Phthalation method

P.O.38 is stable to styrene monomer, but not entirely fast to acetone, which occasionally leads to bleeding if the pigment is processed according to the diallyl-phthalate method (Sec. 1.8.1.2). This is also true if the pigment is treated with a melamine resin solution. 

NIOSH. 1985a. Dibutyl phthalate and di(2-ethylhexyl) phthalate - method 5020. In NIOSH manual of analytical methods. 3rd ed. Cincinnati, OH U.S. Department of Health and Human Services, National Institute for Occupational Safety and Health. 

U.S. Institute for Occupational Safety and Health (NIOSH). Dibutyl Phthalate and Di(2-Ethylhexyl) Phthalate Method 5020.2, In Dibutyl Phthalate and Di(2-Ethylhexyl) Phthalate Method 5020.2, NIOSH manual of analytical methods (NMAM), 4th ed., CassineUi, M. and O Connor, P. F., Eds., 1994. 

Molecular weight p-Toluene sulfonic acid-catalysed acetylation method. Average hydroxyl value (mg KOH/g) Phthalation method. Average hydroxyl value (mg KOH/g) Reaction with phenyl isocyanate. Average hydroxyl value (mg KOH/g)... 

Molecular weight p-Toluene sulfonic acid catalysed acetylation method Phthalation method [2] Reaction with phenyl isocyanate... 

Successful results have been obtained (Renfrew and Chaney, 1946) with ethyl formate methyl, ethyl, n-propyl, iso-propyl, n-butyl, iso-butyl, sec.-butyl and iso-amyl acetat ethyleneglycol diacetate ethyl monochloro- and trichloro-acetates methyl, n-propyl, n-octyl and n-dodecyl propionates ethyl butyrate n-butyl and n-amyl valerates ethyl laurate ethyl lactate ethyl acetoacetate diethyl carbonate dimethyl and diethyl oxalates diethyl malonate diethyl adipate di-n-butyl tartrate ethyl phenylacetate methyl and ethyl benzoates methyl and ethyl salicylates diethyl and di-n-butyl phthalates. The method fails for vinyl acetate, ieri.-butyl acetate, n-octadecyl propionate, ethyl and >i-butyl stearate, phenyl, benzyl- and guaicol-acetate, methyl and ethyl cinnamate, diethyl sulphate and ethyl p-aminobenzoate. 

Method B. Place 125 g. (106 -5 ml.) of diethyl phthalate and 25 g. of molecular sodium (sodium sand see Section 11,50,6) in a 500 ml. round-bottomed flask fitted with a reflux condenser and dropping funnel. Heat the flask on a steam bath and add a mixture of 122 5 g. (136 ml.) of dry ethyl acetate and 2 5 ml. of absolute ethanol over a period of 90 minutes. Continue the heating for 6 hours, cool and add 50 ml. of ether. Filter the sodium salt (VI) on a sintered glass funnel and wash it with the minimum volume of ether. Dissolve the sodium salt (96 g.) in 1400 ml. of hot water in a 3-htre beaker, cool the solution to 70°, stir vigorously and add 100 ml. of sulphuric acid (3 parts of concentrated acid to 1 part of... 

In this experiment the overall variance for the analysis of potassium hydrogen phthalate (KHP) in a mixture of KHP and sucrose is partitioned into that due to sampling and that due to the analytical method (an acid-base titration). By having individuals analyze samples with different % w/w KHP, the relationship between sampling error and concentration of analyte can be explored. 

In the calendering method, a PVC compound which contains plasticizers (qv) (60—120 phr), pigments (qv) (0—10 phr), fillers (qv) (20—60 phr), stabilizers (10—30 phr), and other additives, is kneaded with calender roUs at 150—200°C, followed by extmsion between clearance-adjusted roUs for bonding onto the substrate. This method is employed for products with thick PVC layers, ie, of 0.05—0.75 mm thickness. The main plasticizer used is di-2-ethylhexyl phthalate (DOP). For filler to reduce cost, calcium carbonate is mainly used. A woven or knit fabric made of cotton, rayon, nylon, polyester, and their blend fiber is used as substrate. For foamed vinyl-coated fabrics, the bonded materials are heated in an oven to decompose the foam-blowing... 

Fig. 1. Relative efficiency of plasticizers where H represents Cg phthalate +, C q phthalate A, phthalate and , phthalate phr = parts per hundred mbber. Values for the trimeUitates fall in the shaded area. BSS 35 is equivalent to a Shore A hardness of 80, test method BS2782.

Environmental Effects of Plasticizers. Measurement of the effect of phthalates on environmental species is difficult because standard test methods are not designed to deal with poorly water-soluble substances. Eor this reason a number of early studies are flawed and their results should be disregarded in favor of more recent investigations where these difficulties have been overcome. 

The hydroxyl number can be deterrnined in a number of ways such as acetylation, phthalation, reaction with phenyl isocyanate, and ir and nmr methods. An imidazole-catalyzed phthalation has been used to measure the hydroxyl number for a number of commercial polyether polyols and compared (favorably) to ASTM D2849 (uncatalyzed phthalation) (99). The uncatalyzed method requires two hours at 98°C compared to 15 minutes at the same temperature. 

