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Determination of polyethylene in biodegradable polymer blends and in compostable carrier bags by Py-GC/MS and TGA

机译:通过Py-GC / MS和TGA测定可生物降解的聚合物混合物和可堆肥的运输袋中的聚乙烯

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In this paper, the amount of polyethylene (PE) contained in complex biodegradable polymer blends and in carrier bags claimed to be compostable was determined by thermogravimetry analysis (TGA) and pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS). To validate the method, polymer blends based on polylactide (PLA), poly(butylene adipate-co-butylene terephthalate) 53/47 (PBAT), native starch (NS), and calcium carbonate, with known amount of PE ranging from 0 to 10%, were prepared by melt mixing. Py-GC/MS parameters were optimized. In the first step at 400 degrees C, pyrolysis products originated from thermal cracking of PLA, NS and PBAT were detected. In the second step carried out at 500 degrees C, triplet peaks characteristic for PE, consisting of alpha,omega-dienes, alpha-alkenes and n-alkanes, were revealed together with some signals related to PBAT. TGA under nitrogen atmosphere was used to determine the amount of PE in the blends. An overestimation of about 1.2%, constant for all the blends, was revealed. The overestimation was attributed to the partial overlapping of one of the steps of degradation of the commercial PBAT and that of PE. Additionally, the analytical approach was applied in the characterization of carrier bags claimed to be compostable, recovered directly from the market. The correct determination of the composition of these biodegradable blends is important and crucial to comply with the compostability standard EN 13432-2000. According to this standard, each significant organic constituent of the packaging material must be biodegradable. "Significant" means any constituent present in more than 1% of dry weight of that material. This implies that maximum allowed PE concentration that can be detected in a compostable blend is 1%. In two commercial carrier bags, TGA revealed a component with a degradation temperature of about 455 degrees C corresponding to that of PE. The relative weight loss percentages of these two carrier bags have been estimated 7.6 and 14%. Optimization of the Ay-GC/MS conditions allowed identifying its chemical structure. In fact, the Py-GC/MS at 500 degrees C provided a pyrogram that was a fingerprint for PE with triplets corresponding to linear chains of alpha,omega-dienes, alpha-alkenes and n-alkanes with chain lengths in the range of 9-36 degrees C atoms. Overall, the results show that the combination of TGA and Py-GC/MS can be applied with practical implications. (C) 2015 Elsevier B.V. All rights reserved.
机译:在本文中,通过热重分析(TGA)和热解气相色谱/质谱(Py-GC / MS)确定了复杂的可生物降解聚合物共混物和声称可堆肥的运输袋中聚乙烯(PE)的量。为了验证该方法,使用了基于聚丙交酯(PLA),聚(己二酸丁二酯-对苯二甲酸丁二醇酯)53/47(PBAT),天然淀粉(NS)和碳酸钙的聚合物共混物,已知的PE范围为0至通过熔融混合制备10%。优化了Py-GC / MS参数。在400摄氏度的第一步中,检测到源自PLA,NS和PBAT热裂解的热解产物。在500摄氏度下进行的第二步中,揭示了PE的三重峰,其中包括α,ω-二烯,α-烯烃和n-烷烃,以及一些与PBAT相关的信号。在氮气气氛下使用TGA测定掺合物中PE的含量。结果表明,所有混合物的含量均被高估了约1.2%。高估归因于商业PBAT和PE降解步骤之一的部分重叠。此外,该分析方法还用于表征可堆肥的,直接从市场上回收的手提袋。正确确定这些可生物降解混合物的组成对于遵守可堆肥性标准EN 13432-2000非常重要。根据该标准,包装材料中每种重要的有机成分必须是可生物降解的。 “重要的”是指以该材料的干重的1%以上存在的任何成分。这意味着可堆肥混合物中可检测到的最大允许PE浓度为1%。在两个商用提袋中,TGA揭示了一种降解温度约为455℃的组分,相当于PE的降解温度。这两个搬运袋的相对失重百分比估计为7.6和14%。通过优化Ay-GC / MS条件,可以确定其化学结构。实际上,在500摄氏度下Py-GC / MS提供的热解图是PE的指纹图谱,其三链体对应于链长在9范围内的α,ω-二烯,α-烯烃和n-烷烃的线性链-36摄氏度的原子。总体而言,结果表明,TGA和Py-GC / MS的结合可以实际应用。 (C)2015 Elsevier B.V.保留所有权利。

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