Document 6bVpk9aQE4BgGqnnmm77j0LZ3

29 r^nwi 1999 Anal/ala of Piohamrl-Tarphaa/1 Klnturaa by Pan Chromatonraahr Fhyalaal aad Chaaleal Proportion Balt Organic Soaetora Oronp Atonlea Xataraatlaaal A pi akromatographlo method haa boon developed (or tha quan titative determination of diphenyl, ortho-, mate-, aa< para- terpbeayl la varlona organlo ooolaat mlxturee. taohnique la- volvea rolatlag tha ooapoaaat paak helghta to tha poak height of aa added internal ataadard aftor determination of tka approprlata oallhratioa factore. Tha method baa baaa aaoceaofally aad la tha aaalyala of both aairradlatad aad Irradlatod ooolaat contain- lag up to bO par oaat KBS (High Pollor Beeidaa). Tha iaatrumeat uaedfor tha development of thla method ana aa lap* clall/ aodifiad doalga baaod oa tha Loo engineering'*' Chromat-O-flen aad la ao available aa tha Modal U froa tha eompaa/. Aa/ gaa chromatograph aapabla of atabla aparatloa at JOO*C 1th ooaparabla aeaaltivity aad equipped aith a baok-flaah attachat aoald ba aaad far tha aaal/ala deaorlbed. Tha Modal IX laatruaaat la llluatratad la figure 1, thla Iaatrumeat aaaa a fileaoat-t/po four oloaoat dataator plaead la tha oelaaa ovaa, ,The ooluaa even la a foroad alreulatlaa air bath t/pa with a door epeaiag oat of tha froat paaal, dtrlp-t/pa baaa load baatara (900 att) ooatrollad b/ i variable autotrcnaformer ara looatad aa altkar alda of tha ovaa llaiag. A trio load call-t/po baatar (290 oatt) la plaoad la tha air bath iaat devaetream froa tha circulating faa, Tba dataotor aad ooluan ara aacloaad b/ vertical bafflaa ehioh aarra tha dual fuaotlaaa of dlraotlag air bath nlroulatloa aad of ahlaldiag tha dataator aad aalaaa from trim baatar irradlatioa, Tha froat baffla la removable aad giroa aocaaa to tha apaaa ooouplad by tha dataator aad ooluma. A raalataaoa-balb alaetroala temperature ooatrollar haring praportlonal-band plan raaat raaponaaa la aaad for oraa tamparatara eoatral, figure 2 la a aaotloaal rlam of tha oraa ahavlng tha location of major aoapananta and circulation patha. (1) 29? Vorth Tairente, Paeadena, California 1 oOblbtl The detector circuitry is conventional. Bridga bslsacs is established by the us* of coarss- and fiaa-zaro potentiometers. The appllsd voltags is varied by msans of a rheostat in serlea with the detector bridge circuit and the batteries hich are used for the detector supply. * step-type attenuator (ternary from 1 to 24}) adjusts the signal input to a 1 millivolt recorder. The carrier gas flow path splits Just dosnstreaa froa the pressure regulator. Each stress then passes through s sintered etsl flow restrictor. One streaa flows through the reference side of the detector to the ataosphere. The other streaa flows in ,, aeries through the hypodermic saapls vaporization block, the coluan, the saaple aids of the detector, and to the ataosphere through s esaple outlet-fitting located on the 'front panel. Saapls injection is accomplished by tbs use of a hypodermic syringe (Beckman Liquid Sampler)'*' through an 1/8-inch thiok silastic seal'?). Whan necessary, tha column Is baek-flushed by connecting the reference streaa outlet to the saapls stream outlet and re moving tbs eilaetio injection seal froa the saaple vaporisation block, i flow disgraa of the instrument is shown in Figure J. Column Preparation Weigh the proper aaounts of Aplesoa L^ and >0-60 mesh chroaasorb'5)(weight ratio 1 i 4 for 20 per osnt immobile phase). Dissolve ipleson L in ethyl ether, add cbroaasorb, and evaporate the ether with nixing. (Vaouun evaporation using a Rinoo evapora tor'"' is convenient.) Sieve dry saterlal to >0-60 mesh and load into s 2 aster stainless steel column (1/4-inch O.D.) using an air-operated vibrator to insure ahsenoe of voids. (2 aster