Unsulfonated residue

Deciduous fruit trees are much less susceptible to oil injury in the dormant stage than when in foliage. In practice today, oils having less than about 92% unsulfonated residue are considered unsafe for general use as verdant or summer oils. Less highly refined oil has been used for dormant applications. Within recent years, however, there has... 

Viscoeity (Saybolt, at 100 F.) Viscosity index (kinematic) Gravity (API dem ees) Unsulfonated residue (ASTM) Pour point Homogeneity... 

Viscosity, kinematic, ASTM Designation D 445-39T. Conversion to Saybolt Universal viscosity, ASTM Designation D 446-39. Kinematic viscosity index, ASTM Designation D 567-40T. APIgravity, ASTM Designation D 287-39. Pour point, ASTM Designation D 97-39. Unsulfonated residue, ASTM Designation D 483-40. 

Smith (24) conducted intensive studies of the factors involved in the use of oil sprays to control California red scale and other pests of citrus in southern California. He found that insecticidal efficiency and deleterious effect on the trees were closely related to the so-called weight of the spray oil, as indicated by the distillation range, and that this provided a better basis for classification of spray oils than viscosity. The relationship of the unsulfonated residue of petroleum oils to tree injury had been clearly established previ-... 

Table III. Phytotoxidty and Unsulfonated Residue Exhibited by Isoparaffinie Petroleum Fraction after Storage under Different Light Conditions...

Highly refined isoparaffinic fractions have unsulfonated residues approximating 100%. The per cent unsulfonated residue does not change significantly when these fractions are exposed to light, although the oils become increasingly phytotoxic. 

Am. Soc. Testing Materials, Standard Method of Test for Unsulfonated Residue of Plant Spray... 

Technical DDT solubility at 32 F., % Mixed aniline cloud pt., F. Unsulfonated residue, %... 

The temperature seldom rises above 35°C., and it is necessary to use pure 100 per cent sulfuric acid or part of the naphthalene is not attacked. This is frequently the case in any event, so the mixture is warmed on a water bath to 60° with continuous stirring until all of the naphthalene has disappeared. It is difficult, without considerable practice, to effect smooth sulfonation on a small scale, although no undue difficulties are encountered in large scale sulfonations. To test for the presence of residual naphthalene in the reaction mixture, a small sample is diluted with water. Any unsulfonated naphthalene separates immediately. 

Two drawbacks of petroleum sulfonates are that they are highly colored and always contain rather large amounts of residual (unsulfonated) oil [70]. 

Unsulfonated linear alkylbenzene and linear alkylbenzene sulfones are the main components of unsulfated matter in linear alkylbenzenesulfonate, an anionic surfactant. These residual products can be quantified by high-temperature capillary GC and its application to alkylbenzenesulfonate improves its synthesis process (Molever, 2005). 

A sample of 50-100 mL is deposited on a 3-mL silica SPE column (J. T. Baker) conditioned in CHCI3. The unsulfonated oil is removed by washing the column four times with 0.5-mL aliquots of CHCI3. The sulfonate is then recovered with four 0.5-mL methanol washes. The methanol solution is evaporated to dryness to expel CHCI3, and the residue is redissolved in water or methanol. 

The EtOH/H20 mixture from the monosulfonate determination (Section 2.c), which has been extracted free of unsulfonated and monosulfonated material, is freed of excess HCl by successive evaporations and additions of H2O. The residue is dissolved in 50 mL H2O and passed through a cation exchange column (in the H form). The column is rinsed with an additional 50 mL H2O, and the eluate evaporated to dryness. The evaporation is repeated three times, with 15 mL H2O added each time, to ensure the removal of HCl. The residue is dissolved in H2O and titrated to the phenolphthalein end point with standard NaOH solution. This solution is evaporated to dryness and weighed. This titration and weighing measures the sum of Na2S04 and of disulfonated paraffin. The values are cor-... 

An ethanol/water solution of the sample is extracted with petroleum ether at pH 3 and the residue weighed. This fraction corresponds to the unsulfonated fatty acid and fatty acid ester. The extract is titrated with alkali to determine the fatty acid content, and the ester is determined by difference (120). 

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