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A technique for the double encapsulation of carbofuran in starch urea formaldehyde (Starch-UF) matrix has been developed. The solid particles of carbofuran were first microencapsulated with UF resin and these microcapsules were then dispersed in the Starch-UF matrix to obtain a granular formulation. The rate of release of carbofuran from these granules was found to be governed by its diffusion through the solid UF resin shell and was significantly slower than from the single encapsulated granular formulation prepared by dispersing uncoated carbofuran in Starch-UF matrix. The bioefficacy of these double encapsulated granules (Encecap-D 3G), was evaluated for persistence against rice pests in paddy and against subterranean pests in potato, in comparison with conventional formulations of carbofuran, phorate, quinalphos, aldicarb and cadusafos. The persistence of Encecap-D 3G was found to be better than that of the standard formulation in the cultivation of paddy under flooded conditions and in the cultivation of potato. The order of efficacy was found to be : White grubs - Encecap-D 3G > quinalphos > cadusafos > aldicarb > phorate > Furadan 3G ; Nematodes - cadusafos > Encecap-D 3G > quinalphos > aldicarb > phorate > 'Furadan' 3G.

14C-Methylene labelled phorate was added to nutrient solutions supplying the roots of young broad bean plants and after 24 h absorption, fresh nutrient was substituted. The radiolabel accumulated at the leaf margins was initially associated with solvent-soluble toxic metabolites. Radiolabel extracted from foliage which developed after the treatment was mainly in water-soluble form. The maximum concentration of toxic material occurred in the marginal areas of the leaves after 5 or 6 days and in the central portions after 2 days. The concentrations declined to half of their peak values in 4–6 days from leaf-margin tissue and in 2 days from the central tissues. Water-soluble label did not accumulate to any significant extent. Most was found in the marginal areas but concentrations built up slowly reaching a maximum after about 2 weeks, declining slowly thereafter.

Granular formulations of chlorfenvinphos, chlormephos, disulfoton, phorate and pirimiphos-ethyl were broadcast at 2 kg a.i./ha and incorporated to 100 mm into a sandy-loam soil either in May or in September 1971. The relative persistence of their residues, including insecticidally active oxidation products, after both application dates was disulfoton > chlorfenvinphos > phorate > pirimiphos-ethyl > chlormephos. When applied in September all the insecticides persisted for longer than when applied in May. Degradation was slower during the winter while the mean soil temperature at 100 mm depth remained below 6 to 7°C. Rising soil temperature in the following spring rapidly increased the rates of degradation of chlorfenvinphos, chlormephos and pirimiphos-ethyl residues but not of disulfoton- and phorate-derived residues, predominantly the parent sulphones, which had been leached deeper. Ten months after the September application, half the total residues derived from disulfoton and phorate were found below the initial incorporation depth, whereas the other insecticides showed relatively little downward movement. It was concluded that late summer/early autumn applications for carrot fly control would leave appreciable residues of some insecticides in the soil at the beginning of the next growing season which may contribute to the terminal residues in crops. These would be minimised if moderately persistent compounds were used or if doses of persistent ones were substantially reduced.

Granular formulations of chlorfenvinphos and phorate were applied to sandyloam soil at 2 kg a.i./ha either broadcast and incorporated to 2.5 cm, broadcast and incorporated at 10 cm or by the bow-wave method along the carrot rows. Depth of incorporation did not influence the rates of residue decline in the soil. Bow-wave applications produced the highest residues in root and foliage and also reduced the rate of oxidation of phorate. 30 weeks after sowing the carrots, all treatments gave the highest residue concentrations in the uppermost 6 cm of carrot root. The peel of carrots grown in the soil treated to a depth of 10 cm contained 88 % and 23 % of the total chlorfenvinphos and phorate residues respectively. Significant differences were found in the residue concentrations in five carrot cultivars treated with chlorfenvinphos and phorate by the bow-wave method at 1.5 kg a.i./ha. The concentrations were inversely correlated with root size so that amounts of insecticide (μg/carrot) were similar in all cultivars. Prolonged growth of cv. Norfolk Giant slightly extended the period of uptake of chlorfenvinphos, but the uptake of phorate was ultimately less than its rate of dissipation. Neither the method of application nor the selection of carrot cultivar extended the period of uptake very greatly but differences which were obtained in residue concentrations in the carrot may become significant in the event of regulatory control of residue levels.

