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The Influence of Carrier Water pH and Hardness on Saflufenacil Efficacy and

Solubility

Article  in  Weed Technology · September 2013

DOI: 10.1614/WT-D-12-00154.1

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Weed Technology 2013 27:527–533

The Influence of Carrier Water pH and Hardness on Saflufenacil Efficacy and

Solubility

Jared M. Roskamp, Ronald F. Turco, Marianne Bischoff, and William G. Johnson*

The pH and hardness of water used as agrochemical carrier can influence herbicide efficacy. The objective of this research
was to determine the role of carrier water pH and hardness on saflufenacil efficacy and solubility. Saflufenacil was mixed in
eight different carrier waters with one of five pH levels (4.0, 5.2, 6.5, 7.7, 9.0) or one of three hardness levels (0, 310, 620
mg L1) and applied POST to common lambsquarters and giant ragweed in a field experiment and to field corn in a
greenhouse experiment. Solubility testing was also completed on saflufenacil mixed in the five pH levels used in the field
and greenhouse experiments. Water hardness did not influence the efficacy of saflufenacil on common lambsquarters, giant
ragweed, or field corn. Control of giant ragweed or common lambsquarters in field experiments was reduced by up to 56%
when saflufenacil was applied in water with a pH of 4.0 compared with water with a pH of 7.7. When nonsoluble
saflufenacil was removed from the spray solution, saflufenacil efficacy on field corn in the greenhouse was reduced by 61%
or more when applied in water with a pH of 4.0 than when applied with water with a pH of 5.2 or higher. When
nonsoluble saflufenacil was applied with the soluble saflufenacil in the spray solution, at least a 7% reduction in control of
field corn was observed when applied in water with pH of 4.0 as compared with saflufenacil applied in water with pH of
5.2 or higher. Solubility of saflufenacil was (1) 10.1 mg L1 in water with a pH of 4.0, (2) 3,461.4 mg L1 in water with a
pH of 7.7, and (3) . 5,000 mg L1 at a pH of 9. Some degradation of parent saflufenacil was detected in the pH at 9.0
treatment, with only 90% of added product being recovered after 3 d of storage. This research provides information on
how saflufenacil efficacy and solubility is influenced by carrier water pH and potentially explains some differences noticed
between field applications of saflufenacil.
Nomenclature: Saflufenacil; common lambsquarters, Chenopodium album L. CHEAL; giant ragweed, Ambrosia trifida L.
AMBTR; corn, Zea mays L.
Key words: Carrier volume, water solution, weed control.

El pH y la dureza del agua usada como medio para aplicaciones de agroquı́micos puede influenciar la eficacia de los
herbicidas. El objetivo de esta investigación fue determinar el rol del pH y dureza del agua para aplicación en la eficacia y
solubilidad de saflufenacil. Se mezcló saflufenacil en ocho medios acuosos diferentes con uno de cinco niveles de pH (4.0,
5.2, 6.5, 7.7, 9.0) o uno de tres niveles de dureza (0, 310, 620 mg L1) y se aplicó POST a Chenopodium album y Ambrosia
trifida en un experimento de campo y a maı́z en un experimento de invernadero. También se completaron pruebas de
solubilidad a las mezclas de saflufenacil con los cinco niveles de pH usados en el experimento de campo y en el de
invernadero. La dureza del agua no influenció la eficacia de saflufenacil sobre C. album, A. trifida, o maı́z. En los
experimentos de campo, el control de A. trifida o C. album se redujo hasta en 56% cuando saflufenacil se aplicó en agua
con un pH 4.0 al compararse con agua con pH de 7.7. Cuando saflufenacil insoluble fue removido de la solución de
aplicación, la eficacia de saflufenacil en maı́z en el invernadero se redujo en 61% o más cuando el agua de aplicación tuvo
pH de 4.0 en comparación con agua con pH de 5.2 o mayor. Cuando se aplicó saflufenacil insoluble con saflufenacil
soluble en la solución de aplicación, se observó una reducción de al menos 7% de control en el maı́z cuando se aplicó en
agua con pH de 4.0 en comparación con saflufenacil aplicado en agua con pH de 5.2 o mayor. La solubilidad de
saflufenacil fue (1) 10.1 mg L1 en agua con pH de 4.0, (2) 3,461.4 mg L1 en agua con pH 7.7, y (3) .5,000 mg L1 a
pH 9. Se detectó un poco de degradación de saflufenacil parental en el tratamiento con pH 9.0, con una recuperación de
solamente 90% del producto agregado a la solución después de 3 d de almacenamiento. Esta investigación brinda
información sobre cómo la eficacia y solubilidad de saflufenacil son influenciadas por el pH del agua de solución de
aplicación y potencialmente explica algunas diferencias notadas entre aplicaciones de campo de saflufenacil.

