Document zdM7RBQDjzmQ2Roma1Z70j7eB

Designation: D 3303 - 74 AMERICAN SOCIETY FOR TESTING AND MATERIALS 1916 Race Si.. Philadelphia. Pa.. 19103 Nepnnteo ttoiti the Ai>nul Boo* Ot AS rM Stand Afrit. Copyiighi ASTM if not littod in tha currant combined Index, will apoaar m tha naxt adition Standard Method for RAPID GAS CHROMATOGRAPHIC ESTIMATION OF HIGHER BOILING HOMOLOGUES OF CHLORINATED BIPHENYLS FOR CAPACITOR ASKARELS*1 This Standard it issued undar iha fixed designation D3303: tha number immediately following the designation indicates tha year of original adoption or. in ihe ctM of reviiion. (he year of law revision. A number in parentheae* indicates tha year of law reapproval. 1. Scop* . 1.1 Thia method covers a rapid empirical determination of the level of higher boiling homoioguea in Specification D2233, Types D and A. Higher boiling homologues are de fined in 3.2. This procedure it not intended for the precise analysis of polychlorinated biphenyl products or mixtures. 2. Applicable Documents 2.1 ASTM Standards: D 2233 Specification for Chlorinated Aro matic Hydrocarbons (Askarels) for Transformers' E 260 Recommended Practice for General Gas Chromatography Procedures* E 33$ Recommended Practice for Gas Chro matography Terms and Relationships' J. Summary of Method 3.1 The sample is injected into a supportcoated open tubular gas chromatography column. The components are separated as they pass through the column with helium carrier gas and their presence in the effluent is measured by a flame ionization detector and recorded on a chromatogram. The method is made quantitative by internal normalization comparing the area of the higher boiling homoiogue peaks to the total area of all the peaks in the chromatogram. Note I--Reference should be made to Recom mended Practice* E 260 and E 355. 3.2 This method arbitrarily splits up the chromatogram into two regions. The major region represents mostly mono. di-. trk and tetra-chlorobiphenyis. The lesser region rep resents the higher boiling homologues and is mostly penta- and hexa-chlorobiphenyls. However, there is some overlap of the tetraand penta-chlorobiphenyls between the two regions. Some of the important peaks in the major region contain both tetra- and pentachlorobiphenyls. 3.3 The only way to obtain a closer ap proximation to true composition of these samples is to use a longer column with a gas chromatography-mass spectrometry (GS/MS) combination to correct for the composition of these overlap peaks. Area correction factors must also be used. However, GC/MS instru mentation is not available in many laboratories and is too cumbersome and costly for routine analysis. Therefore, this empirical short method has been adopted. This method yields values that are about 40 % of the true value when the true value is in the range of I %, 4. Significance 4.1 Present knowledge indicates that higher boiling homologues of chlorinated biphenyls are less degradable than the lower 'This method ii under the jurisdiction of ASTM Committee 0-27 on Electrical Insulating Liquids and Gases. Current edition approved Feb. 27, 1974. Published April 1974. 1 1974 Annual Book of ASTM Standards. Part 40. ' 1973 Annual Book of ASTM Standards. Pan 30 1 moms 078< 42 Became of the dl^wil Method of certain type* of capacitors containing these eskaicis, it n iwpoftft to limit the higher hoihog bomoiogac cooust. 4.3 This Method is esed as a process cootroi aad acceptance test for Spedficstka D 2233, Type D. 7.4 Smtplr tor--0.0*5 ml split 1 to 25. 7.5 Inject 5 *1 of the neat sample aad aflow the chromatogram to prnrred at ettcanaiitm aettiag that wifl keep all the peaks on the scale if dm disk chart integrator ia bemg 3.1 Ckromatofnpk--Aay gas chromato graph with flame ioeizatioa detector aad capillary column inkt splitter system. 5.2 Xreorder, 0 to 1 or 10-mV range with fall-teak response time of I s aad chart speed of approximately V* ia./min. $.3 Cetata, 30 ft by 0.02 in. inside diame ter support-coated opea tabular capillary coated with FFAP.' 5.4 /aargnator--Disk chart integrator or electronic digital integrator to measure the peak areas, if aa electronic ietegrator ie osed, it Aould be checked iaitislly sgaiast a disk chart integrator to determine tfcat the eketroak integrator operating parameters bare beta set properly for correctly measoring the late elating smell peaks. *. CMBcartca 0.1 The method of cakculation is peak area normalization. The lack of pare kaowas prevents the accurate determination of re sponse facton (area correctioa factors) for the iadividaal components. Therefore, the icsaks ere reported as area percent of higher boiling koraologues. 0.2 Final check-out of the total chromato graphic system for this analysis can best be done using the reference samples of Aroclor 1010 aad Aroclor 1242* referred to ia Section 9. 7. Procedure 7.1 Adjust the chromatograph to the fol lowing conditions: 7.2 Ttmpemwm.' dmm taS*C (MtMTMl] jjrc m*c 7.3 C Flow Halts: rmiai late*tmr S mi/mm (7 w) Mw JMW/mMm t.l Divide the chromatogram into two regions as ahowa on the accompanying chro matograms. 1.2 Measure the total area of the peeks in each region of the chromatogram. t.3 Calculate the result aa follows: A - (I/O x IOO where: A area % of higher betting bomotogues, B m area of higher hotling bomotogues, aad C total area of ail peaks. 9.1 Reference samples of Aroclor 1014 aad Aroclor 1242 were analyzed in duplicate on two different instruments using both the disk chart integrator and an electronic integrator. Aa Infotronics Model CRS-100 integrator was used on a Perkia-Elmer Model *00 chromatogrepk aad a Hewlett-Packard Model 3370A integrator was used on a Hew lett-Packard Model 7624A ckromatograph. The same column was ased in both instru ments. 9.2 Results are givea in Tabte I. 9.3 The above two reference sampks were each analyzed five times in another labora tory using a Variaa-Aerograph Model 144410-00 gea chromatograph with aa Infotranks Model CRS-II-HS eketroak ietegra tor. The 95 % confidence limits of the mean were cakutatcd as follows: * AnMti tw MMhur Cos. aa Pan Na. means. Sha o ub >! oret ha <mu at Fma Fm WKm (FFAP1 tr*mnk tm tea head fen 4 Viraa taapip, avaUahU dm Vanan lamw Mi 411 Maaaaa Way/Pala AJM, CM UM 2 0 non o_ /- a/5 r . 2.71 for fire measurements. 5 mimated standard deviation. aad . (0.43) (raage of fire measoremests) Remits: Mem 5 W* Aracfcx MM Aradar 1242 0JJ 00043 HU 00053 SJD 0.12a 0.140 10.1 Them values were determined id ac cordance with Recommended Practice E 200 for biphenyl oo the Pertin-Elmer Model *00 Gas Chromatograph. 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