Determination of surfactants from foam-formed products

Tässä Pro gradu -tutkielmassa tutkittiin surfaktanttien (eli pinta-aktiivisten aineiden) jäämiä kiinteistä vaahtorainatuista näytteistä. Työn päätavoitteena oli kehittää sopivat näytteenkäsittely- ja määritysmenetelmät surfaktanttijäämien määrittämiseksi. Työssä määritettiin yhden anionisen surfakta...

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Main Author: Viitala, Janika
Other Authors: Matemaattis-luonnontieteellinen tiedekunta, Faculty of Sciences, Kemian laitos, Department of Chemistry, Jyväskylän yliopisto, University of Jyväskylä
Format: Master's thesis
Language:eng
Published: 2018
Subjects:
Online Access: https://jyx.jyu.fi/handle/123456789/59871
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author Viitala, Janika
author2 Matemaattis-luonnontieteellinen tiedekunta Faculty of Sciences Kemian laitos Department of Chemistry Jyväskylän yliopisto University of Jyväskylä
author_facet Viitala, Janika Matemaattis-luonnontieteellinen tiedekunta Faculty of Sciences Kemian laitos Department of Chemistry Jyväskylän yliopisto University of Jyväskylä Viitala, Janika Matemaattis-luonnontieteellinen tiedekunta Faculty of Sciences Kemian laitos Department of Chemistry Jyväskylän yliopisto University of Jyväskylä
author_sort Viitala, Janika
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description Tässä Pro gradu -tutkielmassa tutkittiin surfaktanttien (eli pinta-aktiivisten aineiden) jäämiä kiinteistä vaahtorainatuista näytteistä. Työn päätavoitteena oli kehittää sopivat näytteenkäsittely- ja määritysmenetelmät surfaktanttijäämien määrittämiseksi. Työssä määritettiin yhden anionisen surfaktantin, natrium dodekyylisulfaatin (SDS), ja yhden nonionisen surfaktantin, Tween 20:n (polyoksietyleenisorbitaanimonolauraatti), jäämiä vaahtorainatuista käsiarkeista. Mitattuja surfaktanttijäämiä verrattiin teoreettisiin arvoihin, jotka laskettiin näytteen kuiva-ainepitoisuudesta ennen kuivausvaihetta ja surfaktantin annoksesta. Surfaktanttijäämien analysoinnin lisäksi tutkittiin 4-dodekyylibentseenisulphonihapon (4-DBSA, anioninen surfaktantti) määritystä vesiliuoksesta UV-spektrofotometrillä. Kirjallinen osa käsittelee surfaktanttien kemiaa ja esittelee suhteellisen uuden paperinvalmistusmenetelmän, vaahtorainauksen. Päähuomio on kohdennettu surfaktanttien analyysimenetelmiin. Näytteenkäsittelymenetelmät ja spektrofotometrian, kromatografian sekä atomispektroskopian käyttö surfaktanttien määrityksessä on käsitelty. Lisäksi käydään läpi kemikaalilainsäädäntöä, surfaktantteihin liittyviä toksikologisia huolenaiheita sekä ruokapakkauksissa käytettävää paperia ja kartonkia koskevia säädöksiä. Surfaktanttijäämien määrittämiseksi käytettiin kahta eri määritysmenetelmää kummallekin surfaktantille. SDS-jäämät määritettiin spektrofotometrillä ja induktiivisesti kytketyllä plasma-optisella emissiospektrometrillä (ICP-OES). Tween 20 -jäämät määritettiin spektrofotometrillä sekä korkean erotuskyvyn nestekromatografilla, jossa oli diodirivi-detektori. ICP-OES -analyysissä näytteenkäsittelymenetelmänä käytettiin ultraääniavustettua typpihappohajotusta. Ennen kromatografista määritystä, Tween 20 uutettiin näytteestä metanolilla käyttäen Soxhlet-uuttoa. Spektrofotometrisessa määrityksessä SDS ja Tween 20 uutettiin veteen. Tulokset osoittivat, että surfaktanttijäämät kasvoivat, kun surfaktantin annos kasvoi ja kun näytteen kuiva-ainepitoisuus (ennen viimeistä kuivausvaihetta) laski. ICP-OES-laitteella ja spektrofotometrillä saadut tulokset SDS-jäämille olivat hyvin samanlaisia. Tulokset osoittivat, että SDS uuttui kuituverkostosta vedellä tehokkaasti. SDS-jäämien määrään vaikutti näytteen valmistuksessa käytetyn veden kovuus, vesi-kuitu -suspension lämpötila ja nonionisen surfaktantin tai tärkkelyksen lisäys. Kun veden kovuus oli °dH = 5, mitatut SDS-jäämät olivat selkeästi korkeampi kuin teoreettiset arvot. Tämä johtuu liukenemattoman kalsium dodekyyli sulfaatin