.3. Instruction Manual, Aminco Mercury Intrusion Porosimeter, Super pressure Inc.
8.2.4. Instruction Manual, PMI Automated Porosimeter, Porous Materials, Inc.
8.2.5. ASTM D2873 The Method for Interior Porosity of PVC Resins by Mercury Intrusion
Porosimetry.
8.3. PRINCIPLE OF TEST METHOD
8.3.1. 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.
8.3.2. 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.
8.3.3. 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 = (-4Γ cos Θ)/p

where d = pore diameter
p = applied pressure
Γ = surface tension of mercury
Θ = contact angle between mercury and pore wall
The pressure required to force mercury into a pore is inversely proportional to the pore
diameter.
8.4.1. Mercury porosimetry is a widely accepted technique of characterizing structure of porous

materials.
18
BCIS-03B Rev. DEC02
8.4.2. The method of test is used to determine properties such as pore diameter, pore size
distribution, and pore volume.
8.4.3. The pore characteristics 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 the pore characteristics. Pore size is a relative term used to
simplify discussion when making comparison between samples of similar materials.
8.5. PRECAUTIONS
8.5.1. Mercury is poisonous. Prevent accumulation of mercury vapor in work spaces through
provision of a 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 a mercury cleaning kit
and/or nitric acid, do so under a well ventilated hood.
8.5.2. Operation of a mercury porosimeter requires high hydraulic pressure. Even though all
porosimeters are equipped with built-in safety features, the operator should observe strict
safety precautions as described in the operating manual.
8.5.3. Spent oil must be handled as mercury waste.
8.6. APPARATUS
8.6.1. Micromeritics Mercury Porosimeter

e.g. Pore Sizer 9320
Auto Pore II 9220
8.6.2. Quantachrome Mercury Porosimeter

e.g. Autoscan - 33 or 60 Porosimeter
8.6.3. Aminco Mercury Porosimeter

e.g. Model J5-7125D, 60K, 5-7107
8.6.4. PMI Automated Porosimeter

e.g. Model No. PMI 30K-A-1
8.7. PROCEDURE
8.7.1. Follow the detailed procedure as described in the instruction manual provided with the
instrument.
8.7.2. A sample weight between 0.1 to 0.7 gram weighed to an accuracy of 0.0001 g is suggested
for commonly available microporous battery separators.
8.8. REPORT
8.8.1. Report the following test conditions:
8.8.2. The instrument used.
8.8.3. The weight of the specimen used.
8.8.4. Values of surface tension, contact angle and density of mercury used.
8.8.5. Report the following test results.
19
BCIS-03B Rev. DEC02
8.8.6. Median Pore Diameter (volume) in μm.
8.8.7. Pore size distribution preferably in the form of a graph showing pore diameter in mm on X-
axis (log scale) and porosity in ml/g on Y-axis.
8.9.1. The precision of this method has not been determined.
20
BCIS-03B Rev. DEC02
9. STANDARD PROCEDURE FOR DIMENSIONAL STABILITY OF SEPARATORS IN

GROUP FORMATION DRY AND WET CHARGE BATTERIES
9.1. SCOPE
9.1.1. This procedure outlines two methods used to determine the degree of dimensional change of
separators used in group formation dry charge (Subsection 9.5) and wet charge (Subsection
9.6) applications.
9.1.2. This procedure uses water that has been acidified to a maximum pH of 3.0 for reason of
safety. While data shows that water will produce larger dimensional changes than sulfuric
acid, using acidified water provides data that is closer to conditions inside the battery.
9.2.1. This procedure is designed to approximate the shrinkage that occurs during battery formation
and life service for separators used in either dry and wet charge battery applications.
9.3. APPARATUS
9.3.1. Hot Plate (capable of boiling water).
9.3.2. 4000 ml stainless steel container or equivalent.
9.3.3. Pyrex dish, 229 mm x 229 mm ( 9 in x 9 in).
9.3.4. Stainless Steel or Teflon Tongs.
9.3.5. Timer (To measure 30 minute intervals).
9.3.6. Hook rule, 0.5 mm ( or 1/64") graduations.
9.3.7. Cutting board.
9.3.8. Perforated spacers and necessary weight or clamps to keep separators submerged in water.
9.3.9. Plastic cover plate ( about 125 mm x 125 mm [4.9 in x 4.9 in]) to hold samples flat.
9.3.10. Safety glasses.
9.3.11. Forced draft oven, minimum temperature of 100°C.
9.3.12. Sulfuric acid acidified distilled or deionized water ( maximum pH of 3.0).
9.3.13. Oven Sample rack ( e.g. test tube rack, VWR Scientific # 60983-007 or equivalent).
9.4. PROCEDURE:
9.4.1. Cut two samples 127 mm x 127 mm ( 5 in x 5 in) from each roll to be tested. Samples must
be cut with ribs parallel to a side. Label the samples for identification.
9.4.2. Apply reference marks at the center of the two adjacent sides of each sample.
9.4.3. Cover the sample with the plastic plate. Apply sufficient pressure to hold samples flat.
21
BCIS-03B Rev. DEC02
9.4.4. Measure the length (Lo ) and the width (Wo) to the nearest 0.1 mm (0.004 in) at the reference
marks (Subsection 9.4.2).
9.4.5. Repeat Subsections 9.4.3 and 9.4.4 for each sample.
9.4.6. Fill the 4000-ml stainless steel container with acidified distilled water. Bring the water to a boil
using the hot plate.
9.4.7. Assemble the samples alternately with the perforated spacers ensuring that the assembly
has a spacer at both ends. Secure assembly lightly with rubber bands. Place this assembly
(all ribs vertical) into the stainless steel container. Cover the assembly with spacer and
weight to keep samples vertically submerged.
9.5. FOR DRY CHARGED APPLICATIONS
9.5.1. Immerse the sample assembly in boiling distilled water bath for 5 minutes + 15 seconds.
NOTE: The sample immersion time starts when the water begins to re-boil.
9.5.2. Remove assembly with the tongs and remove samples from the assembly. Shake off excess
water and immediately place the samples in a forced draft oven set at 93 ± 3oC for 10 ± 0.25
minutes. The samples should be placed in a rack that supports them vertically and separates
them by about 13 mm (0.5 in) before placing them in the forced draft oven.
9.5.3. Remove all samples from the oven and allow to cool. Measure samples as in Subsection
9.4.4. Record the length (LF) and width (WF).
9.6. FOR WET CHARGE APPLICATIONS
9.6.1. Immerse the samples in boiling distilled water bath for 30 + 0.5 minutes.
NOTE: The sample immersion time starts when the water begins to re-boil.
9.6.2. After the 30 minutes of boiling, remove the sample assembly with the tongs. Remove
samples from the assembly. Immediately place samples in Pyrex dish filled with room
temperature distilled water. Immerse the sample for a minimum of 10 minutes.
9.6.3. After the 10 minutes immersion at room temperature, remove the samples with the tongs.
Immediately re-measure sample, as in Subsection 9.4.4. Record the length (LF) and Width
(WF).
9.7. CALCULATIONS
9.7.1. Percent Length Change (PLC) = L F - Lo

_________ x 100
LO
9.7.2. Percent Width Change (PWC) = W F- W o

__________ x 100
WO
9.8. REPORT
9.8.1. Report the PLC and PWC. Shrinkage will yield a negative number. Expansion will yield a
positive number.
9.8.2. Report results as dry charge or wet charge procedure.
22
BCIS-03B Rev. DEC02
10. STANDARD PROCEDURE FOR DIMENSIONAL STABILITY OF SEPARATORS TO AIR

DRYING
10.1. SCOPE
10.1.1. This procedure provides a method to determine the dimensional stability of separators after
being wetted in water and then allowed to air dry.
10.2.1. This procedure is designed to approximate the shrinkage of separators that occurs during air
drying of plates and separators.
10.3. REFERENCED DOCUMENTS
10.3.1. Procedure BCIS-03B-5 Height and Width.
10.4. APPARATUS
10.4.1. Cutting die, 127 mm x 127 mm (5 in x 5 in). If separator is less than 127 mm wide, use the
width of the separator.
10.4.2. 4000 ml stainless steel container or equivalent.
10.4.3. Height and Width gauge. Refer to BCI procedure for Height and Width.
10.4.4. Stainless Steel Tongs.
10.4.5. Timer (To measure 60 minutes interval).
10.4.6. Steel template for setting height gauge to 127 mm (5.0 in).
10.4.7. Perforated spacers and necessary weight to keep separators submerged in water.
10.4.8. Plastic cover plate ( about 125 mm x 125 mm ( 4.9 in x 4.9 in)) to hold samples flat.
10.4.10. Distilled water.
10.4.11. Scale accurate to 0.01 g.
10.5. PROCEDURE
10.5.1. Cut two samples 127 mm x 127 mm (5 x 5 in) from each roll to be tested. Samples must be
cut with ribs parallel to side. Label the samples for identification.
10.5.2. Apply reference marks at the center of the two adjacent sides of each sample. Insert sample
in height and width gauge with an inked reference mark centered on the gauge foot. Make
certain that the base of the separator is squarely against the base plates of the gauge.
10.5.3. Cover the sample with the plastic plate and apply sufficient pressure to hold sample flat
against back plate.
10.5.4. Measure the length (L0) and width (W0) to the nearest 0.1 mm (0.004 in) at the reference
marks (Subsection 10.5.2).
23
BCIS-03B Rev. DEC02
10.5.5. Assemble the samples alternately with the perforated spacers ensuring that the assembly
has a spacer at both ends. Secure assembly lightly with rubber bands.
10.5.6. Fill the 4000-ml stainless steel container with distilled water at 20 ± 3 °C . Do not reuse this
water.
10.5.7. Place the measured, labeled samples (ribs vertical) into the stainless steel container.
Assemble with perforated spacers before putting assembly into the water. Use weights to
keep samples vertically submerged. Cover the container.
10.5.8. Soak the sample for one hour.
10.5.9. After the one hour soak is complete, remove the sample from water and shake off excess
water. Then lay the samples on a flat surface, rib side up. Allow samples to air dry for 2
hours minimum, or until completely dried. This is determined by having no change in the
weight of the separator between measurements that are one hour apart.
10.5.10. After the samples are completely dried, remeasure the dried samples as in Subsection
10.5.4. Record the measurements as Lf and Wf.
10.6. CALCULATIONS
10.6.1. Percent Length Change (PLC) = 100 x (Lf - Lo) / LO
10.6.2. Percent Width Change (PWC) = 100 x (Wf - Wo) / WO
10.7. REPORT
10.7.1. Report the PLC and PWC. Shrinkage will yield a negative number. Expansion will yield a
positive number.
10.7.2. Report results as air dried procedure.
10.8.1. The rate of drying of the separator can influence the values obtained. Repeatability of method
depends on controlling the environment in which the samples are dried.
24
BCIS-03B Rev. DEC02
11. STANDARD TEST METHOD FOR ELONGATION AND TENSILE STRENGTH OF

MICROPOROUS POLYETHYLENE BATTERY SEPARATOR
11.1. SCOPE
11.1.1. This test method describes the use of a constant rate of elongation apparatus to determine
the force per cross sectional area required to rupture a test sample (tensile strength) and the
elongation at maximum force; it may also be used to define the energy absorbed per unit
area of the test sample before breaking -tensile energy absorption (TEA).
11.1.2. This method is suitable for all types of microporous polyethylene battery separators. This
method should not be used for Recombinant Battery Separator Mat (RBSM).
11.2.1. ASTM Standards, D-882-91 "Standard Test Methods for Tensile Properties of Thin Plastic
Sheeting"
11.2.2. British Standard BS 2782.
11.2.3. BCIS-03A-13, Tensile and Elongation of Recombinant Mat
11.2.4. BCIS-03B-3, Backweb Thickness
11.3. TERMINOLOGY (For This Method)
11.3.1. Tensile Strength, the maximum longitudinal stress that the sample is capable of supporting.
11.3.2. Percent Elongation is the maximum tensile strain developed in the test sample before 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 gauge length multiplied by one hundred.
11.3.3. Breakpoint. The point of peak force on the strain/stretch curve, beyond which the force
rapidly diminishes as the separator continues to be stretched.
11.3.4. Tensile Index, the tensile strength in Newtons per meter (N/m) divided by grammage, a
measure of strength per unit weight of material.
11.3.5. Constant-Rate-Of-Elongation Tensile Testing Machine (CRE), a testing machine in which the
rate of an increase of the specimen length is uniform with time.
11.3.6. Machine Direction (MD), refers to the orientation of the separator on a roll; the separator is
unrolled in the machine direction (the direction in which the separator is manufactured).
11.3.7. Cross Direction (CMD or CD), refers to the taking of a sample perpendicular to the MD; i.e.,
across a roll
11.3.8. Tensile Stress, the tensile forces of the test specimen per unit area of the original cross
sectional area.
11.4. SIGNIFICANCE AND USES
11.4.1. The property of tensile strength and elongation is used to decide consistency of quality.
25
BCIS-03B Rev. DEC02
11.4.2. The property of tensile strength and elongation has significance during manufacturing,
especially during the enveloping process. Separators with insufficient tensile could result in
the separator breaking when used in the enveloping process.
11.4.3. The percent elongation shows the ability of the separator to bend and conform to a desired
contour. High elongation suggest a separator with a lot of "spring" or "stretch.” The loss of
elongation is a good indicator of degradation of the separator.
11.5. APPARATUS
11.5.1. Tensile Testing Machine, a constant-rate-of-elongation (CRE) type capable of acting on the
test specimen at a defined rate 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:
11.5.1.1. 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
contact must be perpendicular to the direction of pull so that no sideways stress is applied to
the sample.
11.5.1.2. The rate of separation of the jaws shall be 500 mm/min (20 in/min). The clamping jaws shall
remain parallel to within + 1° for the duration of the test.
11.5.1.3. A load cell should be selected that is suitable for measurements of the samples, typically one
rated at roughly 500 N,(112 lb) maximum capacity. As 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 will result in diminished accuracy for tensile and elongation
measurements.
11.5.1.4. 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 lower accuracy.
11.5.1.5. 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 + 0.1% elongation.
11.5.1.6. An alignment jig may be desirable to simplify 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.
11.5.1.7. 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%.
11.5.2. Cutting Device, a device for cutting test samples of the proper length and width, with straight
parallel sides and a reproducible area, such as a dogbone die or cutting board.
11.6. CALIBRATION
11.6.1. Tensile Tester/Load Cells. These are extremely complex, delicate samples of equipment;
consult the User's Manual for recommendations on method and periodicity of calibration.
11.6.2. 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,” of the cut samples. For separators with ribs the
numbers of ribs on the sample will affect the result.
26
BCIS-03B Rev. DEC02
11.7. SAMPLING AND SAMPLE PREPARATION
11.7.1. Sampling and sample handling is presented here as an incoming goods test for a battery
manufacturer; others using this procedure may wish to modify sampling to fit their different
situations.
11.7.2. Sufficient samples should be taken from a lot of separators to characterize the uniformity of
the lot, typically including at least one sample from each run and set number.
11.7.3. Remove at least two layers of material from the rolls selected, as these outer layers are
susceptible to damage during handling, packaging and shipping.
11.7.4. Using the cutting device, take one sample from each roll to be sampled. The sample should
be large enough to cut the number of specimens needed. Standard specimen size is 25 x
100 mm (1 in x 4 in). The longer dimension denotes the pulling direction.
11.7.5. Samples should be cut to obtain the least number of ribs in the samples. The cut edges of
the sample must be free from nicks or irregularities as these will give false, low readings.
11.8. PROCEDURE
11.8.1. 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.
11.8.2. If possible, prolonged sample storage and/or testing should be carried out in a laboratory with
controlled temperature/humidity levels.
11.8.3. 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 separator being tested. Full-scale sensitivity shall also be set to give
optimum accuracy for the anticipated tensile measurements.
11.8.4. The 25 mm x 100 mm (1 in x 4 in) test strips shall be inserted in the jaws and the clamps set
so that the line contacts are 50 mm ± 2mm (2.0 in ± 0.1 in) apart.
11.8.5. The sample should first be clamped in the upper jaw, and then in the lower jaw after
removing any noticeable slack. Use a clamping pressure satisfactory for the material 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 sample slippage. Be careful not to touch the
sample between the clamping points.
11.8.6. Set the rate of jaw separation at 500 mm/min ± 5 mm/min (20 in/min ± 0.2 in/min). Note: This
method can be used for other types of separators but the rate of jaw separation should be
agreed upon between supplier and user.
11.8.7. 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 the breaking force can be read in
the upper three-fourths of the scale; make preliminary trial tests to decide a full-scale load.
11.8.8. If the test sample breaks within 5 mm (0.2 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
samples for a given sampling are rejected, discard all sample readings and inspect the
apparatus for conformance with specification’s and/or take whatever steps are necessarily to
correct the problem.
27
BCIS-03B Rev. DEC02
11.8.9. 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).
11.9. CALCULATIONS
11.9.1. Tensile strength (nominal) is read directly off the chart by observing the point (breakpoint) at
which the force (curve) decreases rapidly to zero; some instruments provide direct digital
readout of tensile and elongation values. The Tensile strength (nominal) shall be calculated
by dividing the maximum load by the original minimum cross-sectional area of the specimen.
The results are expressed in force per unit area, MPa (lb/in²). The results are reported to
three significant figures.
Note: The ribs will influence the cross sectional area and thus the tensile strength. The use
of backweb thickness only will overstate the actual tensile value.
11.9.2. To calculate the percent elongation from the force/stretch curve, measure the cross head
travel distance to the breakpoint (mm or in), divide by the gauge length of the sample and
multiply by 100. Instruments with digital readouts will give results directly.
11.9.3. For all measurements carried out on a particular lot, set, run or roll, calculate the mean and
standard deviation.
11.10. REPORT
11.10.1. Report Backweb Thickness in mm (in).
11.10.2. Values may be reported for tensile/elongation properties in the machine direction (MD) or
cross direction (CD), or both. Generally, MD values are greater than those for the cross
direction.
11.10.3. Test values should be reported to three significant figures.
11.10.4. Tensile strength is to be reported as MPa (lb/in²) for the mean, standard deviation and range.
Report number of ribs, if any in the test samples.
11.10.5. Elongation values for the mean, standard deviation and range are expressed as percentages.
If a different jaw separation is used, then the separation speed should be recorded.
11.10.6. For each of the above, report all values.
11.10.7. Also report any deviations from the standard test procedure, such as short length or
nonstandard width samples, alternate clamping configurations, nonstandard pull rate or
unusual sampling or conditioning procedures.
11.11.1. Precision
11.11.1.1. No statement can be made on precision based on the test conditions given in this method.
11.11.2. Bias
11.11.2.1. No estimate of bias can be ventured since no standard reference materials exist.
28
BCIS-03B Rev. DEC02
12. STANDARD TEST METHOD FOR TABER STIFFNESS OF LEAF SEPARATORS
12.1. SCOPE
12.1.1. The test is designed to determine separator stiffness of leaf type separators,i.e., glass, PVC,
PE, in the machine and cross-machine direction.
12.1.2. This procedure determines the stiffness by determining the bending moment in gram
centimeters necessary to deflect the free end of a 38 mm (1.5 in) wide vertically clamped
sample 15o from its center line when the load is applied 50 mm (1.97 in) away from the
clamp.
12.2.1. TAPPI'S T-489; Stiffness of paper and paperboard (Taber- type stiffness tester)
12.3.1. Separator stiffness can influence both handling of battery components during assembly
process and resulting battery performance.
12.4. APPARATUS
12.4.1. Taber Stiffness Tester (Teledyne Model 150-B, Type V-5, or equivalent).
12.4.2. Cutting die
12.4.3. 38.1 mm x 38.1 mm (1.5 in x 1.5 in)
12.4.4. 38.1 mm x 70 mm (1.5 in x 2.75 in).
12.4.5. Taber's high sensitivity attachment cat. No. 150-14
12.4.6. Cutting pad
12.5. CALIBRATION
12.5.1. The instrument should be calibrated and the accuracy checked at regular intervals. The
calibration of the instrument should follow manufacturer's instruction. A spring steel test
specimen supplied by the manufacturer is used for calibration purposes.
12.6. SAMPLING
12.6.1. The sample size depends on the stiffness of the separator. The separator is cut to a 38.1±
0.3 mm (1.5 in ± 0.01 in) x 38.1 mm ± 0.3 mm (1.5 in ± 0.01 in) for the medium and low
stiffness separator. An example of a medium stiffness separator is a polyethylene separator.
For the high stiffness separator the specimen size is 38.1 mm ± 0.3 mm (1.5 in ± 0.01 in) x 70
mm ± 1 mm (2.75 in ± 0.05 in). An example of a high stiffness separator is a glass leaf
separator.
12.6.2. Cut five samples to desired dimensions, using the proper die size in both machine and cross
machine direction.
12.6.3. Using the cutting pad to support the sample during cutting, use the die to cut the samples.
Make sure that the samples are perfectly flat before cutting.
29
BCIS-03B Rev. DEC02
12.6.4. For any separator with ribs, cut the sample to assure the least number of ribs on the sample.
12.7. PROCEDURE
12.8. PROCEDURE SETTING UP INSTRUMENT
12.8.1. Connect the tester to a proper power supply.
12.8.2. Set the driving disc to zero on the scale by pushing operative switch.
12.8.3. Level the instrument by adjusting tips on the two front stand legs so that line scribe on
pendulum is directly in line with zero. Tip on rear stand should remain screwed on tight.
12.8.4. Center clamp jaws by turning the clamp screws.
12.8.5. Set up instructions for separator types:
High Medium Low

