Environmental Science and Pollution Research
co m pounds in the feedstock. A sa m ple of 300 μg of paper/ cardboard/ m agazine was placed into a glass sa m pling tube along with an internal standard (1,3,5-tri-tert-butylbenzene). Ther m al desorption was perfor m ed using a unit (Gerstel, Mülhei m an der Ruhr, Ger m any) in the te m perature range 50 to 300 °C for 5 m in, with a heating rate of 60 °C/ m in. Vola- tilized organic co m pounds were concentrated in a cooled injection syste m (CIS) at − 10 °C and subsequently separated on a non-polar HP5 m s colu m n (60 m × 0.25 mm × 0.25 μ m ) under a te m perature progra mm e: 40 °C (2 m in) to 310 °C (10 m in), at a rate of 10 °C/ m in. Identification and quantifi- cation of organic co m pounds were perfor m ed using a m ass spectro m eter (Agilent 5977 B, Santa Clara, USA) within a scan range of m /z 50–650, using external calibration with certified standards. GC/MS quantification of co m pounds was perfor m ed by external standards with the addition of 1 μl of internal standard (1,3,5-tri-tert-butylbenzene) by the calibration curve m ethod. The construction of calibration curves was carried out by the progra m Mass Hunter-MS Quantification.
of crystallinity or cleavage of glycosidic bonds. I m portantly, acetic acid allows for the si m ultaneous re m oval of both PCC and organic additives, without co m pro m ising the cellulose structure. In contrast, traditional acid or alkaline treat m ents (e.g. NaOH and HCl) often exhibit li m itations in selectively re m oving both fillers and additives while preserving fibre integrity. The sa m ple of waste paper was disintegrated for 1 m in using the Vorwerk Ther m o m ix TM6 (Vorwerk Engineer- ing, Wuppertal, Ger m any) and then separated in a centrifuge (Beck m an Avanti JXN-26, Beck m an Coulter, Brea, Califor- nia) at 8000 rp m . The acid–base reaction of the solution was deter m ined according to ISO 10523 (International Organiza- tion for Standardization 2008). Calciu m ion concentration (Ca 2 ၰ , m g/L) was analysed following ISO 6058 (Interna- tional Organization for Standardization 1984). The cellulose sa m ple was subsequently rinsed with 500 m L of deionized water (once or twice). The selection of a suitable extraction agent and its concentration (HCl, H ၸ PO ၹ , and CH ၸ COOH) was based on the studies by Phipps and Lorusso (2001) and Ki m and Ki m (2018).
Processing of results from TD-GC/MS
Methods
A co m prehensive search of the literature, PubChe m data- bases, and additional online sources was conducted to iden- tify the origin of the detected co m pounds. This included infor m ation fro m the “European Printing Ink Association (EuPIA), Inventory List – Version January 2011,” which catalogues packaging ink raw m aterials applied to the non- food contact surfaces of food packaging. The potential haz- ards of the identified co m pounds were assessed according to the “Globally Har m onized Syste m of Classification and Labelling of Che m icals” (GHS Rev. 10, 2023), a guideline for the classification and labelling of hazardous substances. To characterize the broadest possible range of identified che m ical co m pounds, the use of GHS hazard categories was selected as the only viable and consistent m ethod for co m - m unicating their potential risks across international datasets, since GHS-based databases contain infor m ation on hundreds of thousands of substances, including m any that are not reg- istered in the EU. This approach allowed us to retrieve rel- evant hazard data for a large nu m ber of organic co m pounds. For each co m pound, hazard infor m ation fro m the PubChe m database was consulted, with e m phasis on the GHS hazard state m ents: health risks, environ m ental risks, and irritants—the latter being considered part of health risks. Classification into hazard categories was perfor m ed using the co m prehensive category syste m provided by the United Nations Econo m ic Co mm ission for Europe. In cases where a co m pound was associated with risks in all three categories, only one hazard class was reported, following a predefined prioritization: health risks > environ m ental risks > irritants.
The ASTM E1755-01(2020) “Standard Test Method for Ash in Bio m ass” (oxidation at 575 ± 25 °C) was applied (ASTM International 2020). This m ethod is suitable for deter m ining ash content in m aterials such as office waste, boxboard, and newsprint. Moisture content was deter m ined according to ISO 18134-3:2023 (International Organization for Stand- ardization 2023). The calciu m (Ca) concentration in both e m bossed cellulose and waste paper was m easured using the US EPA Method 6200, “Field Portable X-ray Fluorescence Spectroscopy for the Deter m ination of Ele m ental Concentra- tions in Soil and Sedi m ents,” e m ploying the Innov-X Delta Professional analyzer (Oly m pus Innov-X, USA). Identifying m inerals in ash and the character of cellulose fibres was perfor m ed using the auto-e m ission scanning elec- tron m icroscope FEI Quanta-650 FEG ( m anufactured by FEI Co., Hillsboro, USA). The m ineralogical phase co m position of fillers was analysed by X-ray diffraction (Bruker Advance D8 X-ray diffracto m eter). The che m ical co m position and crystallinity of the sep- arated cellulose were analysed using a Fourier transfor m infrared (FTIR) spectro m eter (FT-IR Nicolet 6700, Ther m o Scientific). Measure m ents were conducted using the atten- uated total reflectance (ATR) technique across a spectral range of 4000 to 525 c mၱ 1 , with a resolution of 4 c mၱ 1 . Each sa m ple was scanned 64 ti m es, and the resulting spectra were co m pared to assess structural differences and co m positional features. The TD-GC/MS m ethod (Gerstel, Mülhei m an der Ruhr, Ger m any) was used for the identification of organic
Made with FlippingBook interactive PDF creator