CaDS2 muodostumisesta, joka jää kuituverkostoon. SDS-jäämien määrä laski, kun veden kovuus laski, lämpötilaa nostettiin tai lisättiin nonionista surfaktanttia (Tween 20). Kationisen tärkkelyksen lisäys nosti SDS-jäämien määrää. Tween 20 voitiin määrittää sekä HPLC-DAD-laitteella että spektrofotometrillä. HPLC-DAD:lla saatiin korkeampi tuloksia kuin spektrofotometrisellä menetelmällä, koska Tween 20 ei uuttunut täysin vedellä. Kun vettä, etanolia ja asetonia verrattiin uuttoliuottimina Soxhlet-uutossa, tulokset osoittivat selkeästi, että etanoli ja asetoni uuttivat enemmän Tween 20 -surfaktanttia kuin vesi. Tween 20 -jäämien määrän ei havaittu olevan teoreettisia arvoja suurempia. In this Master’s thesis, determination of surfactant residues from solid foam-formed samples was studied. The residues of an anionic surfactant, sodium dodecyl sulphate (SDS), and a non-ionic surfactant Tween 20 (polyoxyethylenesorbitan monolaurate), were determined from foam-formed hand sheets. The measured surfactant residues were compared with the theoretical values calculated from the water content of the sample before drying phase and the surfactant dosage. In addition to analysis of surfactant residues, determination of 4-dodecylbenzenesulphonic acid (4-DBSA, anionic surfactant) in water solution by UV spectrophotometry was studied. The literature part considers the chemistry of surfactants and introduces the relatively new concept of papermaking, foam forming. The main focus in the literature part is in the analysis methods of surfactants. Sample pre-treatment methods and the use of spectrophotometry, chromatography and atomic spectroscopy in the determination of surfactants are discussed. In addition, the chemical legislation, toxicological concerns of surfactants and the regulations concerning paper and board in food contact materials are discussed. To determine surfactant residues, two different determination methods were used for both surfactants. SDS residues were determined by spectrophotometry and by inductively coupled plasma optical emission spectrometry (ICP-OES). Tween 20 residues were determined by spectrophotometry and by high-performance liquid chromatography equipped with a diode array detector (HPLC-DAD). Ultrasound-assisted nitric acid digestion was used as a sample preparation method for the ICP-OES analysis. Before the chromatographic determination, Tween 20 was extracted from the sample by methanol in Soxhlet extraction. In the spectrophotometric determination, SDS and Tween 20 were extracted by water. The results showed that surfactant residues increased as the surfactant dosage increased and when the dry matter content of the sample (before the last drying stage) decreased. ICP-OES and spectrophotometric methods gave very similar results for SDS residues. The results indicated that SDS was effectively extracted from the fibre network by water. The amount of SDS residues was affected by water hardness, the temperature of the water-fibre suspension and the addition of a non-ionic surfactant or cationic starch. When the water hardness was °dH = 5, the measured SDS residues were clearly higher than the theoretical values. This is due to the formation of insoluble calcium dodecyl sulphate Ca(DS)2 that remains in the fibre network. The amount of SDS residues decreased when water hardness decreased, temperature was raised or a non-ionic surfactant (Tween 20) was added. The addition of cationic starch resulted in the increase of SDS residues. Tween 20 could be determined by both HPLC-DAD and spectrophotometry. HPLC-DAD gave higher results compared to the spectrophotometric determination, because Tween 20 was not fully extracted by water. When water, ethanol and acetone were compared as extraction solvents in Soxhlet extraction, the results showed clearly that more Tween 20 was extracted by ethanol and acetone than water. The amount of Tween 20 residues was not observed to be higher than theoretically estimated.