Test Range, g-cm 10-100 0-10 0-1
Test Length (cm) 5 1 2
Rollers Mounted Down Up *Special
Sample Size (mm) 38.1 x 70 38.1 x 38.1 38.1 x 38.1
Range Weight 0 0 0
10 Unit Compensator Weight No Use Use
Angle of Deflection (degree) 15 15 15
Multiply Scale Indication by 1 0.1 0.01
*High Sensitivity Attachment Cat. No 150-14
Note: If the reading is between 0-10 use a lower test range; if the reading is greater than 100, use a
larger test range.
12.9. SETTING TEST SAMPLE
12.9.1. Insert the test sample between clamp jaws.
12.9.2. Make sure that sample is vertically straight and aligns with center line on clamp jaws.
12.9.3. Check that driving disc is set to zero.
12.10. OPERATION OF EQUIPMENT
12.10.1. With one finger, apply a light pressure to the lever control switch either to the left or right
direction.
12.10.2. Deflect the sample 15° to the left and record reading.
12.10.3. Deflect the sample 15° to the right and record reading.
12.11. REPORT
12.11.1. Report the average of five samples, machine and cross-machine direction in g-cm.
Report range used for the test.
30
BCIS-03B Rev. DEC02
12.12.1. Precision
12.12.1.1. No statement may be made on the precision of this test method for separators, since round
robin testing among laboratories has not been conducted. TAPPI does report in T-489 om -
92 that the repeatability (within laboratory) for the 0-100 g-cm scale is equal to 3-5%, while
the reproducibility (between laboratories) is equal to 9 to 20%. TAPPI is the Technical
Association for Paper and Pulp Industries.
12.12.2. Bias
12.12.2.1. No statement on bias may be made due to the lack of a standard reference material.
31
BCIS-03B Rev. DEC02
13. STANDARD TEST METHOD TO DETERMINE PIN PUNCTURE RESISTANCE OF

BATTERY SEPARATOR USING A MANUAL CHATILLON TESTER
13.1. SCOPE
13.1.1. This method measures the force required to puncture or penetrate the battery separator with
the use of a hand operated Chatillon tester.
13.2.1. Insufficient resistance of a separator to puncture, may contribute to separator damage and
subsequent battery failure.
13.3. APPARATUS
13.3.1. Chatillon Tester Push/Pull Gauge, Model DPP 2.5 kg, mounted on Chatillon Test Stand
Model LTC,or equivalent. Higher range force gauges are suitable, depending on application.
13.3.2. Puncture Tip for Tester, figure 1, Cylindrical Pin with flat Tip. Anvil with a hole size 6.68mm
(0.263 in).
13.3.3. Dial micrometer for backweb thickness measurements as described in BCIS-03B Subsection
3, Backweb Thickness.
13.4.1. Select representative samples. Mark points to be tested.
13.4.2. At marked points measure and record the backweb thickness. Use a gauge with a minimum
precision of 0.01mm or 0.0001 in.
13.5. CHATILLON GAUGE AND STAND SETUP
13.5.1. Lower the platform assembly until it comes to rest at the base of the test stand. Secure the
platform by turning the hand knob. Raise the gauge clamp to the top of the support post and
secure it.
13.5.2. Place the push/pull gauge against the gauge clamp, keeping the longer, narrower end of the
gauge facing down toward the platform.
13.5.3. Insert the support screws through the gauge clamp and tighten until the push/pull gauge is
secure.
13.5.4. Rotate the handwheel to the left until the platform is at its maximum "UP" position.
13.5.5. Loosen the gauge clamp and carefully lower it so that the puncture tip is centered in the
platform hole. The large part of the puncture tip should be just above the platform, yet no
closer than 0.25 mm (0.0098 in). Secure the gauge clamp.
13.6. CALIBRATION
13.6.1. Move the red button on the front of the gauge to the center position.
13.6.2. Screw the flat round tip attachment to the shaft at the top of the gauge (just above the dial
indicator).
32
BCIS-03B Rev. DEC02
13.6.3. Adjust the dial indicator so that the needle is pointing to zero.
13.6.4. Place a known weight of 1.9 kg (4.19 lb) on top of the flat round attachment.
13.6.5. The needle on the dial indicator will move to the left. Use the white scale to measure the
weight or force.
13.6.6. The needle should point to the correct weight ± .025 kg (0.05 lb).
13.6.7. Remove the weight. The needle should return to zero.
13.6.8. If requirements of Subsections 13.6.6 and 13.6.7 are not obtained, recalibrate or replace the
gauge.
13.7. TEST PROCEDURE
13.7.1. Press and move the red button on the front of the gauge to the DOWN position.
13.7.2. Adjust the dial indicator so that the needle points to zero.
13.7.3. Place the sample with ribs facing up on the platform such that the measured backweb/land
area is centered under the puncture tip.
13.7.4. Hold the sample in place using two fingers, one on each side of the platform hole.
13.7.5. Using the other hand, turn the handwheel in 180° turns (½ revolution approximately every
second, or 60 mm/min. (2.4 in/min.) raising the platform, until the puncture tip penetrates the
sample.
13.7.6. Record the dial indicator reading to the nearest 0.025 kg (0.05 lb) and lower the platform.
13.7.7. Push the red button on the front of the gauge back to the MIDDLE position.
13.7.8. Repeat steps 13.7.1 – 13.7.7 until all samples are tested.
13.8. REPORT
13.8.1. Report the following:
13.8.2. The instrument used.
13.8.3. Puncture force: The results of each of ten readings in kg (lb). The results can also be
reported in actual Newtons.
13.9.1. The use of a manual Chatillon Tester has greater within laboratory variation between different
operators than has been experienced with an automatic Chatillon Tester.
33
BCIS-03B Rev. DEC02
FIGURE 13.1: PUNCTURE TIP FOR CHATILLON TESTER
UNF 10-32 4.76 mm (3/16 in)

National Fine Thread tapped (this threads onto gauge)
UNF 10-32 4.76 mm (3/16 in)
34
BCIS-03B Rev. DEC02
14. STANDARD TEST METHOD TO DETERMINE PUNCTURE RESISTANCE OF BATTERY

SEPARATORS USING A TENSILE (INSTRON®) MACHINE
14.1. SCOPE
14.1.1. This method measures the force required to puncture or penetrate the battery separator with
the use of a tensile testing machine.
14.2.1. Insufficient resistance of a separator to puncture, may contribute to separator damage and
potential early battery failure.
14.3. APPARATUS
14.3.1. Tensile testing machine, ie., Instron® Model 1011 or equivalent, with a load transducer 500 N
(112.4 lbf) maximum.
14.3.2. Compression fixture for tensile machine with a 150mm (5.9 in) diameter compression anvil
with a center hole 6.68mm (0.263 in) and a moving crosshead mounted chuck with a flat end
probe 1.90mm (0.075 in) diameter with a 20mm (0.79 in) protruding length. See Figure No.
14.1.
14.3.3. Dial micrometer for backweb thickness measurements as described in BCIS-03B-3, Backweb
Thickness.
14.4.1. Select representative samples. Mark points to be tested.
14.4.2. At marked points measure and record the backweb thickness. Use a gauge with a minimum
precision of 0.01 mm or 0.001 in.
14.5.1. Set the tensile testing machine to "compression" mode.
14.5.2. Set the crosshead speed to 500 mm/minute (20 in/minute).
14.5.3. Check to see that the "load" display is zeroed and reading in Newton (lbf).
14.5.4. Place the sample (rib side up) onto the compression anvil, ensuring that the sample is held
firmly in place and that when the probe is lowered it will be centrally positioned between the
ribs. The anvil should not impinge on the radius corners at the bottom of the ribs.
14.5.5. Take three measurements at three marked points.
14.6. REPORT
14.6.2. The instrument used
14.6.3. Record and report the three readings and/or the average in N (lbf).
35
BCIS-03B Rev. DEC02
14.6.4. Report backweb thickness in mm(in.) if required.
(Not to Scale)
Instron Fixture
Figure No. 14.1
36
BCIS-03B Rev. DEC02
15. TEST VIII - WETTING PROPERTIES PROCEDURE VIIIA - ACID FLOATATION METHOD
15.1. SCOPE
15.1.1. This method tests the wetability of a separator by measuring the time required for sulfuric
acid to wick through the backweb section of the sample separator, when it is placed
horizontally on the surface of the acid.
15.2.1. Separator must wet out thoroughly in electrolyte to function properly in a battery. Electrical
resistance is minimized when all pores are filled with acid.
15.3. APPARATUS AND REAGENTS
15.3.1. A glass or other acid resistant tray of dimensions approximately 150 mm x 150 mm x 50 mm
(6 in x 6 in x 2 in) for a standard test sample, or larger for full size separators. The container
size should be adjusted to provide a sufficient clearance to avoid any acid spillage.
15.3.2. Stopwatch.
15.3.3. Sulfuric Acid, 1.280 ± 0.015 specific gravity (27°C (80°F)). Technical grade.
15.3.4. Cutting board.
15.4. SAFETY
15.4.1. Read and comprehend sulfuric acid safety data sheets and company's safety procedure.
15.4.2. Safety goggles, lab coat and rubber apron must be worn during acid dilution operations. The
glass mixing bottle should be enclosed in a plastic container of sufficient capacity to contain
the solution in case of bottle breakage. To prevent excessive heating, concentrated sulfuric
acid should be added slowly to water with adequate agitation to produce thorough mixing.
The diluted acid is sufficiently corrosive at both ambient and elevated temperatures that
careful handling is necessary to prevent injury or damage. Follow Federal, State, Local
regulations for safe disposal of all chemicals used, including battery acid.
15.5. TEST SPECIMENS
15.5.1. Cut samples to 50 mm x 50 mm (2 in x 2 in) for standard size sample or use a larger size or
full size separator if desired.
15.6. PROCEDURE
15.6.1. Fill tray with sulfuric acid, stabilized at a temperature of 27°C ± 3°C, to a depth of
approximately 25 mm (1 in).
15.6.2. Change acid between each test to avoid contamination which may affect test results,
especially if previous separator samples contained a surfactant which may have leached into
the acid.
15.6.3. Ensure that the test pieces are flat. Any bowing can cause gas entrapment which will void
test results.
15.6.4. Hold the specimen as horizontally as possible, major rib side up, and close to the surface of
the sulfuric acid (10 mm -20 mm).
37
BCIS-03B Rev. DEC02
15.6.5. Drop the specimen onto the surface of the acid and simultaneously start the watch. Avoid
having any edge strike the acid first.
15.6.6. Stop the watch when the top surface of the sample backweb is completely wet with acid.
This is usually noted by a darkening of the surface or no further color change of the backweb.
Note: Some separators have two colors or grey scale changes associated with this test. The
darker color change shall represent the end of test.
15.7. REPORT
15.7.1. Report the wetting time in seconds.
15.7.2. Report any incomplete or spotty wetting.
38
BCIS-03B Rev. DEC02
16. TEST VIII - WETTING PROPERTIES PROCEDURE VIIIB - ACID DROP ABSORPTION
METHOD
16.1. SCOPE
16.1.1. This method defines separator wetability in terms of the time required for a drop of sulfuric
acid to be completely absorbed by the backweb of a separator.
16.2.1. Separator must wet out thoroughly in electrolyte to function properly in a battery. Electrical
resistance is minimized when all pores are filled with acid.
16.2.2. Some separators may have surfactant applied to only one side. These separators will give
different results depending on the side tested.
16.3.1. Automatic burette, three-way, with teflon plug, 10 ml capacity (Kimble 17124F or equivalent)
mounted in burette stand, manual burette or medicine dropper capable of dispensing a 0.05
ml drop.
16.3.2. Support jack with vertical lift to 25 cm (10 in): (VWR Standard Model Cat. #60142-546 or
equivalent).
16.3.3. Stopwatch readable to 0.1 seconds.
16.3.4. Sulfuric Acid, 1.280 ± 0.015 specific gravity (27°C (80°F)). Technical grade.
16.3.5. Acid-resistant covering for support jack.
16.4. SAFETY
careful handling is necessary to prevent injury or damage.
16.4.3. Follow Federal, State, Local regulations for safe disposal of all chemicals used, including
battery acid.
16.5.1. Use a separator test sample of a convenient size.
16.6. PROCEDURE
16.6.1. Place specimen with major ribs down on support jack which is located below the acid
dispensing device.
16.6.2. Raise the support jack so that the backweb of the sample is approximately 10 mm below the
tip of the acid dispensing device. This should be centered between rib locations.
39
BCIS-03B Rev. DEC02
16.6.3. Deliver a single drop (0.05 ml) of sulfuric acid to the sample surface. Immediately start the
stopwatch. The temperature of the acid should be at 25°C ± 3°C (77°C ± 5.4°C).
16.6.4. When the drop is completely absorbed, as evidenced by the disappearance of the shiny
surface of the acid, stop the watch. Record the time.
16.7. REPORT
16.7.1. Report the acid drop absorption time in seconds.
40
BCIS-03B Rev. DEC02
17. TEST VIII - RE-WETTING PROPERTIES PROCEDURE VIIIC - DRY CHARGE PROCESS
SIMULATION
17.1. SCOPE
17.1.1. This test is used to measure the re-wetting properties of leach- proof separators and flat
sheets.
17.2.1. This test simulates a dry charge procedure in which the separators are washed in cold water.
17.3.1. Empty 12 volt battery case or other suitable container.
17.3.2. Constant Temperature water bath at 65°C ± 3°C (149°F ± 5.4°F).
17.3.3. Sulfuric Acid, 1.100 ± 0.005 specific gravity at 26.7°C (80°F).
17.3.4. Sulfuric acid 1.280 ± 0.015 specific gravity at 26.7°C ( 80°F). Technical grade.
17.3.5. Forced draft oven set at 120°C ± 5°C (248°F ± 9°F).
17.3.6. PVC corrugated liners.
17.3.7. Glass trays, 250 mm x 250 mm or larger.
17.3.8. Stop watch.
17.3.9. Perforated pail, 20 liter, for washing, including perforated aluminum spacers to hold samples
vertical and away from the bottom of the washing pail.
17.4. SAFETY
battery acid.
17.5.1. Samples are cut to 140 x 140 mm or the nearest convenient size.
17.6. PROCEDURE
17.6.1. Place 10 separators or flat sheets in each cell of the battery case, separating each with a
corrugated PVC liner.
41
BCIS-03B Rev. DEC02
17.6.2. Fill each cell with approximately 900 ml of 1.100 specific gravity sulfuric acid. Acid must be
21°C ± 3°C (69.8°F ± 5.4°F) when introduced into the cell. Separators must be covered by
the acid.
17.6.3. For each test use clean, fresh acid.
17.6.4. Cover the battery case with heavy gauge polyethylene film and place in a constant
temperature bath at 65°C (149°F), for 2.5 hours.
17.6.5. Following the soak, dump the acid and place the groups of separators with their PVC liners
(separator ribs vertical) into the pail and between the aluminum spacers. The spacers should
hold the separators firmly but not tightly in place. The temperature of the wash water should
be 5°C ± 3°C (42°F ± 5.4°F). The flow rate should be adjusted to approximately 8 liters per
minute. The flow should be delivered by a tube set above the surface of the liquid. Wash the
separators for one hour. Do not wash more than 40 separators at one time. Wash
separators with different wetting systems in different pails.
17.6.6. Remove the washed separators from the pail and dry with rib side up in the forced draft oven
at 120°C ± 5°C (248°F ± 9°F) for 30 minutes.
17.6.7. After drying allow the separators to stand at room temperature for at least 30 minutes. This
allows the separator to reach an equilibrium moisture.
17.6.8. The re-wetting time is measured by carefully dropping the separators onto the surface of an
acid bath and measuring the time in seconds to fully re-wet them per procedure VIII A. Five
separators from each cell are tested in sulfuric acid (1.280 specific gravity) at a temperature
of 26.7°C (80°F), and five separators are tested in the same acid but after the acid is cooled
to -1°C (30.2°F).
17.7. REPORT
17.7.1. Record the time (seconds) to approximately 90% and 100% re-wetting for each separator.
Report the average and range for each acid temperature and percent wet-out.
42
BCIS-03B Rev. DEC02
18. STANDARD TEST METHOD FOR DETERMINING THE ELECTRICAL RESISTANCE OF

