MISCELLANEOUS TECHNIQUES AND IMPURITIES

MT 53 WETTABILITY

INTRODUCTION
The laboratory evaluation of wetters for agricultural purposes has frequently been
based on surface tension measurements. C C Thompson (Notes 1 and 2) has shown
that surface tension is unreliable for evaluating wetters intended for producing
complete wetting of leaf surfaces at high volumes. He has also shown that the
Draves test, based on the wetting of cotton hanks, is a possible laboratory
procedure for evaluating such wetters. However, a modified Shapiro test (Note 3),
based on the sinking times of a standard cotton tape, gives rather better results and
requires considerably less experimental skill. This test may be satisfactorily used
for evaluation of wetters in both soft and hard waters, and for the evaluation of
wetters intended as additives to aqueous dispersions of pesticidal formulations. A
satisfactory wetting solution, for application at high volume spraying rates to leaves
which are difficult to wet, will be given by the concentrations that have a tape
sinking time of not more than 15 sec.
In addition, a standard leaf dipping procedure, which bears a relationship to the
modified Shapiro test, is given for evaluating the performance of wetters on leaf
surfaces (Note 3).
53.1 Wetting time of a standard tape
OUTLINE OF METHOD
A weighted length of cotton tape is dropped into a tall cylinder containing an
aqueous solution of a wetting agent. The time required for the thread connecting
the weight and the tape to relax is recorded as the sinking time. Concentrations of
wetters requiring a sinking time of 15 sec are compared. The test may be used on
formulated pesticides but it does not necessarily apply to cationic wetters.
REAGENTS
Sodium 1,2-bis(2-ethylhexyloxycarbonyl)ethanesulphonate, RE 71, 0.5% standard
stock solution; dry a sample at 95°C for 2 to 3 h and store in a desiccator. Dissolve
5.00 g of the dried compound in 1000 ml of distilled water (Note 4).
APPARATUS
Wire hooks of 16 SWG stainless steel (1.625 mm diameter) of standard weight and
with attached anchors (see Fig 29; Note 5)
Cotton tape (Note 6)
Measuring cylinder 500 ml
Beakers 1500 ml

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Volumetric flasks 1000 ml

Bulb pipette 100 ml or aspirator
Bulb transfer pipettes assorted sizes
Thermostatic water bath, at 25 ± 0.25°C
Stop watch

Figure 29 Diagram of hook and anchor used for determination

of sinking time of cotton tape in the modified Shapiro's
method. The wire hook weighing 0.50 g is connected with a
nylon thread to a cylindrical lead slug weighing 30 to 40 g.,

PROCEDURE

(i) Preparation of solutions.

Weigh (to the nearest mg) about 5 g of sample (unless the solubility is so poor
that a smaller amount must be used), dissolve in water (about 250 ml) at the
minimum temperature at which the material is soluble, transfer to a 1000 ml
volumetric flask, and make up to volume with cold distilled water. Dilute suitable
aliquots to 1000 ml with distilled water and maintain at 25 ± 0.25°C.

(ii) Determination of sinking time.

Pour each of the dilute solutions into a 1.5 litre beaker and thence into the
cylinders, to ensure thorough mixing (Note 7). Put them in the water bath at 25
± 0.25°C, and leave until all the air bubbles have risen to the top. Remove any
foam on the surface with a 100 ml pipette or aspirator (Note 8).

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Lay a length of tape, without tension, on a flat surface, place a ruler on it and cut
22 cm lengths, as required. Insert the hook, with the anchor attached, through the
tape about 0.5 cm from one end of a 22 cm length. Hold the tape by the free end
with the anchor and the bottom of the hook immersed in the wetting solution
contained in a 500 ml cylinder. Start a stop watch as the tape is dropped into the
solution and stop when the tape wets and starts to sink to the bottom of the cylinder
(Note 9). At least five tests must be made for each concentration of wetting agent.

(iii) Standardization of the tape.