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Ty\u00f6n p\u00e4\u00e4tavoitteena oli kehitt\u00e4\u00e4 sopivat n\u00e4ytteenk\u00e4sittely- ja m\u00e4\u00e4ritysmenetelm\u00e4t surfaktanttij\u00e4\u00e4mien m\u00e4\u00e4ritt\u00e4miseksi. Ty\u00f6ss\u00e4 m\u00e4\u00e4ritettiin yhden anionisen surfaktantin, natrium dodekyylisulfaatin (SDS), ja yhden nonionisen surfaktantin, Tween 20:n (polyoksietyleenisorbitaanimonolauraatti), j\u00e4\u00e4mi\u00e4 vaahtorainatuista k\u00e4siarkeista. Mitattuja surfaktanttij\u00e4\u00e4mi\u00e4 verrattiin teoreettisiin arvoihin, jotka laskettiin n\u00e4ytteen kuiva-ainepitoisuudesta ennen kuivausvaihetta ja surfaktantin annoksesta. Surfaktanttij\u00e4\u00e4mien analysoinnin lis\u00e4ksi tutkittiin 4-dodekyylibentseenisulphonihapon (4-DBSA, anioninen surfaktantti) m\u00e4\u00e4rityst\u00e4 vesiliuoksesta UV-spektrofotometrill\u00e4. Kirjallinen osa k\u00e4sittelee surfaktanttien kemiaa ja esittelee suhteellisen uuden paperinvalmistusmenetelm\u00e4n, vaahtorainauksen. P\u00e4\u00e4huomio on kohdennettu surfaktanttien analyysimenetelmiin. N\u00e4ytteenk\u00e4sittelymenetelm\u00e4t ja spektrofotometrian, kromatografian sek\u00e4 atomispektroskopian k\u00e4ytt\u00f6 surfaktanttien m\u00e4\u00e4rityksess\u00e4 on k\u00e4sitelty. Lis\u00e4ksi k\u00e4yd\u00e4\u00e4n l\u00e4pi kemikaalilains\u00e4\u00e4d\u00e4nt\u00f6\u00e4, surfaktantteihin liittyvi\u00e4 toksikologisia huolenaiheita sek\u00e4 ruokapakkauksissa k\u00e4ytett\u00e4v\u00e4\u00e4 paperia ja kartonkia koskevia s\u00e4\u00e4d\u00f6ksi\u00e4.\nSurfaktanttij\u00e4\u00e4mien m\u00e4\u00e4ritt\u00e4miseksi k\u00e4ytettiin kahta eri m\u00e4\u00e4ritysmenetelm\u00e4\u00e4 kummallekin surfaktantille. SDS-j\u00e4\u00e4m\u00e4t m\u00e4\u00e4ritettiin spektrofotometrill\u00e4 ja induktiivisesti kytketyll\u00e4 plasma-optisella emissiospektrometrill\u00e4 (ICP-OES). Tween 20 -j\u00e4\u00e4m\u00e4t m\u00e4\u00e4ritettiin spektrofotometrill\u00e4 sek\u00e4 korkean erotuskyvyn nestekromatografilla, jossa oli diodirivi-detektori. ICP-OES -analyysiss\u00e4 n\u00e4ytteenk\u00e4sittelymenetelm\u00e4n\u00e4 k\u00e4ytettiin ultra\u00e4\u00e4niavustettua typpihappohajotusta. Ennen kromatografista m\u00e4\u00e4rityst\u00e4, Tween 20 uutettiin n\u00e4ytteest\u00e4 metanolilla k\u00e4ytt\u00e4en Soxhlet-uuttoa. Spektrofotometrisessa m\u00e4\u00e4rityksess\u00e4 SDS ja Tween 20 uutettiin veteen.\nTulokset osoittivat, ett\u00e4 surfaktanttij\u00e4\u00e4m\u00e4t kasvoivat, kun surfaktantin annos kasvoi ja kun n\u00e4ytteen kuiva-ainepitoisuus (ennen viimeist\u00e4 kuivausvaihetta) laski. ICP-OES-laitteella ja spektrofotometrill\u00e4 saadut tulokset SDS-j\u00e4\u00e4mille olivat hyvin samanlaisia. Tulokset osoittivat, ett\u00e4 SDS uuttui kuituverkostosta vedell\u00e4 tehokkaasti. SDS-j\u00e4\u00e4mien m\u00e4\u00e4r\u00e4\u00e4n vaikutti n\u00e4ytteen valmistuksessa k\u00e4ytetyn veden kovuus, vesi-kuitu -suspension l\u00e4mp\u00f6tila ja nonionisen surfaktantin tai t\u00e4rkkelyksen lis\u00e4ys. Kun veden kovuus oli \u00b0dH = 5, mitatut SDS-j\u00e4\u00e4m\u00e4t olivat selke\u00e4sti korkeampi kuin teoreettiset arvot. T\u00e4m\u00e4 johtuu liukenemattoman kalsium dodekyyli sulfaatin CaDS2 muodostumisesta, joka j\u00e4\u00e4 kuituverkostoon. SDS-j\u00e4\u00e4mien m\u00e4\u00e4r\u00e4 laski, kun veden kovuus laski, l\u00e4mp\u00f6tilaa nostettiin tai lis\u00e4ttiin nonionista surfaktanttia (Tween 20). Kationisen t\u00e4rkkelyksen lis\u00e4ys nosti SDS-j\u00e4\u00e4mien m\u00e4\u00e4r\u00e4\u00e4.\nTween 20 voitiin m\u00e4\u00e4ritt\u00e4\u00e4 sek\u00e4 HPLC-DAD-laitteella ett\u00e4 spektrofotometrill\u00e4. HPLC-DAD:lla saatiin korkeampi tuloksia kuin spektrofotometrisell\u00e4 menetelm\u00e4ll\u00e4, koska Tween 20 ei uuttunut t\u00e4ysin vedell\u00e4. Kun vett\u00e4, etanolia ja asetonia verrattiin uuttoliuottimina Soxhlet-uutossa, tulokset osoittivat selke\u00e4sti, ett\u00e4 etanoli ja asetoni uuttivat enemm\u00e4n Tween 20 -surfaktanttia kuin vesi. Tween 20 -j\u00e4\u00e4mien m\u00e4\u00e4r\u00e4n ei havaittu olevan teoreettisia arvoja suurempia.", "language": "fi", "element": "description", "qualifier": "abstract", "schema": "dc"}, {"key": "dc.description.abstract", "value": "In this Master\u2019s thesis, determination of surfactant residues from solid foam-formed samples was studied. The residues of an