BATTERY SEPARATOR USING A PALICO MEASURING SYSTEM
18.1. SCOPE:
18.1.1. This method covers the pretreatment, test conditions, apparatus and procedure for the
measurement of the electrical resistance of battery separators.
18.2. SIGNIFICANCE AND USE:
18.2.1. The electrical resistance (ER) of battery separators is a standard measurement used by
separator and battery manufacturers for quality control purposes.
18.2.2. Separator resistance contributes to the internal resistance of the battery and can directly limit
its electrical output. Battery manufacturers can use the ER measurement as a design tool for
establishing battery performance.
18.2.3. Electrical resistance is affected by the porosity, thickness and tortuosity of the pore structure
of the separator and the temperature and concentration of the electrolyte.
18.2.4. Incomplete wetting or saturation of the pore structure limits the lowest ER value obtainable
from a separator structure. Pretreatment procedures (based on the pore size of separators),
are used to wet the separator adequately before testing.
18.2.5. This test method is intended to give a rapid and repeatable measurement that approximates
the ER value of a separator in a battery.
18.3. APPLICABLE DOCUMENTS:
18.3.1. Lead Acid Batteries, Hans Bode, Wiley, New York, 1977, pp. 73-77.
18.3.2. Sulfuric Acid Material Safety Data Sheet.
18.3.3. Applicable Company Safety Policy and Procedure.
18.4. TERMINOLOGY:
18.4.1. Electrical Resistance (ER) of a battery separator is the unit area resistance the separator
adds to battery electrolyte under standard conditions.
18.4.2. ER Bath is a conductivity cell filled with battery electrolyte and fitted with electrodes and
apertures for creating a uniform ionic current flux through separator samples.
18.4.3. A.C. Resistance Meter or Bridge is a low resistance measuring device for determining the
resistance of the ER bath with and without separator samples.
18.4.4. Aperture Area is the area of the flux window in the ER bath
18.4.5. Polarization is a persistent voltage on the bath electrodes due to impurities in the electrodes
or electrolyte.
18.4.6. Porosity is the percentage of the total volume of the separator occupied by the pore volume.
18.4.7. Pore Size is the mean diameter of the separator pores as measured by mercury intrusion.
18.4.8. Tortuosity is the ratio of the mean pore length with respect to the thickness of the separator.
43
BCIS-03B Rev. DEC02
18.4.9. Saturation is the extent to which the pore volume of the separator is wetted or filled with
electrolyte.
18.4.10. Pretreatment is a conditioning procedure to wet the separator for testing.
18.4.11. Battery Electrolyte is a solution of sulfuric acid and water.
18.5. SAFETY
battery acid.
18.6. APPARATUS
18.6.1. Stainless steel container or equivalent to accommodate the separator test samples.
18.6.2. Distilled or deionized water.
18.6.3. Battery electrolyte at a specific gravity of 1.280 ± .005 at 26.7°C (80°F). Battery grade
sulfuric acid is the minimum acceptable purity to produce this electrolyte. For critical
measurements and comparisons, use reagent grade sulfuric acid.
18.6.4. Hot plate or other heating device suitable to boil water.
18.6.5. Stainless steel screen.
18.6.6. Glass or plastic separator tank for presoaking separators in battery electrolyte.
18.6.7. Interval timer.
18.6.9. Thermometer.
18.6.10. Acid resistant gloves and plastic tongs for handling acid laden separators.
18.6.11. ER bath with a fixed aperture area (5 in² is standard) that puts a uniform current flux through
a fixed area of the separator sample for measurement. A drawing of an ER bath (Palico
model 9000-9100) is included in this procedure.
44
BCIS-03B Rev. DEC02
45
BCIS-03B Rev. DEC02
18.6.12. A.C. resistance meter or bridge (Palico model 9100-2) with sufficient sensitivity and resolution
to measure ± 0.1% change in the ER bath resistance in the presence of potentials generated
in the ER bath.
18.7. TEST SAMPLES
18.7.1. Select samples representative of the separator material to be tested.
18.7.2. Cut the samples to a convenient size that is larger than the fixed area window of the acid
bath. A minimum sample size of 120 mm x 120 mm. (4.7 in x 4.7 in) is recommended.
18.7.3. Mark the samples in a corner away from the test area with acid resistant ink or other
non-invasive means of identification.
18.8. PRETREATMENT OR CONDITIONING PROCEDURE
18.8.1. Soaking Procedure
18.8.1.1. Allow the electrolyte to wick into the sample. Do not exceed the wicking rate when immersing
the separator. As the wicking continues, immerse the wet area of the separator thus allowing
air to escape from the pores of the separator. This is especially important in the 20 minute
ER measurement.
18.8.1.2. At the end of 20 minutes and/or 24 hours, measure the ER of the samples using the
procedure in Subsection 18.10 (Measurement Procedure).
18.8.2. Boiling Procedure
18.8.2.1. Place the samples vertically between stainless steel screens and insert with ribs vertical into
the stainless steel container of boiling distilled water.
18.8.2.2. Boil the samples for 10 minutes. Replace the water after boiling each lot of separators.
18.8.2.3. Remove the samples from the water, remove the screens and remove excess liquid.
18.8.2.4. Immediately immerse in the electrolyte in the separator storage tank (not in the storage
compartment of the ER bath).
18.8.2.5. After soaking for 20 minutes, transfer the samples to the ER bath and measure the ER of the
samples using the procedure in Subsection 18.10 (Measurement Procedure).
18.9. PREPARATION OF THE APPARATUS
18.9.1. Fill the ER bath with prepared battery electrolyte to a level above the aperture opening (12-25
mm below the top of the Palico bath) . Adjust the specific gravity to 1.280 ± .005 at 26.7°C
(80°F). Adjust the bath's temperature to 26.7°C ± 2.2°C (80°F ± 4°F).
18.9.2. Connect electrodes to the resistance meter control unit using acid resistant wire and
hardware.
18.9.3. Turn on the resistance meter control unit and allow the equipment to stabilize for at least 20
minutes. If the meter includes a standard reference resistor (place in "Standby" mode and
"Standard" scaling on the Palico and set to the appropriate resistance range scale for a 0.200
ohm resistor reading), the meter reading should be within ± 0.1% of the value of the resistor
or service will be required.
46
BCIS-03B Rev. DEC02
18.9.4. If available, check the resistance standard for the system outlined in Subsection 18.12.4
(Standardization). If this agrees within ± 1%, proceed to Subsection 18.9 (Preparation of the
Apparatus).
18.9.5. Periodically, or when problems occur or changes are made to the system, test the stability,
polarization, current leakage and standardization using the maintenance procedures set forth
in Step 18.12.
18.10. MEASUREMENT PROCEDURE
18.10.1. Measure the temperature of the electrolyte in the ER bath. If the temperature is not within the
range specified in the table in 8.11.5, the bath temperature must be adjusted.
18.10.2. Remove the pretreated samples from the separator storage tank and insert the samples into
the test area of the ER bath. If the separator has no ribs, non-porous ribs or small ribs typical
of automotive batteries, samples may be inserted one at a time. If the rib height is
pronounced, as in industrial batteries, to prevent fringing effects two samples should be
inserted with the ribs (porous) facing each other and slightly offset.
18.10.3. Tap the separator samples to remove any air bubbles clinging to the surfaces.
18.10.4. Close the gate loosely enough to remove the separator without moving the gate. Measure
the total resistance of the tank and the separators. Record as RT. If the resistance drifts,
wait until the unit fluctuates over the same range and then record the mean value of the
range. For the Palico unit, press the "Reset" switch and then the "Preset" switch until a
reading close to zero is obtained.
18.10.5. Remove the sample and remeasure the resistance of the bath (RC) with no separators.
Important: do not move the gate. For the Palico unit with the "Preset" option, the reading
after removing the separators directly gives the difference (RT-RC) used in the calculations in
Step 18.11.1.
18.10.6. If the Palico uses a "Scaled" setting, the appropriate aperture area is automatically multiplied
times the meter reading. If the unit is in the "Standard" mode, aperture calculations must be
made manually.
18.10.7. Repeat this procedure for the remaining samples.
18.11. CALCULATIONS
18.11.1. Electrical Resistance = (RT - RC) x CF x Aperture Area / no. of separator samples where:
RC is the bath resistance obtained in Step 18.10.5 (Measurement Procedure).
RT is the total resistance of the bath and separators obtained in Step 18.10.4.
CF is the temperature correction factor in 18.11.5
If the Palico uses the "Scaled" setting and the "Preset" feature, the appropriate aperture area
is automatically multiplied times the reading and the calculation is simply:
18.11.2. Electrical Resistance = Meter Reading x CF / no. of separator samples
18.11.3. Units for ER are resistance (ohms or milliohms depending on the resistance scale used) x
2 2 2
area (cm or in depending on aperture units) and are typically reported as units of ohm/cm "
2
or "milliohms/in .
47
BCIS-03B Rev. DEC02
18.11.4. Also to be reported are the pretreatment method used, such as "20 minute soak" or "boiled"
and the aperture size of the ER bath and the number of separator samples tested.
18.11.5. If the bath electrolyte temperature is not 26.7°C (80°F), the ER obtained in Step 18.10.1
should be multiplied by the temperature correction factor from the following table derived from
electrolyte conductivity data in Lead Acid Batteries by Hans Bode.
TEMPERATURE CORRECTION FACTOR
o o
C F (CF)
28.9 84 1.04
28.3 83 1.03
27.8 82 1.02
27.2 81 1.01
26.7 80 1.00
26.1 79 0.99
25.6 78 0.98
25.0 77 0.97
24.4 76 0.96
18.12. TESTING AND MAINTENANCE OF EQUIPMENT
18.12.1. Stability
18.12.1.1. Check the resistance of the ER bath (place Palico resistance unit in “Operate” mode and
“Standard scaling and press “Reset”. Set the appropriate resistance range to give the
maximum meter reading without going over scale.)
18.12.1.2. Agitate the electrolyte to make certain that the temperature and specific gravity are uniform.
18.12.1.3. The bath resistance (RC) should be constant within ± 0.5% at a given temperature and
electrolyte concentration.
18.12.1.4. If readings are inconsistent, proceed to Steps18.12.2 (Polarization) and 18.12.3 (Leakage
Current) for polarization and leakage determination.
18.12.2. Polarization
18.12.2.1. Polarization affects the reading of any resistance measuring system differently and should be
dealt with in the manner dictated by the manufacturer.
18.12.2.2. For the Palico system, place the resistance unit in "Operate" mode and Standard" scaling and
press "Reset".
48
BCIS-03B Rev. DEC02
18.12.2.3. Set the appropriate resistance range to give the maximum meter reading (RC) without going
over scale.
18.12.2.4. Press "Test Offset". If the reading is more than half the RC value in Palico systems made
before 1982 or if the display flashes 8's in systems made after 1982, then the polarization is
too high.
18.12.2.5. If the polarization is above the maximum, allow 30 minutes for stabilization and/or discharge
of the polarization and remeasure.
18.12.2.6. If the polarization persists, the electrolyte must be changed and the electrodes cleaned.
18.12.3. Leakage Current
18.12.3.1. If the ER bath has warped or cracked it can have leakage currents out of the flux field that
may affect the ER value measured. The bath should be checked periodically, whenever the
electrolyte is changed or if the bath is moved by using the following procedure.
18.12.3.2. Insert a thin non-porous sheet of acid resistant solid flexible plastic that has the same
dimensions as the separator samples. Close the gate snugly. Adjust the resistance range of
the meter to obtain the fullest scale reading possible and record as the barrier resistance
(RB). The reading may rise for a while after the gate is closed.
18.12.3.3. Remove the barrier sheet and measure the bath resistance (RC).
18.12.3.4. If the ratio of RC/RB is greater than 0.07, bath maintenance or replacement is required. In
the Palico bath, this ratio may be reduced by sealing the leaks or cracks in the partitions. A
bath with sealed partitions is harder to clean but is more stable electrically and mechanically.
18.12.4. Standardization
18.12.4.1. If available, insert a porous plastic sheet that has been standardized for the ER bath into the
test area and close the slide. Read the bath resistance with the sheet in place (RT).
18.12.4.2. Remove the sheet without moving the slide and read the resistance of the bath (RC) without
moving the slide.
18.12.4.3. The difference between these two readings times the aperture area should be equal to the
measured standard within ± 1% corrected for temperature in Step 18.11.4.
18.12.4.4. On the Palico system, the meter can be set to "Scaled" mode and the "Preset" switch
pressed with the plastic standard in the test area with a closed slide. When the standard is
removed, the reading on the meter should equal the standardized value within ± 1% when
corrected for temperature in Step 18.11.5.
18.12.5. Care
18.12.5.1. The surfaces of the bath should be cleaned with each use to remove spilled electrolyte on
the surfaces and connections.
18.12.5.2. The resistance meter should be located far enough from the acid bath to prevent acid and
fumes from entering its case.
18.12.5.3. The electrolyte should be adjusted to the proper specific gravity with each use and changed
periodically or when polarization contaminants begin to affect the readings.
49
BCIS-03B Rev. DEC02
18.12.5.4. Avoid adding hot electrolyte or mixing concentrated acid in the bath to prevent cracking or
crazing.
18.12.5.5. If the bath must be dried for shipment, storage or other reason, pour the electrolyte out and
refill the bath with water. Allow it to stand for 24 hours. Then drain it and allow it to dry at
room temperature. This will minimize the chance of cracking or crazing.
18.13.1. Repeatability of replicate measurements on the same sample, by a single operator on the
same instrument can result in a range as a percent of the average (based on three different
laboratories) from 1.1% to 6.5%.
50
BCIS-03B Rev. DEC02
19. STANDARD PROCEDURE FOR SEPARATOR DEGRADATION TESTING
19.1.1. Battery separators are exposed to distinctive physical and chemical degradation in battery
service. Significant variations in temperature, electrolyte concentration, overcharge, chemical
impurities, physical stresses and service duration are common. Failure modes of separators
due to physical or chemical degradation are generally unique to the type of separator and
type of battery service. Tests to accelerate degradation by high temperatures and corrosive
chemicals or electrochemical treatments can often lead to failure modes not representative of
and/or disproportional to typical service life. Currently, no definitive test will adequately
define separator degradation.
It is therefore the responsibility of the battery producer and separator manufacturer jointly to
agree on a test method(s) that will accelerate degradation modes normally seen in the
service life of a particular type of battery and separator. BCI offers no sanctioned test
method at this time. However, the following types of tests are being used within the industry.
Sulfuric Acid/Hydrogen Peroxide Oxidation

Sulfuric Acid/Dichromate Oxidation
Overcharge Oxidation
51
BCIS-03B Rev. DEC02
20. STANDARD TEST METHOD FOR ACID EXTRACTION BY ACID REFLUX PROCEDURE
A-1
20.1. SCOPE
20.1.1. This procedure provides a method for extracting acid soluble contaminants from battery
separators by refluxing in sulfuric acid followed by analysis for chlorides, metallic and organic
impurities.
20.1.2. The results will be based on volatile free separator weight.
20.2. APPARATUS
20.2.1. 250 ml Erlenmeyer flask with standard ground glass joint.
20.2.2. Reflux condenser with joint.
20.2.3. Thermostat controlled hot plate.
20.2.4. Balance capable of weighing to an accuracy of +0.25% of applied load.
20.2.5. Sulfuric acid - J.T. Baker, Trace Metal Analytical Grade or equivalent.
20.2.7. Scissors.
20.2.8. 500 ml volumetric flask.
20.2.9. Filter unit with 0.45 micron membrane.
20.3. SAFETY
20.3.1. Read and comprehend sulfuric acid material safety data sheet.
The diluted acid is sufficiently corrosive at both ambient and elevated temperatures and
20.3.3. Follow Federal, State and Local regulations for safe disposal of all chemicals, including
battery acid.
20.4. PREPARATION OF REAGENTS
20.4.1. Sulfuric Acid 1.265 Specific Gravity (s.g.) - put 2 liters of distilled water in a 4 liter Erlenmeyer
flask slowly add 644 ml Sulfuric Acid. Stir, cool to room temperature and adjust specific
gravity. Refer to Subsection 20.3 for acid mixing safety information.
20.5. PROCEDURE
20.5.1. Select a 10.0 g sample of separator material, dry at 100°C-110°C for 1 hour and obtain
sample weight to ± 0.1g. Cut the sample into approximately 0.25 cm x 0.25 cm (0.1 in. x 0.1
in.) squares, including ribs.
52
BCIS-03B Rev. DEC02
20.5.2. Transfer the weighed material to the 250 ml Erlenmeyer flask and add 150 ml of 1.260 s.g.
Sulfuric Acid.
20.5.3. Attach reflux condenser, mount on hot plate, bring rapidly to a boil and adjust reflux rate to 1
drop per second.
20.5.4. Prepare on blank, reflux assembly, as above (20.5.2. – 20.5.3) without separators.
20.5.5. After boiling for 3 hours, remove assembly from hot plate and allow to cool to room
temperature. Note: Cooling under running tap water is permitted.
20.5.6. Filter the solution through the filter unit with the use of the water aspirator.
20.5.7. Wash the flask and sample several times with distilled water and transfer the washings to the
filter unit.
20.5.8. Transfer the filtrate to the 500 ml volumetric flask, washing the filter unit with distilled water,
and dilute to the mark with distilled water.
20.5.9. This extract is now ready for analysis.
53
BCIS-03B Rev. DEC02
21. STANDARD TEST METHOD FOR HOT ACID SOAK - PROCEDURE A-2
21.1. SCOPE
21.1.1. This procedure provides a method for extracting acid soluble contaminants from battery
separators by soaking the separators in hot sulfuric acid for a specified time followed by
analysis for metallic and organic impurities and chlorides.
21.1.2. The ratio of separators to sulfuric acid is based on a typical battery cell. This ratio can be
changed to meet the user's specific needs.
21.2. TERMINOLOGY
21.2.1. Working Reference Material (WRM) is a Quality Control sample which closely matches the
sample's matrix. WRMs provide data for estimating precision and verifying analytical control
when analyzed with each sample batch. The WRM has less stringent characteristics and
stability requirements than Standard Reference Material (SRM).
21.3.1. This procedure is designed and verified specifically to leach soluble oxidizable materials from
battery components in preparation for subsequent analyses. Consult Total Organic Carbon
and/or Trace Element Concentration procedures for respective anticipated analytical range,
precision, and accuracy.
21.4. APPARATUS
21.4.1. Forced draft oven capable of maintaining 77°C + 2°C (170°F + 4°F).
21.4.2. Polpropylene Jars, 950 ml (32 oz) 120 mm screw cap. Condition with simulated analysis.
21.4.3. Funnels, long-stem, 65 mm.
21.4.4. Glass filters, 12.5 cm, no binder.
21.4.5. Glass storage bottles, 236 ml (8 oz) (ground glass or polyseal caps).
21.5. REAGENTS
21.5.1. Sulfuric acid (H2S04) 1.265 + 0.005 specific gravity (27°C (80°F))
21.5.2. Analyte concentrations in blank solution should be 0.33 to 0.1 significant sample analyte
concentrations. Technical grade sulfuric acid with reagent grade distilled or deionized water
is usually acceptable for TOC only analysis. Reagent grade sulfuric acid is advised if trace
metals analysis is to be done.
21.6. SAFETY
21.6.1. Read and comprehend sulfuric acid material safety data sheets.
The diluted acid is sufficiently corrosive at both ambient and elevated temperatures so that
54
BCIS-03B Rev. DEC02
21.6.3. Follow Federal, State and Local regulations for safe disposal of all chemicals used, including
battery acid.
21.7. PROCEDURE
21.7.1. Determine the amount of separator needed to obtain 1345 cm2 (208.5 in2) (one side).
21.7.2. With a paper cutter, cut the separators into 32 mm to 38 mm (1.25 in. to 1.5 in.) wide strips
perpendicular to the ribs.
21.7.3. Place the separator strips on edge in the polypropylene jar. Using a graduated cylinder, add
375 ml of 1.265 specific gravity sulfuric acid.
21.7.4. Screw on the plastic cover and seal tight (electrical tape may be used to seal).
21.7.5. Run a WRM (working reference material*) and blank along with the sample(s).
21.7.6. Place the acid containing sample, WRM, and blank jars in a forced draft oven which has been
set and stabilized at 77°C (170°F).
21.7.7. After 20 hours, remove all jars from oven. Filter warm solutions within 2 hours after removal
from the oven as follows:
21.7.7.1. Filter about 15 ml of sample through a glass filter into a glass storage bottle having a ground
glass or polyseal cap. Rinse bottle thoroughly and discard this sample portion.
21.7.7.2. Filter remaining sample to fill bottle, cap, and reserve for the TOC and trace metal tests.
55
BCIS-03B Rev. DEC02
22. STANDARD TEST METHOD FOR METAL ANALYSIS BY INDUCTIVELY COUPLED

