Top

Published in:

2022 | OriginalPaper | Chapter

Analytical Methods for Plastic (Microplastic) Determination in Environmental Samples

Authors : G. Dierkes, T. Lauschke, C. Földi

Published in: Plastics in the Aquatic Environment - Part I

Publisher: Springer International Publishing

Activate our intelligent search to find suitable subject content or patents.

search-config

AI-assisted search

Off

Abstract

Beside several studies about the occurrence of microplastic (MP) there is still a huge gap of knowledge regarding the dynamic processes of MP distribution and fate. Consequently, there is a need for reliable, fast, and robust analytical methods for MP monitoring. However, due to the physicochemical attributes of plastic, new analytical approaches fundamentally different from those for most other environmental contaminants are required. Promising strategies include spectroscopic and thermo-analytical methods. The two vibrational spectroscopic methods, Fourier-transform infrared spectroscopy (FT-IR) and Raman spectroscopy, have been implemented for MP detection. Especially in combination with particle finding software or a focal plane array (FPA) detector, they enable reliable determination of MP particle numbers in environmental samples. In recent years, different thermo-analytical techniques, such as pyrolysis (Py), thermogravimetric analysis (TGA), and differential scanning calorimetry (DSC) have been adapted for MP detection. All thermo-analytical methods are based upon measurement of physical or chemical changes of the polymer under thermal treatment. While DSC measures differences in heat flux caused by phase transitions of the polymer, TGA-MS is based upon detection of specific thermal degradation products. By means of a gas chromatographic separation step, an enhanced detection of the marker compounds is possible, enabling a more sensitive MP detection even in complex matrices. The extent of analytical information obtained as well as the complexity and effort of the methods increase by TGA-DSC < TGA-MS < Py-GC-MS/TED-GC-MS. The results are comparable to those of spectroscopic methods (FT-IR, Raman), but both techniques have different benefits and limitations. While thermo-analytical methods require minor sample pretreatment and reveal mass concentrations, spectroscopic methods are non-destructive and yield particle numbers and size distribution by imaging techniques. Whichever is the most suitable method depends on the scientific question and what kind of information is required.

Dont have a licence yet? Then find out more about our products and how to get one now:

Springer Professional "Wirtschaft+Technik"

Online-Abonnement

Mit Springer Professional "Wirtschaft+Technik" erhalten Sie Zugriff auf:

über 102.000 Bücher
über 537 Zeitschriften

aus folgenden Fachgebieten:

Automobil + Motoren
Bauwesen + Immobilien
Business IT + Informatik
Elektrotechnik + Elektronik
Energie + Nachhaltigkeit
Finance + Banking
Management + Führung
Marketing + Vertrieb
Maschinenbau + Werkstoffe
Versicherung + Risiko

Jetzt Wissensvorsprung sichern!

inform now

Springer Professional "Technik"

Online-Abonnement

Mit Springer Professional "Technik" erhalten Sie Zugriff auf:

über 67.000 Bücher
über 390 Zeitschriften

aus folgenden Fachgebieten:

Automobil + Motoren
Bauwesen + Immobilien
Business IT + Informatik
Elektrotechnik + Elektronik
Energie + Nachhaltigkeit
Maschinenbau + Werkstoffe

Jetzt Wissensvorsprung sichern!

inform now

previous chapter Pitfalls and Limitations in Microplastic Analyses

next chapter Biodegradable Plastics: End of Life Scenarios

Wagner M et al (2014) Microplastics in freshwater ecosystems: what we know and what we need to know. Environ Sci Eur 26(1):1–9CrossRef

Elert AM et al (2017) Comparison of different methods for MP detection: what can we learn from them, and why asking the right question before measurements matters? Environ Pollut 231(Part 2):1256–1264CrossRef

Huppertsberg S, Knepper TP (2018) Instrumental analysis of microplastics – benefits and challenges. Anal Bioanal Chem 410:6343–6352

Li J, Liu H, Paul Chen J (2018) Microplastics in freshwater systems: a review on occurrence, environmental effects, and methods for microplastics detection. Water Res 137:362–374CrossRef

Renner G, Schmidt TC, Schram J (2018) Analytical methodologies for monitoring micro(nano)plastics: which are fit for purpose? Curr Opin Environ Sci Health 1:55–61CrossRef

Zarfl C (2019) Promising techniques and open challenges for microplastic identification and quantification in environmental matrices. Anal Bioanal Chem 411:3743–3756

Silva AB et al (2018) Microplastics in the environment: challenges in analytical chemistry – a review. Anal Chim Acta 1017:1–19CrossRef

Nguyen B et al (2019) Separation and analysis of microplastics and nanoplastics in complex environmental samples. Acc Chem Res 52(4):858–866CrossRef

Peñalver R et al (2020) An overview of microplastics characterization by thermal analysis. Chemosphere 242:125170CrossRef

10.