Water used for herbicide carrier comprises 99% of the
volume of most spray solutions (Altland 2010), and the
elementary qualities of the water, pH and hardness, can
influence herbicide efficacy (Odero 2011). Water hardness is a
measure of cation concentration in water; but for groundwa-
ter, water hardness is primarily a measure of the concentration
DOI: 10.1614/WT-D-12-00154.1
* First and fourth authors: Graduate Research Assistant and Professor,
Department of Botany and Plant Pathology, Purdue University, West
Lafayette, IN 47907; second and third authors: Professor and Research Soil
Microbiologist, Department of Agronomy, Purdue University, West
Lafayette, IN 47907. Corresponding author’s E-mail: wgj@purdue.edu
of dissolved calcium and magnesium. It has been suggested
that extremes in carrier water pH or hardness can influence
the efficacy of some herbicides (Griffin 2009; Ordero 2011);
however, information is lacking on the interaction between
pH or water hardness and the chemical structures of
herbicides in different classes.
Efficacy of weak-acid herbicides can be influenced by the
hardness of carrier water. Carrier water hardness has been
shown to have an antagonistic effect on glyphosate efficacy
(Sandberg et al. 1978; Shea and Tupy 1984). Polyvalent
cations from hard water, especially calcium, magnesium, and
iron, can easily react with glyphosate. The glyphosate