PLASMA EMISSION (ICP) - PROCEDURE C-2
22.1. SCOPE
22.1.1. This procedure provides a method for determining leachable trace metal content in battery
separators. The analyst may select acid leachate from either ACID-EXTRACTION procedure
(A-1 or A-2).
22.1.2. The method described in this procedure utilizes Inductively Coupled Argon Plasma Emission
Spectroscopy (ICP) to determine the level of metallic contamination which is leached from
battery separators.
22.2. REFERENCES
22.2.1. T.J. Schmitt, J.P. Walters, and D.A. Wynn, Appl. Spectrosc. 43,687 (1989).
22.2.2. D.J. Knauer and J.A. Norris, in Methods for Analytical Atomic Spectroscopy, R.A. Storer, Ed.
(ASTM, Philadelphia, 1987), 8th ed., p. 715.
22.2.3. P.W.J.M. Boumans, Line Coincidence Tables for Inductively Coupled Plasma Atomic
Emission Spectroscopy (Pergamon Press, New York, 1980), Vol. 1 & 2, p.1.
22.2.4. M.L. Parsons, A. Forster, and D. Anderson, An Atlas of Spectral Interferences in ICP
Spectroscopy (Plenum Press, New York, 1980), p.10.
22.2.5. R.K. Winge, V.A. Fassel, V.J. Peterson, and M.A. Floyd, Inductively Coupled Plasma-Atomic
Emission Spectroscopy, An Atlas of Spectral Information (Elsevier Science Publishing
Company Inc., New York, 1985), p. 272.
22.2.6. T. Torok, J. Mika, and E. Gegus, Emission Spectrochemical Analysis (Crane Russak, New
York, 1978), p.25.
22.3.1. Range: The range of quantitation and the elemental species determined by the method are
summarized in Appendix I. A total of 35 elements may be quantitatively measured from one
sample.
22.4. SAFETY
22.4.1. The operator must be familiar with the safe operation of the ICP instrument and MSDS's
pertaining to sulfuric acid and standards used for calibration. Always wear lab coat, safety
glasses, and protective gloves. Wash thoroughly when analysis is complete or in the event
contact is made with the acid. Additional information is provided as standard operating
procedures in the appendices.
22.4.2. Follow Federal, State and Local regulations for safe disposal of all chemicals used in this
procedure, including battery acid.
22.5. APPARATUS
22.5.1. An inductively coupled argon plasma emission spectrometer, is used for all analyses.
22.5.2. The sample is aspirated into a high temperature argon plasma ( 8,000°C) where an
emission discharge of the sample is formed. Atoms, excited atoms and ions are produced.
56
BCIS-03B Rev. DEC02
One of the energy forms generated, when the excited atoms and ions return to the ground
state or a lower energy level, is light (UV to visible). This process is known as atomic or ion
emission. Each atom has a characteristic wavelength of light that can be emitted. The
analytical wavelengths are optically separated and focused onto detectors which measure the
intensity of light emitted per unit time. The emission intensity is proportional to concentration.
22.6. CALIBRATION
22.6.1. Calibration Standard Preparation for ICP Analysis
22.6.1.1. Sulfuric Acids - Filename: Acid

See Appendix III for solution series descriptions.
22.6.1.2. Std 5 Multi-Element

STD 5 Multi-element stds 2,3 series stock solution 10.0 ml
Multi-element std 5.5 series stock solution 5.0 ml
Sb (10,000 mg/l) 0.6 ml

Te (1000 mg/l) 5.0 ml
Na (10,000 mg/l) 3.0 ml

Ca (10,000 mg/l) 0.4 ml
Fe (1000 mg/l) 7.0 ml

Mg (1000 mg/l) 7.0 ml
Pb (1000 mg/l) 5.0 ml

Sn (10,000 mg/l) 0.45 ml
Multi-Element Std 1 series stock solution 10.0 ml
Dilute to 100-ml with 30% Sulfuric Acid
Prepare Fresh Daily
22.6.1.3. Std 2
Std 2 "Std 3" (previous) 5 ml
Au (1000 mg/l) 0.05 ml
Pt (1000 mg/l) 0.05 ml
22.6.1.4. Std 1
Std 2 "Std 2" (previous) 15 ml
22.6.1.5. Blank
11% Sulfuric Acid
22.6.2. The polychromator needs to be peaked with 1 ppm Cd before calibration.
22.6.3. A working reference material (WRM) is run by ICP with the samples. No dilution is required.
The dilution factor is 0.91 because the standard concentrations are based on a specific
gravity of 1 g/ml. The WRM contains 9.1 ppm of the following: As, Co, Cu, Fe, Mn, Ni, Sb,
Se, Te, Zn.
22.6.4. Control charts for these elements are used to monitor analysis proficiency.
22.7. REAGENTS
57
BCIS-03B Rev. DEC02
22.7.1. Stock Solutions
22.7.1.1. 11% Sulfuric Acid

Add 110 mL of trace metal free sulfuric acid to 500 ml of ASTM type II water in a 1000-ml
volumetric flask. Let cool to room temperature. Bathing the flask in cold tap water can be
used to speed the cooling process. Dilute to volume with ASTM type II H2O(Refer to ASTM
handbook for details).
NOTE: Adding sulfuric acid to water is a very exothermic reaction. The reaction will be
violent if the acid is added too quickly to water. Significant volumetric errors will occur if
solution is not cooled to room temperature.
22.8. SAMPLING
22.8.1. General Operations
22.8.1.1. All samples are prepared in their respective glassware. Rinse all glassware 3 or more times
with ASTM Type II water before use.
22.8.1.2. All glassware is labeled with dilution factor if applicable. Sample solutions are disposed of
after two days.
22.8.1.3. When done, glassware is rinsed three times with ASTM Type II water and dried.
22.8.1.4. Miscellaneous glassware used for special samples or standards is first soaked in 10% HCI
then 10% HNO3. Then rinse with ASTM Type II water.
22.8.2. Sample Preparation
22.8.2.1. To assure uniform viscosity between samples and standards, all samples should be prepared
according to the following procedure.
22.8.2.2. Using a digital pipette weigh 1.0 ml of the acid to determine the specific gravity (Acid
Extraction procedures A-1 or A-2).
22.8.2.3. Dilute the acid according to the specific gravity determined in 1.1. For 1.265 gravity dilute 4.0
ml to a final 10 ml volume using ASTM type II water. The sample may be analyzed without
dilution when the s.g. is 1.1 g/ml. Dilutions to produce 10ml final volumes for other gravities
are:
(X)(C) = (A)(B)
(X)(C) = (11.0g)(15%)
X = 165
C
X=E
D
110g (0.91) = F
X
X= grams of sample solution.

C= percent of H2SO4 in sample solution determined by the measured specific gravity
and Appendix IId.
A= grams of dilution volume (10ml) of a solution that has 1.10 s.g. (A=11.0g)
58
BCIS-03B Rev. DEC02
B= percent of H2SO4 in a solution that has 1.10 s.g. (B=15%).

D= s.g. of sample solution.
E= volume (ml) of sample solution diluted to 10-ml to make the s.g. 1.10.
F= dilution factor.
Note: The factor 0.91 adjusts the instrument calibration standards which are based on vol to
be based on weight.
22.8.2.4. Use glass and digital pipettes for making dilutions. Remember to add acid to ASTM Type II
water already in the flask. Let solutions cool to room temperature before Step 22.8.2.5.
22.8.2.5. Fill flask to volume mark with ASTM Type II water after the solution has cooled to room
temperature. Record the dilution factor for the sample.
22.8.2.6. Analyze the sample solutions and reference materials for specification elements by ICP.
22.9. PROCEDURE
22.9.1. Quantitative elemental analyses should be performed in accordance with the ICP
manufacturer's recommendations using the standards, reference materials, and prepared
samples described above.
22.9.2. After calibration run the solutions listed below during sample analysis as samples in the order
listed. Some variation of this procedure may be necessary when non-routine samples are
analyzed.
TDBLK, STD4, STD1, WRM'S...5-10 SAMPLES...
Run these at the beginning and at the end of the analysis.
Run STD4 and STD1 in between sample sets.
22.9.2.1. 2nd order calibration is used (except TI).
22.9.3. The polychromator needs to be peaked with 1ppm Cd before calibration.
22.10. REPORTING
22.10.1. Adjustments to measured values must be made for samples that have been diluted.
Q=(M)X(F)
Q=Sample Concentration
M=Measured Concentration
F=Dilution Factor
22.10.2. Compare actual sample concentrations to specification values for the respective elements.
22.11. PRECISION & BIAS
22.11.1. Precision
Instrumental precision in 1-2% RSD for most elements.
22.11.2. Accuracy
Accuracy is determined by analysis of certified and working reference materials (NIST, BCI,
WRM) which are analyzed with the samples.
59
BCIS-03B Rev. DEC02
22.11.3. Interfences
Ba and Pb are not measured by the method because of precipitation as sulfates.
60
BCIS-03B Rev. DEC02
22.12. "APPENDIX 1"
61
BCIS-03B Rev. DEC02
22.13. APPENDIX II
REAGENTS 2
ICP MULTI-ELEMENT STANDARD STOCK CONCENTRATES
Solution Identification Conc. Elements Matrix
Multi-Element STD 1 110 mg/l Si, Mo, Ti, W Tr. HF
600 mg/l S
Multi-Element STD2 100 mg/l Mn, Cd, Ni, Ag, Zn, 3% HNO3
Ba, Cu, Cr, Mg, V, Zr
Multi-Element STD3 100 mg/l Sr, Fe, Co, Ca, Na 3% HNO3
Multi-Element STD 5.5 50 mg/l Be 10% HNO3
250 mg/l B
1200 mg/l AI,P
1500 mg/l As
1700 mg/l Bi, TI
1950 mg/l K
2200 mg/l Se
SINGLE ELEMENT STANDARD STOCK CONCENTRATES

1000 mg/l 10,000 mg/l
Pb, Te, Fe Sb, Na, Ca, Sn
Mg, Au, Pt
62
BCIS-03B Rev. DEC02
23. STANDARD TEST METHOD FOR ATOMIC ABSORPTION SPECTROPHOTOMETER

(AA) PROCEDURE C-1
23.1. SCOPE
23.1.1. This procedure provides a method for determining leachable trace metal content in battery
separators. The analyst may select acid leachate from either acid extraction procedure (A-1
or A-2).
23.2. APPARATUS
23.2.1. Refer to ASTM E885. A corrosion resistant plastic nebulizer is recommended for aspirating
1.265 s.g. Sulfuric Acid matrixes. It should be determined whether any viscosity effects are
present.
23.2.2. Atomic Absorption Spectrophotometer.
23.2.3. Metal ion standards.
23.2.4. Glassware.
23.3. SAFETY
23.3.1. The operator must be familiar with the MSDS's pertaining to sulfuric acid and other reagents
used in this procedure. Always wear lab coat, safety glasses and protective gloves. Wash
thoroughly when analysis is complete or in the event contact is made with the acid or other
reagents.
battery acid.
23.4. PROCEDURE
23.4.1. Analyst is to become familiar with ASTM E885 procedure.
23.4.2. Select leachate sample from ACID EXTRACTION procedure A-1 or A-2, analyst's choice.
23.4.3. Follow procedure outlined in ASTM E 885.
63
BCIS-03B Rev. DEC02
24. STANDARD TEST METHOD FOR TOTAL ORGANIC CARBON (TOC) PROCEDURE
D-1
24.1. SCOPE
24.1.1. This procedure provides a method for determining leachable trace total organic content in
battery separators. The analyst may select acid leachate from either ACID EXTRACTION
procedure (A-1 or A-2).
24.2.1. Instrument operator manual, Dohrmann DC-80 Total Organic Carbon analyzer. Rosemount
Analytical Inc., Dohrmann, Division Santa Clara, CA
24.3.1. Instrument Range

1 to 1000 μg/ml, but range may be extended by changing loop size or by dilution. Most
H2S04 samples will be between 4 and 300 μg/ml.
24.4. APPARATUS
24.4.1. Instrument
24.4.1.1. Total Organic Carbon Analyzer with Auto Sampler.
24.4.1.2. The organic carbon analyzer pumps a sample aliquot into a reactor (see schematic Appendix
1). Organic compounds are oxidized to CO2 by a potassium persulfate solution and UV light.
The CO2 is swept from solution and through an infrared detector with an O2 stream. The IR
signal is Integrated and compared to that from a standard by the control module. The result
is printed in microgram of carbon/ml.
24.4.1.3. Instrument modifications may be necessary to establish baseline stability.
- Sample loop may require adjustment to 140 microliters.

- Insert SO3 trap between reactor and detector in addition to the permeation tube to
remove water vapor. Insert the tin or copper trap to remove chlorine.
24.5. REAGENTS
24.5.1. Reactor Solution

40.0g K2S208 (reagent grade potassium persulfate), 300 microliters H3PO4 dilute to 2 liters
using lowest carbon content H2O available.
24.5.2. Calibration Solution

0.850g dry potassium hydrogen phthalate, 100 microliters H3P04 dilute to 1 liter using the
lowest carbon content H20 available.
24.5.3. Control Solutions
24.5.3.1. 200 microliters (40 micrograms/ml) of glacial acidic acid in 2 liters of 1.265 s.g. sulfuric acid.
24.5.3.2. 1 ml (200 micrograms carbon/ml) glacial acetic acid in 2 liters of 1.265 s.g. sulfuric acid.
24.6. SAFETY
64
BCIS-03B Rev. DEC02
24.6.1. Analyst is to become familiar with the safe operation of the instrument and MSDS's pertaining
to sulfuric acid and standards used for calibration. Always wear lab coat, safety glasses and
protective gloves. Wash thoroughly when analysis is complete or in the event contact is
made with the acid.
24.6.2. Follow Federal, State and Local regulations for safe disposal of all chemicals used in this
procedure, including battery acid.
24.7. PROCEDURE
24.7.1. Select leachate sample from ACID EXTRACTION procedure A-1 or A-2, analyst's choice.
24.7.2. Calibrate instrument with potassium hydrogen phthalate solution to 400 micrograms/ml.
24.7.3. Analyze Samples
24.7.3.1. Fill test tubes:
- Standard at beginning and end of batch.

- Control solution every 5 samples.
- Last test tube in H2O to rinse system.
24.7.3.2. Start autosampler.
24.7.4. Quality Control
24.7.4.1. Oxidizing Strength of Reactor Solution

Analyze a control solution containing acetic acid. Acetic acid is difficult to oxidize and
commonly found in separator leach acid.
24.7.4.2. Observe Baseline

Failure of the unit to returnable baseline(time out error) is indicative of low oxidizer strength
poor pumping or failed SO3 trap.
24.7.4.3. Calibration
Standards should be within 400 ± 10 microgram carbon/ml and control solutions should not
exceed the greater of ±6% or ±3 microgram/ml.
Precision
Acetic Acid in 4.5M H2SO4
Separator WRM
Control Solution (Ref.) 24.5.3.1 24.5.3.2
n 30 33 21
X, microgram/ml 54.0 217.9 191
S, microgram/ml 1.1 4.1 10
CB95 2.3 8.4 21
CB95 = 95% confidence interval
65
BCIS-03B Rev. DEC02
24.8.1. Accuracy
24.8.1.1. Accuracy is a function of sample preparation, calibration, instrument repeatability and

oxidation efficiency. For acids, expect the greater of ±6% or ±3 microgram/ml.
24.8.2. Interference
24.8.2.1. Chloride concentration above 0.1% reportedly produce low results, see manual Appendix B.
24.8.2.2. Polymeric materials may be difficult to oxidize, produce low results and increase background
for subsequent samples. This is not expected to be a problem for the separator application.
66
BCIS-03B Rev. DEC02
25. STANDARD METHOD FOR CHLORIDE ANALYSIS IN SULFURIC ACID BY ATOMIC

