Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 401-a–1 TABLE 401-a Pesticide Analytical Manual Vol. I Table 401-a: Recovery of Chemicals Through Method 401 (E1-E2 + C1 + DL1) (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with post-column derivatization and fluorescence detection) Chemical Recovery 1 Rrt 2 ng 3 Notes 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Retention time, relative to carbofuran, on C-8 column described in DL1. 3 ng that cause 50% full scale deflection detector response in DL1. 2,3,5-trimethacarb C 3,4,5-trimethacarb C 3-hydroxycarbofuran C 0.6 10 3-hydroxymethyl-2,5-dimethyl= P (70%) phenyl methylcarbamate 3-hydroxymethyl-4,5-dimethyl= C phenyl methylcarbamate 3-ketocarbofuran V (67-110%) 0.85 11 4-hydroxymethyl-3,5-dimethyl= C phenyl methylcarbamate aldicarb C 0.83 14 aldicarb sulfoxide P (50-60%) 0.33 9 aldoxycarb C 0.4 9 bendiocarb C 1 10 bufencarb C 1.44 19 Major peak is listed. butocarboxim C 0.75 15 carbaryl C 1.06 7 carbofuran C 1 10 dioxacarb C 0.67 15 ethiofencarb P (70-82%) 1.1 15 Breaks down to 2 peaks; other rrt 0.5. fenobucarb C 1.47 10 isoprocarb C 1.13 8 methiocarb C 1.26 10 methiocarb sulfone C 0.79 11 methiocarb sulfoxide C 0.64 12 methomyl C 0.46 10 32% recovery from peanuts. metolcarb C 0.85 10 oxamyl C 0.44 10 promecarb C 1.31 10 TABLE 401-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 401-a–2 Chemical Recovery 1 Rrt 2 ng 3 Notes Table 401-a: Recovery Through Method 401 (E1-E2 + C1 + DL1) propoxur C 0.98 8 thiodicarb P (40-60%) 0.99 11 Recovery C if analytical breakdown product (methomyl) also measured. XMC C 1.06 10 Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 401-b–1 TABLE 401-b Pesticide Analytical Manual Vol. I Table 401-b: Recovery of Chemicals Through Method 401 (E1-E2 + C1 + DL2) (methanol extraction, cleanup with partitioning and charcoal/Celite column, HPLC with fluorescence detection) Chemical Recovery 1 Rrt 2 ng 3 Notes 4 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Retention time, relative to carbofuran, on C-8 column described in DL1/DL2. 3 ng that cause 50% full scale deflection detector response in DL2. 4 Excitation (Ex) and emission (Em) wavelengths found optimum for the chemical. carbaryl C 1.06 3 Ex L 288, Em L 330. carbofuran C 1 90 Ex L 288, Em L 330. CGA 161149 V (43-99%) 0.73 10 Ex L 288, Em L 330. CGA 195654 S (15-132%) 0.57 300 Ex L 288, Em L 330. dioxacarb C 0.67 180 Ex L 265, Em L 294. fluometuron V (60-100%) 1.09 50 Ex L 288, Em L 330. Low level residues may be obscured by matrix interferences. isoprocarb C 1.13 370 Ex L 264, Em L 292. naphthaleneacetamide P (77%) 0.75 3 Ex L 288, Em L 320. For C rec., elute charcoal with additional 100 mL petr ether napropamide C 1.36 4 Ex L 288, Em L 330. phosalone C 1.7 90 Ex L 288, Em L 330. phosalone oxygen analog C 1.3 90 Ex L 288, Em L 330. piperonyl butoxide C 1.74 5 Ex 288, Em L 330. propoxur C 0.98 40 Ex L 276, Em L 300. TABLE 401-b Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 401-b–2 Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–1 TABLE 402-a Pesticide Analytical Manual Vol. I Table 402-a: Recovery of Chemicals Through Method 402 (E1-E7 + C1 + DG1 or DG3 or DG4) (extraction from acidified mixture, GPC, methylation, and Florisil cleanup, determination by GLC) 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Extraction module used during testing (e.g., E1) is indicated with each result. 3 Florisil eluted with Eluant 1 and Eluant 2 only; chemicals eluted in ethyl ether (EE) are considered NR through basic method as normally performed. 4 Ester/ether elutes from Florisil with Eluant 2 unless otherwise noted. 5 When no reference material available for ester/ether, recoveries calculated against acid/phenol methylated per method. Chemical Recovery 1-3 Notes 4,5 2,3,5,6-tetrachlorotere= E1: NR Methylated completely, but did not elute from phthalic acid GPC. E2: NR 2,3,5-triiodobenzoic acid E1: V (66-86%) No ester reference standard. E2: V (79-138%) 2,3,6-TBA E1: C E2: C 2,3-dihydro-3,3-methyl-2-oxo- E1: NR Chemical did not methylate. 