Roskamp et al.: Water pH and hardness on saflufenacil  527

molecule functions as a chelating agent because of its amine,
carboxylate, and phosphonate groups (Thelen et al. 1995),
and that chelation can limit herbicide penetration into the
plant cuticle or cause precipitation of herbicide from solution,
subsequently decreasing herbicide efficacy (Griffin 2009;
Nalewaja and Matysiak 1991; Thelen et al. 1995). Water
hardness has also been reported to limit the efficacy of
dicamba, 2,4-D, and quinclorac. Dicamba and 2,4-D efficacy
on kochia [Kochia scoparia (L.) Schrad.] was reduced 25 to
45% when applied in water containing 400 to 800 mg L1 of
either calcium or magnesium (Nalewaja and Matysiak 1993b;
Nalewaja et al. 1991). Quinclorac efficacy on green foxtail
[Setaria viridis (L.) Beauv.] was reduced by 23% when mixed
in water containing calcium ions (Wozinca et al. 2003).
Carrier water pH can also influence the efficacy of
herbicides, such as glyphosate. When applied at alkaline pH
levels, glyphosate has been shown to have slower herbicidal
activity on sorghum [Sorghum bicolor (L.) Moench ssp.
bicolor] (Stahlman and Phillips 1979). Glyphosate is a weak-
acid herbicide and is susceptible to alkaline hydrolysis at
solution pH values greater than 7.0 (Altland 2010; Seaman
and Riedl 1986). Carrier water pH can also affect solubility of
herbicides. It has been reported that the solubility of
nicosulfuron, an acetolactate synthase–inhibiting herbicide,
decreased from 500 mg L1 (100% of added amount) in
water with pH 8.7 to 60 mg L1 (12% of added amount) in
water with pH 4.6 (Green and Cahill 2003). When
nicosulfuron solubility was reduced by a solution with low
pH, control of large crabgrass [Digitaria sanguinalis (L.)
Scop.] was reduced by 40% (Green and Cahill 2003). Even
though water with basic pH can increase solubility of some
herbicides, the basic solution can limit the movement of
weak-acid herbicides across the plant cuticle, reducing the
efficacy of the herbicide (Callow and Deveau 2010; Green
and Cahill 2003; Green and Hale 2005; Nalewaja et al.
1997). Research has shown that nicosulfuron, once in
solution, would be more active in low-pH carrier solutions
(Green and Hale 2005). Green and Hale (2005) determined
that once the herbicide was in solution, nicosulfuron efficacy
was most directly influenced by the surfactant used. A more
hydrophilic surfactant should be used at high solution pH
levels, whereas a lipophilic surfactant should be used at low
solution pH levels to provide effective weed control with
nicosulfuron (Green and Hale 2005).
With the widespread use of glyphosate-resistant crops,
glyphosate-resistant weeds are a common concern throughout
the Midwest (Kruger et al. 2009). Several weed species
commonly found in corn and soybean [Glycine max (L.)
Merr.] fields in the Midwest, such as giant ragweed,
horseweed [Conyza canadensis (L.) Cronq.], and common
waterhemp (Amaranthus rudis Sauer), have been confirmed as
glyphosate resistant (Heap 2012). Options to control these
glyphosate-resistant weeds have included preplant burndown
programs that include herbicides other than glyphosate.
Saflufenacil is a new herbicide commercialized in the
marketplace and is often used before planting in a burndown
application to control glyphosate-resistant broadleaf weeds.
Saflufenacil is a pyrimidinedione, which inhibits protopor-
phyrinogen IX oxidase (PPO) (E.C. 1.3.3.4) (Grossmann et
528  Weed Technology 27, July–September 2013
al. 2010). Saflufenacil has activity on broadleaf weeds and
works as a contact herbicide with residual activity in the soil
when use rates are 25 g ai ha1 or more (Knezevic et al. 2009).
Saflufenacil is applied at low use rates, and the label
requires that adjuvants, specifically methylated seed oil
(MSO) and ammonium sulfate (AMS) or urea and
ammonium nitrate (UAN), be added to the tank mixture
(Anonymous 2013). A recent study showed that MSO is the
most effective adjuvant for saflufenacil, followed by crop oil
concentrate (COC) and nonionic surfactant (NIS) (Knezevic
et al. 2010). They reported the lowest saflufenacil rate
required for control of 50% (ED50) of horseweed plants was
85 g ai ha1 for MSO, 111 g ai ha1 for COC, and 154 g ai
ha1 for NIS (Knezevic et al. 2010).
The U.S. Environmental Protection Agency (U.S. EPA)
registration information for saflufenacil indicates that solu-
bility is reduced as the pH of water becomes more acidic (U.S.
EPA 2009). Only 0.0014 g of saflufenacil per 100 ml of water
is soluble at pH of 4.0, whereas, in water at a pH of 7.0, the
solubility increased 150-fold to almost 0.21 g of saflufenacil
per 100 ml of water (U.S. EPA 2009). These data suggest that
carrier water pH could influence solubility of saflufenacil in a
spray solution and influence the efficacy of this herbicide,
similar to that reported for nicosulfuron (Green and Cahill