The application of granules containing 10 % phorate at 1.12,2.24 or 4.48 kg a.i./ha in a narrow slit together with carrot seed significantly reduced seedling emergence in both a mineral and peat soil. When the granules were applied at 2.24 or 4.48 kg a.i./ha in a narrow slit 2.5 cm below the seed, seedling emergence was adversely affected only at the higher rate in the mineral soil. Phorate granules applied with the seed in the peat soil gave a significantly lower plant density than when applied below the seed, but subsequent carrot yields were unaffected because much larger roots were produced. All phorate treatments gave effective reduction of carrot fly larval damage to the roots. On the peat soil, there were significant increases in total phorate residues present in mature carrots with increasing rate of phorate granules placed with the seed. Placement of the granules 2.5 cm below the seed resulted in a 50% reduction in total residues of phorate in whole carrots compared with placing the granules with the seed. Residues resulting from 1.12 kg a.i./ha with the seed or 2.24 kg a.i./ha 2.5 cm below the seed were not significantly greater than residues in untreated carrots.

Following experimental and commercial applications to soil of a granular formulalation of phorate (O,O-diethyl S-ethylthiomethyl phosphorodithioate), residues in the soil and in lettuce were determined by gas-liquid chromatography. When applied by the bow-wave method as a continuous logarithmically-changing dose ranging from approximately 0.9 to 16.0 kg a.i. ha−1, the proportional rate of oxidation in soil of phorate sulphoxide to phorate sulphone was inversely related to dose. Ten weeks after application, total phorate residues in the soil had declined by about 35% at all dose levels. Residues in mature lettuce, from the 1-5 kg ha−1 dose-range, comprised the parent and oxygen analogue sulphoxides and sulphones; the relative proportions of the individual metabolites were independent of dose. Over this dose-range, total residue concentrations in the crop became proportionally slightly greater with increasing dose. When single doses of 1.1, 2.0 or 2.2 kg a.i. ha−1 were applied at drilling, the total residue concentrations in the lettuce declined from 5 mg kg−1 in seedlings from some treatments to

Factors likely to influence the uniformity of treatment and the stability of the insecticides incorporated into peat blocks were investigated. When an Adelphi horizontal mixer was used, 90% of the blocks contained the mean dose (±10%) after dry-mixing the diazinon granules for 3 min. Treatment was slightly less uniform using a concrete mixer or a spade. Between-block variability was greatest when diazinon was applied to the wet surfaces of prepared blocks; in this process, sprinkling granules by hand was less erratic than spraying a liquid formulation. When granular, wettable powder, or emulsifiable concentrate formulations of diazinon were incorporated using the Adelphi mixer, neither the between-block variability nor the subsequent stability of the insecticide were significantly influenced by the formulation used. Insecticide stability was studied by incorporating chlorfenvinphos, chlorpyrifos, diazinon and phorate at 10 mg a.i. per block in January, March, May and July. The relative order of persistence was chlorfenvinphosChlorpyrifos > phorate≫diazinon. There was little loss of insecticide ( < 10%) from the blocks treated with chlorfenvinphos or chlorpyrifos, and the stability of the insecticides was unaffected by seasonal temperature changes, but the rate of loss of diazinon increased markedly from January to July. The rate of oxidation of phorate to its sulphoxide and sulphone analogues increased gradually from January to May but was much slower than in the field after a bow-wave application. With all insecticides, there was no significant difference in loss rates at 25 and 10 mg a.i. per block. After incorporation into three moss peats and two proprietary blocking composts, there was no consistent difference in the rates of loss of either diazinon or of total phorate residues, although the rates of oxidation of phorate and its sulphoxide were not similar in all the peats and composts. It was concluded that, despite the substantial water content and high insecticide concentrations, the principal factor determining insecticide behaviour in the blocks was the adsorptive capacity of the peat.

Carbohydrate metabolism was studied in the hepatopancreas, mantle, intestine and foot of the snail Lymnaea acuminata, exposed to 40% and 80% of the LC50 dose of phorate (12 and 24 mg litre−1, respectively) for 24 and 48 h. Following treatment with the pesticide, the rate of oxygen consumption and the glycogen contents were reduced, while the levels of lactic acid and reducing sugars were enhanced. Withdrawal of the pesticide for 7 days after exposure of the snails to 12 mg of phorate litre−1 for 48 h did not reverse these changes.

An aqueous solution of bromine was used to oxidise 14C-labelled phorate to its metabolites. A substantial amount of [14C]phorate sulphone (O,O-diethyl S-ethylsulphonyl[14C]methyl phosphorodithioate) with minute quantities of [14C]phorate sulphoxide (O,O-diethyl S-ethylsulphinyl[14C]methyl phosphorodithioate) and [14C]phoratoxon sulphoxide (O,O-diethyl S-ethylsulphinyl[14C]methyl phosphorothioate) were recovered using this method. Various concentrations of [14C]phorate and these toxic metabolites were individually incorporated in an artificial diet and fed to Aphis fabae Scop. Mortality was recorded after 48 h. The toxic fractions of the compounds were extracted from the diet and their radioactivity was measured to determine the dose unit. The aphids feeding on diet containing high concentrations of [14C]phorate sulphoxide and [14C]phoratoxon sulphoxide were seen wandering restlessly, which suggested that the acceptability of the diet had been changed by the presence of these metabolites. Phorate appeared to be the most toxic to the aphids, followed by phorate sulphone, phorate sulphoxide and phoratoxon sulphoxide in that order; the reasons for this are discussed.