Tsuge S, Ohtani H, Watanabe C (2011) Pyrolysis-GC/MS data book of synthetic polymers. Elsevier, Oxford

11.

Qian K et al (1996) Rapid polymer identification by in-source direct pyrolysis mass spectrometry and library searching techniques. Anal Chem 68(6):1019–1027CrossRef

12.

Everall NJ, Chalmers JM, Griffiths PR (2007) Vibrational spectroscopy of polymers: principles and practice. Wiley-VCH, Weinheim

13.

Halle AT (2020) Emerging use thermo-analytical method coupled with mass spectrometry for the quantification of micro(nano)plastics in environmental samples. TrAC Trends Anal Chem:115979

14.

Käppler A et al (2018) Comparison of μ-ATR-FTIR spectroscopy and py-GCMS as identification tools for microplastic particles and fibers isolated from river sediments. Anal Bioanal Chem 410(21):5313–5327CrossRef

15.

Müller YK et al (2019) Microplastic analysis – are we measuring the same? Results on the first global comparative study for microplastic analysis in a water sample. Anal Bioanal Chem 412:555–560

16.

Becker R et al (2020) Quantification of microplastics in a freshwater suspended organic matter using different thermoanalytical methods – outcome of an interlaboratory comparison. J Anal Appl Pyrolysis 148:104829CrossRef

17.

Lenz R et al (2015) A critical assessment of visual identification of marine microplastic using Raman spectroscopy for analysis improvement. Mar Pollut Bull 100(1):82–91CrossRef

18.

Dekiff JH et al (2014) Occurrence and spatial distribution of microplastics in sediments from Norderney. Environ Pollut 186

19.

Erni-Cassola G et al (2017) Lost, but found with Nile red; a novel method to detect and quantify small microplastics (20 μm–1 mm) in environmental samples. Environ Sci Technol 51(23):13641–13648

20.

Shim WJ et al (2016) Identification and quantification of microplastics using Nile Red staining. Mar Pollut Bull 113(1–2):469–476CrossRef

21.

Hengstmann E, E.K.J.E.M. Fischer, and Assessment (2019) Nile red staining in microplastic analysis – proposal for a reliable and fast identification approach for large microplastics. Environ Monit Assess 191(10):612CrossRef

22.

Maes T et al (2017) A rapid-screening approach to detect and quantify microplastics based on fluorescent tagging with Nile Red. Sci Rep 7:44501CrossRef

23.

Hermsen E et al (2018) Quality criteria for the analysis of microplastic in biota samples: a critical review. Environ Sci Technol 52(18):10230–10240CrossRef

24.

Käppler A et al (2016) Analysis of environmental microplastics by vibrational microspectroscopy: FTIR, Raman or both? Anal Bioanal Chem 408(29):8377–8391CrossRef

25.

Klein S, Worch E, Knepper TP (2015) Occurrence and spatial distribution of microplastics in river shore sediments of the Rhine-Main area in Germany. Environ Sci Technol 49(10):6070–6076CrossRef

26.

Imhof HK et al (2016) Pigments and plastic in limnetic ecosystems: a qualitative and quantitative study on microparticles of different size classes. Water Res 98:64–74CrossRef

27.

Mani T et al (2019) Repeated detection of polystyrene microbeads in the lower Rhine River. Environ Pollut 245:634–641CrossRef

28.

Stock F et al (2020) Pitfalls and limitations in microplastic analyses. Springer, Berlin, pp 1–30

29.

Harrison JP, Ojeda JJ, Romero-Gonzalez ME (2012) The applicability of reflectance micro-Fourier-transform infrared spectroscopy for the detection of synthetic microplastics in marine sediments. Sci Total Environ 416:455–463CrossRef

30.

Löder MGJ et al (2015) Focal plane array detector-based micro-Fourier-transform infrared imaging for the analysis of microplastics in environmental samples. J Environ Chem 12(5):563–581CrossRef

31.

Käppler A et al (2015) Identification of microplastics by FTIR and Raman microscopy: a novel silicon filter substrate opens the important spectral range below 1300 cm⁻¹ for FTIR transmission measurements. Anal Bioanal Chem 407(22):6791–6801CrossRef

32.