5-benzofuranyl methyl sulfonate E2: NR 2,4,5-T E1: P 79% mean recovery, 31% CV, n=270, nonfat and fat. E2: P 2,4-D E1: P 72% mean recovery, 34% CV, n=186, nonfat and fat. E2: P 2,4-DB E1: C E2: C 2-hydroxy-2,3-dihydro-3,3-methyl- E1: NR Chemical did not methylate. 5-benzofuranyl methyl sulfonate E2: NR 3,5,6-trichloro-2-pyridinol NR Some (<20%) recovered in 100mL ethyl ether. 3,5-dibromo-4-hydroxy= S (0-42%) benzoic acid 3-carboxy-5-ethoxy-1,2,4-thiadiazole NR Methyl ester not eluted from Florisil column. 3-chlorosulfonamide acid NR Complete recovery from Florisil only, 14% from GPC. 3-methyl-4-nitrophenol Methyl ether completely eluted from Florisil, but only 30% from GPC. TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 402-a–2 Chemical Recovery 1-3 Notes 4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) 4-chlorobenzoic acid E1: S (27-66%) Low temperature column needed to detect methyl ester. E2: S (2-76%) 4-CPA E1: S (32-69%) Chromatographs only on wide bore GLC. No ester reference standard. E2: C 6-chloropicolinic acid NR Methylates, but methyl ester does not elute from Florisil. AC 263,222 ammonium salt NR Methyl ester not eluted from Florisil. acifluorfen E1: P (54-69%) alloxydim-sodium E1: NR Does not methylate. E2: NR arsanilic acid Compound did not methylate under method conditions. benazolin E1: NR 28-32% recovered if Florisil eluted with additional 100 mL EE. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. bifenox E1: C Parent is methyl ether. E2: C bromacil E2: NR Complete recovery if Florisil eluted with addi- tional 100 mL EE. bromofenoxim E1: P (57-86%) No ether reference standard. E2: C bromoxynil E1: P (50-68%) No ether reference standard. E2: C chloramben E1: S (40-43%) E2: P (49-59%) chloroxuron E1: NR Does not methylate. E2: NR clofencet potassium salt NR Does not methylate. cloprop E1: P (50-66%) Chromatographs only on wide bore GLC. No ester reference standard. E2: C Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–3 TABLE 402-a Pesticide Analytical Manual Vol. I Chemical Recovery 1-3 Notes 4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) CP 106070 NR Does not methylate. CP 106077 NR Some methylation, but does not elute from GPC. CP 108064 E1: NR NR through method even in 100 mL EE; recovered from GPC only, Florisil only. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. CP 108669 NR Some methylation, but does not elute from GPC. CP 92429 NR Does not methylate. CP 95200 NR Some methylation, but does not elute from GPC. CP 97290 NR Does not methylate. cyclanilide E1: C E2: V (45-67%) dicamba E1: P (71-76%) E2: C dichlorprop E1: C (80%) No ester reference standard. E2: C (72-104%) diclofop E1: S (43-51%) E2: V (81-200%) dinoseb E1: NR Does not methylate. E2: NR disul-Na E1: NR Does not methylate; parent 50% recovered if Florisil eluted with 100 mL EE. E2: NR Does not methylate; complete recovery of parent with 100 mL EE. DNOC E1: S (45-50%) Nitrogen detector required. No ether reference standard. E2: C dodine E1: NR Does not methylate. E2: NR fenac E1: C (74-92%) No ester reference standard. E2: C flumetsulam E1: NR Methylated product not soluble in hexane. E2: NR TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 402-a–4 Chemical Recovery 1-3 Notes 4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) fluroxypyr E1: S (23-30%) Two peaks result; 3-7% more eluted with100 mL EE. No ester ref std. E2: P (64-77%) Two peaks result; complete recovery with 100 mL EE. No ester ref std. haloxyfop E2: P (54%) Florisil elution with 100 mL EE not tested. HOE-038182 E1: NR Methylation was complete, but ester not recovered. E2: S (30-41%) Elution from Florisil only with eluant #2 + 100 mL EE. HOE-099730 NR Does not methylate. imazamox NR Methyl ester not eluted fromFlorisil. ioxynil E1: C (80-87%) No ether reference standard. E2: C iprodione urea NR Methyl ether not eluted from Florisil. MCPA E1: C (78-89%) E2: C MCPB E1: C (70-106%) Chromatographs only on wide bore GLC. No ether reference standard. E2: C mecoprop E1: C (73-84%) Wide bore GLC recommended. No ester reference standard. E2: C PB-7 E1: NR Complete recovery if Florisil eluted with addi- tional 100 mL EE. E2: NR pentachlorophenol E1: P 70% mean recovery, 31% CV, n=275, nonfat and fat. E2: P picloram E1: NR 6-10% recovered if Florisil eluted with additional 100 mL EE. E2: NR Complete recovery if Florisil eluted with additional 100 mL EE. PPG-947 E1: P (49-78%) Two peaks from methylation; only one seen by halogen detector. pyrithiobac-sodium E1: S (7-13%) Additional 31-34% recovered if Florisil eluted with 100 ml EE. Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 402-a–5 TABLE 402-a Pesticide Analytical Manual Vol. I Chemical Recovery 1-3 Notes 4,5 Table 402-a: Recovery Through 402 (E1-E7 + C1 + DG1 or DG3 or DG4) RPA203328 NR Small (0-34%) recovery in 100 mL ethyl ether. silvex E1: C E2: C triadimenol E1: NR Methyl ether not eluted from Florisil. E2: NR triclopyr E1: C Recovery from fatty foods may be <50%. E2: C vinclozolin metabolite B E1: S (26-43%) Methylated product is parent vinclozolin; 62% recovery through Florisil only. E2: S (27-43%) TABLE 402-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96)) Form FDA 2905a (6/92)TABLE 402-a–6 Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 403-a–1 TABLE 403-a Pesticide Analytical Manual Vol. I DL3: Methanol/ DL4: Acetonitrile/ Water Mobile Phase Water Mobile Phase Table 403-a: Recovery of Chemicals Through Method 403 (E1 + C1 + DL3 and DL4) (methanol extraction, cleanup by partitioning and Florisil chromatography, HPLC with post-column photolysis and derivatization, fluorescence detection) Chemical Recovery 1 Rrt 2 Notes 3 Rrt 2 Notes 3 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Retention time, relative to diuron, on the HPLC system described. 3 LD, limit of detection: concentration (ppm) of phenylurea found to cause response three times baseline noise; LQ, limit of quantitation: concentration (ppm) found to cause response 10 times baseline noise. chlorbromuron C 1.16 LD 0.006, LQ 0.022 1.28 LD 0.003, LQ 0.011 chlorotoluron C 0.87 0.91 chloroxuron C 1.25 LD 0.002, LQ 0.008 1.28 LD 0.001, LQ 0.003 diuron C 1 LD 0.002, LQ 0.007 1 LD 0.001, LQ 0.003 fenuron C 0.42 0.49 fluometuron C 0.87 LD 0.002, LQ 0.006 0.93 LD 0.001, LQ 0.003 isoproturon C 0.96 1 linuron C 1.12 LD 0.004, LQ 0.014 1.23 LD 0.005, LQ 0.017 metobromuron C 0.91 LD 0.004, LQ 0.015 1.04 LD 0.004, LQ 0.014 metoxuron C 0.62 0.67 monolinuron C 0.91 0.99 monuron C 0.72 0.75 neburon C 1.34 1.43 siduron C 1.08 1.16 TABLE 403-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 403-a–2 Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92) TABLE 404-a–1 TABLE 404-a Pesticide Analytical Manual Vol. I Table 404-a: Recovery of Chemicals Through Method 404 (E1-E3 + DL5) (methanol extraction, partitioning into methylene chloride, HPLC with ion pairing mobile phase and UV and fluorescence detection) 1 Codes: C: complete (>80%); P: partial (50-80%); S: small (<50%); V: variable (approximate percentage when known); R: recovered but no quantitative information available; NR: not recovered. 2 Residue may result from use of: (1) benomyl, never found as a residue itself, because it is rapidly converted to MBC; (2) thiophanate-methyl, which degrades slowly to MBC; or (3) carbendazim, as MBC is called when used as a fungicide itself (not registered in the U.S.). Chemical Recovery 1 Notes allophanate C Determined by UV detector at 250 nm. benomyl C Determined as MBC (carbendazim) by UV detector at 280 nm. MBC 2 C Determined by UV detector at 280 nm. thiabendazole C Determined by UV detector at 280 nm; confirm, increase sensitivity with DL7. thiophanate-methyl C Determined by UV at 280 nm; degrades in extract, must be determined quickly. TABLE 404-a Pesticide Analytical Manual Vol. I Transmittal No. 96-E1 (9/96) Form FDA 2905a (6/92)TABLE 404-a–2