coluan requires about 20 ga. of packing.) Plug sads of coluan with glsss wool, band, and aount column in chromatograph. Flush column with heliua (ca 100 nl/rnin) for about thirty minutss and bring chromato graph to oparating teapsraturs. (If coluan is laft at JOO'C con tinually, tailing will start to dwvslop in about two to threw wsska which will neowaaitate a coluan ohaage). Operation Conditions Coluan Teaparatura Iwaobile Phaaa Helium Flow Bata Detector Filaaeat Voltage Coluan Length >00*C 20K ipleson L on >0-60 Nsah Cbroaasorb 8? al/ais (>0 palg) 10 volt* 2 sstsrs 0067`>'>`* (2) Beckman Inntruaeats, Fullerton, California (}) Dew Cernlsg Be. >0 Silicons Rmhhsr (4) Jeaes 4. Biddle Co., 1316 irch St., Philadelphia, Penns/lnoie (3) Johas-Naaville Co., Nsnvllle, Sew uereey (6) 1. S. Aloe Co., St. Louis, Missouri Determlnaton of Calibration Factors Accurately weigh .bout 75 mg diphenyl, 200 mg ortho-.erphsnyl, 250 rag triphenylmethane) (as internal standard), 150 mg meta- terphenyl, and 50 rag pcrs-terphenyl into a 10 ml volumetric flask, add tetrahydrofuran, swirl until solution is complete, and dilute to mark. Stopper flask with rubber serum cap, mix thoroughly, and chromatograph at least } - 0.02 ml aliquots of this solution. The compounds elute in the order given above. The first three peaks should be recorded at 5 mu full scale while the later two are recorded at 1 mu full scale. Draw the base line under each peak and measure the height of each peak from its base line to the nearest 0.01 inch. Calculate, the calibration factor for each component using the following formula: ' HT x WC c = Hc x WT where Fc * component calibration factor Wc = weight of component (mg) W<p * weight of triphenylmethane (mg) Hc * component peak height Ht = triphenylmethane peak height Average the factors thus obtained for each component. The devia tion.from the average should be within -2 per cent relative. Analysis of Organic Coolant Mixtures Accurately weigh about 500 mg of Santowax R or 500 mg of Santowax OM and 250 mg of triphenylmethane into a 10 ml volumetric flask, add tetrahydrofuran, 6wirl until solution is complete, and dilute to mark. Stopper with rubber 6erum cap, mix, and chromato graph a 0.02 ml aliquot. If components less volatile than pterphenyl are present, it will be necessary to back-flush the column for ca thirty minutes after each run. Measure peak heights as described under ''Determination of Calibration Factors" and calculate the amount of each component using the following forumula: x Fc x W<j> x 100 where: %C * weight per cent of component Hc s component peak height = triphenylmethane peak height Fc * component calibration factor Wt a weight of triphenylmethane (mg) WB s weight of sample (mg) 006794$ J- TOWOLDMONOQ56750 Aconracr and Praclalon Tha aocuraoy of tba aatbod waa ebaokad by analysing four known ayathatie aiituraa, with and without addad high bailor raaidua. Tba avaraga ralotiaa arror obtaiaad froa fifty-four da- taraiDatioaa waa *1.7 par cant altb a raaga of *4.6 to -6.4 par oaat. To obtala tbla acauraoy, It la naoaaaary that ooapoaant paaka la tba aaalyala of a aaapla ba raeordad at tba aaaa attanua- tloa aa aaa aaad la tba dataralaatloa of tba oallbratioa footora. If tba soapoaltloa of tba aaapla la aucb that aay of tba coapoaaat paaka go off aoala at tba praaerlbad attaauatlona, tba aaapla alto should ba raduead aad tba analysis rapaatad. Saoallbratloa aay ba naoaaaary aftar tao or tbraa daya If tbara baa baan soffi- claot boll off of laaobila pkaaa to algaifloaatly Quango tba ra- taatlon tlaa of tba coaponants. partianlarly aata- aad para- tarphaayl. . 006 1')`lb TOWOLDMONOQ56752 0067>768 TOWOLDMONOQ56753 FIG.3 \ ( x----- 3ACKFLUSH CONNECTOR b h b L t00 TOWOLDMONOQ56754