Cabernard L et al (2018) Comparison of Raman and Fourier transform infrared spectroscopy for the quantification of microplastics in the aquatic environment. Environ Sci Technol 52(22):13279–13288CrossRef

33.

Anger PM et al (2018) Raman microspectroscopy as a tool for microplastic particle analysis. TrAC Trends Anal Chem 109:214–226CrossRef

34.

Schymanski D et al (2018) Analysis of microplastics in water by micro-Raman spectroscopy: release of plastic particles from different packaging into mineral water. Water Res 129:154–162CrossRef

35.

Araujo CF et al (2018) Identification of microplastics using Raman spectroscopy: latest developments and future prospects. Water Res 142:426–440CrossRef

36.

Tagg AS et al (2015) Identification and quantification of microplastics in wastewater using focal plane Array-based reflectance micro-FT-IR imaging. Anal Chem 87(12):6032–6040CrossRef

37.

Primpke S et al (2017) An automated approach for microplastics analysis using focal plane array (FPA) FTIR microscopy and image analysis. Anal Methods 9(9):1499–1511CrossRef

38.

Simon M, van Alst N, Vollertsen J (2018) Quantification of microplastic mass and removal rates at wastewater treatment plants applying focal plane Array (FPA)-based Fourier transform infrared (FT-IR) imaging. Water Res 142:1–9CrossRef

39.

Primpke S et al (2020) EXPRESS: toward the systematic identification of microplastics in the environment: evaluation of a new independent software tool (siMPle) for spectroscopic analysis. Appl Spectrosc:0003702820917760

40.

Paul A et al (2018) High-throughput NIR spectroscopic (NIRS) detection of microplastics in soil. Environ Sci Pollut Res 26:7364–7374

41.

Hahn A et al (2019) Using FTIRS as pre-screening method for detection of microplastic in bulk sediment samples. Sci Total Environ 689:341–346CrossRef

42.

Corradini F et al (2019) Predicting soil microplastic concentration using vis-NIR spectroscopy. Sci Total Environ 650:922–932CrossRef

43.

Peez N, Janiska M-C, Imhof W (2018) The first application of quantitative 1H NMR spectroscopy as a simple and fast method of identification and quantification of microplastic particles (PE, PET, and PS). Anal Bioanal Chem

44.

Peez N, Imhof W (2020) Quantitative 1H-NMR spectroscopy as an efficient method for identification and quantification of PVC, ABS and PA microparticles. Analyst

45.

Peez N et al (2019) Quantitative analysis of PET microplastics in environmental model samples using quantitative 1H-NMR spectroscopy: validation of an optimized and consistent sample clean-up method. Anal Bioanal Chem 411:7603CrossRef

46.

Majewsky M et al (2016) Determination of microplastic polyethylene (PE) and polypropylene (PP) in environmental samples using thermal analysis (TGA-DSC). Sci Total Environ 568:507–511CrossRef

47.

Rodríguez Chialanza M et al (2018) Identification and quantitation of semi-crystalline microplastics using image analysis and differential scanning calorimetry. Environ Sci Pollut Res 25(17):16767–16775CrossRef

48.

David J et al (2019) Introducing a soil universal model method (SUMM) and its application for qualitative and quantitative determination of poly(ethylene), poly(styrene), poly(vinyl chloride) and poly(ethylene terephthalate) microplastics in a model soil. Chemosphere 225:810–819CrossRef

49.

Moldoveanu SC (2005) Moldoveanu SC (ed) Analytical pyrolysis of synthetic organic polymers. Elsevier, Amsterdam

50.

Shin T, Hajime O, Chuichi W (2011) Pyrolysis – GC/MS data book of synthetic polymers. In: Pyrolysis – GC/MS data book of synthetic polymers. Elsevier, Amsterdam

51.

Wampler TP (1999) Introduction to pyrolysis–capillary gas chromatography. J Chromatogr A 842(1):207–220CrossRef

52.

Schindler A et al (2013) A novel direct coupling of simultaneous thermal analysis (STA) and Fourier transform-infrared (FT-IR) spectroscopy. J Thermal Anal Calorim 113(3):1091–1102CrossRef

53.

Pagacz J et al (2015) Thermal decomposition studies of bio-resourced polyamides by thermogravimetry and evolved gas analysis. Thermochim Acta 612:40–48CrossRef

54.

