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Portugalska 2005 A

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Fashion, apparel, textile, merchandising, garments

Fashion, apparel, textile, merchandising, garments

Published in: Business, Lifestyle

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    • 1. DETERMINATION OF FREE FORMALDEHYDE ON TEXTILE SUBSTRATE BY HPLC
      • Bojana VON C INA
      • U niversity of Maribor, Textile Department
      • Smetanova 17, 2000 Maribor, Slovenia
    • 2.
      • Formaldehyde is built in the atmosphere thought photochemical processes of hydrocarbons
      • It is produced during the uncompleted combustion of wood, oil, gas, tobacco
      • Source of formaldehyde :
      • - A utomobile s and airplanes 70-80%
      • - H eating and incineration 13-15%
      • - Formaldehyde in chem . prod . 1%
    • 3.
      • Formaldehyde is found in human body as a building blocks for amino acids and proteins
      • Blood 2-3 mg/kg
      • Apple 17-22 mg/kg
      • Tomatoes 6-7 mg/kg
      • Wood 4-18 mg/kg
      • Formaldehyde is often used as a building block for a number of important chemical products, intermediates and consumer goods : - urea-formaldehyde resins ( 25% ),
      • - phenol- formaldehyde resins (20%),
      • - plastics (15%),
      • - i ntermediates (22%).
    • 4.
      • Toxicity Data
      • Formaldehyde is readily absorbed through skin and is toxic by
      • inhalation
      • It is considered t oxic, c arcinogen, m utagen, c orrosive
      • Health Effects :
      • Inhalation: formaldehide is extremely destructive to tissue of the mucous membranes and that of the upper respiratory tract. Inhalation may be fatal as a result of spasm and inflammation .
      • Eyes/Skin: extremely destructive to the tissue of the eyes and skin. Can cause allergic skin reactions
      • Ingestion: Can cause gastrointestinal disturbances. May alter genetic material. This is considered a carcinogen.
      • Target Organs: eyes, kidneys, liver, heart, potential cancer agent, testis, ovaries   
    • 5. The most effective crosslinking reagents for durable press finishing of cellulose fibers are formaldehyde adducts of urea which release formaldehyde during the production and wearing of in such way treated clothes Formaldehyde durable press finishers are applied to the textile substrate mainly in the form of N-methylol and N-alkoxymethyl compounds
    • 6. Release of formaldehyde from the textile substrate can be measured by:
        • STANDARD TEST METHODS
      • Japan Law 112 (EN ISO 14184-1)
      • AATCC-112
      • The formaldehyde content below 20 mg/kg can not be shown to be caused by the formaldehyde which was released by the crosslinking reagent .
      • ALTERNATIVE TEST METHODS
      • edana recommended test method using HPLC
      • HPLC
    • 7. EN ISO 14184-1 standard test method Standard solutions of formaldehyde with concentration levels of 0.3, 0.6, 0.9, 3.0, 6.0, 15.0 and 30.0 mg/L in the 3,5, - diacetyl –1,4-dihydrolutidin forms were prepared. The formaldehyde derivative solution s w ere prepared in water and in matrix (extract from untreated cotton fibers). Six replicates of each concentration level were prepared From the textile substratef ormaldehyde was extracted with water at 40  C , filtered and then converted by using acetyl - acetone reagent to yellow colored compound
    • 8. V alidation of absorbance measurements on UV/Vis
      • With Grubbs and Beck statistical test were shown that there were no aberrant values
      • An F – test was applied to check heteroscedasticity: standard deviation increase with the concentration
      • Correlation coefficient for standard water and matrix solutions was greater than 0.99
      • Quality coefficient (QC) was lower than permitted 5%
      • Anova test shows that the experimental error was smaller than lack of fit (LOF) for the linear calibration curve
      • Precision of standard water and matrix solutions was better than 10%
      • The limit of detection (LOD) was 0.628 mg/l
      • The limit of quantification (LOQ) was 1.197 mg/l
      • The amount of formaldehyde extracted for each sample can be calculated by:
              • Konc (x) = 7,493 ABS - 0,06356
    • 9. Free formaldehyde measured by HPLC
      • Standard water and matrix solutions of formaldehyde with concentrations levels 0.075, 0.15, 0.3, 0.6, 0.9, 3.0, 6.0, 15.0 and 30.0 mg/L in the 3,5, - diacetyl –1,4-dihydrolutidin forms were prepared
      • Formaldehyde was extracted from textile substrate with water at 40  C , filtered and then converted by using acetylacetone reagent to yellow colored compound
      • HPLC Varian Prostar 210 pump ,
      • Varian Prostar 310 UV/Vis detector (at 410 nm ) ,
      • STAR Chromatography Workstation Varian 4.5 ,
      • LiChrosorb RP-18 coloum with particle size 7  m ,
    • 10. V alidation of the HPLC analytical method
      • T he optimisation of the
      • method (the proper column,
      • mobile phase, solvents,
      • temperature of the column
      • etc.) was done.
      • The concentration of free
      • formaldehyde in the aqueous
      • solution was determined using
      • peak areas from the standard
      • and sample chromatograms.
      • M obile phase methanol-water (70:30 v/v).
      • The retantion time for formaldehyde derivative was 2.7 min
    • 11. V alidation of the HPLC analytical method
      • With Grubbs and Beck statistical test were shown that there were no aberrant values
      • An F – test was applied to check heteroscedasticity: standard deviation increase with the concentration
      • Correlation coefficient for standard water and matrix solutions was greater than 0.99