2003).
Inconsistent control of weeds from saflufenacil has been
observed for burndown applications in corn and soybean
fields (W. G. Johnson, personal observation). Preliminary
research indicated that carrier water pH and hardness could
influence the efficacy of saflufenacil (data not shown). A
survey of Indiana groundwater provided by the Indiana
Department of Natural Resources (1999) showed that the
water hardness and pH of Indiana groundwater ranged from 0
to 800 mg L1 and 5.5 to 9.0, respectively, with an average
hardness and pH of 313 mg L1 and 7.3, respectively (IDNR
1999). Therefore, understanding the influence that carrier
water pH and hardness has on the efficacy of saflufenacil will
assist growers and herbicide applicators in achieving the
highest levels of efficacy and reducing field-to-field variability
in weed control. The objectives of this research were twofold:
(1) to determine whether carrier water pH or hardness has an
effect on the efficacy of saflufenacil, and (2) to determine
whether pH of carrier water influences saflufenacil solubility.
Materials and Methods
Influence of Water pH and Hardness on Saflufenacil
Efficacy. The water pH and hardness levels tested throughout
this study were chosen to represent water samples found
throughout Indiana that would typically be available for use as
herbicide carrier.
Field Study. A field experiment was conducted at Throck-
morton Purdue Agricultural Center (TPAC) in Lafayette, IN,
during the summer of 2011. Saflufenacil (Sharpen herbicide,
BASF Corporation, Research Triangle Park, NC) was applied
in carrier water with one of five pH levels (4.0, 5.2, 6.5, 7.7,
and 9.0) or carrier water with one of three hardness levels (0,
310, and 620 mg L1 as calcium carbonate) for eight water
treatments. Hardness levels were adjusted using calcium
chloride (calcium chloride 93% granular, Sigma-Aldrich
Corporation, St. Louis, MO) and magnesium sulfate
(magnesium sulfate 99% anhydrous, Mallinckrodt Baker,
Inc., Paris, KY) mixed at a 3 : 1 ratio of calcium to
magnesium into deionized water. The pH treatments were
created by mixing organic salts into deionized water at 0.1 M.
Water pH levels of 4.0 and 5.2 were created with potassium
hydrogen phthalate (Acros Organics, Geel, Belgium) and
titrated to the proper level with hydrochloric acid (HCl 37%,
Mallinckrodt Baker) or sodium hydroxide (NaOH pellets,
Mallinckrodt Baker) or both. Water pH levels of 6.5 and 7.7
were created with potassium phosphate monobasic crystals
(Avantor Performance Materials, Inc., Phillipsburg, NJ) and
were titrated with HCl or NaOH or both. Water pH of 9.0
was created with tris(hydroxymethyl)aminomethane (Acros
Organics) and was titrated with HCl or NaOH or both. All
solutions were tested with a pH meter (Oakton Waterproof
pH Testr 30, Oakton Instruments, Vernon Hills, IL) to
ensure the desired pH levels.
Saflufenacil was applied at 12.5 g ha1 in each of the eight
water treatments described previously. Ammonium sulfate
(AMS) (APF S-Sul Sprayable AMS 99.5%, American Plant
Food Corporation, Galena Park, TX) and MSO (Sundance II,
Bayer CropScience, Kansas City, MO) were included in all
pH and hardness treatments at 20.37 g L1 and 1% (v/v),
respectively. AMS was added first to the spray solution to
counteract the effect of hardness ions in the water on the
herbicide (McMullan 2000). Saflufenacil was added to the
dissolved AMS solution, followed by the MSO, as suggested
by the label (Anonymous 2013). After addition of adjuvants
and herbicide, solution pH was lowered by 0.5 to 1.0 pH
units from the initial pH level for water sources having a pH
of 6.5, 7.7, and 9.0. For water sources with a pH of 4.0 and
5.2, the initial pH was changed less than 0.5 pH units after
adding the adjuvants and herbicide (data not shown).
The experiment was conducted as a randomized complete-
block design with four replications. The experiment was
repeated in the summer of 2011 for two experimental runs.
The treatments were applied to a fallow area with plot sizes of
3.1 m wide by 9.1 m long. The soil type at TPAC was a
Toronto–Millbrook silt loam with 2.9% organic matter and a
pH of 6.2. The plots contained an evenly distributed
population of common lambsquarters and giant ragweed.
For the first run of the experiment, treatments were applied to
giant ragweed and common lambsquarters at an average
height of 46 cm and 20 cm with densities of 16 and 6 plants
m2, respectively. The second run of the experiment was
applied to giant ragweed and common lambsquarters with an
average height of 25 cm and 15 cm with densities of 8 and 7
plants m2, respectively, approximately 2 weeks later in the
growing season. Treatments were applied at 4.8 km h1 using
a N2-propelled backpack sprayer calibrated to deliver 140 L
ha1 using TeeJet XR11002 nozzles (TeeJet Technologies,
