-FISHERIES AND MARINE SERyICE.

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1 ' -FISHERIES AND MARINE SERyICE. e :1 Translation Stries No Errors made during analysis of fatty acid composition by gas. chromategraphy by Augustyn Jakubowski Original title:. 0 bitedach pope/nionych.priy analizie sk/adu kwasdw t/uszczowych za pomocg chromatografii gazowej From: T/uszcze Jadalne (Edible Fats), 17(2) : 65-70, 1973 Tranelated by the Translation Sureau(JNO) Multilingual Services Division Department 6f the SeCretary of State'of Canada Department of the Environment Fisheries and Marine 'Service Halifax Laboratorv Halifax, M.S pages typescript el

2 h ^ DEPARTMENT OF THE SECRETARY OF STATE TRANSLATION BUREAU SECRÉTARIAT D'ÉTAT BUREAU DES TRADUCTIONS 4 TRANSLATED FROM - TRADUCTION DE Polish MULTILINGUAL SERVICES DIVISION INTO - EN English DIVISION DES SERVICES MULTILINGUES I FfM..S 3z)1 7 AUTHOR - AUTEUR Augustyn Jakubowski TITLE IN ENGLISH - TITRE ANGLAIS Errors made during analysis of fatty acid composition by gas chromatography TITLE IN FOREIGN LANGUAGE (TRANSLITERATE FOREIGN CHARACTERS) TITRE EN LANGUE ETRANGERE (TRANSCRIRE EN CARACTÉRES ROMAINS) 0 blgdach popelnionych przy analizie skladu kwasôw ttuszczowych za pomoca chromatografii gazowej. REFERENCE IN FOREIGN LANGUAGE (NAME OF BOOK OR PUBLICATION) IN FULL. TRANSLITERATE FOREIGN CHARACTERS. REFERENCE EN LANGUE ÉTRANGERE (NOM DU LIVRE OU PUBLICATION), AU COMPLET, TRANSCRIRE EN CARACTÉRES ROMAINS. Tluszcze Jadalne REFERENCE IN ENGLISH - REFERENCE EN A'IGLAiS PUBLISHER - EDITEUR PLACE OF PUBLICATION LIEU DE PUBLICATION Edible Fats Not given Not given (Poland). YEAR ANNEE 1973 DATE OF PUBLICATION DATE DE PUBLICATION VOLUME 17 ISSUE NO. NUMÉRO 2 PAGE NUMBERS IN ORIGINAL NUMEROS DES PAGES DANS L'ORIGINAL NUMBER OF TYPED PAGES NOMBRE DE PAGES DACTYLOGRAPHIÉES 8 REQUESTING DEPARTMENT MINISTÉRE-CLIENT Environment TRANSLATION BUREAU NO. NOTRE DOSSIER NO BRANCH OR DIVISION DIRECTION OU DIVISION Fisheries Service Office of the Editor TRANSLATOR (INITIALS) TRADUCTEUR (INITIALES) PERSON REQUESTING DEMANDÉ PAR Dr. R. G. Aclman /.: 11 1 YOUR NUMBER VOTRE DOSSIER NO \`^`... DATE OF REQUEST DATE DE LA DEMANDE Yarch 21, SoS (REV.2/ee)

3 r DEPARTMENT OF THE SECRETARY OF STATE CLIENT'S NO. NO DU CLIENT BUREAU N0. NO DU BUREAU TRANSLATION BUREAU MULTILINGUAL SERVICES DIVISION DEPARTMENT MINISTERE Environment LANGUAGE LANGUE 6 SECRÉTARIAT D'ÉTAT BUREAU DES TRADUCTIONS DIVISION/BRANCH DIVISION/DIRECTION DIVISION DES SERVICES MULTILINGUES office of the Editor Fisheries Service ^TRANSLATOR (INITIALS TRADUCTEUR ( INITIALES) Polish J. No. CITY VILLE MAY -e, i974 Tluszcze Jadalne, T. XVII, Edible Fats, vol. 17, pp blgdaeh popelnianych przy analizie skladu kwas6w tluszczowych za pomoca chromatografii gazowej. Errors made during analysis of fatty acid composition by.a. gas chroma t ography. V ^;' ^ü`^ y By s Augustyn Jakubowski Ç t Institute of the Fat Industry N-9-0 During analyses carried out by means of gas chromato- *65 graphy, as is the case whén iaà.king..use of any other technique, there occurs the possibility of making errors. In the case of gas chromatography used for evaluating the composition of fatty acids in particular fats the errors in the result obtained may arise from three sources, namely as a result of: - a defectively carried out transformation of the fat to esters, - a defectively conducted chromatographic analysis, - mistakes in calculating the chromatogram obtained. SOS ^ The figures in the right-hand margin indicate the corresponding pages in the original text.