anionic surfactant, sodium dodecyl sulphate (SDS), and a non-ionic surfactant Tween 20 (polyoxyethylenesorbitan monolaurate), were determined from foam-formed hand sheets. The measured surfactant residues were compared with the theoretical values calculated from the water content of the sample before drying phase and the surfactant dosage. In addition to analysis of surfactant residues, determination of 4-dodecylbenzenesulphonic acid (4-DBSA, anionic surfactant) in water solution by UV spectrophotometry was studied. The literature part considers the chemistry of surfactants and introduces the relatively new concept of papermaking, foam forming. The main focus in the literature part is in the analysis methods of surfactants. Sample pre-treatment methods and the use of spectrophotometry, chromatography and atomic spectroscopy in the determination of surfactants are discussed. In addition, the chemical legislation, toxicological concerns of surfactants and the regulations concerning paper and board in food contact materials are discussed.\nTo determine surfactant residues, two different determination methods were used for both surfactants. SDS residues were determined by spectrophotometry and by inductively coupled plasma optical emission spectrometry (ICP-OES). Tween 20 residues were determined by spectrophotometry and by high-performance liquid chromatography equipped with a diode array detector (HPLC-DAD). Ultrasound-assisted nitric acid digestion was used as a sample preparation method for the ICP-OES analysis. Before the chromatographic determination, Tween 20 was extracted from the sample by methanol in Soxhlet extraction. In the spectrophotometric determination, SDS and Tween 20 were extracted by water.\nThe results showed that surfactant residues increased as the surfactant dosage increased and when the dry matter content of the sample (before the last drying stage) decreased. ICP-OES and spectrophotometric methods gave very similar results for SDS residues. The results indicated that SDS was effectively extracted from the fibre network by water. The amount of SDS residues was affected by water hardness, the temperature of the water-fibre suspension and the addition of a non-ionic surfactant or cationic starch. When the water hardness was \u00b0dH = 5, the measured SDS residues were clearly higher than the theoretical values. This is due to the formation of insoluble calcium dodecyl sulphate Ca(DS)2 that remains in the fibre network. The amount of SDS residues decreased when water hardness decreased, temperature was raised or a non-ionic surfactant (Tween 20) was added. The addition of cationic starch resulted in the increase of SDS residues.\nTween 20 could be determined by both HPLC-DAD and spectrophotometry. HPLC-DAD gave higher results compared to the spectrophotometric determination, because Tween 20 was not fully extracted by water. When water, ethanol and acetone were compared as extraction solvents in Soxhlet extraction, the results showed clearly that more Tween 20 was extracted by ethanol and acetone than water. 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spellingShingle Viitala, Janika Determination of surfactants from foam-formed products surfactants surfactant residues foam forming Epäorgaaninen ja analyyttinen kemia Inorganic and Analytical Chemistry 4031
title Determination of surfactants from foam-formed products
title_full Determination of surfactants from foam-formed products
title_fullStr Determination of surfactants from foam-formed products Determination of surfactants from foam-formed products
title_full_unstemmed Determination of surfactants from foam-formed products Determination of surfactants from foam-formed products
title_short Determination of surfactants from foam-formed products
title_sort determination of surfactants from foam formed products
title_txtP Determination of surfactants from foam-formed products
topic surfactants surfactant residues foam forming Epäorgaaninen ja analyyttinen kemia Inorganic and Analytical Chemistry 4031
topic_facet 4031 Epäorgaaninen ja analyyttinen kemia Inorganic and Analytical Chemistry foam forming surfactant residues surfactants
url https://jyx.jyu.fi/handle/123456789/59871 http://www.urn.fi/URN:NBN:fi:jyu-201810184450
work_keys_str_mv AT viitalajanika determinationofsurfactantsfromfoamformedproducts