ABSORPTION SPECTROPHOTOMETER (AAS)
25.1. SCOPE
25.1.1. This procedure provides a method to determine the leachable chlorides from battery
separators by the use of an Atomic Absorption Spectrophotometer (AAS). In the procedure,
known amounts of silver standards are reacted with the sample. Essentially all chloride is
precipitated out and then removed either with a vacuum filter or a centrifuge. The final silver
concentration is determined by AAS. Using the method of standard additions, adapted for
this procedure, the total amount of silver lost is determined. This concentration is converted
to chloride in the sample using standard stoichiometric and dilution factors.
25.2.1. Hockgesang, Frank P., in “Treatise on Analytical Chemistry”, Pt. I, V.5, Ch.63, I.M. Kolthoff &
P.J. Elving eds., Interscience, NY, 1964.
25.2.2. BCI Standard Test Method to Determine Chlorides In Sulfuric Acid By Turbidimetry, BCIS-
03B Subsection 26.
25.2.3. BCI Standard Test Method to Determine Elemental Chlorine in Sulfuric Acid Solution by
Inductively Coupled Argon Plasma Optical Emission Spectroscopy (ICP/OES). BCIS-03B
Subsection 33.
25.2.4. BCI Standard Test Method for Chloride by Potentiometric Chloride Determination in Aqueous
Extracts. BCIS-03B Subsection 34.
25.2.5. BCI Standard Test Method for Chlorides by Ion Selective Electrode (ISE). BCIS-03B
Subsection 27.
25.2.6. BCI Standard Test Method For Acid Extraction By Acid Reflux. BCIS-03B Subsection 20.
25.3.1. Soluble chloride in the electrolyte of the battery can increase the rate of positive grid
corrosion and can increase the solubility of the active material in the sulfuric acid.
25.3.2. This is one of five BCI methods for the determination of soluble chloride in battery separators.
This method may provide different results than the other BCI Chloride methods.
25.3.3. As indicated in the “Apparatus” list, only Type I (also called Class I or nanopure) water may
be used. This water is defined as that having had a specific resistance of 18 MΩ-cm or
greater. Commercially available, bottled distilled water is not acceptable because it may not
meet the necessary guidelines (these distilled waters may be no better than Type III, defined
as water having 0.1MΩ-cm or greater specific resistance—although ASTM has a different
definition). Such water usually has enough chloride to cause problems.
25.3.4. Cleanliness is crucial when testing for chlorides. The results of the analysis will be
dependent upon suitable laboratory practice to avoid chloride contamination. Rinse all
glassware with Type I water while wearing powder-free laboratory gloves. The powder-free
gloves are necessary to avoid contaminating the glassware with the high levels of chloride
found on human skin and in some kinds of powdered gloves. DO NOT wash glassware with
bare hands to avoid serious contamination. Furthermore, detergents of any kind may not be
used because they tend to be high in chloride. Depending on what glassware gets
contaminated, such interferences can be either positive or negative.
67
BCIS-03B Rev. DEC02
25.3.5. All glassware must be acid washed in dilute H2SO4 (2-hour soak with pH < 2) as part of the
cleaning procedure. This dilution must be made with Type I water.
25.3.6. Other halides or materials that precipitate silver will cause a positive interference with the
method.
25.3.7. Report all results as μ m /ml (mg/l)
25.3.7.1. The term μm/ml and μg/g are equivalent only if the specific gravity is 1.0.
25.3.7.2. To convert from μg/g to μg/ml use the following formula: μG/ml = (μg/g)/(S) (where 'S' is the
specific gravity)
25.3.7.3. To convert from μg/ml to μg/g use the following formula: μg/g = (μg/ml)/S
25.4. APPARATUS
25.4.1. All containers must be glassware. (Plasticware may cause problems.)
25.4.2. All volumetric glassware must be equivalent to Class A as defined by NIST circular 602.
25.4.3. Three 100 ml volumetric flasks (Pyrex).
25.4.4. 1- 200 ml volumetric flask (Pyrex).
25.4.5. 1- 1000 ml volumetric flask (Pyrex).
25.4.6. 1- 1 ml pipet.
25.4.7. 2- 2 ml pipets.
25.4.8. 2- 5 ml pipets.
25.4.9. 1- 10 ml pipet.
25.4.10. 1- 20 ml pipet.
25.4.11. 1 Centrifuge or vacuum filtration unit with 0.45 μm glass-fiber filter paper.
25.4.12. 50 ml glass centrifuge tubes (quantity needed varies).
25.4.13. 1- 1000 ml graduated cylinder.
25.4.14. 1- 4000 ml Erlenmeyer flask.
25.4.15. 1 Hydrometer with 1.265 S.G. in range.
25.4.16. 1 Atomic absorption spectrophotometer with associated equipment and supplies.
25.4.17. 1 Ag lamp.
25.4.18. Nitric acid, HNO3. Trace metal analysis grade.
25.4.19. Sulfuric acid, H2SO4. Trace metal analysis grade.
68
BCIS-03B Rev. DEC02
25.4.20. 1000 mg/l (ppm) AAS Silver Standard.
25.4.21. Type I water. Substitutes are not allowed. See Subsection 25.3.3.
25.5. SAFETY
25.5.1. The operator must be familiar with the MSDS’s pertaining to H2SO4 and other reagents.
Always wear lab coat, safety glasses and protective gloves. Wash thoroughly when analysis
is complete or in the event contact is made with the acid.
25.5.2. As listed under Step 25.6.1, H2SO4 must be diluted under constant agitation (e.g. a stir plate)
and under a fume hood. Failure to stir while adding H2SO4 to water will create a strong
thermal gradient that could break the glass, severely injuring the analyst. Using the fume
hood is necessary because H2SO4 liberates harmful fumes when diluted. The glass mixing
bottle must be enclosed in a plastic container of sufficient capacity to contain the acid in case
of bottle breakage.
battery acid.
25.6. PREPARATION OF REAGENTS
25.6.1. Sulfuric acid 1.265 specific gravity (S.G.) as follows: To two (2) liters of Type I water in a four
liter Erlenmeyer Flask (under constant agitation with a stirbar and stirplate and under vacuum
hood), SLOWLY add 644 mL of concentrated H2SO4 in approximately 100 mL aliquots. This
step is dangerous and extreme caution must be used. After the acid has cooled to room
temperature, verify that the specific gravity is 1.265 with an appropriately scaled hydrometer.
(If adjustments are needed, add H2SO4 to increase the S.G. and Type I water to lower it.)
This procedure is that of Subsection 20.4.1 in BCIS-03B Subsection 20: Standard Test
Method for Acid Extraction by Acid Reflux.
25.6.2. Silver standard 10.00 ppm. Pipette 2.00 mL silver standard of 1000 ppm into a 200 mL
volumetric flask and add 2 mL HNO3. Dilute to mark with Type I water. Mix well.
25.7. PROCEDURE
25.7.1. For each sample, label three 100mL volumetric flasks with sample name on each flask. On
one flask write “1”, on the second “1.5” and on the third “2”.
25.7.2. Add about 50 ml of Type I water into each of the flasks.
25.7.3. Pipet 5.00 ml of the acid extract obtained from BCI Standard Test Method for Acid Extraction
by Acid Reflux, Subsection 20.5.9 into each of the flasks. Alternate volumes may be used,
but must be precisely measured.
25.7.4. Pipet 1.00 ml HNO3 into each flask.
25.7.5. Pipet 10.00 ml of the 10.00 ppm silver standard into flask “1”, 15.00 ml into flask “1.5” and
20.00 ml into flask “2”.
25.7.6. Dilute to volume with Type I water.
25.7.7. Stopper flasks and mix thoroughly by inversion. Place samples in a dark place. Every 15
minutes repeat the mixing by inversion. Allow at least two hours for reaction to complete. A
stirplate may be used—at low speed with samples protected from excess light—for two
69
BCIS-03B Rev. DEC02
hours. In both cases, this is a reaction to completion: longer periods of time may be needed.
Allowing the reaction to sit overnight is acceptable.
25.7.8. After the reaction is complete, determine whether the solutions are visibly turbid. If they are,
filter them through Whatman™ 541 filter paper or equivalent. However, if the samples are
highly turbid (milk-colored) then there is too much chloride and the test must be repeated
using a smaller amount of sample.
[Note: All three flasks for each sample should appear to have the same turbidity. A major
difference suggests that there was too much chloride in the sample or that there was
contamination. In either case, the experiment has failed and must be repeated using cleaner
apparatus or less sample volume, whichever is appropriate.]
25.7.9. Place aliquots in centrifuge tube and centrifuge for not less than 15 minutes. Alternately,
where available, the samples may be vacuum filtered (in order of increasing silver
concentration) through pre-rinsed and dried 0.45 μm glass-fiber filter paper. The latter
provides better precipitate separation; however, it requires the most extreme cleanliness.
25.7.10. Analyze the samples with an AA spectrophotometer in absorbance mode—it is not necessary
to calibrate the AA other than properly zeroing it. If these absorbances are outside the linear
range, use a shorter burner head or other standard technique to decrease sensitivity. Use
the laboratory’s standard operating procedure for AA. Obtain at least three readings for each
sample. [While running the AA, it is advisable to verify the intermediate silver standard with
a second-source quality control, using appropriate AA methods.]
25.8. CALCULATIONS
25.8.1. Perform a linear regression on the samples, with the labeled concentration being “x” and the
absorbance being the “y” value. Do not include any blank readings in the calculation. A
correlation coefficient of 0.99 or better should be achieved. If it is less than 0.98, then the
procedure has failed and must be repeated.
[Note that a point-to-point line graph may not be substituted for the regression due to
precision and accuracy loss.]
25.8.2. Find the x-intercept (not the y-intercept). If the x intercept is less than zero, then the
procedure has failed and must be repeated. This value is the decrease in the silver
concentration due to chloride.
25.8.3. Convert the silver loss to chloride in the original extract as follows:
25.8.3.1. Let C= concentration of chloride in the original extract, in ppm.
25.8.3.2. Let V= the volume of the sample used in Step 7.3.
25.8.3.3. Let A= silver loss as determined above, in ppm.
25.8.3.4. C = A(35.453)(100) = (32.867)(A)

V (107.868) V
25.9. REPORT
25.9.1. The Chloride content in μg/mL.
25.9.2. The BCI Method, leaching procedure and instrument used.
70
BCIS-03B Rev. DEC02
26. STANDARD TEST METHOD TO DETERMINE CHLORIDES IN SULFURIC ACID BY

TURBIDIMETRY
26.1. SCOPE
26.1.1. This procedure provides a method for determining the leachable chlorides from battery
separators by the use of turbidimetry. The chloride content of a separator is leached into
1.265 S.G. sulfuric acid. Then the solution is reacted with silver nitrate to form a turbid
suspension of silver chloride. The turbidity of the suspension is measured in a turbidimeter,
which is then correlated, to concentration with an empirical calculation.
26.1.2. Chloride at low concentration (<20 ppm) forms a turbid suspension with the silver nitrate in
the H2SO4 solution. Silver chloride above this concentration will not provide a stable
suspension and the correlation between concentration and turbidity will drop.
26.1.3. Because turbidity (nucleation and particle growth) is dependent on time, temperature, pH and
sample motion these parameters consistently must be controlled.
26.1.4. In turbidimetry, light passes through a sample and is scattered by suspended particles. The
amount of light scattered at 90 º to the beam (proportional to turbidity present) is received by
a photomultiplier tube and the signal displayed on the meter.
26.1.5. Bromide and iodide ions will also form precipitates with silver ions, giving a positive
interference. Foreign particulate matter or color also interferes.
26.2.1. Hockgesang, Frank P., in ‘Treatise on Analytical Chemistry’, Pt. 1, V.5, Ch. 63, I.M. Kolthoff
&P.J. Elving Eds, Interscience, NY, 1964.
26.2.2. Instrumental Manual, Hach Chemical Co., Loveland, CO.
26.2.3. BCI Standard Test Method for Chlorides by Ion Specific Electrode, BCIS-03B Subsection 27.
26.2.4. BCI Standard Test Method for Chloride Analysis by Atomic Absorption Spectrophotometer
(AAS), BCIS-03B Subsection 25.
26.2.5. BCI Standard Test Method for Acid Extraction by Acid Reflux, BCIS-03B Subsection 20.
26.2.6. BCI Standard Test Method for Acid Extraction by Hot Acid Soak, BCIS-03B Subsection 21.
26.3. SIGNIFICANCE & USE
26.3.1. Soluble chloride in the electrolyte of the battery can increase the rate of positive grid
corrosion and can increase the solubility of the active material in the H2SO4.
26.3.2. This is one of three BCI methods for the determination of soluble chloride in battery
separators: the user should determine if this procedure simulates the conditions in the battery
under consideration. This method may produce different results than the other BCI Chloride
methods.
26.3.3. As indicated in the “Apparatus” list, only Type I (also called Class I or nanopure) water may
be used. This water is defined as that having a specific resistance of 18 MΩ-cm or greater.
Commercially available, bottled distilled water is not acceptable because it may not meet the
necessary guidelines (these distilled waters may be no better than Type III, defined as water
71
BCIS-03B Rev. DEC02
having 0.1 MΩ-cm or greater specific resistance—although ASTM has a different definition).
Such water usually has enough chloride to cause problems.
dependent upon suitable laboratory practice to avoid chloride contamination. Rinse all
glassware with Type I water while wearing powder-free laboratory gloves. The powder-free
gloves are necessary to avoid contaminating the glassware with the high levels of chloride
found on human skin and in some kinds of powdered gloves. DO NOT wash the glassware
with bare hands to avoid serious contamination. Furthermore, detergents of any kind may not
be used because they tend to be high in chloride. Depending on what glassware gets
contaminated, such interferences can be either positive or negative.
26.3.5. All glassware must be acid washed in dilute H2SO4 (2 hour soak with pH < 2) as part of the
cleaning procedure. This dilution must be made with Type I water.
26.3.6. Report all results as μg/ml (mg/L)
26.3.6.1. The terms μg/ml and μg /g are equivalent only if the specific gravity is 1.0.
26.3.6.2. To convert from μg /g to μg/ml use the following formula: μg/ml = (μg /g)( S) (where ‘S’ is
the specific gravity)
26.3.6.3. To convert from μg/ml to μg /g use the following formula: μg /g = (μg/ml)/
26.4. APPARATUS
26.4.1. All reagents must conform to ACS reagent grade specifications.
26.4.2. Water must be Type 1. Substitutes are not allowed. See Subsection 26.3.3.
26.4.3. Nitric Acid, HNO3
26.4.4. Silver Nitrate, AgNO3
26.4.5. Sodium Chloride, NaCl
26.4.6. Sulfuric Acid, H2SO4
26.4.7. Gelex Standard solutions; 0-l, 0-10, 0-100 and 0-1000 NTU
26.4.8. All containers must be glassware. (Plasticware may cause problems.)
26.4.9. All volumetric glassware must be equivalent to Class A as defined by NIST circular 602.
26.4.10. Volumetric flasks - 100 ml.
26.4.11. Volumetric flasks - 500 ml.
26.4.12. 4 liter Erlenmeyer flask.
26.4.13. 1- 1 ml pipet.
26.4.14. 1- 2 ml pipet.
26.4.15. Balance, capable of weighing 5.000g.
72
BCIS-03B Rev. DEC02
26.4.16. Turbidimeter 2100 A. Hach Chemical Co., Loveland, CO or equivalent.
26.5. SAFETY
26.5.1. The operator must be familiar with the MSDS’s pertaining to H2SO4 and other reagents.
is complete or in the event contact is made with the acid.
26.5.2. As listed under Step 26.6.5, H2SO4 must be diluted under constant agitation (e.g. a stir plate)
and under a fume hood. Failure to stir while adding H2SO4 to water will create a strong
thermal gradient that could break the glass, severely injuring the analyst. Using the fume
hood is necessary because H2SO4 liberates harmful fumes when diluted. Enclose the glass-
mixing bottle in a plastic container of sufficient capacity to contain the acid in case of bottle
breakage.
battery acid.
26.6. PREPARATION
26.6.1. Samples are aliquots of separator leaching/extracting solution from either BCI Standard Test
Method for Acid Extraction by Acid Reflux BCIS-03B Subsection 20 or BCI Standard Test
Method for Hot Acid Soak BCIS-03B Subsection 21.
26.6.2. A blank of the leaching solution must be run with each batch of samples to verify a low or
chloride-free background.
26.6.3. Gelex standards or equivalent are used to calibrate the turbidimeter. Standards are available
for ranges of 0-1, 0-10, 0-100 and 0-1000 NTU.
26.6.4. Calibration of the turbidimeter is in accordance with manufacturer’s instructions.
26.6.5. Sulfuric Acid 1.265 specific gravity (S.G.) as follows: To two (2) liters of Type I water in a 4 L
Erlenmeyer flask (under constant agitation with a stirbar and stirplate and under vacuum
hood). SLOWLY add 644 ml of concentrated H2SO4 in approximately 100 ml aliquots. This
step is dangerous and extreme caution must be used. After the acid has cooled to room
temperature, verify that the specific gravity is 1.265 with an appropriately scaled hydrometer.
(If adjustments are needed, add H2SO4 to increase the S.G. and Type I water to lower it.)
This procedure is that of Subsection 20.4.1 in BCIS-03B Subsection 20: Standard Test
Method for Acid Extraction by Acid Reflux.
26.6.6. To prepare a 1% silver nitrate solution, weigh out 1.0 gram silver nitrate. Transfer to 100 ml
volumetric flask. Add about 75 ml Type I water and 1.00 ml nitric acid. Swirl to dissolve the
silver nitrate. Dilute to volume. Mix well.
26.7. PROCEDURE
26.7.1. Transfer approximately 5 g of sample weighed to the nearest mg to a 100 ml volumetric flask.
A blank must also be run.
26.7.2. Pipette 2.00 ml concentrated HNO3 to flask and swirl to mix.
26.7.3. Add 1.265 S.G. H2SO4 to bring the volume up to approximately 95 ml.
26.7.4. Pipette 2.00 ml of the 1% silver nitrate solution to the flask and dilute to the mark with the
1.265 S.G. H2SO4
73
BCIS-03B Rev. DEC02
26.7.5. Stopper the flask and mix well by inverting about 10 times.
26.7.6. Rinse the sample cell with the sample solution two times.
26.7.7. Fill the cell to the 25 ml mark; wipe free of fingerprints, dust and lint, and then place the cell in
the turbidimeter to incubate for 30 minutes. (Note: meter should be set at 1000).
26.7.8. After 30 minutes replace the sample cell with the 100-Range NTU standard and standardize
by switching over to the 100 scale and setting the meter to read the indicated value on the
standard with the standardize knob.
26.7.9. Switch back to the 1000 scale and replace the standard with the sample.
26.7.10. Switch to the 100 scale to read the sample and switch back to the 1000 scale. If reading is
too low, per instrument operating manual, recalibrate to a lower NTU standard and repeat
steps 26.7.8 and 26.7.9, except using the lower standard and not waiting an additional 30
min.
26.7.11. Repeat calibration and sample reading.
26.8. CALCULATION
26.8.1. Where only approximate values are needed the following empirically-derived formula may be
used.
26.8.1.1. Let A=NTU instrument reading.
26.8.1.2. Let B= sample weight in grams
26.8.1.3. The Chloride content, ppm = (A x 3.6 µg Cl/NTU)

B
26.8.2. Report the chloride content in ppm and state the method used for extraction.
26.8.3. Where more accurate data are needed consult the modifications in Appendix A.
26.9.1. Range: The normal working range for the method is 0.1 to 12 ppm Chloride in 1.265 S.G.
H2SO4 sample. In this procedure, samples are diluted by 1:20 to bring them into range.
26.9.2. Precision: Repeated analyses of a working reference material (WRM) in 1.265 S.G. H2SO4
was done.
26.9.3. WRM 86-01 gave these results:

n= 191
x = 45.2 ppm
s = 2.7 ppm; 95% conf, int =±5.3 (RSD = 12%)
True value = 48.0 ppm Cl
26.9.4. Accuracy: With one determination, the precision of the method and the cleanliness of the
analyst to avoid chloride contamination of the equipment used limit accuracy.
27. STANDARD PROCEDURE TO DETERMINE CHLORIDES BY ION SPECIFIC ELECTRODE
27.1. SCOPE
74
BCIS-03B Rev. DEC02
separators by Ion Specific Electrode. The exact protocol should follow specific instructions
based on the electrode and equipment used. The specific calibration of the electrode and
standards are dependent on specific manufacturers instructions.
27.2.1. Hockgesang, Frank P., in “Treatise on Analytical Chemistry”, Pt. I, V.5, Ch.63, I.M. Kolthoff &
27.2.2. BCI Standard Test Method for Chloride Analysis By Atomic Absorption Spectrophotometer
(AAS), BCIS-03B Subsection 25.
27.2.3. BCI Standard Test Method To Determine Chlorides In Sulfuric Acid By Turbidimetry, BCIS-
03B Subsection 26.
27.2.4. BCI Standard Test Method To Determine Elemental Chloride in Sulfuric Acid Solution by
Inductively Coupled Argon Plasma Optical Emission Spectroscopy (ICP/OES), BCIS-03B
Subsection 33.
27.2.5. BCI Standard Test Method for Chloride by Potentiometric Chloride Determination in Aqueous
Extracts, BCIS-03B Subsection 34.