4 In this paper we will not concern ourselves with the mistakes which occur as a result of defectively conducted esterification and chromatographic analysis but will be concerned however with mistakes resulting from the interpretation of the chromatograms. In 1972 the Institute of the Fat Industry conducted investigations on a commercial scale on a highly selective hydrogenation of rapeseed oil, with the aim of divesting this of linoleic acid while retaining the linoleic acid. The process was controlled by the method of gas chromatography, by an analysis of samples of the oil collected from the autoclave during the hydrogenation. 2 The oil samples were sent out for chromatographic analysis, and the results which were sent to the Institute of the Fat Industry are presented in Tables I and II. From Table II it can be seen that there are differences in the summed content of fatty acids of a particular chain length, and these are greater than may be explained by the normal level of the error occurring in the G. C. analysis. For example, in lot No. 6 in the initial oil the estimated content of the C 18 acids comprised 31.6%, while in the hydrogenated oil this was 25.8%. In the case of the C 22 acids these values are 54.7% and 59.6% respectively. From observation of the chromatograms it is apparent that the peaks of the erucic acid were not symmetrical, while some of the acids of the 0 :2 18 group, in particular C 18, manifested a partial separation. In this situation the suggestion arose that the chromatograms were not calculated correctly.

5 ;., ! C. Table I. Fatty acid composition of rapeseed oil during selective hydrogenation. Tabl a Sad 1cwas6w tluszczow -jc oleju cztioakowt13o podczas seléktywneso uwotior.11un5at -1 q- Cc I 0.18 C! `la e >3 s l.2 I CrI pr31;ki 6! : 22 _ 1= _ I 1, ! 9,8 0 1 «de. 5/ D ,3.d9 56, 1 5/2 2,9 0, 2 1,2 1 14,1 c ,0 1,2 9 2!; 14,8 8,2 1, C- 5/ , ,3 r 5/4 3,0 0, c 15,1 ; ,4 56,9 5/5. 2,6 0,2 1,2 14, ,2 8,2 0,4. 1,3 59,0 ; r /e i 16,6! 7,2 1,6 eoe , ÇJ 9 M ; 5/7 30 0,2 r, 1,5 t 17, 6 1 6,5 0,6 0,9. 8, rt " ,5 0,6 0, ,7 0,6 --, ueuemiaill 1,6 ' n e) r 1,5 1,7 ti CL6T'IIMCI*2 T: a; 6/1 6/2 6/3 6/4! 6/ /6 6/7 if 6/2 2,0 8 0,2 2,0 4 0;2 3,0 0,2 2,6 0,2 3,0 0,2 3, ,0 0,3 3,0. 0,2 * Sample 1\lumber. "I , , , t 5 10,5 9, ,7' 6,7 6, , , ,0 y 1, S : , , ', ,6 1,9 J-e, r ,7 56, , , , ""

6 4 Table II. Summed content (j) o of fatty acids of different chain length calculated on the basis of the data contained in Table I.,Tabl:iaa II - Sumaryczna zawartosé /5^/ k.vras6,,v txuszczocrich o rôznej dxugosci lancucha obl.iczona na pods tlawie danych zarvaxtych w tablxcy x.,.. ' --_-_^-? n i n Yr Pr6bki C ' { 18 It u 4 ==-_;=--=57}4 28 2Y==1 9, 3!2 ^ 5/2 26s3 ^ 9,9 '+ 59,5, n 5/3 3.,,.0 26#1. 10r0 1 59g, 3 ii 5992 ii 5/4 ;.. 3,g2 25j /5 2t8 24.,^7 ^ 9^8 ^ 61j0 it 26$6 1 9rg ; 58#3 5/6-5/7 3, %9 5gIA9 It u 6/1. = 39,0 31.,,6 9,1 54^7 it ii n + 2!6. 9,0 58a8-6/2 I i+ 28^ + n 1' 6/3 1 3$2 it,'..` ^0^5 + 9*4 ^. 55 t4 + ; 6/4 + 2R8' ; 9*5, 58, 0 ; 6/5 ^ it If 2 i s9 I 56t8 it 6/6 i 3,,,4 26r,8 i 10^ r3 6/7 3#3 36i7 10 ^ t 594^ i i: 6/8 It 3,l2 ; 25,a8.. ' 59,,6 _-^ %g + We decided to carry out calculations of the chromatograms applying a different method for interpreting these. We accepted the known and sometimes recommended gravimetric method, i.e. the chromatograms were redrawn onto tracing paper, the individual peaks were cut out, weighed and their weight was compardd to the total weight of all of the peaks. In the case of the peaks with an incomplete separation, these were

