Technical manual section 03a

BCI Battery Technical Manual BCIS-03A REV FEB02 Issued Current Revision: 1993-05 2002-02 RECOMMENDED BATTERY MATERIALS SPECIFICATIONS VALVE REGULATED RECOMBINANT BATTERIES TABLE OF CONTENTS 10 11 12 13 14 15 16 17 18 19 20 21 22 23 Organizations for Referenced Test Methods Suppliers of Testing Equipment and Materials Sampling Procedure for Recombinant Battery Separator Mat Standard Test Method for Thickness of Recombinant Battery Separator Mat Standard Test Method for Basis Weight (Grammage) of Recombinant Battery Separator Mat 14 Standard Test Method for Volume Porosity of Recombinant Battery Separator Mats 18 Test for Pore Size by the First Bubble Method Of Recombinant Battery Separator Mat 20 Test for Pore Size by the Liquid Porosimetry Method of Recombinant Battery Separator Mat 23 Test for Pore Size by the Mercury Intrusion Method of Recombinant Battery Separator Mat 28 Test Method for Surface Area of Recombinant Battery Separator Mat 31 Test Method for Determining Percent Moisture Content of Recombinant Battery Separator Mat 34 Test Method For Percent Ignition Weight Loss of Recombinant Battery Separator Mat 36 Test Method for Tensile Strength and Elongation of Recombinant Battery Separator Mat 39 Acid Wetting and Wicking of Recombinant Battery Separator Mat 45 Test Method for Determining the Compressibility of Recombinant Battery Separator Mat 46 Test for Determining Acid Weight Loss of Recombinant Battery Separator Mat (Reflux Method) 48 Extractable Metallic Impurities of Recombinant Battery Separator Mat 51 Extractable Chloride of Recombinant Battery Separator Mat 57 Test Method for Electrochemical Compatibility of Recombinant Battery Separator Mat 58 Total Organic Carbon For Recombinant Battery Separator Mat 71 Identification of Organic Impurities In Recombinant Battery Separator Mat 72 Electrical Resistance of Recombinant Battery Separator Mat 77 Conversion Factors for SI Units 78 BCIS-03a Rev Feb02 ORGANIZATIONS FOR REFERENCED TEST METHODS Referenced Test Method Procurement Addresses 1.1 American National Standard Institute, Inc (ANSI) 1430 Broadway New York, NY 10018 USA Tel: 212-260-5400 1.2 ASTM 1916 Race Street Philadelphia, PA 19103 USA Tel: 212-260-5400 1.3 British Standard Institution Park Street London W1A 2BS, England Tel: 266933 BSI LON G 1.4 Technical Association of Pulp and Paper Industries (TAPPI) PO Box 105113 Atlanta, GA 30348-5113 USA Tel: 800-333-8686 (USA) Tel: 800-446-9431 (Canada) Tel: 404-446-1400 Fax: 404-446-6947 BCIS-03a Rev Feb02 SUPPLIERS OF TESTING EQUIPMENT AND MATERIALS 2.1 Summary The following list of manufacturers and suppliers of testing materials, instruments and machines is published by BCI solely for the convenience of its members BCI has made no investigation of its own with respect to the listed company compliance, however, and makes no certification, representation or warranty, express or implied, with respect to such compliance nor with respect to the quality of performance of such materials, instruments or machines Publication of this list or any reference to it in BCI Test Methods shall not be construed to be any such certification, representation or warranty Any purchaser or user of such material equipment or machinery desiring any certification or warranty with respect thereto must negotiate the same directly with the manufacturer or supplier from whom he makes such purchases This equipment supplier listing is not intended to be inclusive, only a reference point, any manufacturer or supplier wishing to have his name included in this list should direct a request to BCI Headquarters 2.2 General Supplies 2.2.1 Cole-Parmer Instrument Company Vernon Hills, IL 60061 Tel: 800-323-4340 Fax: 847-247-2929 2.2.2 Fisher Scientific 711 Forbes Avenue Pittsburgh, PA 15219 2.2.3 Nalge Company Rochester, NY 14602-0365 Tel: 716-586-8800 2.2.4 Omega Engineering, Inc PO Box 4047 Stamford, CT 06907 2.2.5 SGA Scientific Inc 735 Broad Street Bloomfield, NJ 07003 Tel: 800-245-2300 2.2.6 Thomas Scientific 99 High Hill Road PO Box 99 Snedesboro, NJ 08085-0099 Tel: 800-345-2100 2.2.7 VWR Scientific Products 1310 Goshen Pkwy West Chester, PA 19380 Tel: 610-431-1700 2.2.8 EG&G, Princeton Applied Research PO Box 2565 BCIS-03a Rev Feb02 Princeton, NJ 05840 Tel: 609-452-2111 2.3 Surface Area (1) and Porosity (2) 2.3.1 Coulter Electronics, Ltd (2) Northwell Drive Luton, Beds LU3 3RH England Tel: (0582) 582442 590 West 20 Street Hialeah, FL 33010 Tel: 305-885-0131 Tel: 800-653-4306 2.3.2 Micromeritics Instruments (1) (2) One Micromeritics Drive Norcross, GA 30093 Tel: 770-662-3633 2.3.3 Quantachrome Corporation (1) (2) 1900 Corporate Drive Boynton Beach, FL 33426 2.3.4 PMI (Porous Material, Inc.) (2) 83 Brown Road Ithaca, NY 14850 Tel: 607-257-5544 Tel: 800-332-1764 2.4 Atomic Absorption 2.4.1 Spectro Analytical Institute 160 Authority Drive Fitchburg, MA 01420 Tel: 2.4.2 Spectra Instrumentation 11850 Industrial Court Auburn, CA 95603 Tel: 916-823-1638 2.4.3 Buck Scientific, Inc 58 Fort Point Street East