MISCELLANEOUS TECHNIQUES AND IMPURITIES

MT 23 MISCIBILITY WITH HYDROCARBON OIL

OUTLINE OF METHOD

The sample is mixed with a suitable oil and is then allowed to stand at 30 °C for
1 h. The solution is examined for layering or separation of solid material.

SCOPE

The test is intended to determine whether a pesticide solution is suitable for

application after dilution with oil instead of water.

REAGENT

Hydrocarbon oil; RE 36.1, or as specified by the manufacturer of the pesticide

solution

APPARATUS

Beaker 250 ml
Burette 50 ml
Measuring cylinder 100 ml
Water bath maintained at 30 °C (Note 1)

PROCEDURE

Pour into the beaker a sufficient quantity of the sample to obtain 100 ml of final
solution at the dilution for use recommended by the supplier (Note 2). Add the
oil from a burette to make up the volume to 100 ml. The oil is added at the rate
of about 25 ml per minute while the solution is stirred with a glass rod at the rate
of three turns per second. Pour the resulting solution obtained into a clean, dry,
graduated measuring cylinder. Maintain for 1 h at 30 ± 1 °C (Note 1).
At the end of 1 h note whether (a) the solution is homogeneous, (b) there has
been any separation of solid matter, or (c) any separation into layers.

Note 1 Or the prescribed time and temperature.

Note 2 Use the highest and lowest dilutions recommended in the instructions
for use.

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MT 24 PHOSPHORUS(V) OXIDE

REAGENT
Phosphorus(V) oxide
Vermiculite exfoliated ; mesh size 2.4 to 1.68 mm or 1.68to 0.85 mm

APPARATUS
Screw cap bottle 1000 ml

PROCEDURE
Place a weighed amount of vermiculite in the bottle, add an equal quantity of
phosphorus(V) oxide quickly, and close the bottle. Shake the bottle and contents
(only half full) vigorously for 5 min. The powdered phosphorus(V) oxide is thus
incorporated completely within the pores of the exfoliated carrier. The finished
product is a dust-free, free-flowing, granular material.

Note 1 Based on the method described by G F Smith and H Diehl,

Talanta, 1962, 9, 84.

MT 25 SAND FOR GERMINATION TESTS

SPECIFICATION (Note 1)
Toxic substances. The sand shall not contain toxic substances which could
cause injury to seedlings during the germination test. Control tests should be
made periodically to determine whether a particular lot of sand has any effect
on seedling development.
Particle size. The sand shall be free from both fine and large particles and
particles shall pass through a sieve having holes of 0.8 mm diameter and shall
be retained on a sieve having holes of 0.05 mm diameter.
pH. The pH shall be within the range 6.0 to 7.5.
Specific conductance. The specific conductance shall be within the range 0.1 to
0.2 × 10-4 (MT 32).

STERILIZING
Pick out any seed remaining in the sand (Notes 2 and 3). Heat the sand in mild
steel pans about 60 x 70 x 15 cm deep. After the sand is dry, heat for a further
2 h at 150 °C. During heating turn the sand regularly, firstly, to aid drying and

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later to prevent overheating. Leave the sand to cool. Any seeds which were
overlooked will be charred and are removed by sieving.

WATER

Add tap water to the sand (the amount depending on the seed to be tested) in the
following quantities:

Seed Water
Cereals 8 of water to 96 of sand by weight
Vegetables 11 of water to 96 of sand by weight
Pulses 10 of water to 96 of sand by weight

Sprinkle additional water on when the seed is planted to bring the water levels
to 50% of the water holding capacity for cereals and vegetables and 60% for
pulses.

Note 1 Suitable sand (Garside grade 60) may be purchased from George
Garside (Sand) Ltd, 39 Hockliffe Street, Leighton Buzzard, England.
Note 2 Discard the sand at the end of the test to avoid accumulation of
poisons where seeds have been treated with pesticides.
Note 3 Use new sand for vegetable seeds but, for other kinds of seeds, the
sand can be used several times.