Phenethyl alcohol may be identified as the phenethyl -nitrobenzoate [57455-00-2] (mp 106—108°C), as phenethyl -nitrobenzyl phthalate [65997-34-4] (mp 84.3°C), and also by its formation of styrene on treatment with alkaU. Use of these derivatives has, however, been superseded by physical methods. Infrared (75,76), mass spectroscopy (77), and nmr spectra (78) are useful for identification. 

Mixed cellulose esters containing the dicarboxylate moiety, eg, cellulose acetate phthalate, have commercially useful properties such as alkaline solubihty and excellent film-forming characteristics. These esters can be prepared by the reaction of hydrolyzed cellulose acetate with a dicarboxyhc anhydride in a pyridine or, preferably, an acetic acid solvent with sodium acetate catalyst. Cellulose acetate phthalate [9004-38-0] for pharmaceutical and photographic uses is produced commercially via the acetic acid—sodium acetate method. 

Mixed esters containing the dicarboxylate moiety, eg, cellulose acetate phthalate, are usually prepared from the partially hydroly2ed lower aUphatic acid ester of cellulose in acetic acid solvent by using the corresponding dicarboxyhc acid anhydride and a basic catalyst such as sodium acetate (41,42). Cellulose acetate succinate and cellulose acetate butyrate succinate are manufactured by similar methods as described in reference 43. 

Vehicles are selected by two methods. In one a concentrate is designed directiy for a resin system, the resin itself, or a compatible resin. Thus when the concentrate is made there is a minimal effect on the properties of the final color. In PVC, often a plasticizer such as dioctyl phthalate (DOP) is used. In the other method, concentrates are made with a commercial universal concentrate vehicle. Concentrate manufacturers and some resin manufacturers have developed vehicles that can incorporate many types of colorants and can be used across many classes of polymers without adversely affecting final product performance. 

The other analytical methods necessary to control the typical specification given in Table 5 are, for the most part, common quality-control procedures. When a chemical analysis for purity is desired, acetylation or phthalation procedures are commonly employed. In these cases, the alcohol reacts with a measured volume of either acetic or phthalic anhydride in pyridine solution. The loss in titratable acidity in the anhydride solution is a direct measure of the hydroxyl groups reacting in the sample. These procedures are generally free from interference by other functional groups, but both are affected adversely by the presence of excessive water, as this depletes the anhydride reagent strength to a level below that necessary to ensure complete reaction with the alcohol. Both procedures can be adapted to a semimicro- or even microscale deterrnination. 

The method of detecting dimethylterephthalate (DMTP), dibuthyl-phthalate (DBP) and diocthylphthalate (DOP) in aqueous extract is based on their extraction with an organic solvent (hexane) and subsequent concentration using gas-liquid chromatography and an electron-absorbing detector. The detection limit is 0.05 mg/dirf for DMTP and DBP, and 0,01 mg/dm for DOP. 

The resolution of sec.-octyl alcohol was first described by Pickard and Kenyon. The method employed by these authors differed from the foregoing in the following respects. The brucine salt of sec.-octyl hydrogen phthalate was crystallized several times from acetone until it reached optical purity and was then decom-... 

Dioctyl phthalate Lab method using Tenax sorbent tubes, solvent desorption and gas chromatography 32... 

Two different methods have been used for the incorporation of the activating ogliomer (or monomer) in the seed particles. The first method involves the application of a small organic chemical, such as chloroundecane or dibutyl phthalate, which is incorporated into the particles in the first swelling step. In the second method, an ogliomer compound is formed by polymerization of monomers that are absorbed inside the seed particles. 

A better combination of fiber and polymer is achieved by an impregnation of [44] the reinforcing fabrics with polymer matrixes compatible with the polymer. Polymer solutions [40,45] or dispersions [46] of ]ow viscosity are used for this purpose. For a number of interesting polymers, the lack of solvents limits the use of the method of impregnation [44]. When cellulose fibers are impregnated with a bytyl benzyl phthalate plasticized polyvinylchloride (PVC) dispersion, excellent partitions can be achieved in polystyrene (PS). This significantly lowers the viscosity of the compound and the plasticator and results in cosolvent action for both PS and PVC [46]. 

The thin-layer technique (CA 60, 6691) utilizes aliquots of proplnt ether extract (I) and the ether soln (II) of a known mixt. II consists of nitrates of glycerol and glycol, di-Bu or di-Et phthalates, Et or Me centralites, DNT, and diphenylamine. The chromatoplates are made of 85 15 silica gel and plaster of Paris. These plates, containing spots of I and 11, are developed with 1 1 C6H6-petroleum ether, then sprayed with specific detectors by color. The method is much quicker and easier than chemical analysis and simpler than infrared spectroscopy and column chromatography... 

Laboratory method using porous polymer adsorbent tubes, thermal desorption and gas chromatt raphy MDHS 32 Dioctyl phthalates in air Laboratory method using Tenax adsorbent tubes, solvent desorption and gas chromatography MDHS 33 Adsorbent tu standards Preparation by the syringe loading technique MDHS 34 Arsine in air Colorimetric field method using silver diethyl-dithiocarbamate in the presence of excess silver nitrate... 

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