Technical manual section 03b

Standard Test Method for Overall Thickness of Battery Separator Including Attached Retainer Mat .... Standard Test Method to Determine Pin Puncture Resistance of Battery Separator Using

Technical Manual

DEC02

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

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

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)

1.2.1 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

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

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

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

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

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

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)

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

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

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

5.5.1.1 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

5.5.2.1 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.)

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

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

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)

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

7.2.1 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

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

7.7.1 Expected reproducibility is ± 1%

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

8.2.1 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

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

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-X-axis

8.9.1 The precision of this method has not been determined

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

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)

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 SIGNIFICANCE AND USE

10.2.1 This procedure is designed to approximate the shrinkage of separators that occurs during air

drying of plates and separators

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

10.4.9 Safety glasses

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)

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 PRECISION AND BIAS

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

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

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

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

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 PRECISION AND BIAS

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 SIGNIFICANCE AND USE

12.3.1 Separator stiffness can influence both handling of battery components during assembly

process and resulting battery performance

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

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 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

12.12 PRECISION AND BIAS

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 T489 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

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 SIGNIFICANCE AND USE

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)

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

13.7.1 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 PRECISION AND BIAS

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

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)

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 SIGNIFICANCE AND USE

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

14.6.1 Report the following:

14.6.2 The instrument used

14.6.3 Record and report the three readings and/or the average in N (lbf)

14.6.4 Report backweb thickness in mm(in.) if required

(Not to Scale) Instron Fixture Figure No 14.1

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 SIGNIFICANCE AND USE

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

15.5.1 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)

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

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 SIGNIFICANCE AND USE

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 APPARATUS AND REAGENTS

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

16.4.3 Follow Federal, State, Local regulations for safe disposal of all chemicals used, including

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

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