Determine the sinking time of each batch of tape by the standard procedure with a
0.02% solution of sodium 1,2-bis(2-ethylhexyloxycarbonyl)ethanesulphonate
prepared by dilution of the stock solution with distilled water. The mean of five
determinations at 25°C should normally give a sinking time of 15.0 ± 1.0 sec.
(iv) Interpretation of results. Plot the values for the concentrations of wetting
agents, expressed as g/100 ml, on the horizontal scale of log - log graph paper.
Similarly, plot mean sinking time, in seconds, on the vertical scale. Draw a smooth
curve and determine the concentration of wetting agent which corresponds to a
sinking time of 15.0 sec (Fig 30).

Figure 30 Evaluation of wetting agents, on log - log scale. See text for interpretation
53.2 Wetting of leaf surfaces
OUTLINE OF METHOD
A freshly picked leaf is immersed in a solution of wetting agent under standardized
conditions and a visual examination of the area wetted is made.

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The minimum concentration of wetting agent, which will produce complete

wetting of a cabbage leaf, is normally that concentration which will give a sinking
time of 15 sec by the tape test (MT 53.1).

REAGENT
Cabbage leaves variety, January King

APPARATUS
Beakers 500 ml
Thermostatic water bath at 25 ± 0.25°C

PROCEDURE
(i) Method.

Transfer 400 ml portions of solutions of wetting agents at suitable concentrations

to beakers and immerse the beakers to solution level in a water bath at 25°C (Note
10). Immerse a freshly picked undamaged leaf in the test solution (Note 11) for 1
sec and withdraw it, and examine after 5 sec. With the leaf held vertically make a
visual estimate of the percentage area wetted (Note 12 and Note 13).
Make at least 20 tests with 5 leaves from each of 4 separate plants.

(ii) Evaluation of results.

To compare the wetting properties of a group of wetting agents for a leaf such as
cabbage, which is difficult to wet, determine the minimum concentration of wetting
agent which produces 100% wetting of 4/5ths of the number of leaves tested. A
comparison of the wetting of the tape and cabbage leaves is given in Table I.

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TABLE I
Tape test Leaf wetting test*
Concentration of wetter to give
Wetter Concentration of wetter to 100% visual wetting of
Sample give a 15 sec wetting time January King Cabbage leaves
(g/100 ml) (g/100 ml)
A 0.057 0-025 - 0.500
B 0.540 > 0.500
C+ 0.020 0.025 - 0.050
D 0.055 0.025 - 0.050
E 0.066 0.050 - 0.100
F 0.032 0.020 - 0.050
*
The results are recorded as ranges of wetter concentrations to produce 100 %
wetting on cabbage leaves from plants between 6 to 20 weeks old.
+
Standard wetter - sodium 1,2-bis(2-ethylhexyloxycarbonyl)ethanesulphonate
With cabbage of the January King variety, largest leaves from the middle of the
stem, from plants of the same age, should be used for comparative wetting tests
since they are more difficult to wet than the lower or higher positioned leaves.

53.3 Wetting of wettable powders

SCOPE
The method describes a procedure for the determination of the time of complete
wetting of wettable powders.
OUTLINE OF METHOD
A weighed amount of the powder is dropped on water in a beaker from a specified
height. The time for complete wetting is determined.
REAGENT
Standard Water MT 18 (Note 14)

APPARATUS
Beaker 250 ml, internal diameter 6.5 ± 0.5 cm, height 9.0 ± 0.5 cm
Weighing bottle
Stop watch accurate to the nearest second
Measuring cylinder 100 ml