Norwalk, CT 06855-1097 203-853-9444 2.4.4 Cathodeon, Ltd Nuffield Road Cambridge, England CB4 1TW Tel: 1-022-346-0100 2.4.5 Fisons Instruments, Inc 24911 Avenue Sanford Valencia, CA 91356 Tel: 800-551-8741 BCIS-03a Rev Feb02 2.4.6 Leeman Labs, Inc 600 Suffolk Street Lowell, MA 01854 Tel: 508-454-4442 2.4.7 The Perkin-Elmer Corp Norwalk, CT 06859-0177 Tel: 800-762-4000 2.4.8 Phillips Export B.V Lelyweg Almelo, Netherlands 7602EA Tel: 1054-903-9440 2.4.9 Preiser Scientific, Inc 94 Oliver Street St Albans, WV 24177 Tel: 800-624-8285 2.4.10 Spectro Products, Inc 385 State Street North Haven, CT 06473 Tel: 203-281-0122 2.4.11 Biomed Instruments, Inc 1020 S Raymond Ave., No B Fullerton, CA 92631 Tel: 714-870-0290 2.4.12 Stackpole/Ultra Carbon PO Box X924 Baycity, MI 48707 Tel: 517-894-2911 2.4.13 Thermo Jerrell Ash Corp Forge Pkwy Franklin, MA 02038 Tel: 800-225-4087 2.4.14 Varian Instrument Group 220 Humboldt Court Sunnyvale, CA 94089 Tel: 800-231-8134 2.4.15 VWR Scientific Products 1310 Goshen Pkwy West Cjester {A 19380 Tel: 215-891-2782 2.5 Thickness (1) and Tensile (2) 2.5.1 Customer Scientific Instruments, Inc (1) 13 Wing Drive Kearny, NJ 07927 Tel: 201-538-8500 BCIS-03a Rev Feb02 2.5.2 EMUECO Inc (1) PO Box 16 Newberg, OR 97132 Tel: 503-538-8616 2.5.3 Huygen Instruments Assoc (1) 8782 Gull Road Richland, MI 49083 Tel: 816-629-5824 2.5.4 Instron Corporation (2) 2500 Washington Street Canton, MA 02021 2.5.5 H.E Messmer, Ltd 144 C Off Road London N1 1NS England Tel: 01-607-2416/7 2.5.6 Testing Machines Inc (1) (2) 400 Boyview Avenue Amityville, NY 11701 Tel: 516-842-5400 2.5.7 Thwing-Albert Instrument Co (1) (2) 10960 Dutton Road Philadelphia, PA 19154 Tel: 215-637-0100 2.5.8 Tinius Olsen Testing Machine Co (2) Easton Road Willow Grove, PA 19090-0429 Tel: 215-675-7100 2.5.9 B.C Ames Co (1) 131 Lexington Street Waltam, MA 02254-0070 Tel: 617-893-0095 BCIS-03a Rev Feb02 SAMPLING PROCEDURE FOR RECOMBINANT BATTERY SEPARATOR MAT 3.1 Scope 3.1.1 This method summarizes sampling requirements for recombinant battery separator mat (RBSM) and outlines the sample size needed for each BCI RBSM Test Method 3.1.2 Prior to purchase, there should be agreement between supplier and purchaser on details of the sampling and acceptance procedure as well as on the required physical and chemical properties, dimensional tolerance, etc., and the test methods to be employed to determine frequency (and/or need) of testing 3.2 Reference Documents 3.2.1 BCI’s RBSM Test Methods, BCIS-03a 3.2.2 TAPPI’s T 400 – Sampling and accepting a single lot of paper, paperboard, fiberboard, or related product 3.2.3 ASTM’s – D585 – Sampling and accepting a single lot of paper, paperboard, fiberboard, or related products 3.3 Terminology 3.3.1 LOT – a quantity of RBSM of a single grade, making (manufacture run), grammage, and thickness about which it is desired to make a judgement (usually as to conformance to specification) by examining or testing a small fraction called the sample 3.3.2 SAMPLE – a specified number of test units selected according to a prescribed procedure to represent a lot Each test method should be reviewed for any special procedures 3.3.3 TEST UNIT – an area of RBSM sufficient to obtain a single adequate set of test result for all the properties to be measured 3.3.4 SPECIMEN – a test unit, or a portion of a test unit, upon which (for a specified property) a single test determination is to be made 3.3.5 TEST DETERMINATION – the process of carrying out the series of operations specified in the test method whereby one or more readings (observations) are made on a test specimen and the observations combined to obtain the value of a property of the test specimen, or the value obtained by the process 3.3.6 TEST RESULT – the value obtained for one test unit of the sample by carrying out the complete protocol of the test method, the value being (as specified in the test method) either a single test determination or specified combination of a number of determinations 3.3.7 ROLL – A coil of RBSM of continuous length 3.3.8 QUALIFICATION 3.3.8.1 RBSM test which are done for initial acceptance of vendor’s material 3.3.8.2 An agreement between user and supplier on subsequent testing frequency 3.4 Procedure BCIS-03a Rev Feb02 3.4.1 RBSM generally is a very delicate product Any rough handling or misuse of the test specimen may result in test results, which are not representative of the material 3.4.2 RBSM may have specific aging characteristics These aging characteristics may have no effect on the RBSM performance inside a battery but will result in different results of physical properties such as tensile and elongation This aging effect is believed to be accelerated by hot and humid conditions 3.4.3 If a lot number or roll identification system is needed then reference should be made to either TAPPI’s T400 or ASTM’s D-585 for guidance 3.4.4 Table No should be referenced for a summary of test specimens needed and the size of each specimen Table No Test Method Thickness Sample Size Needed 1000 cm2 Frequency (Per Lot) per roll Grammage Volume Porosity Pore Size 1000 cm2 1000 cm2 300 cm2 per roll Qualification Qualification Surface Area 10 g Qualification Moisture Content Ignition Loss Tensile and Elongation 10 g g 25 x 150 mm – strips per roll Qualification Qualification Comments Thickness should be checked right after sampling Moisture must be subtracted Use thickness and grammage results RBSM, which has been densified, will give smaller pore size values Sample size depends of sample surface area and may vary depending on whether the test specimen is taken from the wire of felt side of the RBSM Tensile is extremely sensitive to handling Sufficient sample should be obtained to cut strips without any damage 1000 cm2 Qualification Compression g Qualification Acid Weight Loss g Qualification Extractable Metal Analysis No Method Qualification Extractable Chlorine Analysis x 10 cm Qualification Electrochemical Compatibility Qualification Organic Impurities Variable Variable When Required Organic Identification Notes: Remove the outer two wraps before sampling BCIS-03a Rev Feb02 STANDARD TEST METHOD FOR THICKNESS OF RECOMBINANT BATTERY SEPARATOR MAT 4.1 Scope 4.1.1 This method covers the determination of the thickness of recombinant battery separator mat (RBSM) which is used in a recombinant lead acid cell This method is to be used, except as otherwise required by materials specification 4.1.2 This method covers RBSM from 0.127 mm (0.005 in) to 3.048 mm (0.125 in) 4.1.3 This method covers measurement of RBSM using a pressure of 10 kPa (1.5 psi) and a 29 mm (1.14 in) presser foot 4.2 Referenced Documents 4.2.1 ASTM Standards 4.2.1.1 ASTM D-374 Standard Test Method for Thickness of Solid Electrical Insulation 4.2.1.2 ASTM D-645 Standard Test Method for Thickness of Paper and Paperboard ISO No 534 4.2.2 TAPPI Standards T 411 Thickness (Caliper) of Paper and Paperboard 4.3 Significance Thickness and its consistency is an important property of RBSM RBSM is used at various thicknesses and degrees of compression The thickness of RBSM allows for the proper selection of the mat for a given cell construction and the electrical characteristics desired 4.4 Description of Terms 4.4.1 RECOMBINANT BATTERY SEPARATOR MAT (RBSM) – Any material intended for use as a separator between the cathode and anode plates in a VRLA battery 4.4.2 THICKNESS – The perpendicular distance between the two principal surfaces of a material, as determined by the prescribed procedure 4.5 Apparatus 4.5.1 Method A – Manually-Operated Dead Weight Type Thickness Gauge 4.5.1.1 The gauge shall be a dead-weight type having a presser foot and a lower anvil parallel to within 0.002 mm (0.0001 in) The presser foot shall move on an axis perpendicular to the anvil face 4.5.1.2 The diameter of the presser foot and anvil shall measure 29 mm (1.14 in) The presser foot shall apply pressure of 10 ± 0.6 kPa (1.5 psi) on the specimen 4.5.1.3 If a dial gauge is used, the dial spindle shall be vertical The dial shall be at least 50 mm (2 in) in diameter and shall be continuously graduated to read directly to 0.002 mm (0.0001 in) If necessary, it will be equipped with a revolution counter recording the number of complete revolutions of the large hand The dial indicator shall be essentially friction free BCIS-03a Rev Feb02 4.5.1.4 The indicator shall give readings repeatable to 0.001 mm (0.00004 in) at a zero setting or on a steel gauge block 4.5.1.5 The frame of the indicator shall be of such rigidity that a load of 13 N applied on the dial housing, out of contact with either the weight or the presser foot spindle, will produce a deflection of the frame not greater than the smallest division on the indicator 4.5.2 Method B – Motor-Operated Dead Weight Gauge: 4.5.2.1 Except as additionally defined in this Subsection, the instrument shall meet the requirements of 4.5.1.1 4.5.2.2 The dead weight dial spindle shall be raised and lowered by a constant-speed motor through a mechanical linkage such that the rate of descent (for a specified range of distance between the presser foot and the anvil) and the dwell time on the specimen are within the limits specified for the material being measured Downward force on the presser foot shall be only that of gravity on the weighted spindle with no addition from the lifting-lowering mechanism 4.6 Calibration (General Considerations for Care, Use and Calibration of Thickness Measuring Apparatus) 4.6.1 Surfaces of Micrometer Apparatus 4.6.1.1 Cleaning Surfaces of Micrometers – Before and during instrument calibration and thickness measurements, the micrometer surface shall be maintained in a clean condition Cleaning can be accomplished by pulling through a sheet of smooth paper Warning When using a motorized micrometer, caution should be exercised in pulling a sheet of RBSM through the anvil while in motion, since this may negatively effect the life of the instrument 4.6.1.2 Parallelism of Surfaces of Micrometers: 4.6.1.2.1 A hardened calibrated gauge or a calibrated tread measuring cylinder of suitable