7 Table III. Fatty acid composition of rapeseed oil during selective hydrogenatiàn calculated by the gravimetric method. Tablica III - Sklad kwas6w oleju rzepakowego w czasie selektywnego. _ uwodornienie obliczony metodz1 wagowa I G * O it I X/. 0 4 * C- C 1-0 I C. I 0 :1 szar Nr ** ' la is " 5/1 5/2 5/3 5/4 5/5 5/6 5/7 érednia average 6/1 W2: É/3 É/4 - É/5. ÉjÉ Étt )8 avéragé r e ,2 4,1 3,0 4,0 3,7-0, ,3 0,3 0,3 0, , , , ,3 à,33 - riz/ J i -18 I-. I, I J r a 14 07i12,4 5 e '8 11, , ,5 1 3,0 31,6 16,4 11,6 2,7 31,9 18,3 11,6 18,0 12,0 L' e , ,3 e :565 (15 ;3 3 5 Ë t99 14d7/ b. ( J 1 5C 14, ,5 J e5 d e J 1 Je 4J ,4 12, b bej ,5 e ,1 3ei b e : , e9 4 13,0 I'M p.a41 iï, 5 1 i. 17,8 li e ' 2,0 2,8 34, ,6, i.) blimeir'jàkià,àà* -ii.t'àâ.;.,' 1..àààbi i datej dltigcol.1alicucha Summeà bbntent Of acidb of the given chan length, ,5 32,9 3? ,1.33, x/ :o. G "C i : - 22 I. L r J.- _ * "{ 1, , _ 91. 1, ,3 98" "0,6 11, , ,4 11,7 9,4 0,8 1 9,3 0,6 11,3 9 / ,6 8,7 8, , ,5 0,8 0,5 0,7 0, ,5 1 10,6 1.2,2 11,3 10,7 ii 6 11, yl '0' 1, , , 2 1,6 1, 5.w. *====4=ic====fe=====t= 48 / « ,0 48,4 46,8 49, ,9 47, ,6 * Batch Number ** Sample Number 49,6 50,3 49,9 49;3 n / ^ I I ri Sc. 1,,iXt e1 3%.) I ç.g2 t -'')2 1' '20 et I. I , , 3 0 e ' ,3 50,6 49, ,7 49,8 48,1 1 49,4 0,4!, ,9 _ , 6..== ==.4L---1========d1 0,8 0, , ,

8 6 Table IV. The content of unsaturated fatty acids of the 0 18 group during hydrogenation of rapeseed oil according to the results obtained from outside (Z) and from our own interpretation (W). -Tellies. IV Zawartoe nienasyconych kws,s6w tluszczowych grupy 0 w czasie uwodornlenia cleju rzepakowego wg wynik6w uzyskanych z zewnaltrz /Z/ 1 wlasnaj interpretacji 11 li :Hr preiloki. I , Sample No. I It t Z' t 1 5/1 5/2 '5/3 5/4 5/5.5/6 5/7 14,2 14,1 14, D 1,6 v 6 17, , o 8 8,7 8, ,3 7,2 6,5 12,4 11, ,6 12, ,3 1, , ,9' ,0 2, ,0 6/1 6/2 6/a 6/4 6/5' - ri r 6)7 6/8 12,0 130' 1. 14,843e 12, ,2.15, ,1 tre 16,6. 17,8 12, ,5.9,7 8,0 ' 7,7 ee 13,6 12,9 14, , ,3 6,8 4, , = , ,1 2,0 - H Il u 9 eut perpendicularly to the base line at the point closest to the latter. The results obtained are presented in Table III. As can be seen from the comparison of the calculations obtained by the above described method, the results differed

9 considerably from those presented in Table I. In the first place there is a good agreement in the summed content of the acids of particular chain lengths; moreover, the content of the 0 18 group of acids is higher than that estimated in Table I, while the content of the 0 22 group of acids is con- siderably lower. The analyses discussed here were carried out with the aim of evaluating the process of the highly selective hydrogenation of rapeseed oil. The changes which were of interest to us occur primarily in the region of the unsaturated 0 18 acids. The results obtained by the two methods of calculation are presented in Table IV. From Table IV it is apparent thàt the greatest dif- :2 ferences occurred in the evaluation of the C 18 acid, i.e. where there occurred a partial separation of the isomers. the product the amount of this acid calculated by the gravimetric method is almost twice as great as that given in the results obtained from outside. Thus, in the case of hydrogenated fats particular attention should be paid to the evaluation of the content of this acid. At the same time, the considerable overestimation of the content of the 0 22 group of acids is disturbing. With the accepted method of calculation (comparing the area of a given peak to the sum of the areas of all of the peaks), an underestimation of the content of some of the components causes an overestimation of the content of the remaining com- ponents. The gravimetric method of calculation indicates that the 022 acids are present at a level of about 51%, while 7 In

10 8 according to the data obtained from outside these should be present at a level of up to 5.9%; this difference is therefore in the teens* expressed as a comparative percentage. The evaluation carried out above indicates that a verification should probably be made of the standard for determining the composition of fatty.acids to avoid mistakes in the evaluation of the content of the C18 and C22 acids, which are standardized in many products of the oil industry. ^ Translator's note. _"kilkanascie" - between ten and twenty.