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{. du Font &e Memours & Co. (inc.) .tie Proa-acts and. Resins Department TEg-LOK" FEP-PLUOBOCARBOH SESIH, AQUEOUS AR226-2376 Code Ho. T 212.200 Revised.: 2-16-76 Page 1 of 2 PISPERSIOH (^/ ^ ^,c^'Vr,i1^' t ^ C-8/o/r Deteraination of EqmYalenttC-9 Dispersing Agent Applicability (L-i)^ This nethod is applicable to determining the equivalent.C~9 dispersing agent in FEP dispersion. 11. Unusual Safety Considerations III. IV. Principle Percent C-9 is dstemined 'by titrating PEP dispersion with a solution of cetyltriBethylaBnaoni-um Tsromiae. Sensitivity, Precision, and Accuracy The prscision (sigma) of this test based on five runs made on one sample is 0.0005 -with an X of 0.125^ C-9. V. Fieagents 1. CetyltriiEathylaanaoniual bromide (CTMAB) 1 e/liter - (HE^&eC^VT^fAETML P>IAAt>*M^ lROA.\-fcfc) (RC 190.127) V1- Procedure 1. Weigh 25 t 0.01 g FEP dispersion into a oOO-ml beaker. 2. Add 20C ml (grad cyl) deiaineralized water to the dispersion. 3. S-tir the beaker using a Eagaetic stirrer until the dispersion and water are mixed (ca. 30 seconds). ^> It. Fill a buret vith 1 g/liter CTMAB solution- Record the reading. it 5. Using the bm-et, add CTMAB solution to the dispersion slowly, -with CTMAB is added, polymer vill begin constant magnetic stirring. As -When appears that most of the polymer has coagulated, to coagulate. stop adding CTMAB and then stop agitation a few seconds later. If 6. Alilqlouvidt.he buli-tk oisf tchloeupdoyl,ymreesruntoe sagetittaletioonutanandd aoddbs0e.r2vetothe0.5suapleron.atant CTMAB. 7. Stop agitation and allow to settle. * Reg. U.S. Pat- Off. \ Ife J^ . - 1 w > ^-1 EID933920 2 of 2 8. Repeat steps 6 and. 7 until the supernatant liquid is perfectly clear. A clear supernatarrt liquid, is the end. point of the titrafcion- 9. Record, the "buret- reading. 10. Find specific gravity of the dispersion and percent solids, using Method T 202.8o4. 11. Calculate % C-9 and. g C-9/g 'STSP. VII. Calculations 1. Calculation of % C-9 ml CTMA3 = (step 9 - step Ftv- 6-?' A^/fl^t- ^(5 3 .--> >^ ^3 / ml CTMAB 46l 1000 v' 364 x _sr_t _o_f_d_i_sp_e_r_s_io_n. 0.12T2 x ml CTtJAB vt of dispersion where: saolecular vt C-9 = 463 molecular irt CIMAB = 364 2. Calculation of g C-9/g PEP % PEP = ^ solids (step 10) % C-9 from step 1, Calculations g F2? % C-9 % PEP WL C-1A ^^c-^-.o.n^ <^ii-^ VIII. References 1. Couture, M. J-, -Washington Vorks Technical Moratory Hotebooh Mo. 1026, pp 88-89 2. Plastics Department Laboratory Test Method T 202.80^ 3. Original M^.od, ^as^nston Works Technical Laboratory. 3-11-T1 Hevised to reduce s^le size to .ive hetter enc, point and to spec.ry ' deaineralized instead of deionized water. S^ i..^ g:1^.^^" ^""^^^^^.".'rs^iiu ^ o,^,., w.i^-.;.. ?a C..~i,.tl.n cot... E-16-76 a 0 . 3 ^00\ ?-n-r-2939 00 EID933921