Aphis fabae colonies were established on both leaflets of the second leaf of young broad bean plants. Doses of phorate sublethal to the aphids were applied to the roots or to the third leaf. The aphids, their honeydew and the foliage on which they were feeding were analysed and the quantities of toxic and non-toxic radiolabel determined at intervals. Toxic metabolites were found in the aphids and the leaves but whereas the aphid colonies in all experiments contained approximately similar amounts of the toxic metabolites, the residues in the leaves on which they were feeding differed considerably. The leaves contained more than 100 times as much of these metabolites following the root treatment than after the foliar treatment. These results are discussed in relation to the aphids' feeding site and the probable transport routes of the toxicants.

Aphid colonies were established on one second-node leaflet of young broad bean plants and sublethal treatments of 14C-labelled phorate were applied to the adjacent leaflets. After 3 days, the amounts of toxic and non-toxic 14C-labelled compounds in the aphids, their honeydew and the untreated foliage were determined. There were no significant differences between the amounts in leaves at the same level on the plant when infested and aphid-free plants were compared, but the aphids and their honey-dew contained two and 23 times as much of the toxic and non-toxic 14C-compounds, respectively, found in the host leaflets. Following translocation to aphids on leaves above or below treated leaflets, the aphid colonies again contained more labelled compounds than the host-plant leaves. The movement of non-toxic compounds into the roots was reduced when the aphid colonies were situated on foliage between the site of treatment and the roots. More of the toxic and the non-toxic fractions were translocated downwards from the third to the second leaf than in the reverse direction.

Phorate residues in peat blocks and lettuce were determined following incorporation of the insecticide into different block and ‘Speedling’ cell sizes. Between-block variability was influenced little by block size. Phorate oxidation was most extensive in the largest blocks containing the smallest dose. Total residue concentrations in the lettuce declined from the time of planting to harvest, although accumulation of insecticide continued and was related more to dose than to block or cell size. Residues in the lettuce at harvest exceeded the proposed maximum limit of 0.2 mg kg−1 in some treatments. Residues at planting comprised mainly the parent sulphoxide and sulphone, but by harvest, the oxygen analogue sulphoxide and sulphone predominated. Lettuce weight was not influenced by dose but was related directly to block size. Carbofuran and chlorfenvinphos residues were determined in calabrese sown into two sizes of blocks. At planting time, carbofuran residue concentrations were 100 times greater than those of chlorfenvinphos but residues of both insecticides in the mature heads were < 0.01 mg kg−1. Seedling weights in both sowings declined with increasing concentrations of the insecticides. It was concluded that manipulations of block size and the dose of insecticide need to be evaluated for individual insecticide/crop combinations to exploit the technique fully.

Carbaryl, chlorfenvinphos, diazinon, disulfoton, parathion, phorate, fenitrothion, thionazin and trichlorphon were tested for their effectiveness in killing wireworms by broadcast treatments. Each insecticide was tested once or more in two field trials cropped with wheat and two cropped with potatoes. Phorate and parathion were very lethal to wireworms at 4 Ib active ingredient per acre (4?48 kg/ha). Thionazin and diazinon were intermediate in effectiveness and the other insecticides ineffective.

Analytical methods are described for the determination of residues of chlorfenvinphos, diazinon, fonofos and phorate in soils and carrots. The insecticides, applied in June 1969 at 2 kg (a.i.)/ha, persisted longer in peaty loam than in sandy loam. After 7 months, the sandy loam contained 1% of the applied diazinon and 20–30% of the applied chlorfenvinphos, fonofos and phorate, the latter as its sulphone; the corresponding figures for the peaty loam were 10, 40–50, 40–50 and 30–40% respectively. None of the residues showed any substantial change from October to January. Although high initial concentrations (up to 50 ppm) of the residues in carrots were diluted by plant growth, it is shown that concentrations >1 ppm could be present in marketable crops 12–14 weeks after application at recommended rates. Carrots harvested 26 weeks after sowing contained

Factors influencing the performance of various granular formulations of disulfoton and phorate after foliar application to field beans were investigated by bioassay in controlled environment rooms. Frequent rainfall and high temperature increased activity considerably but humidity had little effect. With disulfoton formulation on pumice rather than fuller's earth, and toxicant concentrations of 7.5% rather than 10% increased toxicity, but effects of formulation were small with phorate. The influence of rainfall and formulation were confirmed in a field experiment. There was evidence for an initial fumigant effect, particularly for phorate, in both laboratory and field experiments. The detailed effects of the various factors at different intervals after applying the granules are discussed in relation to the physical properties of the insecticides and granular carriers. It is suggested that the possibilities of controlling performance by influencing release rates from granules are limited for chemicals such as phorate and disulfoton which are appreciably adsorbed by soil.