Wheaton, IL) at 275 kPa. Weed control was estimated
visually at 14 d after treatment (DAT) using a scale of 0 to
100%, where 0% was no weed control (same as the
nontreated check), and 100% was complete weed control.
Roskamp et al.: Water pH and hardness on saflufenacil
Foliar chlorosis, necrosis, and plant stunting were considered
when making visual estimates.
Greenhouse Study. A bioassay was conducted in the greenhouse
on field corn (‘33W84 0 , formerly, Pioneer Hi-Bred Interna-
tional, Inc., now, DuPont Pioneer, Johnston, IA) to compare
the activity of saflufenacil in solution to total saflufenacil
(both suspended and in solution) in carrier water with five
different pH levels. Saflufenacil was also applied to field corn
to evaluate the differences in efficacy when applied in hard
water. Water hardness and pH treatments were created using
the same procedure as described previously. Saflufenacil at 25
g ha1 was mixed into water in each of the three levels of
hardness which were used in the field experiments. For the pH
treatments, two samples of water from each of the five pH
levels (4.0, 5.2, 6.5, 7.7, 9.0) were mixed with saflufenacil at
25 g ha1. All treatments were mixed with AMS and MSO as
described previously. All of the water pH treatments were
shaken for 1 h on a shaker table. One sample from each pH
level was filtered, whereas the other sample of each pH level
remained unfiltered. To create the filtered treatment, the
water sample containing saflufenacil was pushed through a
0.45-lm nylon filter (Nylaflo Membrane Disc Filters 47mm,
Pall Life Sciences, Ann Arbor, MI) to remove all of the
suspended solids. The solution that had passed through the
filter contained only saflufenacil that entered into solution
after 1 h of continuous shaking. The other samples at each pH
level were left unfiltered and, therefore, containing both
saflufenacil in solution and in suspension.
Field corn was planted in the greenhouse at a depth of 4.5
cm in 655-cm3 cone-containers (Deepots, Stuewe & Sons,
Tangent, OR) filled with potting soil (Redi-Mix, Sun-Gro
Redi-Earth Plug and Seedling Mix, Sun Gro Horticulture,
Bellevue, WA). Plants were watered daily and fertilized weekly
(Miracle-Gro Water Soluble All Purpose Plant Food [24-8-
16, N–P–K], Scotts Miracle-Gro Company, Marysville, OH]
to maintain active growth. The greenhouse temperatures were
maintained at 22/30 C night/day temperatures. Supplemental
lighting was used to provide a 14-h photoperiod. The
experiment was designed as a randomized complete block
with 5 replications. This experiment was repeated August
2011 through March 2012 for three experimental runs.
Treatments were applied once the corn plants reached the V2
collar stage (Abendroth et al. 2011) using compressed air in a
track spray chamber at 140 L ha1 using a TeeJet 80015EVS
nozzle (TeeJet Technologies) at 275 kPa. Plants were
harvested at 14 DAT and placed in a forced-air dryer at 30
C for 1 wk before dry wt measurement. The percentage of
reduction in corn dry wt was calculated and compared with
the nontreated check.
Effect of Water pH on Saflufenacil Solubility. Laboratory
Experiment. The solubility of saflufenacil at each pH level used
in the previous experiments (4.0, 5.2, 6.5, 7.7, and 9.0) was
determined. A concentration gradient was established by
creating a scale of increasing concentrations of saflufenacil
mixed in water at each pH level and comparing them to a
standard concentration gradient created using analytical-grade
saflufenacil mixed in acetonitrile (ACN). Concentrations of
saflufenacil used to create the gradients were the following: (1)
 529
5 mg L1 to 30 mg L1 for a pH of 4.0, (2) 50 mg L1 to 300 ration, Redmond, WA). Solubility values were found by
mg L1 for a pH of 5.2, (3) 500 mg L1 to 5,000 mg L1 for a solving for the maximum value in the curve.
pH of 6.5, (4) 1,000 mg L1 to 12,500 mg L1 for pH 7.75,
and (5) 1,000 mg L1 to 15,000 mg L1 for pH 9.0.
Saflufenacil concentrations were mixed and shaken for 1 h. Results and Discussion
Aliquots were then removed and filtered through 0.2-lm Influence of Water pH and Hardness on Saflufenacil
nylon syringe filters (VWR International, West Chester, PA) Efficacy. Field Study. Control of common lambsquarters and
into vials (Target DP 9–425 Screw-Thread Vials, Thermo
giant ragweed was not influenced by hardness at P  0.05
Fisher Scientific, Pittsburgh, PA) for solubility testing. To
(data not shown). Saflufenacil was applied with full adjuvant
ensure that all of the saflufenacil was detected during
rates, which included AMS and MSO, as required by the
solubility testing, the saflufenacil caught in the filter was
product label (Anonymous 2013). Because of the inclusion of
measured and compared with the amount that was found to
AMS into the spray solution, the negative effects of calcium
be in solution. To extract the solid saflufenacil from the used
