Document Z8BnnqLE8LNo89Yxrkab9prnd

1 J .-~v v * ,,* -iTM . > 7 * \ HViiiUJ MONSANTO RESEARCH CORPORATION / DAYTON LABORATORY / DAYTON, OHIO 4 5 4 0 7 EASC - Dayton (DEPT./SE CTION) Analytical TYPE OF REPORT _ REPORT ** aa h<2 H (X o iX a o ao IX w XI o a &o a co id X 6 o Gw 1-1 < 2 *H K M X<M t~ U Ot o H Q IX Q O1 A a 0 CO 1 H IX o U LO CS3 0) X 2 TJ X I EX <D < O U 2 2> IX < Q in a O X LU H Z> h < 1- o m m I < Q S ` :;1 REPORT NO.: MDA-330 JOB/PROJECTNO.: 320.2220 DATE: PERIOD COVERED: October 12, 1982 TITLE: ANALYSES OF PARACHLOROPHENOLS F O R CHLORINATED DIBEN ZO-p-DIOXINS -r'K ABSTRACT: Five samples of parachlorophenol from the Krummrich Plant were analyzed at the Dayton Laboratory in the Ultratrace Facility, The samples were analyzed for the presence of chlorinated dibenzo-p-dioxins. Technical Approval Frederick D. Hileman Senior Research Chemist Approved by : c - + - ^ c J <,-- .__________ Robert F. Ivory O Environmental Analytical Sciences Center Service Project Manager Approval date: RESTRICTED DISTRIBUTION (see over) o z f- Q. >a-. LCUC OO C O M P A N Y C O N FI D E N T I A L T hi. document it the property of Monsanto-Research Corporation and the recpiem it responsible for hs M feie e p rrB end d.sp o.iu jn . It conta.ns CONFIDENTIAL INFORMATION wh-ch must not be produced rvcled to unauthorized persons or sent outside Monsanto Retearrh (.out proper eull r p . . ^ ^ T V T 1 3 T t T l l T S T TM . _ - i u ______ ^ _____ TMV SAMPLE PREPARATION AND ANALYSIS Five samples of parachlorophenol were received for the analysis of chlorinated dibenzo-p-dioxins (CDD). The samples were assigned MRC log number 1-82-09-14-02. The samples were prepared for analysis by dissolving five grams of the.phenol in IN KOH. The basic solution was extracted with 40 mL of petroleum ether by shaking the mixture for 15 minutes. ' The base layer was removed and the petroleum ether was washed with - 50 mL of organic free water. This water wash was removed and the petroleum ether was dried over anhydrous.sodium sulfate. The petroleum ether was concentrated to 0.5 mL and applied to a chromatography column .containing 2.5 grams of Woelm basic alumina. .This column was first eluted with 10 mL of 2% dichloromethane/ hexane and this fraction discarded. An additional elution was made with 15 mL of 50% dichloromethane/hexane and 300 pL of dodecane was added to this eluant as a keeper. The eluant was concentrated to 300 pL and submitted for GC/MS analysis. The GC/MS analysis was carried out on a Hewlett Packard 5985B GC/MS system. A 30 meter Se-54 capillary column was used for all gas chromatographic separations. The mass spectrometer was used in the selected ion monitoring mode analyzing for ions characteristic of various CDDs. The results of the analyses are given in Table 1. In all cases the results are given as the sum total of all iosmers of a given degree of chlorination. In the case for the tetrachlorodibenzo-p-dioxins (TCDDs), the 2,3,7,8-TCDD has been listed separately. Thus for KB-5043 there was a total of 2.6 ppb TCDDs, however less than 1 ppb coeluted with the-"2,3,7,8-TCDD. In most instances the TCDDs consisted of the 1,3,6,8-TCDD and 1,3,7,9-TCDD. 1 5" T U A W TADLE 1. ANALYSIS OF PARACHLOROPIIENOLS FOR CHLORINATED DIBENZO-p-DIOXINS ng/gm (ppb) J 00 N0 Sample ID Cli Cl2 CI 3 ClU Clu* Cl5 Cl6 CI-, Clo KB-5043 ND ND ND 2.6 ND ND ND ND KB-5043 Replicate ND ND ND 2.4 ND ND ND ND KB-5044 ND ND ND 3.2 ND ND ND ND KB-5045 ND ND ND ND ND ND ND ND KB-5046 ND ND ND 2.7 ND ND ND ND KB-5047 ND ND ND ND ND ND ND ND Blank ND ND ND ND ND ND ND ND Method Detection Limit 1.0 1.0 1.0 1.0 1.0 1.0 1.0 1.0 Spike Level 2.5 2.5 2.7 -- 2.0 2.4 2.3 2.5 KB-5043 2.2 2.5 2 . 6 -- 1.7 1.7 1.9 2.4 Recovery % 88 100 96 -- 85 71 83 96 Spike Level 25 25 27 -- 20 24 23 25 KB-5043 18 20 22 -- 16 22 21 22 Recovery % 72 81 81 -- 80 92 91 88 = analysis of the 2,3,1 ,8-tetrachlorodibenzo-p -dioxin. ND ND ND ND ND ND ND 1.0 2.0 1.9 95 20 17 85 <