dimensions to fit conveniently between the presser foot and the anvil of the thickness gauge shall be measured at several locations Note the maximum variations of readings 4.6.1.2.2 In calibrating the gauge, it is important that the gauge block or cylinder is inserted only under the edge of the pressure foot 4.6.1.3 Flatness of Surfaces of Micrometers: 4.6.1.3.1 The anvil and spindle surfaces of the micrometer shall be flat to within 0.0013 mm (0.00005 in) The flatness may be determined by use of an optical flat 4.6.1.3.2 A flat surface forms straight, parallel, and equidistant fringes 4.6.1.3.3 A grooved surface forms straight parallel fringes at unequal intervals The estimated maximum displacement of any line from its normal position, where all lines would be equidistant, is a measure of deviation from flatness 4.6.1.3.4 A symmetrical concave or convex surface forms concentric circular fringes, and their number is a measure of deviation from flatness 10 BCIS-03a Rev Feb02 and 5mA Average the voltage difference and report as the change in anodic polarization Example (Figure 19.6) Pure Acid Pure Acid Pure Acid Pure Acid Pure Acid Pure Acid Pure Acid Leach Polarization @3mA 1.658 1.610 1.604 1.603 1.603 1.602 1.602 1.601 -1 @4mA 1.661 1.626 1.621 1.620 1.619 1.619 1.619 1.617 -2 @5mA 1.671 1.638 1.632 1.631 1.631 1.631 1.630 1.629 -1 Avg = -1mV 19.6.3.3.6 In addition, the anodic scan in pure acid after cycling (see Figure 4) shall be compared to the scan in the acid leach solution to determine the following: Figure 19.4 – Anodic Scan 19.6.3.3.6.1 Changes in the current voltage characteristics of the charge (PbSO4 PbO2) – discharge (PbO2 - PbSO4) peaks 19.6.3.3.6.2 Presence of additional peaks which may represent secondary or simultaneous reactions 64 BCIS-03a Rev Feb02 Figure 19.5 – Cathodic Scan of Disc Electrode Figure 19.6 – Anodic Scan of Disc Electrode 19.7 Report 19.7.1 Cathodic Scans Report values obtained from graph of cathodic scans Figure 19.7.1.1 Cathodic voltage shift (hydrogen) Report average voltage shift between last curve of standard pure acid and leach acid at 2mA and 3mA as shown in Paragraph 19.6.3.2.6 19.7.1.2 Cathodic Current charge Peak Report percent of charge peak current of leach to charge peak current of standard acid Example (Figure 19.5): 19.7.1.3 current, mA (leach / current, mA (standard) x 100 = 0.83 / 0.94 x 100 = 88% charge peak of standard Cathodic Voltage Charge Peak Report voltage charge peak shift between standard acid and leach acid 65 BCIS-03a Rev Feb02 Example (Figure 19.5): 19.7.1.4 Cathodic Current discharge Peak Report percent of discharge peak current of leach acid to that of standard acid Example (Figure 19.5): 19.7.1.5 voltage, mV (standard) – voltage, mV (leach) = (-990 mV) – (-993 mV) = +3 mV shift current, mA (leach) / current, mA (standard) x 100 = 1.90/2.40 x 100 = 79% discharge peak of standard Cathodic Voltage Discharge Peak Report voltage discharge peak shift between standard acid and leach acid Example (Figure 19.5): Voltage, mV (standard) – voltage, mV (leach) = (-898 mV) – (-900 mV) = + mV shift 19.7.2 Anodic Scans – Report values obtained from graph of anodic scans Figure 19.6 19.7.2.1 Anodic Voltage Shift (Oxygen) Report average voltage shift between last curve of standard pure acid and leach acid at 3, 4, and mA as shown in Paragraph 19.6.3.3.5 19.7.2.2 Anodic Current Charge Peak Report percent of charge peak current of leach solution to that of standard acid Example (Figure 19.6): 19.7.2.3 Anodic Voltage Charge Peak Report voltage charge peak shift between standard acid and leach acid Example (Figure 19.6): 19.7.2.4 current, mA (leach) / current, mA (standard) x 100 = 5.69 / 5.95 x 100 = 07% discharge peak of standard Anodic Voltage Discharge Peak Report voltage discharge peak shift between standard acid and leach acid Example (Figure 19.6): 19.8 Voltage, mV (standard) – voltage mV (leach) = 1357 mV – 1370 mV = 13 mV shift Anodic Current discharge Peak Report percent of discharge peak current of leach acid to that of standard acid Example (Figure 19.6): 19.7.2.5 current, mA (leach) / current, mA (standard) x 100 = 0.83 / 0.99 x 100 = 88% charge peak of standard voltage, mV (standard) – voltage, mV (leach) = 1030 mV – 1033 mV = mV shift Precision and Bias The precision of this test method has not been determined 19.9 Appendix 1: Pre-Electrolysis of Acid Preparation of Pure Acid 19.9.1 Prepare eight liters of 1.210 s.g sulfuric acid from reagent grade concentrated acid and deionized water 66 BCIS-03a Rev Feb02 19.9.2 Insert two cleaned 13 cm x 15 cm (5 1/8 in x 29/32 in) 99.999% lead electrodes with 12.7 mm (1/2 in) grids into the acid Connect the positive lead from the power supply to the positive lead electrode and the negative lead to the negative electrode 19.9.3 Turn on power supply and increase the voltage until there is visible gassing from both electrodes Check the current after hour of electrolysis and adjust it to a level of 1.0 to 1.5 amps 19.9.4 Allow the electrolysis of the acid to