Supporting Information. Occurrence of dichloroacetamide herbicide safeners and co-applied herbicides in. Midwestern US streams
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1 1 2 3 Supporting Information Occurrence of dichloroacetamide herbicide safeners and co-applied herbicides in Midwestern US streams 4 Emily E. Woodward, 1,* Michelle L. Hladik, 1 and Dana W. Kolpin U.S. Geological Survey, 6000 J. Street, Placer Hall, Sacramento, California U.S. Geological Survey, 400 S. Clinton St., Iowa City, Iowa, * Corresponding author address: ewoodward@usgs.gov; phone:
2 Experimental Methods GC/MS Analysis. Herbicide safener extracts were analyzed using GC/MS. The column used was an Agilent DB-5MS+DG (30 m, 0.25mm, 0.25 µm). The initial run temperature was 80 C, and the temperature ramped to 300 C over 15 min. Temperature settings were 150 C for the MS quad, 230 C for the MS source, and 280 C for the MS transfer line. Retention times and MS ions for each compound are reported in Table S3. Quality Assurance Field blanks were collected (n=8). AD-67, benoxacor, dichlormid, furilazole, and the two herbicides were not detected in any of the field blanks. Field replicates were collected (n=4). Relative percent differences (RPD) between the regular and replicate sample were calculated, when possible, for each compound: AD-67 not detected in regular sample or replicate, 90% for benoxacor, 0% for dichlormid, 15 to 23% for furilazole, 0 to 8% for acetochlor, and 0.5 to 7% for metolachlor. For this study, surrogate recovery of d 14 -triflurlain ranged from 55 to 127%, the mean recovery was 86%, and 98% of the samples collected (188 out of 192) had recoveries between 70 and 130%. Data were not recovery corrected
3 47 48 Table S1. Site information and safener detection frequencies for the seven streams sampled. [km 2, square kilometers: %, percent: N, number] Site Name USGS ID Drainage Area a (km 2 ) Corn Cover b (%) Samples (N) Detection Frequency (%) AD-67 Benoxacor Dichlormid Furilazole WB Wapsinonoc Creek at College St. at West Branch, IA Spoon River near St. Joseph, IL Clear Creek near. Oxford, IA Old Mans Creek near Iowa City, IA English River at Kalona, IA Vermilion River near Danville, IL Iowa River at Wapello, IA a Data from USGS National Water Information System 1. b Percent corn cover (%) represents cover within each drainage basin and was calculated using Geographic Information Systems (crop data layer from United States Department of Agriculture Statistics Service 2 )
4 Table S2. Herbicide safeners and stream flow for the samples collected across Iowa and Illinois. [Parentheses are used to indicate concentrations that are between the compound specific limit of detection and method reporting limit values: Q, discharge: m 3 /sec, cubic meter per second: ng/l, nanograms per liter: nd, concentration less than the limit of detection (not detected): nr, near] Site Date Q a Concentration (ng/l) (m 3 /sec) AD-67 Benoxacor Dichlormid Furilazole Acetochlor Metolachlor WB 3/16/ nd nd nd nd nd 50 Wapsinonoc 4/06/ nd nd nd nd Creek at 4/20/ nd nd nd nd College St. 4/27/ nd nd nd nd at West 4/28/ nd nd Branch 4/30/ nd 12 nd nd /09/ nd ,000 2,400 5/24/ nd nd nd nd /28/ nd nd nd nd /15/ nd nd nd nd /22/ nd 22 nd ,000 9/7/ nd nd nd nd /3/ nd nd nd nd nd 18 10/11/ nd nd nd nd nd 20 10/26/ nd nd nd /9/ nd nd nd nd nd 29 11/23/ nd nd nd /28/ nd nd nd /6/16 - nd nd nd nd nd 4,000 12/13/16 - nd nd nd nd nd 20 1/11/16 - nd (5) nd nd nd 19 1/16/17 - nd nd nd nd /17/17 - nd nd nd nd /8/17 - nd nd 10 nd nd 12 3/7/ nd nd nd nd nd 12 3/27/ nd nd nd nd nd 31 3/29/ nd nd nd nd nd 38 3/30/ nd nd nd nd nd 250 4/5/ nd nd nd nd nd 120 4/10/ nd nd nd nd /16/ nd nd nd nd /17/ nd nd nd nd /27/ nd nd 7 nd /28/ nd nd (6) nd /29/ nd 14 nd nd /1/ nd nd nd nd /11/ nd ,000 4,800 5/18/ nd /20/17 * 0.6 nd 10 nd nd /20/17 * 0.6 nd 63 nd 9 2,100 5,000 5/26/ nd 25 nd (4) /8/ nd nd nd nd
