1、Designation: D 7129 05An American National StandardStandard Test Method forDetermination of Ammonia Trapping in a Grafted BatterySeparator1This standard is issued under the fixed designation D 7129; the number immediately following the designation indicates the year oforiginal adoption or, in the ca
2、se of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the measurement of the abilityof a material to capture ammonia.1.
3、2 This test method is intended primarily for testing graftedpolyolefin materials used as a battery separator, although othermaterials could be tested.1.3 The values stated in SI units are to be regarded as thestandard.1.4 This standard does not purport to address all of thesafety concerns, if any, a
4、ssociated with its use. It is theresponsibility of the user of this standard to establish appro-priate safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Referenced Documents2.1 ASTM Standards:2D 123 Terminology Relating to TextilesE 438 Specificat
5、ion for Glasses in Laboratory ApparatusE 1272 Specification for Laboratory Glass Graduated Cyl-inders3. Terminology3.1 Definitions:3.1.1 For definitions on other textile terms in this testmethod, refer to Terminology D 1234. Summary of Test Method4.1 A predetermined amount of separator and ammoniumh
6、ydroxide is added together in a KOH solution. The specimensare conditioned under a controlled temperature for 24 h. Afterthe solution is cooled, the solutions are distilled to determinethe amount of ammonia the separator retained.4.2 Results are calculated as mol/g using the appropriateequations.5.
7、Significance and Use5.1 Nickel metal hydride (Ni-MH) cells can exhibit highself-discharge rates. Nitrate impurities in the positive electrodecan be reduced to ammonia on the negative electrode. Thiscauses rapid self-discharge. Technical publications have re-ported a link between the separator ammoni
8、a trapping capa-bilities and the cells charge retention. Grafted polyolefinseparators can absorb or trap these impuritieshence, reduc-ing self-discharge rates. The level of ammonia trapping fromthis method gives an indication of the efficiency of a separatorto trap these contaminates, thus helping a
9、 battery self discharge( charge retention). A higher value should provide a cell withgreater charge retention.6. Apparatus6.1 Flask, Erlenmeyer, wide mouth, 250 mL capacity with ascrew cap.6.2 Flask, Erlenmeyer, wide mouth, 500 mL capacity.6.3 Cylinder, Graduated, Class A, 250 mL capacity.NOTE 1The
10、tolerance on the accuracy of the graduations in Specifi-cation E 1272 for this apparatus is 61.4 mL. If greater accuracy isrequired for a test result, the graduated trap(s) should be calibrated.6.4 Pipette, Volumetric, Class A, 10 mL capacity.NOTE 2The tolerance on the accuracy of the graduations in
11、 Specifi-cation E 438 for this apparatus is 60.02 mL3. If greater accuracy isrequired for a test result, the graduated trap(s) should be calibrated6.5 Pipette, Volumetric, Class A, 3- mL capacity.NOTE 3The tolerance on the accuracy of the graduations in Specifi-cation E 438 for this apparatus is 60.
12、01 mL. If greater accuracy isrequired for a test result, the graduated trap(s) should be calibrated.6.6 Distillation Unit, Micro or macro Kjeldhal apparatus.6.7 Oven.7. Reagents7.1 Ammonium Hydroxide, 0.3M (NH4OH), ACS grade.7.2 Hydrochloric Acid, 0.1M (HCL), ACS grade.1This test method is under the
13、 jurisdiction of ASTM Committee D09 onElectrical and Electronic Insulating Materials and is the direct responsibility ofSubcommittee D09.19 on Dielectric Sheet and Roll Products.Current edition approved March 1, 2005. Published March 2005.2For referenced ASTM standards, visit the ASTM website, www.a
14、stm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.7.3 Met
15、hyl Red, ACS grade.7.4 Potassium Hydroxide Solution, 8MPrepare a suffi-cient quantity of KOH solution for the testing programimmediately at hand as follows.7.5 To a 1500-cm3(mL) beaker add 800 to 850 cm3(mL) ofdistilled water. Slowly add 448 g of potassium hydroxidepellets, certified ACS grade, to t
16、he beaker. Allow cooling toroom temperature.7.6 Potassium Hydroxide, 0.1M (KOH), ACS grade.(WarningFollow appropriate safe handling procedureswhen using acids or bases.)8. Conditioning8.1 Determine sampling based on grafting process. Then cuttest specimen to a weight of 2.00 6 0.05 g.8.1.1 Cut speci
17、men into 1-cm2pieces.8.1.2 Place cut pieces into Erlenmeyer flask as stated in 6.1.8.2 Measure out 120 mL of KOH solution as stated in 7.3.8.2.1 Add to the Erlenmeyer flask containing the cut speci-men.8.3 Using the 3 mL volumetric pipette, add 3 6 0.01 mL ofammonium hydroxide to the Erlenmeyer flas
18、k and immediatelycap the flask.8.4 Place the bottle into the oven at 40 C for 24 6 0.5 h.8.5 Condition a control specimen along with the test speci-men.8.6 The control is prepared the same way but without anytest specimen placed in the bottle.9. Procedure9.1 Allow bottles to cool so that the ammonia
19、 returns toliquid phase.9.2 Precondition the distillation apparatus before distillationas follows:9.2.1 Distill a 1:1 mixture of ammonia-free water and 50 %NaOH for 5 min just before sample distillation to reducecontamination from atmospheric ammonia. (WarningFollow appropriate safe handling procedu
20、res when using acidsor bases.)9.3 Prepare receiving solution as follows:9.3.1 Add 150 6 0.1 mL of ammonia-free water to theErlenmeyer flask as stated in 6.2.9.3.2 Add 10 6 0.01 mL of 0.1M HCL to the same flask.9.3.3 Add four drops of methyl red to the flask; this willcause the color to change to red
21、. If the solution does not changeto red, check for problems with the procedure.9.4 Measure out 100 mL of the solution in 8.1 and washingsand add to the distillation tube.9.5 Place tube into the machine.9.6 Place receiving flask into the machine.9.7 Begin distillation at a rate of 7.5 mL/min.9.8 Dist
22、illation is complete when receiving solution hascaptured 200 6 1 mL of distillate.9.9 Titrate the receiving flask solution with 0.1N potassiumhydroxide. The control sample is titrated using 0.1N hydro-chloric acid.10. Calculation10.1 Calculate the non-trapped ammonia as follows:N25 10 A! 3 1.25 3 0.
23、1!/1000 (1)where:N2= amount of non-trapped ammonia andA = volume of KOH used in titration.10.1.1 Calculate the control sample as follows:N15 10 1 B! 3 1.25 3 0.1!/1000 (2)where:N1= amount of ammonia remaining in the control andB = volume of KOH used in titration.10.1.2 Amount of Ammonia TrappedN1N2!
24、/2 (3)10.1.2.1 Record results in mol/g.11. Report11.1 State that the specimens were tested as directed in TestMethod D 7129.11.2 Report the following information:11.2.1 The amount of ammonia trapped to the nearest 1xE-512. Precision and Bias12.1 PrecisionThe precision of this test method is to beest
25、ablished on or before 2008.12.2 BiasThe procedure in this test method has no biasbecause the values of ammonia trap can only be defined interms of a test method.13. Keywords13.1 ammonia; battery separator; grafted polyolefin,nonwovenASTM International takes no position respecting the validity of any
26、 patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revi
27、sion at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are invited either for revision of this standard or for additional standardsand should be addressed to ASTM International Headquarters. Your
28、comments will receive careful consideration at a meeting of theresponsible technical committee, which you may attend. If you feel that your comments have not received a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyri
29、ghted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 7129 052