continue for 24 hours Remove the lead electrodes and turn off the power supply Allow the acid to outgas for one hour Then store the acid in glass bottles 19.10 Appendix 19.10.1 Fabrication of the Rotating disc Electrode 19.10.1.1 In the fabrication of the rotation disc electrode, it is essential that there are no voids in the lead rod or the epoxy jacket The lead rod, if cast, must be made in a mold (Figure A) whose cavity is fed via the bottom of the mold with a 6.3 mm (1/4 in) hole and using lead at a temperature 550°C (1022°F) tends to form reproducible and uniform castings Prior to encapsulation in epoxy, the lead rod is cleaned with 600 micron aluminum oxide wet or dry abrasive paper It is preferable to provide a constant washing during the cleaning process to keep the abrasive paper from clogging with lead Figure 19.A – Split Hold for Casting Lead Rod (Aluminum) 19.10.1.2 A concentric holding piece (Figure 19.B) is fitted over one end of the lead rod The lead rod, with holding piece, is then mounted in the 12.7 mm (1/2 in) diameter mold (Figure 19.C), which has been sprayed with Teflon, allowing 3.2 mm of the lead rod to protrude from the end of the mold 67 BCIS-03a Rev Feb02 Figure 19.B – Concentric Holding Piece (Polyethylene) Figure 19.C – Split Mold for Casting Epoxy Jacket 19.10.1.3 Epoxy resin (Araldite 502 and Hardener 951) which has been preevacuated to remove all air bubbles is then carefully poured into the 12.7 mm (1/2 in) mold around the lead rod It is best to this under a vacuum; i.e., in a vacuum desiccator equipped with an addition funnel to facilitate addition of the epoxy to the mold which is standing upright in the desiccator When the mold is filled with epoxy resin, a second concentric holding piece is then pressed over the end of the protruding lead rod and pushed into the 12.7 mm (1/2 in) diameter cavity The resin is allowed to pre-cure for four hours after which time the mold is placed in a 93°C (200°F) oven for three hours as a final cure After it has cooled, open the mold and remove the holding pieces from the ends of the lead rod and cut it into two equal sections using a saw 68 BCIS-03a Rev Feb02 19.10.1.4 Machine the ends of the pieces, make a small shallow hole in one end of each and solder a cm (25/32 in) piece of 0.508 mm (20 mil) platinum wire onto the end (The hole serves to hold the Pt wire in position while soldering) Place the rod in the lathe and machine off enough of the outside area of the Pt wire end so that the lead forms a 3.2 mm (1/8 in) long nub which makes a snug fit inside a piece of mm (15/64 in) glass tubing 19.10.1.5 Take a 170 mm long piece of mm (15/64 in) glass tubing, polish the ends, and slide a concentric holding piece of 80 mm (3 5/32 in) onto one end Put a dab of epoxy over the lead protrusion at the base of the platinum wire and fit the long end of the glass tubing over the platinum wire and lead tip (epoxy should fill 3.2 mm (1/8 in) of the glass tubing) The entire assembly is mounted in the 12.7 mm (1/2 in)diameter mold which has been sprayed with Teflon mold release (Figure 4) until the epoxy is cured The clamping pressure on the mold is released and the entire assembly is pushed upward in the mold such that the concentric holding piece is 25.4 mm (1 in) above the top of the mold The clamping screws are then retightened Approximately ml of epoxy is added into the mold and allowed to run down the sides and the concentric holding piece is pressed into the mold opening After two hours of pre-cure at room temperature, the mold is placed in a 93°C oven for three hours, allowed to cool, and the finished electrode removed 19.10.1.6 The electrode can then be dressed and filled with mercury to make contact with the platinum filament of the rotator 19.10.1.7 Throughout the fabrication of this electrode it must be stressed that the epoxy resin must be pre-evacuated to remove all entrained air In general, it can be stated that it is the small bubbles of entrained air which cause instability and inconsistent scans 19.10.2 Machining of the Face of the Disc Electrode 19.10.2.1 In the evaluation of electrochemical Compatibility it is critical that the surface of the electrode is clean; that all traces of previous sample scans are removed, and that the texture of the surface can be reproduced consistently 19.10.2.2 To this end, the tool edge (Figure D) must be very sharp The tool is first ground to the proper configuration on a medium grit grind wheel The upper flat surface is then lightly deburred by rubbing the surface over a piece of 600 micron grit paper which is placed on a flat surface Polish the curved surface of the tool by repeatedly rubbing it over the 600 micron paper until the tool edge is smooth and free of all rough edges Be careful not to cause the sharp edge to dig into the grit paper as it will easily dull the tool Figure 19.D – Cutting Took (High Speed Tool Steel) 69 BCIS-03a Rev Feb02 19.10.2.3 Mount the tool in the tool holder such that the leading edge passes exactly through the rotational axis