5 63 Table S2. Continued Site Date Q a Concentration (ng/l) (m 3 /sec) AD-67 Benoxacor Dichlormid Furilazole Acetochlor Metolachlor WB 6/14/ nd nd nd nd Wapsinonoc 6/15/ nd nd nd nd Creek Cont. 6/17/17 - nd 44 nd , Spoon River nr. St. Joseph, IL Clear Creek nr. Oxford, IA 9/15/ nd nd nd nd nd 94 10/4/ nd nd nd nd /20/ nd 11 nd nd 90 1,600 11/3/ nd nd nd nd /14/ nd nd nd nd nd 47 11/29/ nd nd nd nd /12/ nd nd nd nd nd 62 1/11/ nd nd nd nd nd 48 1/18/ nd nd nd nd /28/ nd nd nd nd nd 60 3/8/ nd 14 nd nd nd 730 3/31/ nd nd nd nd /1/17 21 nd nd nd 30 1,600 9,700 5/25/ nd nd nd nd /15/ nd nd nd nd /21/ nd nd nd /28/ nd 13 nd nd /1/ nd 12 nd /10/ nd 32 nd /23/ nd nd nd nd nd 37 5/28/ nd 15 nd nd /15/ nd 11 nd ,900 6/22/16 13 nd 14 nd ,000 9/8/ nd nd nd nd /3/ nd nd nd nd nd 23 10/11/ nd nd nd nd /27/ nd nd nd nd /9/ nd nd nd nd nd 30 11/23/ nd nd nd nd /28/ nd nd nd nd nd 76 12/6/ nd 7 nd nd /13/ nd nd nd nd nd 20 1/11/ nd 16 nd nd /17/17 - nd nd nd nd /8/ nd (6) nd nd nd 12 3/7/ nd 7 nd nd nd 13 3/27/ nd nd nd nd nd 31 3/30/ nd nd nd nd nd 43 4/6/ nd nd nd nd /16/ nd nd nd /17/ nd nd nd nd /27/ nd nd (5) nd
6 65 Table S2. Continued Site Date Q a Concentration (ng/l) (m 3 /sec) AD-67 Benoxacor Dichlormid Furilazole Acetochlor Metolachlor Clear Creek 4/30/ nd nd (5) Cont. 5/1/ nd nd , /11/ nd ,800 4,200 5/18/ nd ,000 7,100 5/20/ nd 11 nd ,600 5/26/ nd 58 nd (5) 130 4,600 6/8/ nd nd nd nd /15/ nd 11 nd nd /17/ nd ,000 5,300 Old Mans Creek nr. Iowa City, IA English River at Kalona, IA 3/16/ nd nd nd nd nd 53 4/7/ nd nd nd nd /21/ nd nd nd /29/ nd 31 nd /1/ nd 12 nd 25 1,900 2,300 5/10/16 15 nd ,900 4,100 5/23/ nd nd nd nd /28/16 13 nd 31 nd ,800 6/15/ nd 10 nd /22/16 25 nd 14 nd ,700 9/8/ nd nd nd nd nd 81 10/3/ nd nd nd nd nd 25 10/11/ nd nd nd nd nd 45 10/27/ nd nd nd nd /9/ nd nd nd nd nd 30 11/23/ nd nd nd nd nd 31 11/29/ nd nd nd nd /6/ nd (5) nd nd nd 31 12/13/ nd nd nd nd nd 20 1/11/ nd nd nd nd nd 18 1/17/17 33 nd nd nd nd /8/ nd nd nd nd nd 10 3/7/ nd (4) nd nd nd 12 3/27/ nd nd nd nd /30/ nd nd nd nd nd 53 4/6/17 34 nd nd nd nd /17/ nd nd nd nd /27/ nd nd (6) /2/17 14 nd nd ,100 1,000 5/11/17 22 nd ,100 4,900 5/18/17 27 nd ,800 5,800 5/20/17 31 nd ,000 3,700 6/8/ nd nd nd nd /15/ nd nd nd nd /18/17 16 nd ,200 2,100 3/17/16 16 nd nd nd /17/16 14 nd nd nd /21/ nd nd nd nd /29/ nd 24 nd
7 66 Table S2. Continued Site Date Q a Concentration (ng/l) (m 3 /sec) AD-67 Benoxacor Dichlormid Furilazole Acetochlor Metolachlor English 5/2/16 26 nd 35 nd 30 2,600 3,600 River Cont. 5/10/ nd ,300 6,900 5/25/16 12 nd nd nd /28/16 61 nd 60 nd 43 3,700 6,700 6/15/ nd nd nd nd /8/16 16 nd nd nd nd /3/ nd nd nd nd nd 35 10/11/ nd nd nd nd nd 41 10/27/16 25 nd nd nd nd 680 1,900 11/9/ nd nd nd nd nd 43 11/23/ nd nd nd nd nd 44 11/29/16 11 nd nd nd nd 410 1,700 12/6/ nd nd nd nd /17/ nd nd nd nd /8/ nd (5) nd nd nd 24 3/7/ nd (4) nd nd /27/ nd nd nd nd /30/17 25 nd nd nd nd /6/ nd nd nd nd /17/17 22 nd nd nd nd /27/17 11 nd nd (6) /2/17 62 nd ,900 4,600 5/11/17 57 nd ,000 4,200 5/18/17 50 nd ,900 2,200 5/20/17 85 nd 25 (6) 26 3,400 7,100 6/8/ nd nd nd (5) /15/ nd nd nd nd /18/17 27 nd ,300 4,300 Vermilion River nr. Danville, IL Iowa River at Wapello, IA 9/15/16 31 nd nd nd nd /4/16 12 nd nd nd nd nd 34 10/20/16 14 nd nd nd nd /3/16 20 nd nd nd nd /14/16 11 nd nd nd nd nd 59 11/29/ nd nd nd nd nd 95 12/12/16 - nd nd nd nd /11/17 26 nd nd nd nd /18/ nd nd nd nd /28/17 16 nd nd nd nd nd 61 3/8/17 31 nd nd nd nd nd 26 3/31/17 87 nd nd nd nd /1/ nd ,500 4,900 5/25/17 56 nd nd nd ,000 6/15/17 23 nd nd nd /24/ nd nd nd nd /6/ nd nd nd nd nd 56 5/11/ nd 43 nd 30 2,600 3,700 5/24/ nd nd nd nd