MT 26 JOHN INNES COMPOST

26.1 Seeding Compost - with fertilizer

INGREDIENTS

Sand. Clean and free from humus, silt, lime and organic matter.
Peat. Moss or sedge peat, particle size from 1.3 to 1.9 cm in diameter.
Loam. Sterilize by steaming, so that the temperature reaches 95 °C throughout
the mass; maintain at this temperature for 20 min. To achieve an even
distribution of steam, sieve the loam through a 1 cm sieve before treatment.
John Innes base fertilizer. Mix three fertilizers in the following proportions:
2 parts of hoof and horn meal (13% nitrogen)
2 parts of calcium superphosphate (nominally 18% P2O5)
1 part of potassium sulphate (48% K2O)

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PREPARATION

Mix together the following constituents:

2 parts of sand
3 parts of peat
9 parts of sterilized loam
Add to each bushel (8 gallons; 36 litres) of this mixture 113 g(0.25 lb) of the
John Innes base fertilizer and 22 g (0.75 oz) of powdered chalk or limestone.
Add water until the consistency of the compost is such that a ball can be formed
by squeezing in the palm of the hand, but when pressed between two fingers the
ball will break easily. Rub the compost through a sieve and put into the
containers without packing.

26.2 Seeding compost - without fertilizer

INTRODUCTION
When seedlings on standard test media exhibit symptoms indicating damage by
seed treatment (or blackening of tissues in broad beans) re-tests are carried out
in John Innes seeding compost without added fertilizer.

INGREDIENTS as for MT 26.1, except that the base fertilizer is not needed.

PREPARATION. As for MT 26.1, except that the base fertilizer and powdered
chalk are omitted.

MT 27 MATERIAL INSOLUBLE IN ACETONE

OUTLINE OF METHOD

The sample is refluxed with acetone, the solution is filtered, and the weight of
insoluble material is determined

APPARATUS
Conical flask 250 ml fitted with ground glass joint
Reflux condenser to fit flask
Sintered glass crucible porosity P40 (pore size 16-40 µm)
Flameproof oven at 110 °C
Water bath

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REAGENT

Acetone {(CH3)2CO} dried over anhydrous sodium sulphate; RE 34

PROCEDURE

Weigh about 10 g of sample (w g) into the conical flask, add acetone (150 ml)
and reflux for a period of 10 min. Filter the hot solution through the tared
crucible (x g) and wash well with more acetone (3 × 20 ml). Dry at 110 °C for
30 min, cool and weigh (z g).

100 ( z − x)
Content of material insoluble in acetone = % m/m
w

Note 1 The crucible porosity is only given as a guide; it may be necessary to

use a coarser or finer pore size according to the particle size of the
insoluble material.

MT 28 DIMEDONE DERIVATIVE

OUTLINE OF METHOD

The aldehyde is heated with dimedone, the condensation product filtered off,
and recrystallized from ethanol. The aldehyde is characterized by the melting
point of this derivative.

O O R O

R CH O + 2
CH3 CH3 + H2O
H3C O O CH3
O CH3 CH3

REAGENTS

Dimedone (5,5-dimethylcyclohexane-1,3-dione; RMM 140.2) solution; dissolve

dimedone (0.7 g) in ethanol (30 ml of 50% m/v)
Ethanol (CH3CH2OH) or Industrial Methylated Spirit

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APPARATUS

Weighing bottle
Measuring cylinder 50 ml
Beaker 100 ml
Water bath

PROCEDURE

Add the aldehyde (0.2 g; Note 1) to the dimedone solution (30 ml) warm on the
water bath to 50 °C and allow the solution to stand for 2 to 3 h. If the derivative
does not precipitate easily, stir vigorously to coagulate. Filter off the precipitate,
wash with ethanol and dry. Crystallize from ethanol and determine the melting
point by MT 2.

Dimedone derivative with Melting Point

°C
Acetaldehyde 140
Acrylaldehyde (acrolein) 192
Formaldehyde 189
Metaldehyde (Note 2) 140

Note 1 For formaldehyde, use 1 ml of a 40% solution or equivalent amounts

for other strengths.
Note 2 First warm with one drop of concentrated sulphuric acid to convert to
acetaldehyde.

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