of the lathe spindle and approaches the electrode at a 30 to 45 degree angle (Figure 19.E) Figure 19.E 19.10.2.4 Adjust the motion of the tool table such that its motion perpendicular to the axis of the spindle is offset by 2° as per Figure 19.D This is extremely important since it prevents “smearing” of the lead surface as the tool edge passes through the rotational axis of the electrode 19.10.2.5 To obtain a smooth easily reproducible surface the spindle should have a rotational speed of 900 rpm and the feed rate of the tool should be 25.4 mm/min (1.0 in/min) To resurface the disc electrode position the electrode in the lathe chuck and clamp lightly with the set screw With the spindle rotating at 900 rpm bring the tool into contact with the face of the electrode and then retract the tool with the feed screw Using the axial screw turn the tool 0.127 mm (0.005 in) into the electrode and again using the feed screw, pass the tool across the face of the electrode at a rate of 25.4 mm/min (1.0 in/min) Loosen the set screw and remove the electrode from the spindle 19.10.2.6 Always be careful, particularly after polishing, not to touch the face of the electrode against anything as it may become contaminated 70 BCIS-03a Rev Feb02 20 TOTAL ORGANIC CARBON FOR RECOMBINANT BATTERY SEPARATOR MAT The industry at this time is unable to offer a recommendation of any one procedure over another Current practice employs several different test procedures for Total Organic Carbon (TOC) of recombinant battery separator mat (RBSM) For those interested in reviewing examples of test methods for the measurement of TOC in RBSM, several procedures are on file at BCI Additional comments or examples of test methods of TOC may be submitted to BCI for inclusion to this file 71 BCIS-03a Rev Feb02 21 IDENTIFICATION OF ORGANIC IMPURITIES IN RECOMBINANT BATTERY SEPARATOR MAT 21.1 Scope 21.1.1 This test procedure covers the qualitative identification of organic impurities in recombinant battery separator mat (RBSM) 21.1.2 A sample of RBSM is extracted with an organic solvent (e.g chloroform) After evaporation of the solvent, an infrared spectrum is run on the residue The contaminant spectrum is compared to published reference spectra and/or spectra that have been run on suspected sources of contamination 21.1.3 Other spectral techniques, such as ultraviolet, near-infrared, far-infrared and nuclear magnetic resonance may also be useful Chromatographic techniques may be useful in separating mixtures of extracted organic contaminants 21.2 Referenced Documents 21.2.1 Sadtler Spectra Collections; Sadtler Research Laboratories, Inc 21.2.2 Infrared Analysis of Polymers, Resinsand Additives – An Atlas – Volumes I & II; Hummel D.O and Scholl, F; Wiley Interscience (1969) 21.2.3 Identification and Analysis of Surface-active Agents by Infrared and Chemical Methods; Hummel, D.; Interscience Publishers (1962) 21.2.4 Identification and Analysis of Plastics; Haslam, J and Willis, H.A.; Van Nostrand (1965) 21.2.5 An infrared Spectroscopy Atlas for the coating Industry; Federation of Societies for Coatings Technology (1980) 21.2.6 The Aldrich Library of Infrared Spectra; Pouchert, C J.; Aldrich Chemical Company 21.2.7 Perkin-Elmer Infrared Application Studies and Perkin-Elmer Infrared Bulletins; Instrument Division, Perkin-Elmer Corporation 21.3 Significance and Use Some organic impurities in RBSM may adversely affect the performance of RBSM by oxidation to gaseous products, causing pressure build up in the battery; by oxidation to acetic acid and other lower organic acids resulting in reaction with the grids and subsequent deposit of lead during battery cycling; or by direct reaction with gaseous oxygen 21.4 Apparatus 21.4.1 Infrared or FTIR spectrometer 21.4.2 Sodium chloride salt plates 21.4.3 Infrared solvent cell with sodium chloride windows 21.4.4 Thermostat controlled electric drying oven 21.4.5 Ventilated fume hood 72 BCIS-03a Rev Feb02 21.4.6 Hot plate-magnetic stirrer 21.4.7 Erlenmeyer flasks (125 ml and 250 ml), flat bottom, with ground glass joints 21.4.8 Soxhlet extractor 21.4.9 Reflux condenser, Liebig or Fredricks 21.4.10 Magnetic stirring bar 21.4.11 Funnel 21.4.12 Filter paper, fast running (Whatman No 4), fluted 21.4.13 Boiling stones 21.4.14 125 ml Erlenmeyer flask 21.4.15 10 ml Erlenmeyer flask 21.4.16 Watch glass, Pyrex (7 or inch diameter (178 mm or 203 mm)) 21.4.17 Scalpel 21.4.18 Spatula (small) 21.4.19 Medicine dropper 21.4.20 Needle probe 21.4.21 Ringstand and clamps 21.4.22 Long tweezers 21.5 Reagents and Materials 21.5.1 Purity of Reagents – The use of spectroanalyzed organic solvents is recommended 21.5.2 The Choice of extraction solvent(s) is at the discretion of the analyst and will depend on the chemical nature of the suspected contaminant Solvents recommended for consideration include chloroform, carbon tetrachloride, methanol, and acetone and hexane 21.6 Sampling 21.6.1 Each occurrence of organic impurities in RBSM may differ, thus some judgment must be used in sampling and sample