Hessian fly was controlled to a maximum of 95% with organophosphate insecticides, in terms of the number of puparia and percentage tiller infestation at harvest. Granules: phorate at 1.68 kg/ha (1 1/2 lb/acre) as 10% granules in the seed furrow was most effective on durum wheat in 1967–8, with 69–92%, control, of tillers infested. 1.12 kg/ha gave 74–89% control, 0.56 kg/ha in the seed furrow 35–54%. Seed furrow treatment was more effective than band or broadcast treatment over young plants, although granules broadcast over young barley at 1.68 kg/ha of phorate gave 74% control in 1967–8. Fonofos (Dyfonate) granules at 1.55 kg fonofos/ha were most effective on barley in 1968–9, with 66% control. After fonofos and phorate, disulfoton at 1.68 kg disulfoton/ha was next in effect, with up to 86%, control in 1967-8 and 24% in 1968–9, but variable and not much more effective than at 0.56 kg/ha. Other insecticides were less effective. Seed dressings: disulfoton was the most effective, giving 79% control in 1967-8 on wheat and 77% on barley at a high rate of application that was phytotoxic in 1968–9. Diazinon, bromophos and ethion gave 15–38%, control and chlorfenvinphos and dimethoate less. Carbaryl dust at 1.12 kg carbaryl/ha gave 32% control. Yields were poor, but grain yield was increased by up to 33% in wheat in 1967-8, averaging about 15%. Barley yield was increased by 7% in 1967–8, and from 9–23% in 1968-9 by fonofos and phorate granules. Insect control reduced the number of tillers, increased the number of heads and increased the grain weight per head. In observation plots, chlormequat (CCC) spray alone at the 5-leaf stage reduced infestation of wheat by between 22% and 43%, but CCC with fertilizer, and fertilizer alone had no conclusive effect. High fly populations are partly due to leaving crop residues in the field at harvest. When these can be ploughed in, infestation should decrease. The use of insecticides may not be economic unless more consistent increases in yield can be obtained.

Since mint oil is used as a flavouring agent for foods and cosmetics, pesticide residues in the oil are undesirable. The residual behaviour of two pesticides, phorate and methomyl, was studied as replacements for chlorinated hydrocarbon pesticides which leave residues in the oil. Phorate applications of 1.1 kg/ha resulted in oil residues of 0.24 mg/kg total phorate in Oregon samples and 1.69 mg/kg in Washington samples. Less than 1% of the residues in the hay distilled with the oil. Mint oil undergoes a 100- to 1000-fold dilution in commercial use with a corresponding reduction of residues in the final product. No residues of methomyl were found in the oil, even with hay residues as high as 5.34 mg/kg. Residues in hay decreased to half of initial levels in 2 to 4 days, independently of use conditions. It was concluded that the proposed use of phorate or methomyl for control of mint pests does not present a residue hazard. Details of the analytical methods used are also presented.

Effects of granule distribution relative to carrot rows are discussed and further results described. Placing insecticides 5 to 10 cm deep 7.5 cm away from the centre line of the carrot row usually, but not always, improved their performance compared with bow-wave applications. Both sides of the row need to be protected. The efficiency of chlorfenvinphos in a sandy loam, and phorate in a peaty-loam, decreased with increasing distance from the row but they were slightly effective even 19 cm away. The optimum depth for side-placing granules at sowing time varied from 5 to 10 cm, and combining side-placement with a bow-wave application did not greatly enhance efficiency. The most effective combination on a peaty-loam was a bow-wave application of 3 kg phorate/ha at sowing time followed 6 to 9 weeks later by a similar amount side-placed 7.5 cm deep 7.5 cm from the row centre. Comparison of the performance of phorate broadcast, applied by the bow-wave method or deep side-placed indicated that efficiency was improved by restricting the granule distribution but that higher concentrations of granules were then needed in the treated zones to be equitoxic with more uniformly broadcast granules. Uptake by the carrot root system is an important factor in the action of insecticides against carrot fly larvae.

Thin-layer chromatography was used to assess semi-quantitively the persistence of six organophosphorus insecticides in hen-house litter. Malathion disappeared within 4 h of application. Carbofenthion was the most persistent. Four weeks after treatment the proportions of the applied doses extracted from the litter were: carbofenthion 46%, phorate 21%, diazinon 13%, coumaphos 7% and fenitrothion 3%.