      • Quality coefficient (QC) was lower than permitted 5%
      • Anova test shows that the experimental error was smaller than lack of fit (LOF) for the linear calibration curve
      • Precision of standard water and matrix solutions was better than 10%
      • The limit of detection (LOD) was 0. 0199 mg/l
      • The limit of quantification (LOQ) was 0.066 mg/l
      • The amount of formaldehyde extracted for each sample can be calculated by:
              • Konc (x) = 0,2055 * 10 -4 AREA – 0,222
    • 12. CONCLUSIONS
      • The results obtained by the standard test method, Japan
      • Law112, were compared with the results obtained by HPLC
      • method where separation was performed on RP C 18 column
      • with water-MeOH as a mobile phase.
      • The limit of detection (LOD) for Japan Law 112 was 0.628 mg/l and t he limit of quantification (LOQ) was 1.197 mg/l
      • The limit of detection (LOD) for HPLC method was 0. 0199 mg/l and t he limit of quantification (LOQ) was 0.066 mg/l  
      • Matrix has no influence on the formaldehyde content in the analysed solution.
    • 13.
      • FORMALDEHYDE IN MICROENCAPTULATED TEXTILE MATERIALS
      Bojana VON C INA U niversity of Maribor, Textile Department Smetanova 17, 2000 Maribor, Slovenia
    • 14. Introduction
      • Essential oils from plants Lavandula sp.
      • (lavender), Rosmarinus sp (rosemary) and
      • Salvia sp. (sage) are natural fungicide and
      • antibacterial agents.
      • These oils were microencapsuled in melamine-
      • formaldehyde microcapsules and cross l inked on
      • PES nonwoven textile materials .
      • Such textile material is capable of
      • releasing formaldehyde by decomposition
      • of microcapsules .
    • 15. S ources of the formaldehyde
      • Textile material (PES)
      • cross-linking reagent
      • m i c ro c apsule s
      • wall : melamine-formaldehyde resins
      • core : 25 % mixture of essential oils , 75 % solvent
      • 80 % mixture of essential oils , 20 % solvent
          • mixture of essential oils : - lavender 70 %
              • - rosemary 20 %
              • - sage 10 %
          • solvent: isopropyl mirystate
    • 16. Experimental
      • Release of formaldehyde from the textile substrate was determined by
      • EN ISO 14184-1 ( Japan Law 112 method ) ,
      • AATCC test 112-1998 ,
      • HPLC method, where the separation was achieved with elution using methanol-water, as eluents on a reverse phase column and was monitored at 410 nm with a UV/VIS detector.
      • In all three methods the e xtracted
      • formaldehyde was converted by
      • using acetylacetone reagent to
      • yellow coloured compound .
    • 17.
      • The formaldehyde contents were determined in
      • different textile samples :
      • a)   untreated textile material (PES nonwoven)
      • b) textile material with cross-linking reagent (suspension of latex and acrilate emulsifier )
      • c)   textile material with empty microcapsules,
      • d)   textile material with cross-linkin ked empty microcapsules ,
      • e) textile material with cross-link ed microcapsules filled with oils ( 25 % mixture of essential oils , 75 % solvent )
      • f) textile material with cross-link ed microcapsules filled with oils ( 80 % mixture of essential oils , 20 % solvent)
      • The formaldehyde contents were determine also in mixture of
      • oils and pure rosemary and sage oil.
    • 18.
      • U ntreated textile material and cross-linking reagent do not contain formaldehyde (7 mg/kg) .
      • Microcapsule’s wall s contribute to the amount of of the formaldehyde significantly :
        • The average formaldehyde content for the microencaptulated textile material with empty microcapsules is 715 mg/kg and 766 mg/kg for microencaptulated textile material with microcapsules filled with oils ( both results are obtained by Japan Law method ) .
        • Results from AATCC test for the same samples are 5.126 mg/kg and 4.174 mg/kg respectively .
      • .
      Results and conclusions
    • 19.
      • Results obtained by HPLC method :
      • indicate that only formaldehyde is released from the textile samples microencaptulated w ith and without essential oil.
      • Although some amount of formaldehyde is proved in pure essential oil s , amount of essential oil which is applied on textile material with microcapsules (160 g/m 2 ) contribute v e ry little to total amount of formaldehyde. This was proved by the measurements of released formaldehyde after the mechanical damages of microcapsules on the textile substrate
    • 20.
      • Lavender: 0,54 ml/L
      • Rosemary: 0,15 ml/L
      • Sage: 0,32 ml/L
      • mixture of essential oils :
              • Average amounts of formaldehyde : 0,61 ml/L
              • Results: from 0,18 to 0,75 ml/L (dependent on extraction conditions)
      Formaldehyde measurements in essential oils:
    • 21. Conclusion
      • Results given by AATCC test 112-1978 method are expected proportionally higher as results given by EN ISO 14184-1 method.
      • The a verage results obtained from samles prapered in production line are lower . T hose samples satisfy eco-labeling system’s requirement. T he explanation for this phenomenon is found in different processes of curing and drying.
      • B y HPLC it was proven that there are no other aldehydes or ketones present on microcapsulated textile materiale
      I t was proven that the amount of formaldehyde in essential oils is negligible
      • M icrocapsule’s wall contributes to the highest degree of the amount of formaldehyde
      • After washing of textile substrate, the results are considerable lower