preparation Since the weight of impurity compared to the RBSM is usually quite small, the objective is to extract as much of the impurity as possible 21.6.2 In cases in which the impurity is present as visual spots or streaks on the surface of the mat, remove the spots (streaks) with a needle probe, taking a minimum amount of adjoining mat 21.6.3 For surface coatings or discoloration, remove the contamination along with a thin layer of RBSM for extraction 21.6.4 For impurities distributed throughout the thickness of the mat or suspected impurities that are not visible, a random sample is used in the extraction 73 BCIS-03a Rev Feb02 21.7 Procedure CAUTION: Due to the presence of potentially toxic solvent fumes, the extraction, filtration, evaporation and infrared sample preparation steps must be carried out in a properly vented fume hood 21.7.1 Boiling Extraction 21.7.1.1 Place the spots or streaks and adjoining mat (21.6.2) in a ground glass-jointed Erlenmeyer flask (21.4.7) of appropriate size and add a magnetic stirring bar 21.7.1.2 Fill the flask to approximately 2/3 to 3/4 of its designated volume with extraction solvent (21.5.2) Attach a condenser (no silicone grease), place the assembly on a hot platemagnetic stirrer and clamp it to the ringstand 21.7.1.3 Heat and stir the solvent-RBSM mixture under vigorous reflux for a minimum of 16 hours, then remove the hot plate-stirrer and allow the contents of the flask to cool to ambient temperature 21.7.2 Soxhlet Extraction 21.7.2.1 For surface coating or uniformly distributed impurities (21.6.3 and 21.6.4) cut the specimen containing the contamination into rectangular strips of about 6mm (1/4 inch) width and length; about 6mm (1/4 inch) less than the height of the soxhlet sample compartment 21.7.2.2 Place the strips in the soxhlet sample compartment using the tweezers (no thimble) 21.7.2.3 Temporarily attach the soxhlet to a ground glass-jointed Erlenmeyer flask (21.4.7) Pour extraction solvent (21.5.2) through the top opening of the soxhlet until the solvent in the sample compartment siphons to the flask 21.7.2.4 When the solvent has stopped dripping, temporarily clamp the soxhlet to the ringstand Remove the flask, add additional solvent to a level of about 2/3 the capacity of the flask and add three boiling stones 21.7.2.5 Attach the condenser and flask to the soxhlet (no silicone grease), place on the hot platemagnetic stirrer and clamp the assembly to the ringstand 21.7.2.6 Adjust the hot plate setting so that the boiling solvent condenses into the sample compartment at the rate of about one drop per second and extract for a minimum of 24 hours (Note: It may be necessary to wrap insulation around the flask and soxhlet to achieve the above condensation rate) 21.7.2.7 Remove the hotplate and allow the assembly to cool to ambient temperature 21.7.3 Filtration and Solvent Evaporation 21.7.3.1 Place the funnel containing a piece of fluted filter paper (21.4.12) into a 125 ml Erlenmeyer flask 21.7.3.2 Filter the solvent extract containing the organic impurities into the Erlenmeyer flask (Note: In the case of boiling extraction (21.7.1) and possibly soxhlet extraction (21.7.3), the glass fibers present may clog the pores of the filter paper before its contents have fully drained When this occurs, carefully lift the fluted paper from the funnel, place a fresh piece in the funnel and pour the contents of the plugged paper into the fresh paper In some instances, this step will have to be repeated several times 74 BCIS-03a Rev Feb02 21.7.3.3 Remove the funnel, add two boiling stones, place the flask on the hotplate and reduce the volume of solvent extract to about 25 ml, then allow the flask to cool to ambient temperature 21.7.3.4 Pour the concentrated extract into the watch glass, place it on the hot plate and evaporate the remaining solvent (Note: solvent bumping may be reduced by the addition of a boiling stone at the start of evaporation This stone should be removed at about 10-15 ml volume) When the volume of extract reaches the final ml, hold the watch glass above the hotplate (use insulated gloves) and swirl slightly 21.7.3.5 Place the watch glass in a thermostatically controlled oven, set at a temperature of 20°C ± 5°C (36°F ± 9°F) above the boiling point of the extraction solvent, for 20 minutes to remove any residual solvent Remove the watch glass from the oven and allow it to cool to ambient temperature 21.7.4 Infrared Sample Preparation 21.7.4.1 The sample preparation technique chosen will depend upon the physical nature of the organic impurity residue on the watch glass Judgement by the analyst is required More than one technique may be applicable in many cases 21.7.4.2 NaCl Plate Smear – this technique is applicable for semi-solid or liquid residues (e.g grease) Remove the residue from the watch glass with a scalpel or spatula Place on a NaCl plate and sandwich with a second NaCl plate 21.7.4.3 Film Cast on NaCl Plate – this technique is applicable for film-forming residues (e.g polymer binders or