and magnesium cations in the hard water solutions may have
filter, a 60 : 40 mixture of ACN and distilled water were
been prevented, as was shown in previous AMS experiments
pushed through the syringe filters. The ACN and water
with glyphosate and 2,4-D (Nalewaja and Matysiak 1993a,b;
mixture dissolved the saflufenacil that would not normally
O’Sullivan et al. 1981), which are also weak-acid herbicides.
dissolve in water, allowing it to pass through the filter.
The main effect of run was significant (a ¼ 0.05) for
Aliquots of this ACN and water mixture pushed through the
filters were placed into vials for detection. The concentration common lambsquarters and giant ragweed control when
gradient for each pH level was created three separate times saflufenacil was applied in water with varying pH levels. For
and processed in separate high-pressure liquid chromatogra- the first experimental run, the treatments with pH of 4.0 and
phy (HPLC) runs before analysis. 5.2 had less injury than did the treatments with a pH of 6.5 or
Additional samples were made at pH 9.0 to determine higher on common lambsquarters (Table 1). The pH 4.0
degradation of the product. Two concentrations were created treatment only provided 15% control of common lambsquar-
(5,000 mg L1 and 10,000 mg L1) and sampled after 1, 24, ters as compared with 71% control with the pH 7.7 treatment
48, and 72 h of mixing. Samples were kept at room (Table 1). Control of giant ragweed was lowest in water with a
temperature and shaken for 1 h before each aliquot was pH of 4.0, providing only 44% control compared with 84%
removed for testing. control in water with a pH of 7.7 (Table 1). In both weed
Solubility detection of saflufenacil was determined by species, saflufenacil applied in water with a pH of 4.0 or 5.2
conducting HPLC on samples from the concentration provided less control than did saflufenacil applied in water
gradients created previously. Reverse HPLC was performed with a pH of 7.7 or 9.0.
using a Zorbax Eclipse XDB-C18, 150 mm by 4.6 mm, 3.5- The second experimental run showed similar patterns to
lm column (Agilent Technologies, Santa Clara, CA) operated the first run in common lambsquarters control over varying
at 22 C with a mobile phase of 0.1% formic acid (FA) in carrier water pH levels. Saflufenacil applied in water with pH
water and 0.1% FA in ACN at a flow rate of 1 ml min1. The of 4.0 and 5.2 provided lower control of common
elution profile was 50% of the FA and water mixture plus lambsquarters, 10 and 20%, respectively, as compared with
50% of the FA and ACN mixture for 11 min. Concentrations the 7.7 pH treatment, which provided 45% control (Table 1).
were detected using a diode array detector (Agilent Technol- No differences were observed between the pH treatments on
ogies) at 271 nm. Saflufenacil retention time was 7.5 min. the giant ragweed. The increased control of giant ragweed and
Peak heights and area below the peak were converted into lack of separation in the second run was caused by smaller
milligrams per liter for analysis.
Table 1. Control of common lambsquarters and giant ragweed at 14 d after
Statistical Analysis. Weed control ratings and percentages of application when saflufenacil was applied in water at five different pH levels.a
biomass reduction were analyzed using ANOVA in the PROC Weed species pH Run 1 Run 2
MIXED procedure in SAS 9.2 (SAS Institute Inc., Cary, NC).
b,c
Before analysis, data were checked for normality using PROC % control
UNIVARIATE and transformed when necessary. In the field Common lambsquarters 4.0 15 b 10 c
5.2 17 b 20 bc
experiment, a significant run interaction was present for 6.5 55 a 31 ab
common lambsquarters and giant ragweed at a ¼ 0.05; 7.7 71 a 45 a
therefore, data were analyzed separately by run for each weed. 9.0 58 a 28 ab
However, no significant run interactions were noted for any of Giant ragweed 4.0 44 c 94 a
the greenhouse studies; therefore, data were pooled over 5.2 47 bc 97 a
6.5 69 ab 97 a
experimental runs. All transformed data were back-trans- 7.7 84 a 98 a
formed for presentation after analysis. Data for the hardness 9.0 80 a 98 a
treatments were analyzed separately from the data collected a
Saflufenacil was applied at 12.5 g ai ha1 with ammonium sulfate at 20.37 g
from the pH treatments in all trials. Means for significant L1 and methylated seed oil at 1% v/v.
effects were separated using Tukey’s pairwise comparison test b
Visual ratings on a scale from 0 to 100%, where 0% was no control and
at P  0.05. Laboratory experiment data for the overall 100% was complete control.
solubility of saflufenacil were plotted and modeled using a c
Within each weed species, means followed by the same letter in each column
quadratic formula in Excel (Office 2007, Microsoft Corpo- do not differ according to Tukey’s pairwise comparison test at P  0.05.