dependent upon suitable laboratory practice to avoid chloride contamination.
27.3.2. This is one of five BCI methods for the determination of soluble chloride in battery separators.
Each method may provide different results, and the comparison of results from different
methods should be used with caution. This method could have more variance between
instruments, due to different instruments, electrodes or make-up procedure required for the
electrode used. Variability among these methods are due to different sample size, solvent
systems used in procedure, and extraction conditions.
27.4. APPARATUS
27.4.1. Reagents
27.4.1.1. All reagents must conform to ACS reagent grade specifications.
27.4.1.2. Water must be deionized and distilled (Class 1).
27.4.1.3. Nitric acid
27.4.1.4. Chloride standard, 100 ppm
27.4.1.5. Ionic Strength Adjustment Buffer (ISAB)
27.4.1.6. Methanol
27.4.2. Equipment
27.4.2.1. All volumetric glassware must be equivalent to “Class A” as defined by NIST circular 602.
27.4.2.2. Volumetric flasks - 100 and 500 ml
75
BCIS-03B Rev. DEC02
27.4.2.3. Beaker - 250 ml
27.4.2.4. Pipets - 1.00, 2.00, 5.00 and 10.0 ml
27.4.2.5. Balance, capable of weighing 5.000 g.
27.4.2.6. Ion specific electrode and meter. (Example: Corning model 250/255 or 350/355 pH/mV/ion
meter plus suitable electrodes)
27.4.2.7. Powder free lab gloves
27.5. SAFETY
27.5.1. The operator must be familiar with the MSDS pertaining to Nitric acid and other reagents.
is complete or in the event contact is made with the acid
battery acid.
27.6. GENERAL PREPARATION
27.6.1. Electrode Preparation
27.6.1.1. Make sure the electrodes are filled with the required fluids as outlined in equipment
instructions.
27.6.2. Electrode Slope Check
27.6.2.1. Check electrode each day as per manufacturer's instructions.
27.7. PROCEDURE
27.7.1. Weigh out approximately 5 g. of the sample.
27.7.2. Cut the sample into small pieces about 5 mm x 5 mm. Reweigh the cut pieces, record the
weight to the nearest 0.01 g. Record the weight as W.
27.7.3. Transfer the sample into a 100 ml volumetric flask, rinsing out any residue with methanol.
Add 5 ml of concentrated Nitric acid, 1 ml of ISAB and dilute to 100 ml with methanol.
27.7.4. Stir the sample for 30 minutes.
27.7.5. After the 30 minutes, transfer the solution and sample to a 250 ml beaker. Take a reading
with. The Specific Ion Meter (R).
27.7.6. Make sure the reading, calibration and standards are per instruction of the equipment
manufacturer.
27.8. CALCULATION
27.8.1. The Chloride content, ppm = meter reading ( R) / sample weight (W).
Note: Check to assure the instrument used reports reading in ppm. If not report results in
mg/L.
27.9. REPORT
76
BCIS-03B Rev. DEC02
27.9.1. Report the Chloride content in ppm and the instrument used. (See note in 27.8.1)
27.10.1. Precision
27.10.1.1. Complexation
27.10.1.1.1. Total concentration consists of free ions and complexed or bound ions in solution. Since the
electrode only responds to free ions, any complexing agent in the solution reduces the
measured concentration of ions.
27.10.1.2. Temperature Influence.
27.10.1.2.1. Samples and standard should be within ± 1 °C of each other, since electrode potentials are
influenced by changes in temperature.
27.10.2. Accuracy
27.10.2.1. The accuracy is limited by the precision of the method and good technique.
77
BCIS-03B Rev. DEC02
28. STANDARD TEST METHOD TO DETERMINE PIN PUNCTURE RESISTANCE OF

BATTERY SEPARATOR USING A MOTORIZED CHATILLON TESTER
28.1. SCOPE
28.1.1. This method measures the force required to puncture the battery separator with the use of a
motorized Chatillon tester.
28.2.1. Insufficient resistance of a separator to puncture may contribute to separator damage and
potential early battery failure.
28.3.1. BCI Procedure BCIS-03B Subsection 13, Standard Test Method To Determine Pin Puncture
Resistance Of Battery Separator Using A Manual Chatillon Tester.
28.3.2. BCI Procedure BCIS-03B Subsection 03, Standard Test Method For Backweb Thickness Of
Battery Separator.
28.4. APPARATUS
28.4.1. Digital force gauge (Chatillon DFI-10 or similar).
28.4.2. Motorized test stand (Chatillon TCM-200 or successor), or equivalent.
28.4.3. Puncture tip with flat bottom of 1.93 mm (0.076 in) diameter. See TM-3.213.
28.4.4. Puncture base with hole of 6.7mm (0.26 in.) diameter and 10mm (0.4 in.) in depth.
28.4.5. (Optional Printer) Mitutoyo Digimatic Mini-Processor (DP-1 HS or equivalent).
28.5. TERMINOLOGY
28.5.1. Puncture Resistance - The peak force during puncturing of the separator.
28.6. SAFETY
28.6.1. Set UPPER Travel Limit (located at back of vertical test stand column) to position the
puncture tip approximately 6 mm (0.24 in) above puncture base. This prevents accidental
insertion of fingers below pin.
28.6.2. Set LOWER Travel Limit to position the puncture tip no more than 8 mm (0.32 in) below
puncture level surface. This prevents excessive column travel causing compression in
excess of gauge range.
28.6.3. (Only for TCM-201) According to Operating Instructions set Compression Limit to upper limit
of Force Gauge range. In case of emergency hit RED button at right of column for immediate
STOP.
28.7.1. Select representative samples.
78
BCIS-03B Rev. DEC02
28.7.2. Mark points to be tested. At marked points, measure and record backweb thickness, BCIS-
03B Subsection 03. Use a gauge with a minimum precision of 0.01 mm (for Metric) and
0.0001 in. (for English).
28.8.1. Turn on power switch of test stand, force gauge and mini-processor.
28.8.2. Set left selector button on control panel to "Start Upper Limit" position.
28.8.3. The speed of the pin travel can be between 100 to 500 mm/min (4 to 20 in/min).
28.8.4. Press "Peak" key on force gauge to show "C (compression PEAK).
28.8.5. Select appropriate Unit (N or lbs) by pressing UNIT key on force gauge.
28.8.6. Press CL (clear) key on printer keyboard.
28.8.7. Reset gauge to zero by pressing ZERO key on digital gauge.
28.8.8. Insert separator sample below the puncture tip, positive ribs facing up, and keep it flat across
puncture base.
28.8.9. Press DOWN key on test stand. The unit will puncture sample and return automatically to
Upper Limit.
28.8.10. Press XMIT key on gauge to transmit result to printer or record result manually and reset
gauge to zero (Step 28.8.7).
28.8.11. Continue with next sample going through Steps 28.8.7 through 28.8.7.
28.8.12. Press FEED to advance recording tape.
28.9. REPORT
28.9.1.1. The instrument used and the speed of the pin.
28.9.1.2. Puncture force in g (lb). The results can also be reported in actual Newtons.
28.9.1.3. Report the back-web thickness mm (in).
28.10.1. A study dated 12-19-96 and on file at BCI showed that the values do not change with regards
to pin speed travel. The same study suggested that variations can be obtained with changes
in the anvil hole size. Different puncture test method will provide different results.
79
BCIS-03B Rev. DEC02
29. STANDARD TEST METHOD TO DETERMINE RESISTANCE OF BATTERY

SEPARATORS TO OXIDATIVE DEGRADATION USING HYDROGEN PEROXIDE IN
SULFURIC ACID AS OXIDIZING MEDIUM
29.1. SCOPE
29.1.1. This test procedure provides a test method to determine resistance of separator material to
degradation by hydrogen peroxide in sulfuric acid used as oxidizing medium.
29.1.2. This test procedure is intended to simulate resistance of separator to oxidative degradation in
lead-acid batteries at an accelerated rate.
29.1.3. This procedure is one of the four test methods made available by BCI that require exposure
of separators to various corrosive environment which include:
29.1.3.1. Heated sulfuric acid
29.1.3.2. Hydrogen peroxide in sulfuric acid
29.1.3.3. Potassium dichromate in sulfuric acid
29.1.3.4. Simulated electrochemical oxidative conditions in battery cell under charging
29.1.4. Oxidative degradation resistance of a separator sample is expressed by weight loss, tensile
strength and/or elongation of oxidized sample in relation to untreated control sample.
29.2.1. BCIS-03B Subsection 30, "Standard Test Method to Determine Resistance of Battery
Separators to Corrosive Using Hot Sulfuric Acid as Corrosion Medium."
Separators to Oxidative Degradation Using Potassium Dichromate in Sulfuric Acid as
Oxidizing Medium."
Separators to Oxidative Degradation Using Simulated Electrochemical Cell Environment as
Oxidizing Medium."
29.2.4. BCIS-03B Subsection 11, "Standard Test Method for Elongation and Tensile Strength of
Microporous Polyethylene Battery Separators."
29.2.5. Tappi's TIP 0606-15, Physical and Chemical Properties of Hydrogen Peroxide (H2O2)1.
1
Available from TAPPI PRESS, Technology Park, P.O. Box 105113, Atlanta, GA 3048-
5113, USA.
29.2.6. American Chemical Society, Monography Series No. 128, "Hydrogen Peroxide", by
SCHUMB, Satterfield & Wentworth2
2
Available from Xerox University Microfilm, Ann Arbor, MI, USA
impurities, physical stresses and service duration are not uncommon. Failure modes of
separators due to physical or chemical degradation are generally unique to the type of
80
BCIS-03B Rev. DEC02
separator, battery design construction and type of battery service. Tests to accelerate
degradation through high temperatures and corrosive chemicals or electrochemical
treatments can often lead to failure modes not representative of and/or disproportional to
physical service life.
29.3.2. Due to conditions described above, there may not be one definitive test that will adequately
29.3.3. It is the responsibility of battery producer and separator manufacturer to jointly agree on test
method(s) that will accelerate degradation modes normally seen in the service of a particular
type of battery and separator.
29.3.4. Adoption of proper degradation resistance test method of a particular type of battery
separator should be determined by the similarity between the test method and actual
degradation mode of the separator in the applicable battery cells during the service.
29.3.5. This test procedure, in general, can be used as qualification testing, verification testing or
validation testing of separator materials.
29.4. SAFETY
29.4.1. Read and comprehend safety data sheets for sulfuric acid and hydrogen peroxide, and
company’s safety procedure.
battery acid and hydrogen peroxide.
29.5. APPARATUS
29.5.1. Laboratory balance with a sensitivity of 0.1 mg. (Must be large enough to weigh a 40 X 40
mm piece of separator).
29.5.2. Laboratory oven capable of maintaining prescribed temperature within ±2 C.
29.5.3. Desiccator and desiccant
29.5.4. Clean scissors or paper cutter
29.5.5. Precision ASTM Specific Gravity Hydrometer with 0.001 subdivision
29.5.6. Tensile tester e.g. Instron 1011 or equivalent.
29.5.7. Water Bath or air circulating oven, suitable to hold a 80 ± 2°C
29.5.8. Beakers, 600 ml, 4000 ml
29.5.9. Wide mouth reagent bottles, 500 ml and 100 ml
29.6. REAGENTS
81
BCIS-03B Rev. DEC02
29.6.1. Sulfuric acid, reagent ACS grade (1.83-1.84 specific gravity, 95-98% H2SO4)
29.6.2. Hydrogen Peroxide, 30% solution, ACS grade H2O2
29.6.3. Deionized or distilled water
29.7. PREPARATION OF ACID SOLUTIONS
29.7.1. 1.280 Specific Gravity Sulfuric Acid

Caution: Exercise precaution when adding concentrated sulfuric acid to water to dilute the
acid due to heat evolution that causes explosive spattering. Always add the acid to water,
never the reverse.
29.7.2. Fill 1447 ml of deionized water into 4000 ml beaker and slowly add 553 ml of concentrated
sulfuric acid while stirring the solution. Allow to cool before using.
29.7.3. Check specific gravity of solution with a hydrometer. Adjust specific gravity to 1.280±0.002 at
26.7°C (80°F).
29.7.4. Hydrogen peroxide in 1.280 Specific Gravity Sulfuric Acid Oxidizing Solution
29.7.4.1. In 4000 ml beaker, fill 997 ml of 1.28 specific gravity H2SO4. Carefully add, while stirring, 336
ml of concentrated H2SO4 . Allow to cool and then add 667 ml of 30% H2O2. This is a 10%
hydrogen peroxide solution assuming the hydrogen peroxide is at 30%. Check specific
gravity of solution with a hydrometer. Adjust specific gravity to 1.280 ± 0.002 if needed.
29.7.5. Hydrogen peroxide solution concentration should be checked by approved analytical

method. Reference Subsections 29.2.5 and 29.2.6.
29.8. PREPARATION OF TEST SPECIMEN
29.8.1. Specimen for Weight Loss Test
29.8.1.1. Cut the separator sample into approximately 40 mm by 40 mm square piece.
29.8.2. Specimen for Tensile Strength and Elongation Test. Reference should be made to BCI Test
Method in Subsection 11.
29.8.3. Cut the separator sample into 25 mm x 100 mm rectangular piece.
29.9. PROCEDURE FOR ACCELERATED OXIDATION
29.9.1. Preheat water bath or air circulating oven to 80°C ± 2°C (176°F ± 2.6°F).
29.9.2. Cut specimens to prescribed size and shape.
29.9.3. Place the samples in the oven and dry for one hour at 70°C ± 2°C (158°F ± 3.6°F).
29.9.4. Remove the specimens from drying oven and place in the desiccator for cooling. Weigh the
samples as rapidly as possible to the nearest 0.001 g using the laboratory balance. Note
initial weight Wi.
29.9.5. Fill the appropriate size wide mouth glass reagent bottle with ground glass stopper (e.g. 500
ml or 1000 ml bottle) with oxidizing solution. Use 150 ml of oxidizing solution for each 1 gram
of sample.
82
BCIS-03B Rev. DEC02
29.9.6. Place the beaker into water bath and heat it until temperature of oxidizing solution reaches
80°C ± 2°C (176°F ± 3.6°F).
29.9.7. Introduce samples into the wide mouth reagent glass bottle making certain that the samples
are immersed under oxidizing solution by using glass rods or other chemically inert material
allowing separation of samples and circulation of oxidizing solution and heat. Close the bottle
with ground glass stopper.
29.9.8. Heat the bottle with samples in the water bath or air circulating oven for 3 hours. NOTE: the
minimum time of exposure is three hours. It is recognized that to obtain meaningful results a
different time may be selected (or a different concentrations of reagent), depending on the
type and dimensions of material being tested. If a different time or reagent concentration is
used, these changes should be so noted when the data is reported.
29.9.9. Remove the samples from beaker and rinse them gently with water.
29.9.10. Place the sample into a clean 600 ml beaker and add approximately 500 ml of fresh water
and allow to soak at least one hour to ensure that no residual oxidizing solution will remain in
the pores of separator material.
29.9.11. Gently and thoroughly rinse the sample again with water.
29.9.12. Dry the sample for 90 minutes at 70°C ± 2°C (158°F ± 3.6°F) and cool sample in desiccator.
Weigh sample as rapidly as possible after removing from desiccator. Note final weight Wf.
29.10. SAMPLE EVALUATION TESTS AND CALCULATIONS
29.10.1. Oxidation Weight Loss Test
⎛ W − Wf ⎞
% Oxidation Weight Loss = ⎜⎜ i ⎟ × 100
⎟
⎝ W1 ⎠
Where,
Wi = Initial sample weight from Subsection 29.9.4
Wf = Final sample weight from Subsection 29.9.12
29.10.2. Tensile Strength and Elongation Test
29.10.2.1. Perform tensile strength and elongation tests on control sample and oxidized sample. Test
samples in machine direction (MD) and cross machine direction (CD). Refer to BCIS-03B
Subsection 11 Standard Test Method for Elongation and Tensile Strength of Microporous
Polyethylene Battery Separator.
29.10.2.2. Record tensile strength of untreated control sample in MPa. Note tensile strength of control
sample A.
29.10.2.3. Record tensile strength of oxidized sample in MPa. Note tensile strength of oxidized sample
B.
29.10.2.4. % Retention of Tensile Strength
⎛A - B⎞
% Retention of Tensile Strength = ⎜ ⎟ × 100
⎝ A ⎠
Where,
83
BCIS-03B Rev. DEC02
A = Tensile Strength of Control Sample from Subsection 29.10.2.2

B = Tensile Strength of Oxidized Sample from Subsection 29.10.2.3
29.10.2.5. Record elongation of untreated control sample in %. Note elongation of control sample C.
29.10.2.6. Record elongation of oxidized sample in %. Note elongation of oxidized sample D.
29.10.2.7. % Retention of Elongation
⎛C-D⎞
% Retention of Elongation = ⎜ ⎟ × 100
⎝ C ⎠
Where,
C = Elongation of Control Sample from Subsection 29.10.2.5
D = Elongation of Oxidized Sample from Subsection 29.10.2.6
29.11. REPORT
29.11.1.1. Report % weight loss to nearest 0.1%.
29.11.1.2. Report oxidative degradation test procedure used for the test.
Tensile Strength and Elongation Test
29.11.1.3. Report tensile and elongation test procedure used.
29.11.1.4. Report tensile strength MPa and elongation in % of untreated control sample and oxidized
sample in MD and CD. Report backweb thickness of sample.
29.11.1.5. Report % retention of puncture resistance.
29.11.1.6. Report the exposure time in hours.
29.12.1. Precision
29.12.1.1. No statement on precision can be made due to lack of test data.
29.12.1.2. A round robin test study using various separator materials is required to establish precision of
the test method.
29.12.2. Bias
29.12.2.1. No statement on bias can be made due to lack of a standard reference material.
84
BCIS-03B Rev. DEC02

SEPARATORS TO HOT SULFURIC ACID
30.1. SCOPE
hot sulfuric acid.
30.1.2. This test procedure is intended to simulate resistance of separator to oxidative degradation in
lead-acid batteries at an accelerated rate.
of separators to various corrosive environment which include:
30.1.4. The resistance of a separator sample in this procedure is expressed in weight loss of the
sample after subjecting it to hot sulfuric acid.
30.2.1. BCIS-03B Subsection 29, A Standard Test Method to Determine Resistance of Battery
Separators to Oxidative Degradation by Hydrogen Peroxide in Sulfuric Acid as Oxidizing
Medium.
Separators to Oxidative Degradation Using Potassium Dichromate in Sulfuric Acid as
Oxidizing Medium.
Oxidizing Medium.
30.2.4. BCIS-03B Subsection 20, Standard Test for Determining Percent Acid weight Loss of
Recombinant Battery Separator Mat (Reflux Method)
service. Significant variations in temperature, electrolyte concentration, overcharge,
chemical impurities, physical stresses and service duration are not uncommon. Failure
modes of separators due to physical or chemical degradation are generally unique to the type
of separator, battery design construction and type of battery service. Tests to accelerate
85
BCIS-03B Rev. DEC02
30.3.4. Adoption of proper degradation resistance test method of a particular type of battery
30.3.5. This test procedure, in general, can be used as qualification, verification or validation testing
of separator materials.
30.4. SAFETY
30.4.1. Read and comprehend safety data sheets for sulfuric acid and hydrogen peroxide, and
company's safety procedure.
30.4.2. Safety goggles, lab coats and rubber apron must be worn during acid dilution operations.
The glass-mixing bottle should be enclosed in a plastic container of sufficient capacity to
contain the solution in case of bottle breakage. To prevent excessive heating, concentrated
sulfuric acid should be added slowly to water with adequate agitation to produce thorough
mixing. The diluted acid is sufficiently corrosive at both ambient and elevated temperatures
that careful handling is necessary to prevent injury or damage.
30.4.3. Follow current Federal, State, and Local regulations for safe disposal of all chemicals used,
including battery acid and hydrogen peroxide.
30.5. APPARATUS
30.5.1. Laboratory balance with a sensitivity of 0.1 mg
30.5.2. Laboratory oven capable of maintaining prescribed temperature within ± 3°C
30.5.5. Precision ASTM Specific Gravity Hydrometer with 0.001 readings.
30.5.6. Hot plate
30.5.7. Reflux condenser and 500 mL Erlenmeyer flask 24/40 or equivalent.
30.6. REAGENTS
30.6.1. Sulfuric acid, reagent ACS grade (specific gravity 1.83-1.84, 95-98% H2SO4)
30.7. PREPARATION OF ACID SOLUTIONS