impurities) Scrape the film from the watch glass with a scalpel Place the scraping in a 10 ml Erlenmeyer flask and add a minimum amount of solvent to dissolve the residue Place a few drops of the impurity solution on a NaCl late and allow the solvent to evaporate, leaving a film (Note: Chloroform and carbon tetrachloride are preferred solvents because of their transparency in most infrared regions) 21.7.4.4 Solvent Cell – This technique is applicable to solid organic impurities, which are not film forming (e.g hard polymers) Dissolve the scraped residue in a solvent, fill the infrared solvent cell with the residue solution and fill the reference cell with pure solvent 21.7.4.5 KBr Pellet – This technique may be used for preparation of samples not possible by the methods described in 21.7.4.2, 21.7.4.3, and 21.7.4.4 Spectrum quality is poorer than the other techniques Consult infrared spectrometer manufacturers’ instructions 21.7.5 Running of Infrared Spectra Follow instructions provided by infrared spectrometer manufacturers 21.8 Interpretation of Spectra 21.8.1 Observe the position of the major bands of the contaminant spectrum to determine which organic functional groups are present (e.g only unsaturated hydrocarbon bands suggests the presence of some types of grease or a polyolefin; carbonyl and C-O single bond groups together suggest an acrylic polymer or a phthalate plasticizer) 21.8.2 Based on conclusions drawn in 21.8.1 and from the physical nature of the extracted contaminant, compare the contaminant spectrum to appropriate classes of reference spectra (21.2.1 – 21.2.7) It is also very valuable to have infrared spectra for reference of all raw materials used in the manufacturing of all products made on the same equipment, in addition to lubricating greases and oils used in the production facility 75 BCIS-03a Rev Feb02 21.9 Report In cases not restricted by proprietary information limitations, a complete report should include RBSM sample identification, conclusions as to the identity and/or chemical nature of the organic impurity, a brief description of techniques used in the analysis, a spectrum (or spectra) of the impurity and photocopies of reference spectra 21.10 Precision and Bias Precision and bias data for the methods described above are not available at this time 76 BCIS-03a Rev Feb02 22 ELECTRICAL RESISTANCE OF RECOMBINANT BATTERY SEPARATOR MAT The Battery Council International Technical Subcommittee on Separators has reached a consensus that equipment suitable for measuring the electrical resistance of recombinant battery separator mat (RBSM) in the partially saturated state does not presently exist If such equipment is developed at some future date, the Subcommittee on Separators may be reactivated to draft an appropriate method In the interim, some laboratories have chosen to use BCIS03b-18, Standard Test Method for Determining the Electrical Resistance of Battery Separator Using a Palico Measuring System for measurements on RBSM in the flooded state The use of this test method for RBSM is not sanctioned 77 BCIS-03a Rev Feb02 23 CONVERSION FACTORS FOR SI UNITS Quantity or Test Value in Trade or Customary Unit Conversion x Factor = Value in SI Unit Symbol Area square inches square feet square yards acres 6.45 0.0929 0.836 0.405 square centimeters square meter square meter hectares cm2 m2 m2 Basis Weight* or Substance lb (17x22-500) lb (24x35-500) 3.760 1.627 grams per sq meter * g/m2 ** (500 sheet ream) lb (25x38-500) 1.480 * ** or Grammage* when expressed in g/m2 lb (25x40-500) pounds per 1000 sq ft 1.406 4.882 * * * ** Caliper mils 0.0254 millimeters Force kilograms pounds 9.81 4.45 newtons newtons Length angstroms microns mills feet 0.1 0.0254 0.305 nanometers micrometers millimeters meters Mass tons (2000 lbs) pounds ounces (avdmp.) 0.907 0.454 28.3 metric tons kilograms grams Mass per Unit Volume ounces per gallon pounds per cubic ft 7.49 1.60 kg per cubic meter kg per cubic meter kg/m3 kg/m3 Stiffness (Taber) gram centimeters (taber units) 0.0981 millinewton meters mN•m Tear Strength grams 9.81 millinewtons Tensile Breaking Load pounds per inch kilograms per 15 mm 0.175 0.654 kilonewtons per meter kilonewtons per meter Volume, fluid ounces (US Fluid) gallons 29.6 3.79 milliliters liters mL L Volume, Solid cubic inches cubic feet cubic yards 16.4 0.0283 0.765 cubic centimeters cubic meters cubic meters cm3 m3 m3 78 mm N N nm um mm m t kg g mN kN/m kN/m ... could be realized 11 BCIS -03a Rev Feb02 4.7.3 Testing should be conducted in a controlled atmosphere (if possible) of 23°C (73°F) and 50% RH See Subsection 4.6.2.1 4.7.4 Manual Gauge 4.7.4.1 Place... Reference Documents 9.2.1 Instruction Manual, Micromeritics Mercury Intrusion Porosimeter 9.2.2 Instruction Manual, Quantachrome Mercury Porosimeter 9.2.3 Instruction Manual, Aminco Mercury Intrusion... RBSM sample Find the intersection of this (one-half dry-flow) line and the wet flow line or curve as shown in Figure 8.5 Determine the pressure coordinate of the intersection and substitute into