An iodometric method was developed for the determination of P(III) in cotton fabrics finished with Thpc/amide flame retardants. The method is applicable to a wide range of Thpc/amide resins, including those of urea, melamine, the cyclic ureas, and the carbamates, but not those of iodine-sensitive compounds such as thiourea, dihydroxyethyleneurea, or the triazones. The validity of the method was corroborated by experiments with the phosphorus-free resins and their precursors. The phosphorus in the Thpc/amide resins was found to be predominantly trivalent, surviving both the heat cure and the soap-soda boil largely intact.
CokeE. C.CalvoJ. M.HuelsenW., The Reactions of Iodine and Iodates with Thiourea and Thiouracil, Bol. Soc. Biol., Santiago, Chile2, 330–336 (1945); Chem. Abstr. 41, 2003 (1947).
3.
DaigleD. J.ReevesW. A.BeninateJ. V., The Oxidation State of Phosphorus in Flame-Retardant Polymers based upon THPC, J. Fire Flam. 1, 178–182 (1970).
4.
DaigleD. J.ReevesW. A.DonaldsonD. J., The Reaction of THPOH with Secondary Amines, Textile Res. J. 40, 580–581 (1970).
5.
FrankA. W.DrakeG. L.Jr., The Iodometric Determination of P(III) in Flame Retardants for Cotton. Part I: Development of the Method, Textile Res. J. 43, 633–38 (1973).
6.
FrankA. W.VailS. L., The Use of Trimethylamine in Flame-Retardant Finishes based on THPC and Various Amides, (in preparation).
7.
FrankA. W.VailS. L., The Iodometric Determination of P(III) in Flame Retardants for Cotton. Part III: Application of the Method to THPOH/Ammonia Resins, Textile Res. J., 46793–797 (1976).
8.
GonzalesE. J.BeneritoR. R.BerniR. J.ZacharisH. M., Kinetics of the Reactions of Ethyleneurea Derivatives with Cotton Cellulose. Part II: The Cellulose-Dimethyloldihydroxyethyleneurea Reaction, Textile Res. J. 36, 571–578 (1966).
9.
GuthrieJ. D.DrakeG. L.Jr.ReevesW., Application of the THPC Flame-Retardant Process to Cotton Fabrics, Amer. Dyest. Rep. 44, 328–332 (1955).
10.
JungH. Z.BeneritoR. R.GonzalesE. J.BerniR. J., Influence of Structure of Cyclic Urea Derivatives on their Reactivities with Cotton, J. Appl. Polym. Sci. 13, 1949–1963 (1969).
11.
KasemM. A.RichardsH. R.WalkerC. C., Preparation and Characterization of Phosphorus-Nitrogen Polymers for Flameproofing Cellulose. I. Polymers of THPC and Amines, J. Appl. Polym. Sci. 15, 2237–2243 (1971).
12.
KolthoffI. M.BelcherR., “Volumetric Analysis,”Vol. 3, Interscience Publ., New York, 1957; (a) pp. 199–235, (b) p. 293, (c) p. 403.
13.
KosolapoffG. M., “Organophosphorus Compounds,”John Wiley and Sons, Inc., New York, 1950, p. 98.
14.
LouisG. L.FioriL. A., Utilization of Medium Staple Discount Cotton in Printcloth, U. S. Dept. Agr., ARS 72–95, 14–21 (1972).
15.
MazzenoL. W.Jr.TraskB. J.YeadonD. A.DannaG. F., Oxidation of THPOH/NH Flame Retardant Cotton Fabrics to Increase Resistance to Weatherometer Exposure and Outdoor Line Drying, J. Coated Fibrous Mater. 2, 178–82 (1973).
16.
MillerW. H.RoblinR. O.Jr.AstwoodE. B., Studies in Chemotherapy. XI. Oxidation of 2-Thiouracil and Related Compounds by Iodine, J. Amer. Chem. Soc. 67, 2201–2204 (1945).
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NelsonM. L.RousselleM.-A.CanjemiS. J.TrouardP., The Iodine Sorption Test. Factors Affecting Reproducibility and a Semimicro Adaptation, Textile Res. J. 40, 872–880 (1970), and references therein.
18.
NuessleA. C.BernardJ. J., Some Aspects of Chlorine Retention by Resin-treated Fabrics, Amer. Dyest. Rep. 39, 396–403 (1950).
19.
PetersenH., Recent Developments in the Chemistry of Crosslinking Agents, Textile Res. J. 40, 335–344 (1970).
20.
ReevesW. A.PerkinsR. M., Chemistry of THPC in Flame Retardants for Cotton, Colourage1971, 1–7 (1971).
21.
SkramovskyS., Determination of Thiourea by Titration, Cas. Lek. Cesk. 21, 1–4 (1941): Chem. Abstr. 38, 2288 (1944).
22.
SmithA. R., in “Chemical Aftertreatment of Textiles,”MarkH.WoodingN. S.AtlasS. M., Eds., Wiley-Interscience, New York, 1971, pp. 553–581.
23.
SoignetD. M.BoudreauxG. J.BerniR. J.GonzalesE. J., Nuclear Magnetic Resonance Studies of Substituted Cyclic Ureas, Appl. Spectrosc. 24, 272–276 (1970).
