Document qaLbYwE8EEB2okEREmBr6gv5x

A/X cl bl- ./luilSijlD MONSANTO RESEARCH CORPORATION / DAYTON LABORATORY / DAYTON. OHIO 45407 Lrs } '/ EASC - Dayton (DEPT /SECTION) Analytical TYPE OF REPORT REPORT ua E-< <Mz os o a uo* CO zo w & c0 rj c: e0 0 J CQ =Z -H O 1-- MX O .M Q fc. Q 0r a U to 1 u0 U tn oi <D >4 z TO |J Ed 0 <a U Zw Cl. < O ato: O .. DHz I-w-J <H ri n I < Q Z o z H UQ(4C. > . oO REPORT NO.: JOB/PROJECT NO.: DATE: PERIOD COVERED: TITLE: AUTHORS: MDA-331 320.2270 , October 12, 1982 ANALYSES OF DICHLOROPHENOLS FOR CHLORINATED DIBENZO-p-DIOXINS Frederick D. Hileman ABSTRACT: Three samples of dichlorophenol from the Krummrich Plant was 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 : 7^- U-r . ______ Robert F. Ivory cJ Environmental Analytical Sciences Center Service Project Manager Approval date 1 0 - / 3 - %SL RESTRICTED DISTRIBUTION (see over) IV I T h .* (feeum .nt .. tht property of M o n ae m o R e se arch C o rp o r ,o n end the recp,e m r p o r , p i for as U # k , * p r,B #nd a ' * * " " c o n i. m -i---C--O---N F ID E N T IA L. .I.N..F O R M A T IiOvNn ww hn,nc.ihi nmuun nnooti dbo rr^HwOoQd uUcCeNd , revealed to u n a u th o r,ted personnsy y e mn u i r tl * ^ M>o.m---a--n--t-o-B R--e--s-a--a--r-c.hC* *orporenon and M onsanto Com pany without proper authoraaten C C 0N F iI5ii^3T 3A L C0204 SUBJECT TO PROTFOT1VF ORPiFD DISOTIBJUTTWO N COPY NUMBER 1 J. A. Gloeckner 2 E. A. Fay 3 J. D. Wilson 4 R. B. Hudson 5 D. B. Edwards 6 T. A. Taulli 7 R. F. Ivory 8 F. D. Hileman 9 Central'Files 10 Technical Reports Library 1740 1740 G3WG N3A B2SG N1D 1250 1250 1250 R3C ABSTRACT ONLY R. K. Flitcraft R. M. Scott W. B. Witmer 1250 1250 1250 NOTE: Distribution of this report is restricted. Requests for additional copies should be made through the principal contact at the Monsanto location involved or the Manager, Environmental Analytical Sciences Center, Dayton Laboratory, Dayton, Ohio. ACKNOWLEDGEMENT Contributions of the folllowing Dayton Laboratory personnel to this project are gratefully acknowledged: Analyses : D. E. Kirk C O M P A N Y-^C O N FI D E N T I A L CONFIDE! 77IA SUBJECT TO PROTECTIVE ORDER Three chlorophenols were received for the analysis of chlorinated dibenzo-p-dioxins. They were assigned MRC Log. Number 1-82-10" 05-02. The samples were prepared for analysis by dissolving five grams of the phenol in IN KOH. The dioxins were then extracted with 40 mL of petroleum ether by shaking for 15 minutes. The base layer was removed and the petroleum ether was washed a second time with base followed by -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 a 50% dichloromethane/hexane and 300 yL of dodecane was added to this eluant as a keeper. The eluant was concentrated to 300 yL 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 in the selected ion monitoring mode analyzing for ions characteristic of various CDDs. The results'of the 'analyses are given in Table 1. Note that the results are reported as the sum of all isomers for a given degree of chlorination. Quality control results have been reported for both the 2,4-dichlorophenols and for the crude monochlorophenol. 1 COMPED 7 SUBJECT TO PROTECTIVE ORDER. SUBJECT TO PROTECTIVE ORDEF IS) O 0 Z a wA --i TABLE 1. ANALYSIS OP C1ILOROP1IENOLS FOR CHLORINATED DIBENZO-p-DIOXINS ng Dioxin/gm phenol (ppb) Sample Cl, Refined 2,4-D 10-3-82 J-1Q1 ND* Refined 2,4-D 10-2-82 1-102 HD Refined 2,4-D (Rep) 10-2-82 1-102 ND Crude Mono 10-3-82 J-l ND Crude Mono (Rep) 10-3-82 J-l ND Blank ND Method Detection Limit 1 Low Level Spike 2.5 Refined 2,4-D 10-2-82 1-102 1.7 Recovery t 68 Crude Mono 10-3-82 J-l 2.1 Recovery 4 84 High Spike Level 25 Refined 2,4-D 10-2-82 1-102 18 Recovery % 72 Crude Mono 10-3-82 J-l 22 Recovery 1 88 Cla Ci a Cl I. ci ND ND ND ND ND ND ND ND ND ND ND ND ND ND 1.4 3.0 1 ND ND 1.6 3.0 ND ND ND ND 1 1 11 2.5 2.7 2.0 2.4 2.1 2.3 2.0 2.3 84 84 100 96 l.B 3 3.1 4 . B 72 111 80 75 25 27 20 24 18 22 17 22 72 81 85 92 20 24 19 24 B0 09 90 88 Cl. ND ND ND 3.8 4.3 ND 1 2.3 2.4 104 5.3 23 21 91 26 96 Cl7 ND ND ND 4.5 4.9 ND 1 2.5 2. B 112 5.6 25 22 68 27 89 Cl. ND ND ND 5.9 5.1 ND 1 2.0 1.9 95 6.4 20 19 95 28 110 *ND = none detected at the method detection limit. - Spike levels were not sufficiently larger than the amount of dioxin originally in the sample to be considered valid.