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~Ward Period: ~Rom I Lj+'Ljf;J. to 3)30/Y::{ (Performance) ------(Reporut Lponsor Amount: Total Estimated: S L;;J., Yt? Funded: S__ I,....;J.=T-1 _lJRGIA INSTITUTE OF TECHNOLOGY OFFICE Of l,;UN I 1'11-\\.. I "'LIIYIII•I"" 1 ''~ • ,...,. •• '· PROJECT Al>MINISTRATION LlATA SHEET 00 ORIGINAt D REVISION NO. --- roject No. A '34 3 0 GTRIK*=f DATE _....1...101.J..~J J-'-4+-/ ~Yk=--- Seheei/Lab _- __;t_~-~M..;...;s~· =~;.._ ______ roject Director: ·1ft· -~n9 /.... Wt.t. ponsor: Get _11 (Qr_o. Ve I cLo:sf a, 6-11- 'yr,e Agreement: na l\()e111 en I= d zd~d Jl/2 rjf;J.. ~ward Period: ~rom I lj+'ljf;J. To 3)30/Y::{ (Performance) ------- (Reporut lponsor Amount: Total Estimated: S l;;J., yt? Funded: s__ I,....;J.=t-1 ......Y __ i_3 ______ _ I ,~-----~~~-2V~~--~--- ~[)MINISTRATIVE DATA OCA Contact z;tn d a If. I$()(.J&l 411 ;( ff).(J I) Sponsor Technical Contact: 2) Sponsor Admin/Contractual Matters: M.s, LJ',d7L t:l//ot . , Defense Priority Rating: __fJ~l .... 11,..7...,£ ____ _ Military Security Classification: /] ()0 ( (or) Company/Industrial Proprietary: RESTRICTIONS See Attached __.,1)+-+-/ .. zu..::;... _____ Supplemental Information Sheet for Additional Requirements. I l'ravel: Foreign travel must have prior approval - Contact OCA in each case. Domestic travel requires sponsor approval where total will excee~ greater of $500 or 125% of approved proposal budget category. Equipment: Title vests with 0 QO e 0(0 r;?p~cf_ ~ I COPIES TO: Research Administrative Network Research Security Services Research Communications (2) Research Property Management "'Aepnrb Coordinator (OCAL-­ Project F ile Accounting GTRI Other P•D Procurement/EES Supply Services · Library Other ------------------------------- GEORGIA INSTITUTE Of ·.TECHNOLOGY OFFICE OF CONTRACT ADMINISTRATION SPONSORED PROJECT TERMINATION SHEET . ·_ Project Title: Analysis of Berbici~e Material , . A-3430 . Project No: Dr. Tung L. Wu Project Director: , Sponsor: Griffin Corporation Effective Termination Date: ___._3.,/-.30..,./~81(M3~------ Clearance of Accounting Charges: _ __.,3....,/3_0_/....._8...,3 ______ Grant/Contract Closeout Actions Remaining: · [!] Final Invoice axkelusi•f'&bi'iliiWN&I 0 Final Fiscal RePQrt 0 Final Report. of Inventions 0 Govt. Property Inventory & Related Certificate 0 Classified Material Certificate []~her ________________________ EMS~ Assigned to: ---------·-------- ~R.aboratory) COPIES TO: Administrative Coordinator E ES Public Relations (2) Research Property Management Computer Input Accounting Project !)J. Procurement/EES Supply Services Library ~her'M.< Final Report ANALYSIS AND RESEARCH OF GRIFFIN LINURON PRODUCT by Tung L. Wu Energy and Materials Sciences Laboratory Engineering Experiment Station Georgia Institute of Technology Atlanta, Georgia 30332 Research Project Number A-3430 Project Officer Ms. Linda Elliot Griffin Corporation P.O. Box 1847 Valdosta, Georgia 31601 i. Table of Contents 1. Product Chemistry Data a. Product chemistry . 1 b. Product assay .. 2 2. Description of Manufacturing Process a. Raw material . .. 3 b. Step by step Description of Manufacturing Process . 3 c. Discussion of impurity formation . 4 3. Analytical Hethods and Data a. High performance liquid chromatography (HPLC) . 