Caution: Exercise caution when adding concentrated sulfuric acid to water to dilute the acid
due to heat evolution that causes explosive spattering. Always add the acid to water, never
the reverse.
86
BCIS-03B Rev. DEC02
30.7.1.1. Fill 1333 ml of deionized water into 4000 ml beaker and slowly add 667 mL of concentrated
sulfuric acid while stirring the solution. Allow cooling before using.
30.7.1.2. Check specific gravity of solution with a hydrometer. Adjust specific gravity to 1.280 ± 0.002
at 25°C
30.8.1. Cut approximately 1 g of the separator sample into conveniently sized rectangular pieces.
30.9. PROCEDURE TO DETERMINE HOT ACID RESISTANCE
30.9.1. Place the sample in an oven. Dry for one hour at 70°C ± 3°C.
30.9.2. Remove the sample from the drying oven and place in the desiccator for cooling. Weigh the
sample as rapidly as possible to the nearest 0.001 g using the laboratory balance. Note
initial weight WI.
30.9.3. Introduce the samples into a 500 ml Erlenmeyer flask with 1.280 specific gravity sulfuric acid
solution. Use 150 ml of sulfuric acid as corrosion medium for each 1 gram sample. Make
certain that the samples are immersed under the solution by using either glass rods or other
chemically inert material, allowing separation of samples and circulation of solution and heat.
30.9.4. Reflux for 3 hours (or mutually agreed time) in the reflux apparatus at the rate of one drop per
second.
30.9.5. At the end of three-hour reflux, remove the flask from the hot plate. Allow the flask to cool for
30 minutes.
30.9.6. Gently and thoroughly rinse the sample with water.
30.9.7. Place the sample into a clean 600 ml beaker and add approximately 500 ml of fresh water.
Soak at least one hour to ensure that no residual acid solution will remain in the pores of
separator material.
30.9.9. Dry the sample for 90 minutes at 70°C ± 3°C and cool the sample in a desiccator. Weigh the
sample as rapidly as possible after removing the sample from the desiccator. Note final
weight Wf.
30.10.1. Weight Loss Test:

% Weight Loss = ‡(Wi - Wf)/ Wi Ž x 100
Where
30.11. REPORT
30.11.1. Report % weight loss to nearest 0.1%.
30.11.2. Report test procedure used for the test.
87
BCIS-03B Rev. DEC02
30.11.3. Report reflux time.
30.11.4. Report visual physical conditions of sample after reflux
30.12.1. Precision
30.12.1.1. No statement on precision can be made due to lack of test data.
30.12.2. Bias
30.12.2.1. A limited number of tests conducted on polyethylene and hard rubber separators at one
laboratory showed polyethylene separators lost significantly more weight than hard rubber
separators. The weight loss of the polyethylene may be associated with loss of wetting
agent, retained oils, etc, rather than degradation of polyethylene structure.
88
BCIS-03B Rev. DEC02

SEPARATORS TO OXIDATIVE DEGRADATION USING POTASSIUM DICHROMATE IN
SULFURIC ACID AS OXIDIZING MEDIUM
31.1. SCOPE:
degradation by potassium dichromate used as oxidizing medium in sulfuric acid.
31.1.2. This test procedure is intended to simulate the resistance of separators to oxidative
degradation in lead-acid batteries at an accelerated rate.
of separators to various corrosive environments which include:
31.1.4. Oxidative degradation resistance of a separator sample is expressed by weight loss, tensile
strength, elongation, puncture resistance or physical defects of oxidized sample in relation to
an untreated control sample.
31.2.1. BCIS-03B Subsection 29, “Standard Test Method to Determine Resistance of Battery
Separators to Oxidative Degradation Using Hydrogen Peroxide in Sulfuric Acid as Oxidizing
Medium.”
31.2.2. BCIS-03B Subsection 30, “ Standard Test Method to Determine Resistance of Battery
Separators to Corrosive Degradation Using Hot Sulfuric Acid as Corrosion Medium.”
31.2.3. BCIS-03B Subsection 32, “ Standard Test Method to Determine Resistance of Battery
Oxidizing Medium.”
31.2.4. BCIS-03B Subsection 11, “Standard Test Method for Elongation and Tensile Strength of
Microporous Polyethylene Battery Separators”.
31.2.5. BCIS-03B Subsection 13, “Standard Test Method to Determine Pin Puncture Resistance to
Battery Separator Using a Manual Chatillon Tester.”
31.2.6. BCIS-03B Subsection 14, “Standard Test Method to Determine Puncture Resistance of
Microporous Polyethylene, Rubber and PVC Battery Separator Using Tensile (Instron)
Machine.”
31.2.7. BCIS-03B Subsection 28, “ Standard Test Method to Determine Puncture Resistance to
Battery Separator Using an Automatic Chatillon Tester.”
89
BCIS-03B Rev. DEC02
31.3.4. Adoption of proper degradation resistance test methods for a particular type of battery
31.4. SAFETY
31.4.1. Read and comprehend the sulfuric acid and potassium dichromate, safety data sheets and
your company’s safety procedure.
31.4.2. Safety goggles, lab-coat and rubber apron must be worn during acid dilution operations. The
glass-mixing bottle should be enclosed in a plastic container of sufficient capacity to contain
careful handling is necessary to prevent injury or damage. Testing samples can cause
corrosion to the equipment.
31.4.3. Follow current Federal, State, and Local regulations for the safe disposal of all chemicals
used, including sulfuric acid and especially potassium dichromate.
31.5. APPARATUS
31.5.1. Laboratory balance with a sensitivity of 0.1 mg
31.5.2. Laboratory oven capable of maintaining prescribed temperature within ±3°C (5.4°F)
31.5.5. Precision ASTM Specific Gravity Hydrometer with 0.001 subdivision (at 25°C for all
measurements)
31.5.6. Tensile tester e.g. Instron 1011 or equivalent
31.5.7. Digital force gauge, Chatillon DFI-10 or equivalent
31.5.8. Motorized test stand Chatillon TCM-200 or equivalent
31.5.9. Glass reagent bottles, 500 and 1000 ml with ground joint.
90
BCIS-03B Rev. DEC02
31.5.10. Beakers, 4000 and 600 ml
31.5.11. Volumetric flask, 2000 ml
31.6. REAGENTS
31.6.1. Sulfuric acid, reagent ACS grade (specific gravity 1.83-1.84, 95-98% H2SO4)
31.6.2. Potassium dichromate, reagent ACS grade K2Cr2O7
31.7. PREPARATION OF OXIDIZING SOLUTION

Caution: Exercise precaution when adding concentrated sulfuric acid to water to dilute the
acid due to heat evolution that causes explosive spattering. Always add the acid to water,
never the reverse.
31.7.2. Fill 1447 ml of deionized water into 4000-ml beaker and slowly add 553 ml of concentrated
sulfuric acid while stirring the solution. Allow the solution to cool before using.
31.7.3. Check specific gravity of solution with a hydrometer. Adjust specific gravity to 1.280 ± 0.002
at 26.7°C (80°F).
31.7.4. 1% Potassium Dichromate in 1.28 Specific Gravity Sulfuric Acid Oxidizing Solution
31.7.5. Dissolve 20 grams ±0.1 grams of potassium dichromate into 1.280 specific gravity sulfuric
acid in 2000-ml volumetric flask. Fill the acid to the graduation line.
31.8.1. Specimen for Weight Loss Test
31.8.1.1. Cut the separator sample into approximately 40 mm by 40 mm square pieces.
31.8.1.2. Specimen for Tensile Strength and Elongation Test. Reference should be made to
Subsection 11.
31.8.1.3. Cut the separator sample into 25 mm x 100 mm rectangular piece. Square pieces, cutting
parallel to the ribs and include ribs in the sample.
31.8.2. Specimen for Puncture Resistance Test
31.8.2.1. Cut the separator sample into approximately 40 mm by 40 mm square piece.
31.8.3. Specimen for Delamination Testing of Glass Fiber Type Separator
31.8.3.1. Cut separator sample into approximately 70 mm long by 38 mm wide. Square pieces, cutting
parallel to the ribs and include ribs in the sample.
31.9. PROCEDURE FOR ACCELERATED OXIDATION
31.9.1. Preheat oven to 80°C ± 2°C (176°F ± 3.6°F).
31.9.2. Cut specimens to prescribed size and shape.
91
BCIS-03B Rev. DEC02
31.9.3. Place the specimens in oven and dry for one hour at 70°C ± 2°C (158°F ± 3.6°F).
31.9.4. Remove the specimens from drying oven and place in the desiccator for cooling. Weigh the
specimens as rapidly as possible to the nearest 0.001 g using a laboratory balance. Note
initial weight Wi.
31.9.5. Fill the appropriate size wide mouth glass reagent bottle, containing a ground glass stopper
(e.g. 500 or 1000 ml bottle) with oxidizing solution. Use 150 ml of oxidizing solution for each 1
gram of sample.
31.9.6. Place the bottle into an oven and heat it until temperature of oxidizing solution reaches 80°C
± 2°C (176°F ± 3.6°F).
31.9.7. Introduce samples into the wide mouth, reagent glass bottle. Make certain that the samples
are immersed under oxidizing solution by using glass rods or other chemically inert material
allowing separation of samples and circulation of oxidizing solution and heat. Close the bottle
with ground glass stopper.
31.9.8. Heat the bottle with the samples immersed in the oxidizing solution for 3 hours. Maintain the
solution temperature at 80°C ± 2°C (176°F ± 3.6°F).
NOTE: The recommended time of exposure is three hours. It is recognized that to
obtain meaningful results a different time may be selected (or a different concentration
of reagent), depending on the type and dimensions of materials being tested. If a
different time or reagent concentration is used, these changes should be so noted
when the data is reported.
31.9.9. Remove the samples from beaker and rinse them gently with water.
31.9.10. Place the sample into a clean 600 ml beaker and add approximately 500 ml of fresh water
and allow to soak at least for one hour to ensure that no residual oxidizing solution will remain
in the pores of separator material.
31.9.12. Remove the sample from the rinse bottle. Either air-dry the sample or remove excess water
with a paper towel. Use this step for Tensile Strength and Elongation Test (Subsection
31.10.2) and Puncture Resistance Test (Subsection 31.10.4).
NOTE: The samples can still be corrosive and oxidize the jaws of the tensile or
puncture tester.
31.9.13. To determine Oxidative Weight loss (Subsection 31.10.1) dry the sample in an oven for 90
minutes at 70°C ± 2°C (158°F ± 3.6°F) and cool the sample in desiccator. Weigh the sample
as rapidly as possible after removing from desiccator. Note final weight Wf.
% Oxidation Weight Loss = ((Wi - Wf)/ Wi) x 100

Where
92
BCIS-03B Rev. DEC02
31.10.2.1. Perform tensile strength and elongation tests on control sample and oxidized sample. Refer
to Subsection 11: Standard Test Method for Elongation and Tensile Strength of Microporous
Polyethylene Battery Separator.
31.10.2.2. Record tensile strength of untreated control sample in MPa. Note tensile strength of control
sample A.
31.10.2.3. Record tensile strength of oxidized sample in MPa. Note tensile strength of oxidized sample
B.
31.10.2.4. % Retention of Tensile Strength = (B/ A) x 100
Where
A = Tensile Strength of Control Sample from Subsection 31.10.2.2
B = Tensile Strength of Oxidized Sample from Subsection 31.10.2.3
31.10.2.5. Record elongation of untreated control sample in %. Note elongation of control sample C.
31.10.2.6. Record elongation of oxidized sample in %. Note elongation of oxidized sample D.
31.10.2.7. % Retention of Elongation = ((C - D)/ C) x 100
Where C = Elongation of Control Sample from Subsection 31.10.2.5

D = Elongation of Oxidized Sample from Subsection 31.10.2.6
31.10.3. Puncture Resistance Test
31.10.3.1. Perform puncture resistance tests on control sample and oxidized sample. Refer to
Subsection 13: Standard Test Method to Determine Pin Puncture Resistance of Battery
Separator Using a Manual Chatillon Tester, Subsection 28: Standard Test Method to
Determine Puncture Resistance to Battery Separator Using an Automatic Chatillon Tester, or
Subsection 14: Standard Test Method to Determine Puncture Resistance of Microporous
Polyethylene, Rubber and PVC Battery Separator Using Tensile (Instron) Machine
31.10.3.2. Record puncture resistance force of untreated control sample in kg (or Newton). Note
puncture resistance of control sample A.
31.10.3.3. Record puncture resistance force of oxidized sample in kg (or Newton). Note puncture
resistance of oxidized sample B.
31.10.3.4. Report % Retention of Puncture Resistance = ((A - B)/ A) x 100

Where A = Puncture Resistance of Control Sample from Subsection 31.11.3.2.
B = Puncture Resistance of Oxidized Sample from Subsection 31.11.3.3.
31.10.4. Delamination of Glass Fiber Test
31.10.4.1. Proceed with accelerated oxidation test procedure Subsection 31.9.1. through Subsection
31.9.12.
31.10.4.2. Remove the sample and visually inspect individual sample for blisters or other signs of
delamination.
31.11. REPORT
93
BCIS-03B Rev. DEC02
31.11.1.1. Report % weight loss to nearest 0.1%.
31.11.1.2. Report oxidative degradation test procedure used for the test.
31.11.2.1. Report tensile and elongation test procedure used.
31.11.2.2. Report tensile strength MPa and elongation in % of untreated control sample and oxidized
sample. Report backweb thickness of sample.
31.11.2.3. Report % retention of elongation and tensile strength.
31.11.3. Puncture Resistance Test
31.11.3.1. Report puncture tester and puncture resistance test procedure used.
31.11.3.2. Report puncture resistance of untreated control sample and oxidized sample. Report
backweb thickness of sample.
31.11.3.3. Report % retention of puncture resistance.
31.11.4. Delamination of Glass Fiber Test
31.11.4.1. Report presence of blisters or other signs of fiber delamination after visual inspection.
31.12.1. Precision
31.12.1.1. A round robin test study conducted with very limited number of tests on polyethylene
separators and hard rubber separators showed very wide variations of test results among
testing laboratories.
31.12.1.2. No statement on repeatability (within a laboratory), comparability (between materials) or

reproducibility (between laboratories) can be made due to lack of sufficient test data.
31.12.2. Bias
31.12.2.1. No statement on bias can be made due to lack of a standard reference material.
94
BCIS-03B Rev. DEC02

SEPARATORS TO OXIDATIVE DEGRADATION USING SIMULATED
ELECTROCHEMICAL CELL ENVIRONMENT AS OXIDIZING MEDIUM
32.1. SCOPE
oxidative degradation by simulated electrochemical cell environment as oxidizing medium.
32.1.2. This test procedure is intended to simulate the resistance of separators to oxidative
degradation in lead-acid batteries at an accelerated rate.
32.1.2.1. If used for quality control (comparative) purposes the test can be terminated after a prescribe
time, e.g. 50 or l00 h.
32.1.2.2. If used for initial evaluation and acceptance purposes, the test should be continued until
failure (Subsection 32.9.6).
32.1.3. Procedure is one of the four test methods made available by BCI that require exposure of
separators to various corrosive environments which include:
32.1.3.2. Hydrogen peroxide in sulfuric acid.
32.1.3.3. Potassium dichromate in sulfuric acid.
32.1.3.4. Simulated electrochemical oxidative conditions in battery cell under charging.
Separators to Oxidative Degradation Using Hydrogen Peroxide in Sulfuric acid as Oxidizing
Medium.”
32.2.2. BCIS-03B Subsection 30,”Standard Test Method to Determine Resistance of

BatterySeparators to Corrosive Degradation Using Hot Sulfuric Acid as Corrosion Medium.”
Separators to Oxidative Degradation Using Potassium Dichromate In Sulfuric Acid As
Oxidizing Medium.”
95
BCIS-03B Rev. DEC02
32.3.4. Adoption of proper degradation resistance test methods for a particular type of battery
32.3.5. This test procedure, in general, can be used as qualification testing, verification testing or
validation testing of separator materials.
32.4. SAFETY
32.4.1. Read and comprehend the sulfuric acid, safety data sheets and your company’s safety
procedure.
32.4.2. Safety goggles, lab coats and rubber apron must be worn during acid dilution operations. The
32.4.3. Test cells may explode since the sulfuric acid in the cell produces an explosive mixture of
hydrogen and oxygen. Extreme caution should be taken to make sure that the test cells are
stored, and worked on, in a well-ventilated area. Always wear safety glasses and a face
shield when working on or near the test cells. Keep all sparks, flames and cigarettes away
from the test cells.
32.4.4. Follow current Federal, State, and Local regulations for the safe disposal of all chemicals
used, including sulfuric acid.
32.5. APPARATUS
32.5.1. The assembly of electrochemical test apparatus including electric circuits is shown in figure 1.
32.5.2. Lead Plates.
32.5.2.1. Electrodes for both anode and cathode are fabricated by cutting a 1 mm thick lead plate as
shown in Figure 35.2. Thicker lead plates can be used. A thickness of 1 mm, is the minimum
that is recommended.
32.5.2.2. Dimension of an electrode for effective testing area is 50 mm x 50 mm.
32.5.2.3. The surface of the electrode facing the separator must be clean (free of oxide) smooth and
flat.
32.5.2.4. The electrode should be replaced with a fresh electrode after each test.
32.5.3. Polyethylene or Polypropylene cable ties.
32.5.4. Lead wire and connecting hardware made of type 316 stainless steel.
32.5.5. Glass plate, 75mm high x 75mm wide x 5 to 20 mm thick.
32.5.6. Container, 200 mm high x 80 mm wide x 120 mm long or a battery container having a cell
compartment 170 to 270 mm high x 35 to 85 mm wide x 120 to 190 mm long, e.g. BCI Group
96
BCIS-03B Rev. DEC02
Numbers 24 or 75 for 12 volt batteries, with 6 compartments; or Group Numbers 1 or C2 for 6