530  Weed Technology 27, July–September 2013

plant size at application as well as by a larger amount of
variability within treatments. The height of giant ragweed in
the second run was much smaller at the time of application,
which likely caused differences in efficacy between the two
runs.
Although the two runs of the field trial could not be pooled
for analysis, a pattern among the treatments was observed. A
lower solution pH of 4.0 or 5.2 resulted in reduced control of
common lambsquarters as compared with a solution a pH of
7.7. Conversely, effects on the control of giant ragweed were
inconsistent but showed that carrier water pH of 4.0 or 5.2
can reduce efficacy of saflufenacil as compared with carrier
water with a pH of 7.7 or 9.0.
Greenhouse Study. Similar to the weed control in the field
study, water hardness of 310 and 620 mg L1 did not reduce
the control of corn, as compared with the deionized water
treatment at a ¼ 0.05 (data not shown). The herbicide
treatments used in the greenhouse study included full rates of
AMS and MSO as required by the product label (Anonymous
2013). As stated earlier, previous research on other weak-acid
herbicides, specifically glyphosate and 2,4-D, suggest that the
addition of AMS to the spray solution can counteract the
negative effects of cations on herbicide efficacy (Nalewaja and
Matysiak 1993a,b; O’Sullivan et al. 1981), which could
explain lack of differences between hardness treatments.
However, water pH did have an effect on herbicide efficacy.
For the greenhouse study, one-half of the treatments were
filtered to remove the nondissolved herbicide from the spray
solution; therefore, those treatments contained only herbicide
that entered into solution. These filtered treatments were
compared with the unfiltered treatments that contained both
dissolved herbicide and suspended, solid herbicide particles.
Comparing the filtered with the unfiltered treatments
provided information on how much activity the solid
herbicide particles provided at each pH level. Both filtered
and unfiltered spray solutions showed reduced efficacy at a pH
of 4.0. In the filtered treatments, water with a pH of 4.0
provided less control than did all other treatments. The pH
4.0 treatment reduced corn dry wt by 19%, whereas all other
pH treatments reduced corn dry wt between 80 and 86%
(Table 2). In the unfiltered treatments, water with a pH of 4.0
provided less control at 79% dry wt reduction, as compared
with water with a pH of 7.7 or 9.0, which provided 87 and
86% dry wt reduction, respectively (Table 2). Irrespective of
filtering, saflufenacil applied in water with pH from 5.2 to 9.0
reduced corn dry wt by at least 80% (Table 2). When
comparing growth reduction of corn across the pH levels
within the filtered or unfiltered treatments, the pH 4.0
treatment always provided reduced efficacy as compared with
treatments with a pH of 7.7 or 9.0. At a water pH of 4.0,
there was a difference in efficacy between filtered and
unfiltered treatments. The unfiltered treatments provided
more control (79% growth reduction) than did the filtered
treatment (19% growth reduction) (Table 2). This suggests
that the difference in corn dry wt between the nonfiltered
treatment and filtered treatment could be due to the activity
of suspended solids of saflufenacil in the nonfiltered
treatment.
Roskamp et al.: Water pH and hardness on saflufenacil
Table 2. Percentage of reduction in corn dry wt when saflufenacil was applied in
water at five different pH levels and with or without filtering.a,b
Carrier water pH Filtered treatmentsc,d Nonfiltered treatmentsc,d
%
4.0 19 b** 79 b**
5.2 80 a 83 ab
6.5 84 a 83 ab
7.7 84 a 87 a
9.0 86 a 86 a
a
Data were pooled over experimental runs.
b
Saflufenacil was applied at 25 g ai ha1 with ammonium sulfate at 20.37 g
L1 and methylated seed oil at 1% v/v.
c
Means in each column followed by the same letter do not differ according to
Tukey’s pairwise comparison test at P  0.05.
d
Differences (at P  0.05) in Bonferroni pairwise comparisons across rows are
denoted with asterisks (**).
Effect of Water pH on Saflufenacil Solubility. Laboratory
Study. Evaluation of saflufenacil solutions resulted in clear
evidence of a pH effect on the solubility of the herbicide.
Immediately after mixing, visual differences in clarity of
solution could be seen between the pH 4.0 and 9.0 solutions
(Figure 1). HPLC analysis supported the hypothesis that, at
higher pH levels, more herbicide enters into solution.
Detection of saflufenacil by the HPLC procedure showed a
recovery range of 95% or higher from all pH levels, except for
pH 9.0 (Table 3). Model parameters used for solubility
analysis are listed in Table 3. At a pH of 7.7, solubility was
3,687.3 mg L1, whereas at pH 6.5, solubility was only 382.8
mg L1 (Figure 2). Solubility of saflufenacil at a pH of 4.0
and 5.2 was 10.1 mg L1 and 55.2 mg L1, respectively
(Figure 2). Water with a pH of 9.0 supported higher
solubility as compared with the water at a pH of 7.7 (Table
3); however, not all of the added saflufenacil could be