5 b. Thin layer chromatograhy (TLC) ... ..... 14 c. Gas chromatography - mass spectrometry (GC/MS) . 15 d. Combination of TLC & GC/MS . 24 4. Physical and Chemistry Properties a. Physical properties . 27 b. Chemical properties . 27 ii. List of Tables Table 1. Analytical Results of Technical Linuron Samples using HPLC . 7 Table 2. RF values of TLC Analysis of the "B" Technical Linuron Product 14 Table 3. GC Run Conditions for Analysis of Technical Linuron 16 Table 4. Nass Spectrometer Run Conditions and Tuning. Report . 17 Table 5. List of Mass of TLC Fraction #4 25 Table 6. Library Search for TLC Fraction #4 . 26 iii. List of Figures Page Figure 1. Chromatogram of HPLC Analysis 9 a. "A" Technical Linuron (T0110682) 10 b. "B" Technical Li.nuron 11 c. "A" Technical Linuron (Tll02798) 12 d. "A" Technical Linuron (Tll02584) 13 e. II C" Kayaku Technical Linuron 14 Figure 2. Thin Layer Chromatogram of "B" Technical Linuron 14 Figure 3. ,Reconstructed Ion Chromatogram of Technical Linuron 19 a. "A" T0110682 19 b. "B" product 20 c. II B 11 Tll02798 21 d. "A" Tll02584 22 e. ' II C" product •· 23 iii. List of Figures Pp.ge Figure 1. Chromatogram of HPLC Analysis 9 a. "A" Technical Linuron (T0110682) 10 b. "B" Technical Linuron 11 c. "A" Technical Linuron (Tll02798) 12 d. "A" Technical Linuron (Tll02584) 13 e. "C" Technical Linuron 14 Figure 2. Thin Layer Chromatogram of "B" Technical Linuron .... 14 Figure 3. Reconstructed Ion Chromatogram of Technical Linuron 19 a. "A" T0110682 19 b. II B" product 20 c. "B" Tll02798 21 d. "A" Tll02584 22 e. "C" product . 23 1. Product Chemistry Data a. Product Chemistr~ - Linuron is the active ingredient of a herbicide which is conunercially available under several trade names, such as: Afalon (Hoechst) Hoe-2810 (Hoechst) Herbicide-326 (du·Pont) Lorox (duPont) Linuron is a substituted urea herbicide, the molecular fonnula, chemical nomenclature and structural formula are depicted below. Molecular formula CgH 10 ci 2N2o2 Chemical Nomenclature 3-(3J4-dichlorophenyl) -1-methoxY-l-methYl - urea H ./ OCH 3 Cl N- C- N Structural formula -@- Cl / I CH b '-.. 3 Substituted urea herbicides are generally synthesized by four different routes: (1) Reaction of isocyanate with at-nines, (2) Reaction of carbamic acid chlorides with amines, (3) Reaction of carbamic acid phenyl esters with amine, and (4) Transamination of ureas with amines. These synthetic routes are depicted below, where R1 , R2 are alkyl or phenyl groups. -2- H H / (1) - C= 0 + R2-NH.L0 ~ R1-N-C-N 0" \ R2 H H H (2) R -N-c-Cl + RL~-NH ~ R -N-c-N-R0 + HCl 1 II 2 1 ll . ~ 0 0 H H H (3) R 1 -N:.:~-o- 0 + R2-NH 2 ---?>- R 1 -N-~-NR2 + 0 -OH 0 0 H H /H (4) R -N-~-NH 2 + R2 i~H 2 ~ R 1 -N-~-N, + . NH 3 o o R2 Specifically, "B" Technical Linuron is made according to the following scheme. H .. @ H / Cl -fo\-N == C = O+NH OH . NaOH> Cl ·-o-N- C-N, p 2 Cl / . lb OH Cl CH 0H H CH 3 Cl --!0\-- N-c _N ~ 3 (CH3)2S04 Cl p il " oc~ ~--......._.NaOH 0 b. Product Assay: Typical analysis of "B" Technical Linuron is summarized in the following: Chemical Name Structural Formula Percent 3-(3,4-dichloro­ 95% phenyl)-1-methoxy- Cl -0 -~-~-N_,CH3 1-methyl urea C1 G 'oCH3 3,4-dichlorophenyl­ H H 0.3% hydroxy-urea Cl -0 -N-c-N/ Cl ~ 6 'OH bis-(3,4-dichloro­ phenyl) urea H H 1.8% Cl -0-N-c-N- @-Cl Cl / b , Cl -3-· Chemic-al Name Structur.al Formula Percent 3-(3,4-dichloro­ H H phenyl) methoxy Cl ~0 -N-c-N-"' -urea c1 " S 'ocH3 Biuret HN-c-NH-c-NH 0.5% 2 II II 2 0 0 Methoxybiuret H HN-c-NH-c-N -0CH 0.2% 2 II ft 3 0 0 Inorganic salts & Acetone insolubles 0.5% Residual Solvent 0.5% 100% 2. Description of Manufacturing Process a. Raw Material: The starting materials and their sources for manufacturing "B" Technical Linuron are summarized below: Chemicals Sources (1) 3,4-dichlorophenylisocyanate Bayer (West Germany) (2) Hydroxylammonium sulfate BASF · (West Germany) (3) Dimethylsulfate Hoechst (West Germany) (4) Methanol Many sources b. Step by Step Description of Manufacturing Process: (1) Dissolve 82 parts hydroxylamine sulfate in 300 parts water by adding 100 parts solution of 40% strength sodium hydroxide -4- (2) To the aqueous solution of hydroxylamine formed in the above step, a toluene solution of 3,4-dichlorophenylisocyanate (188 parts in 400 parts) is added with good stirring and external cooling. (3) After completion of the addition, the mixture is stirred at 25°-30°C for 1 hour. The pre­ cipitate of 3-(3,4-dichlorophenyl)~l-hydroxy- urea is filtered and washed with water and dried. (4) 400 parts methanol are added to the dried 3-(3,4-dichlorophenyl)-1-hydroxyurea with stirring. Subsequently, 190 parts dimethyl- sulfate are also added. (5) 320 parts of 25% sodium hydroxide solution is slowly added to the reaction mixture. The re- action vessel is maintained at temperature between 10 to 20°C with external cooling. (6) The mixture is stirred for 1/2 hour, then 400 parts water are added to precipitate Linuron (3-(3,4-dichlorophenyl)-1-methoxy-1- methylurea). (7) Linuron is filtered, washed and dried. c. Discussion of Impurity Fomation: Since 3,4-dichlorophenyl hydroxyurea is the intemediate -5- material in the manufacturing of Linuron, small parts of 3,4-dichlorophenyl hydroxyurea remains in the Technical Linuron product as impurity. Two major impurities are formed, however, in the methylation process of the reaction inter- mediate, 0,4-dichlorophenyl hydroxyurea). 3-(3,4-dichloro- phenyl) methoxyurea is resulted from incomplete methylation, while bis-(3,4-dichlorophenyl) urea is formed when two mole­ cules of 3,4-dichlorophenyl hydroxyurea react. 3. Analytical Methods and Data Five samples of Technical Linuron were provided by the Griffin Corporation, and were analyzed for Linuron and im- purities. Technical Linuron samples were dissolved in Methanol and analyzed with the following four analytical methods. a. High Performance Liquid Chromatography (HPLC) Instrument: Micrometric Model 7000 High Performance Liquid Chromatograph Column: Microsil Cl8 Micrometric packing Solvent System: Isocratic mode 10/o isopropanol 90% isooctane Run Mode: Constant pressure (1900psi) Flow Rate approximately 1.7 ml/min Temperature: 25oc Chart Speed: 0.2 in/min -6- UV Wavelength: 254 nm Injection: volume: 8·1-11 concentration: 10 pg/pl quantity: 80 pg Reference J.F. Laurence, 1976, "High Performance Liquid Chromatographic Analysis of Urea Herbicides in Food", J of the AOAC, 59, pp. 1066-1070. -7- Table 1. Analytical Results of Technical Linuron Using HPLC. Manufac- Compo- Ret en- turing Lot nents tion time Pk fo Company 4fo .
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