volt batteries, with 3 compartments.
32.5.7. Container must be washed with water after each test or once a week.
32.5.8. Bundle of separators and glass mats (battery retainer type or RBSM type) cut to 79 mm x 70
mm for shimming.
32.5.9. Water bath equipped with thermostat capable of maintaining bath temperature at 50°C ± 2
°C.
32.5.10. Ammeter
32.5.11. Voltage recorder
32.5.12. DC stabilizing power supply
32.6. REAGENTS
32.6.1. Sulfuric acid, reagent ACS grade or battery grade, specific gravity 1.300 at 2O °C.
32.7. PREPARATION OF SEPARATOR TEST
32.7.1. Specimen
32.7.1.1. Cut a separator to 70 mm by 70 mm.
32.7.1.2. Leave ribs on any separator if the separator has ribs.
32.7.1.3. Remove any glass mat from the separator if it has glass mat attached.
32.8. PROCEDURE TO SET UP ASSEMBLY OF TEST EQUIPMENT
32.8.1. Prepare a separator test stack by placing glass plate, anode, separator sample, cathode, and
glass plate in the order as shown in Figure 3.
32.8.2. The entire stack must be centered, aligned and tied with Polyethylene cable ties as shown in
Figure 32.3.
97
BCIS-03B Rev. DEC02
32.8.3. Build shimming material by stacking separator sheets and glass mats (flooded battery
retainer type or valve regulated RBSM type) cut to 75 mm x 75 mm wide which consists of
separators / glass mats / separators at approximately 40% / 20% / 40% of space between
separator test stack and container wall respectively. Sheets of glass mat, acting as a
cushion, are inserted between bundles of rigid separators to provide adequate fit under
compression for separator test stack.
32.8.4. Insert the separator test stack in the middle and shimming stack on each end in a vertical
position in the container as shown in Figure 1. Make certain that adequate fit or compression
is provided to the separator test stack by selecting the proper number of separator (s), and
glass mat sheets used as the shim stock.
32.8.5. Fill the test container with 1.300 (20°C) specific gravity sulfuric acid to a level 25 mm above
the top of the test stack. Allow the separator test stack to be wetted with the acid at least 3
hours before starting the test. This allows the test cell to be warmed up and separator test
piece to be thoroughly wetted.
98
BCIS-03B Rev. DEC02
32.8.6. If a commercial battery container with multiple compartments is used, fill the unused
compartments with 1.30 specific gravity sulfuric acid or water to provide appropriate heat
transfer to the test cell.
32.8.7. Place the test container in water bath with thermostat, (or air oven) which is capable of
maintaining water temperature at 50°C ± 2°C.
32.8.8. Maintain the temperature of test container and the bath at 50°C ± 2°C throughout the test
period.
32.9. PROCEDURE FOR ACCELERATED DEGRADATION TEST
32.9.1. Set up the test assembly as described in Subsection 32.88 and shown in Figure 32.3.
32.9.2. After wiring as shown in Figure 32.1, turn on the power. Adjust current to 2.5 A before
commencement of testing.
32.9.3. Set the voltage recorder paper so that one can see the timer easily.
32.9.4. Start the test.
32.9.5. Initial electrolyte level should be maintained by adding distilled water when the level
decreases during the prolonged test period.
32.9.6. Terminate the test when either the voltage fluctuates more than 0.2 V/minute or if a short
circuit occurs. Note time (in hours) and type of failure.
32.10. REPORT
32.10.1. Report
32.10.1.1. If following the protocol in Subsection 32.1.2.1, report whether the material passed or failed
and the length of time used.
32.10.1.2. If following the protocol in Subsection 32.1.2.2, report the time to failure in hours and method
(Subsection 32.9.6).
32.11.1. Precision
32.11.1.1. No statement on precision can be made.
32.11.2. Bias
32.11.2.1. No statement on bias can be made due to a lack of standard reference material.
99
BCIS-03B Rev. DEC02
33. STANDARD TEST METHOD TO DETERMINE ELEMENTAL CHLORINE IN SULFURIC

ACID SOLUTIONS BY INDUCTIVELY COUPLED ARGON PLASMA OPTICAL EMISSION
SPECTROSCOPY (ICP/OES)
33.1. SCOPE
33.1.1. This procedure provides a method for determining the leachable elemental chlorine from
battery separators by Inductively Coupled Argon Plasma Optical Emission Spectroscopy
(ICP/OES) at a wavelength of 134.724 nm. This low UV ICP emission spectrometer is
specially designed for analysis of atomic line emissions down to 120.000 nm (ref. 2.1, 2.2,
2.3, 2.4). The separator leach solution (ref. 2.5, 2.6) is analyzed directly for chlorine along
with other leachable elemental impurities. No additional sample preparation is needed as
required by other methods.
33.1.2. Interference's such as bromide and Iodide do not affect the ICP/OES analysis because the
ICP/OES is measuring chloride directly and not a precipitate (ref. 2.7, 2.8). Chloride
concentrations can be measured down to 1.0 part per million (ppm) in solution by the
ICP/OES method.
33.1.3. The type of ICP/OES needed for this method is quite specific: Most units will not meet these
requirements. A unit must be able to read the atomic line spectra for chloride that is at
134.724 nm.
33.2.1. Spectro Analytical Instruments, News of the Americas, “New Spectro M120 ICP”, spring
1998.
33.2.2. JY Emission Horiba Group, The SpectraLink, “Analysis of Chlorine in an Aqueous Matrix”,
Vol. 1, issue 1, September 1998.
33.2.3. LaFreniere, B.R.; Houk, R.S.; Fassel, V.A. Anal. Chem. 1987, 59, 2276-2282.
33.2.4. Denton, M.B.; Pilon, M.J.; Babis, J.S., Appl. Spectrosc. 1990, 44, 975-978.
33.2.5. BCI Standard Test Method for Acid Extraction By Acid Reflux, BCIS-03B Subsection 20.
33.2.6. BCI Standard Test Method for Acid Extraction By Hot Acid Soak, BCIS-03B Subsection 21.
33.2.7. BCI Standard Test Method for Chloride Analysis By Atomic Absorption Spectrophotometer
(AAS), BCIS-03B Subsection 25
33.2.8. BCI Standard Test Method to Determine Chlorides in Sulfuric Acid By Turbidimetry, BCIS-
03B Subsection 26.
33.3.1. Soluble chloride in battery electrolyte can increase the rate of positive grid corrosion and can
increase the solubility of active material in the electrolyte.
33.4. APPARATUS
33.4.1. All reagents must conform to American Chemical Society (ACS) reagent grade specifications
(chlorine free).
33.4.2. Purified water must be Type I, 18 MΩ•cm.
100
BCIS-03B Rev. DEC02
33.4.3. Matrix matched Calibration Standards made from chlorine free elemental stock solutions.
33.4.4. Concentrated sulfuric acid (18 M).
33.4.5. Spectro’s M120 ICP, low UV ICP/OES (down to 120.000 nm) or equivalent instruments that
can read down to 120.000 nm.
33.4.6. Purified Water System.
33.4.7. Pipettes, 0.05 to 10.0 mL.
33.4.8. Class A, volumetric flasks, 10, 25, 50, 100, 1000 ml.
33.4.9. Analytical balance with 3 decimal place accuracy.
33.5. SAFETY
33.5.1. The operator must be familiar with the Material Safety Data Sheets for all reagents used and
follow company Standard Operating Procedures. Always wear lab coats, safety glasses, and
protective gloves (powder free). Know where safety showers and eyewash stations are in
case of accidental contact. Always wash hands thoroughly after reagent use.
33.5.2. Always handle all reagents and prepare sample solutions in an acid fume hood.
33.5.3. Sulfuric acid and water mixing can be a violent exothermic reaction if improper mixing takes
place. Always add sulfuric acid very slowly to water under agitation, and the solution will
generate heat, but under controlled conditions. It is important to agitate the dilution too avoid
the possibility of a thermal gradient breaking the glass.
33.5.4. Follow site disposal procedures for old samples and unwanted reagents.
33.6. PREPARATION
33.6.1. No further preparation is needed for the resulting leached solution which is 1.265 g/mL
sulfuric acid obtained by following BCIS-03B Subsection 20: Standard Test Method for Acid
Extraction by Acid Reflux- Procedure A-1 or BCIS-03B Subsection 21: Standard Test Method
for Hot Acid Soak-Procedure A-2.
33.6.1.1. Either method can be used.
33.6.1.2. The procedure used should be reported, either BCIS-03B Subsection 21.
33.6.2. Prepare two to three matrix matched calibration standards from 1.000 μg/ml Cl to 50.00 μ
g/ml Cl in 1.265 g/mL sulfuric acid.
33.6.2.1. Failure to have exactly the same acid concentration in the standards as in the samples will
lead to inaccurate results.
33.6.3. If the calibration standards are made in sulfuric acid solutions other than 1.265 g/ml sulfuric
acid solutions, then the leach sample solution must be diluted so that the resulting diluted
leach sample solution matches the sulfuric acid concentration of the calibration standards.
Then an appropriate dilution factor is calculated and is used to obtain the original
concentration in the 1.265 g/ml sulfuric acid leach solution.
Note: Failure to have exactly the same acid concentration in the standards as in the
sample will lead to inaccurate results.
101
BCIS-03B Rev. DEC02
33.7. PROCEDURE
33.7.1. Calibrate low UV ICP/OES.
33.7.2. Run samples directly using a dilution factor of 0.79. The dilution factor will convert the result
from μg/mL to μg/g.
33.7.3. If the original leach sample was diluted as described in Subsection 33.6.3, then the dilution
factor for the μg/mL to μg/g conversion will be different and it will have to be determined by
the user.
33.8. CALCULATION
33.8.1. Calculations are done using the instrumental software and the results are reported as μg/g Cl
in the sample.
Report the leaching procedure used
Comparative Data for Chloride Analysis
Table 1
ICP/OES Turbidemetric
Low UV method
No. (mg/kg Cl) (mg/kg Cl)
Test Period (9/98-11/98) ('96 - '98)
1 51.1 45.1
2 49.0 45.4
3 53.1 46.6
4 49.0 45.3
5 53.7 46.5
6 50.4 47.4
7 50.4 47.6
8 49.0 44.2
9 49.9 47.3
average 50.6 46.2

std.dev. 1.7 1.2
3 std dev. 5.1 3.6
Theoretical 48.0 48.0

% Difference 5.4 -3.8
102
BCIS-03B Rev. DEC02
Note: Each of the above tests represent different samples
Table ll
Table II
Supplemental Individual Data Points
1070 acid 10.5 10.4

water soln. #1 21.9 20.0
water soln. #2 21.0 19.2
water soln. #3 26.9 25.6
water soln. #4 26.8 25.0
water soln. #6 14.8 14.3
water soln. #7 <1 <1
Note: Above ICP/OES and Turbidity analysis conducted on each sample for side-by-side
comparison
103
BCIS-03B Rev. DEC02
34. STANDARD TEST METHOD TO DETERMINE CHLORIDES BY POTENTIOMETRIC

CHLORIDE DETERMINATION IN AQUEOUS EXTRACTS
34.1. SCOPE
separators by the use of aqueous extracts with a silver nitrate solution and potentiometric
titration, to determine the chloride content.
34.2.1. Hockgesang, Frank P., in "Treatise on Analytical Chemistry", Pt. I, V.5, Ch.63, I.M. Kolthoff &
34.2.2. BCI Standard Test Method for Chloride Analysis by Atomic Absorption Spectrophotometer
(AAS). BCIS-03B Subsection 25.
34.2.3. BCI Standard Test Method to Determine Chlorides in Sulfuric Acid by Turbidimetry, BCIS-
03B Subsection 26.
34.2.4. BCI Standard Test Method for Chloride by Ion Specific Electrode, BCIS-03B Subsection 27.
34.2.5. BCI Standard Test Method to Determine Elemental Chloride in Sulfuric Acid Solution by
Inductively Coupled Argon Plasma Optical Emission Spectroscopy (ICP/OES), BCIS-03B
Subsection 33.
dependent upon suitable laboratory practice to avoid chloride contamination. An example is
the use of powder-free gloves which are required since the powder typically contains chloride
as a contaminant, or direct contact of the sample with the operators bare hands.
34.3.2. This is one of five BCI methods for the determination of soluble chloride in battery separator.
This method may provide different results than other BCI chloride methods.
34.4. APPARATUS
34.5. REAGENTS
34.5.1. All reagents must conform to ACS reagent grade specifications.
34.5.2. Water must be deionized and distilled (Class 1).
34.5.3. Silver Nitrate (AgNO3 solution 0.01 N).
34.5.4. Chloride Standard Solution ( 20 mg Cl/ l Acetic Acid).
34.5.5. Reference certified solution, e.g. NIST SRM 3182, or equivalent.
34.6. EQUIPMENT
34.6.1. All volumetric glassware must be equivalent to "Class A" as defined by NIST circular 602.
34.6.2. Titrator, e.g. Mettler DL40 or equivalent.
104
BCIS-03B Rev. DEC02
34.6.3. Silver Electrode, e.g. Mettler’s Model M 141 SC or equivalent.

34.6.4. Pipette - 10 mL
34.6.5. Balance, with a minimum precision of 0.01 g.
34.6.6. 25 mL graduate cylinder.
34.6.7. 100 mL Erlenmeyer Flask.
34.6.8. Laboratory hot plate.
34.7. SAFETY
34.7.1. The operator must be familiar with the MSDS's for sulfuric acid and the other reagents.
is complete or if skin contact is made with the acid.
battery acid.
34.8. PROCEDURE
34.8.1. Weigh out a 2 g sample of separator material. Cut the sample into approximately 10 mm X
10 mm pieces and place into a tared 100 ml Erlenmeyer flask.
34.8.2. Weigh the flask with the sample in it and record the difference between the flask and the flask
with the sample.
34.8.3. Add 50 mL of demineralized water into the 100 mL Erlenmeyer Flask. This level should be at
the 50 mL mark on the flask. Mark the fluid level on the flask.
34.8.4. Place the flask on a hot plate and bring the flask to a boil. After five minutes of boiling,
remove the flask and allow the flask to cool to room temperature.
34.8.5. After the flask has cooled to room temperature, re-adjust the flask with deminerlized water to
the level marked in Step 34.8.3. Swirl the flask.
34.8.6. Decant 25 ml of the supernatant liquid into a 25 ml graduated cylinder. Transfer the
supernatant liquid to the titration vessel.
34.8.7. Add 10 ml of the standard chloride acetic acid solution to the transferred supernatant liquid.
34.8.8. Titrate the sample in the titrator, with a silver electrode, following the manufacturer’s
instructions. Understand and use the manufacture's end point for titration for the equipment
being used. The titrator should be calibrated with a traceable standard following the specific
instructions of the manufacturer. Follow manufacturer’s instruction for calibration of
equipment.
34.8.9. Make a blank solution by following above Steps 34.8.3 to 34.8.8. Run the blank sample,
before and after each test series. Average these two readings. Use this average in Step
34.8.10.
34.8.10. Take the reading of the test specimen directly from the meter. Subtract the average blank
reading from this number and report this value as the results used as the meter reading in
Step 34.10.
34.9. CALCULATION
105
BCIS-03B Rev. DEC02
34.9.1. The Chloride content (μg = Meter reading/ dry sample weight). Meter reading from Step
34.8.10 minus the reading from the blank average reading in Step 34.8.9).
34.10. REPORT
34.10.1. Report the chloride content in μg/g and the method used for extraction.
34.10.2. Report the titrator used.
34.11.1. Precision
34.11.1.1. No statement is made with regards to Precision of this method.
34.11.2. Accuracy
34.11.2.1. No statement is made with regards to the accuracy of this method. It will be dependent on
many factors, such as if all the chloride is leached out and the cleanliness to avoid chloride
contamination of the equipment used and the handling of the specimen.
34.11.2.2. The user should undertake a precision statement from replicate tests using a certified
reference material, e.g. diluted NIST SRM 3182.
106

Technical Manual Section - 03b

Uploaded by

Document Information

Original Title

Copyright

Available Formats

Share this document

Share or Embed Document

Sharing Options

Did you find this document useful?

Is this content inappropriate?

Copyright:

Available Formats

Technical Manual Section - 03b

Uploaded by

Copyright:

Available Formats

BCIS-03B REV.

BCI RECOMMENDED MATERIALS SPECIFICATIONS

1. Standard Test Method for Overall Thickness of Battery Separator........................................... 3

1. STANDARD TEST METHOD FOR OVERALL THICKNESS OF BATTERY SEPARATOR

1.2. SIGNIFICANCE AND USE

1.6.2. Report apparatus type used.

2. STANDARD TEST METHOD FOR OVERALL THICKNESS OF BATTERY SEPARATOR

2.2. SIGNIFICANCE AND USE

2.5.3. Record all readings and locations measured.

3. STANDARD TEST METHOD FOR BACKWEB THICKNESS OF BATTERY SEPARATOR

3.2. SIGNIFICANCE AND USE

3.3.5. Non-fibrous, non-compressible separators, such as polyethylene, PVC, microporous rubber

3.4.4. SHOULDER MINI-RIBS - The ribs in the area of the shoulders.

3.6.2. Center the measurement foot between ribs.

3.7.1. Report all readings per customers / vendor requirements.

3.7.2. Fibrous - nearest 0.1mm or 0.001 in.

3.7.3. Non-Fibrous - nearest 0.01mm or 0.0001 in.

3.7.5. The gauge used and the loading of this gauge.

4. STANDARD TEST METHOD TO DETERMINE SQUARENESS OF BATTERY SEPARATOR

4.2. SIGNIFICANCE AND USE

4.3.2. Steel rule graduated in a 0.5 mm or 1/64 in. increments.

4.5.5. Repeat above procedure after rotating separator 180 degrees.

4.6.1. Report side squareness in mm (in).

4.6.2. Record width and height of the separator in mm (in).

5. STANDARD PROCEDURE TO DETERMINE HEIGHT AND WIDTH OF BATTERY

5.1.2. Method A uses a graduated measuring device, such as a rule or a square.

5.2. SIGNIFICANCE AND USE

5.5.2.5.2. The gauge used and that method B was used.

6. STANDARD TEST METHOD TO DETERMINE THE SKEW OF ROLL STOCK BATTERY

6.2. SIGNIFICANCE AND USE

6.4. SAMPLE PREPARATION

7. STANDARD TEST METHOD TO DETERMINE VOLUME POROSITY AND MOISTURE

7.2. SIGNIFICANCE AND USE:

7.3.1. Balance, accurate to 0.001 grams, such as a Mettler PM 460 or equivalent.

7.3.3. Moisture extraction oven, such as Genlab ME/156/HYD or equivalent.

7.3.5. Distilled or deionized water

7.3.6. Timer, accurate to + 1 second.

7.3.7. Beakers, 1000 ml and 150 ml.

7.4. SAMPLE PREPARATION

7.5.6. Place sample into 1000 ml beaker containing distilled water.

7.5.7. Assemble the density determination kit.

7.5.7.1. Place bridge over balance pan.

7.5.7.3. Place sample support onto wire frame.

7.5.7.4. Tare the balance to zero.

7.5.10. Remove the sample from the sample support.

7.6.1.1. Volume of pores = (Wet Weight in air) - ( Dry Weight).

7.6.1.2. Volume of sample = (Wet Weight in air) - (Wet Weight in water).

7.6.1.3. Volume Porosity, % = (W3 - W1) x 100

7.6.1.4. Moisture, % = W0 - W1 x 100

7.7. PRECISION AND BIAS

7.7.1. Expected reproducibility is ± 1%.

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

8.2. REFERENCE DOCUMENTS

8.2.1. Instruction Manual, Micromeritics Mercury Intrusion Porosimeter.

8.2.2. Instruction Manual, Quantachrome Mercury Porosimeter.

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

8.3. PRINCIPLE OF TEST METHOD

d = (-4Γ cos Θ)/p

8.4. SIGNIFICANCE AND USE

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

8.5.3. Spent oil must be handled as mercury waste.

8.6.1. Micromeritics Mercury Porosimeter

8.6.2. Quantachrome Mercury Porosimeter