8 67 68 Table S2. Continued Site Date Q a Concentration (ng/l) (m 3 /sec) AD-67 Benoxacor Dichlormid Furilazole Acetochlor Metolachlor Iowa River 6/8/ nd nd nd Cont. 9/30/ nd nd nd nd /19/ nd nd nd nd /6/ nd nd nd /15/ nd nd nd /8/ nd nd nd /22/ nd nd nd nd /12/ nd nd nd /26/ nd nd nd /1/ nd nd nd (6) a Data from USGS National Water Information System 1. * One sample taken at 7:15 and one sample taken at 15: Table S3. GC/MS retention times (RT), quantitation ions (Quant), qualitative (Qual) ions, average laboratory spiked water sample recoveries (n=3), and percent relative standard deviation (RSD) for dichlormid, furilazole, AD-67, and benoxacor. Compound RT (min) Quant Qual Recovery (%) RSD (%) Dichlormid Furilazole AD Benoxacor
9 Figure S1. West Branch Wapsinonoc Creek at College St. at West Branch ( ). Seasonal views looking immediately downstream of the sampling location (left photos) and a representative field upstream of the sampling location (right photos), for stream-water collection on. A: April 6, 2016 (0.08 m 3 /sec); B: May 9, 2016 (0.5 m 3 /sec); C: June 22, 2016 (0.7 m 3 /sec); D: October 26, 2016 (0.2 m 3 /sec); E: December 13, 2016 (discharge data unavailable); F: February 8, 2016 (discharge data unavailable); G: March 29, 2017 (0.1 m 3 /sec). A B
10 C D E Figure S1. Continued
11 F G Figure S1. Continued
12 Figure S2. Concentrations of AD-67, benoxacor, dichlormid, and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for West Branch Wapsinonoc Creek ( ), March 2016 through June The shaded area is the typical corn planting season in Iowa. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
13 Figure S3. Concentrations of benoxacor, dichlormid, and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for Old Mans Creek ( ), March 2016 through June AD-67 was not detected at this site. The shaded area is the typical corn planting season in Iowa. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
14 Figure S4. Concentrations of benoxacor, dichlormid, and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for Clear Creek ( ), March 2016 through June AD-67 was not detected at this site. The shaded area is the typical corn planting season in Iowa. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
15 Figure S5. Concentrations of benoxacor and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for Iowa River ( ), March 2016 through June AD-67 and dichlormid were not detected at this site. This site was not sampled using a hydrologic sampling approach, and this site had the largest drainage area out of all of the sites sampled. The shaded area is the typical corn planting season in Iowa. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
16 Figure S6. Concentrations of benoxacor and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for Spoon River ( ), September 2016 through June AD-67 and dichlormid were not detected at this site. The shaded area is the typical corn planting season in Illinois. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
17 Figure S7. Concentrations of benoxacor, dichlormid, and furilazole, the herbicides acetochlor, and metolachlor, and stream discharge for Vermilion River ( ), September 2016 through June AD-67 was not detected at this site. The shaded area is the typical corn planting season in Illinois. [ng/l, nanogram per liter: m 3 /sec, cubic meter per second]
18 References (1) National Water Information System: USGS Water Data for the Nation 2017 (US Geological Survey). Available at (accessed 11 August 2017). (2) USDA National Agricultural Statistics Service Cropland Data Layer 2016 (US Department of Agriculture). Available (accessed 1 August 2017)
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