The Detection Method Of Phosphate Flame Retardants In Textiles

Flame retardants are used to reduce the flammability of the polymer materials,improve their self-extinguishing and avoid the flame from spreading. In recent years,phosphate flame retardants, which is the most important class of flame retardants, arewidely used in textile. Meanwhile, among those retardants, phosphate retardants willbe more harmful to humans. Flame retardants could block the contact of the synthesismaterials with oxygen by forming a nonvolatile protective film and carbide film. Theeffect of flame retardant does not mean that after the precursor modification and flameretardant finishing process, the material will not burn, but that the anti-flammable getimproved after the these treatments, thus slow down the spread speed of the flam, thenself-extinguishing. By means of chemical bonding, Van der Waals force, hydrogenbonding, adsorption deposition, physical bonding et.al, the flame retardant finishingprocess attach the flame retardant to the polymer chain, to obtain flame retardancy.There are lots of methods in retardant finishing process, compare with other methods,the advantages of the retardant enzyme treatment are mild reaction conditions, highcatalytic efficiency, strong specificity and little environmental pollution, thus, reducethe harm to human body. But long-time contact with the phosphate flame retardantswill cause thyroid disease, liver damage, immune system function decline, motor nervedamage and highly carcinogenic. The daily used clothing, bedclothes and other textileshave the possibilities to potential risks, especially the school uniforms, infant clothesand the clothing contact to the body directly. The United States, Germany, Britain,Japan and other countries have already formulate some appropriate standards andregulations, to regulate and restrict the use category and dosage of flame retardants, forinstance, the " American Society for Testing and Materials Standards","Food and DailyConsumer Goods Act,""Hazardous Substances Safety Regulations","HouseholdHazardous Substances Control Act." This paper established a better phosphate flameretardant HPLC-MS/MS method to detect the content of Tris-(aziridinyl)- phosphineoxide(TEPA), Tris-(2-chlorisopropyl)-phosphate(TCPP),Tris-(2,3-dibromo-propyl)-phosphate(TDBPP), Tris-(2-chloroethyl)-phosphate(TCEP) in textiles.The pre-treatment methods of phosphate flame retardants of textiles are following:Samples are extracted by50mL methanol twice, ultrasound extraction twice for20minand30min, respectively. Rotary evaporated in40℃water bath to near dryness,reconstituted with1mL acetonitrile, analysis on a HPLC-MS/MS instrument. HPLC-MS/MS instrument conditions are optimized as followed: electrospray ion source,American Agilen C183.5μm,150×2.1mm column, pure acetonitrile and5mmolammonium acetate serve as the mobile phase, positive ion scan, multi-reactionmonitoring (MRM) mode, quantitative test of external standard method, then establishfour kinds of phosphate flame retardant in textiles detection and analysis methods. Thepeak time of the four kinds of phosphate flame retardants are: TEPA1.8min, TCPP11.46min, TDBPP13.38min, TCEP10.05min, respectively. The recovery rate of thefour kinds phosphate flame retardants are up to80%～100%. And the standard curveshows a good linear relationship, the correlation coefficient r2values are larger than0.9998. The detection limit is0.1μg/mL.This pre-treatment method is simple, fast to operate and easy to repeat. Theadvantage of the HPLC-MS/MS is less affected by the external environment, andexhibit higher sensitivity, repeatability and efficiency. This detection method could laida theoretical and experimental basis for the further detect of the phosphate flameretardants in textiles.