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PROCEDURE

53.3.1 Without swirling.

Pour Standard Water (100 ± 1 ml) into the beaker. Weigh out 5 ± 0.1 g of a
representative sample of the powder, taking care that it remains in a non-compacted
state. Add all the powder at once, by dropping it on the water from a position level
with the rim of the beaker, without undue agitation of the liquid surface.
When the powder is added, start the stop watch and note the time taken (to the
nearest second) for it to become completely wetted (Note 15).
Report the time, to the nearest second, required for complete wetting of the powder
as the wetting time.
53.3.2 With swirling.
Carry out the procedure given in MT 53.3.1 except that the contents of the beaker
should be swirled by hand at the rate of 120 swirls per minute after the addition of
the powder. Report the results as wetting time with swirling.
Note 1 C C Thompson, J Sci Food Agric, 1958, (9-10), 650-657.
Note 2 Modified from the method described by L Shapiro, American Dyestuff
Reporter, 1950, 39, 38 - 45, 62.
Note 3 R de B Ashworth and G A Lloyd, J Sci Food Agric, 1961, 12, (3), 234.
Note 4 Sodium 1,2-bis(2-ethylhexyloxycarbonyl)ethanesulphonate for the
preparation of standard solutions should be of such purity that only 2-
ethyl- hexan-1-ol is detectable by gas chromatography. Sodium 1,2-
bis(2-ethyl- hexyloxycarbonyl)ethanesulphonate may be obtained from
Messrs Hard- man and Holden, Clayton Works, Manchester 11, England.
Note 5 Make the hook and attached anchor as follows:
Bend a piece of No 16 SWG (1.625 mm diameter) stainless steel wire
about 3.5 cm in length into a two pronged hook (Fig 30). File the ends to
sharp points and adjust the weight to exactly 0.500 g. Attach the hook
with a length of nylon thread to a loop of wire secured to the centre of a
cylindrical lead weight (ca 35 g). The distance between the base of the
hook and the anchor should be 2.0 cm.
Note 6 One inch tape conforming to BS 1626:1972, 'Woven Cotton Tape Light,
Medium and Heavy Quality' with 73 warp ends and 36 weft picks per inch
is suitable and may be obtained from Rykneld Mills Ltd. Bridge Street,
Derby DE1 3LH, UK. The tape is uniformly woven from untreated yarn,
freed from defects and has straight and firmly woven selvedges. The width
of the tape should be 1 ± 0.04 inch, the weight per 144 yd should be 25 ±
1.25 oz and the minimum breaking load 70 lb.

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Note 7 If the more dilute solutions are tested first, the beakers and cylinders used
need not be rinsed and dried each time.
Note 8 The same diluted solution may be used many times without apparent
exhaustion of the wetting agent, but cationic wetters are perhaps better in
this respect.
Note 9 In cloudy solutions it may be difficult to observe sinking of the tape in
emulsions or suspensions. Where great accuracy is not required, attach a
short length of nylon thread to the free end of a length of tape and
counter balance over the side of the cylinder with a 20 mg weight.
Upward movement of the weight indicates the sinking time. For greater
accuracy, use a square sided vessel with side illumination from a
powerful light source or, alternatively, wind a length of insulated single
core copper wire closely round a 500 ml cylinder to a height of 2 cm
from the base of the cylinder. Similarly, construct a secondary coil of
four to five times the number of turns of the primary. Connect the
primary coil to a source of alternating current at 6 to 12 volts and the
secondary coil to a sensitive milliammeter. When a hook of iron wire
enters the field produced by the primary coil, a current is induced in the
secondary coil. Thus, record the sinking time by observing the movement
of the ammeter needle.
Note 10 Remove foam or air bubbles from the surface of a solution before tests of
leaf wetting are made, using a filter paper pad.
Note 11 The area wetted by dipping a leaf in the solution gives results comparable
to high volume spraying.
Note 12 Do not touch any surface with the leaf when withdrawing it from the
beaker.
Note 13 Visual assessment of percentage area wetted may be subject to large errors
between 5 and 95% levels, particularly with cabbage leaves; hence the
need to relate the concentration to 100% wetting.
Note 14 Use CIPAC Standard Water D (MT 18.1.4) unless otherwise agreed.
Note 15 Neglect a film of fine particles remaining on the surface.

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