recovered. The U.S. EPA registration sheet for this product
(U.S. EPA 2009) suggests that saflufenacil will undergo
alkaline hydrolysis, which suggests that lower recovery levels
of saflufenacil may result from degradation of the product,
similar to that observed by Mudge et al. (2010) with
Figure 1. Visual observation of saflufenacil solubility at five pH levels.
 531
Table 3. Parameters and amounts of saflufenacil in solution for predicted the activity of the herbicide when proper adjuvants are
solubility models of saflufenacil in carrier water at five different pH levels.
included in the spray solution (Nalewaja et al, 1997).
Maximum R2 However, the ionic form of the herbicide (present at higher
Carrier water pH Solution parametersa solubility value pH levels) is less likely to cross plant membranes (Sterling
mg L1 1994). Green and Hale (2005) showed that adjusting the pH
4.0 0.016(conc)2 þ 0.004(conc) 1.813 10.1 0.81 to an optimum range can increase nicosulfuron efficacy when
5.2 6e4(conc)2 þ 0.308(conc) þ 15.846 55.2 0.97 the proper adjuvants were used. Water with a pH of 5.2
6.5 1e5(conc)2 þ 0.093(conc) þ 167.13 382.8 0.92
7.7 7e6(conc)2 þ 0.292(conc) þ 635.91 3,687.3 0.97
limited the amount of saflufenacil in solution in both the
9.0 1e5(conc)2 þ 0.619(conc) þ 353.79 . 5,000.0 0.97 greenhouse and field rates. The pH 5.2 water treatments in
a
the greenhouse and field studies showed reduced control, as
Abbreviation: conc, original concentration (in milligrams per liter) of mixed
solution.
compared with the pH 7.7 treatment, but were still higher
than the pH 4.0 treatment. This suggests that larger amounts
of saflufenacil in solution can provide more control of
flumioxazin. Only 95 and 90% of the added product could be susceptible plants.
recovered 2 and 3 d after mixing, respectively. Knowledge of saflufenacil solubility at specific pH levels
The data from the solubility experiments provided some can be important. More saflufenacil in solution resulted in
explanation as to why there were differences between better control in corn; therefore, if water pH cannot be
treatments in both the greenhouse and field experiments. changed, increasing the carrier volume will allow for more
Treatments in the field and greenhouse were applied using a saflufenacil to enter into solution. For example, when
12.5 g ha1 and 25 g ha1 of saflufenacil, respectively. Using a applying a field rate of saflufenacil (25 g ai ha1) at 47 L
carrier volume of 140 L ha1, the concentration of saflufenacil ha1, the concentration of saflufenacil is 534 mg L1. In water
in the solution was equivalent to 89 mg L1 and 178 mg L1, with a pH of 6.5, not all of the saflufenacil in the tank will
respectively. With the knowledge that saflufenacil solubility at enter solution. However, when the carrier volume is increased
a pH of 4.0 is 10.1 mg L1, the saflufenacil mixed in the pH to 187 L ha1, the concentration of saflufenacil in the tank is
4.0 treatments for both the field and greenhouse experiments lowered to 133 mg L1, allowing all of the saflufenacil in the
did not completely enter solution. When herbicides are left as tank to enter into solution at a pH of 6.5.
a suspension in the spray solution, there is a potential for From the field and greenhouse experiments, the reported
deposition in the spray tank (Chahal et al. 2012), which could data suggest that water hardness of 310 or 620 mg L1 does
pose an issue in commercial spray operations. The samples in not influence the efficacy of saflufenacil when applied with
this study were shaken immediately before spraying to MSO and AMS. However, water pH does have an influence
eliminate this issue. The reduced control could also be from on saflufenacil solubility and efficacy. Control of common
reduced herbicide absorption. Liu (2004) found that lambsquarters was reduced with water pH treatments of 4.0
bentazon, another weak-acid herbicide, was less soluble at and 5.2 as compared with pH of 7.7. Further work in the
low pH levels and was more likely to crystallize on the leaf greenhouse revealed that saflufenacil in water at pH of 4.0
surface during droplet dry down; therefore, it did not enter provided less control of corn than water with a pH of 7.7 or
the plant. At lower pH levels, saflufenacil has a smaller 9.0. Lastly, the solubility of saflufenacil was greatly reduced at
amount in solution, which may limit the amount of the lower pH levels.
herbicide available for absorption. When solubility is a
limiting factor for herbicides, increasing the pH can increase
Acknowledgments
The authors would like to thank BASF for their support
and contribution of technical-grade saflufenacil for the
chromatography experiments. Thanks also to the members
of the Purdue Integrated Weed Science laboratory for their
assistance with the labor and other tasks of this research.

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Received October 23, 2012, and approved February 22, 2013.
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