David J et al (2018) Quantitative analysis of poly(ethylene terephthalate) microplastics in soil via thermogravimetry–mass spectrometry. Anal Chem 90(15):8793–8799

55.

Dierkes G et al (2019) Quantification of microplastics in environmental samples via pressurized liquid extraction and pyrolysis-gas chromatography. Anal Bioanal Chem 411(26):6959–6968

56.

Fischer M, Scholz-Böttcher BM (2017) Simultaneous trace identification and quantification of common types of microplastics in environmental samples by pyrolysis-gas chromatography–mass spectrometry. Environ Sci Technol 51(9):5052–5060CrossRef

57.

Okoffo ED et al (2020) Identification and quantification of selected plastics in biosolids by pressurized liquid extraction combined with double-shot pyrolysis gas chromatography–mass spectrometry. Sci Total Environ:136924

58.

Steinmetz Z et al (2020) A simple method for the selective quantification of polyethylene, polypropylene, and polystyrene plastic debris in soil by pyrolysis-gas chromatography/mass spectrometry. J Anal Appl Pyrolysis:104803

59.

Unice KM, Kreider ML, Panko JM (2012) Use of a deuterated internal standard with pyrolysis-GC/MS dimeric marker analysis to quantify tire tread particles in the environment. Int J Environ Res Public Health 9(11):4033–4055CrossRef

60.

Fries E et al (2013) Identification of polymer types and additives in marine microplastic particles using pyrolysis-GC/MS and scanning electron microscopy. Environ Sci Process Impacts 15(10):1949–1956CrossRef

61.

Fabbri D, Trombini C, I.J.J.o.c.s. Vassura (1998) Analysis of polystyrene in polluted sediments by pyrolysis – gas chromatography – mass spectrometry. J Chromatogr Sci 36(12):600–604CrossRef

62.

Fischer M, Scholz-Böttcher BM (2019) Microplastics analysis in environmental samples – recent pyrolysis-gas chromatography-mass spectrometry method improvements to increase the reliability of mass-related data. Anal Methods 11(18):2489–2497CrossRef

63.

Duemichen E et al (2014) Assessment of a new method for the analysis of decomposition gases of polymers by a combining thermogravimetric solid-phase extraction and thermal desorption gas chromatography mass spectrometry. J Chromatogr A 1354:117–128CrossRef

64.

Dümichen E et al (2015) Analysis of polyethylene microplastics in environmental samples, using a thermal decomposition method. Water Res 85:451–457CrossRef

65.

Duemischen E et al (2019) Automated thermal extraction-desorption gas chromatography mass spectrometry: a multifunctional tool for comprehensive characterization of polymers and their degradation products. J Chromatogr A 1592:133–142CrossRef

66.

Eisentraut P et al (2018) Two birds with one stone – fast and simultaneous analysis of microplastics: microparticles derived from thermoplastics and Tire Wear. Environ Sci Technol Lett 5(10):608–613CrossRef

67.

Krauskopf L-M et al (2020) Critical aspects on off-line pyrolysis-based quantification of microplastic in environmental samples. J Anal Appl Pyrolysis:104830

68.

Hermabessiere L et al (2018) Optimization, performance, and application of a pyrolysis-GC/MS method for the identification of microplastics. Anal Bioanal Chem 410(25):6663–6676CrossRef

69.

Peters CA et al (2018) Pyr-GC/MS analysis of microplastics extracted from the stomach content of benthivore fish from the Texas Gulf Coast. Mar Pollut Bull 137:91–95CrossRef

70.

Dümichen E et al (2017) Fast identification of microplastics in complex environmental samples by a thermal degradation method. Chemosphere 174:572–584CrossRef

71.

Fuller S, Gautam A (2016) A procedure for measuring microplastics using pressurized fluid extraction. Environ Sci Technol 50(11):5774–5780

72.

Lithner D et al (2009) Leachates from plastic consumer products--screening for toxicity with Daphnia magna. Chemosphere 74(9):1195–1200CrossRef

73.

Lithner D, Larsson A, Dave G (2011) Environmental and health hazard ranking and assessment of plastic polymers based on chemical composition. Sci Total Environ 409(18):3309–3324CrossRef

74.

Luft A et al (2017) Nontarget analysis via LC-QTOF-MS to assess the release of organic substances from polyurethane coating. Environ Sci Technol 51(17):9979–9988CrossRef

75.

Zimmermann L et al (2019) Benchmarking the in vitro toxicity and chemical composition of plastic consumer products. Environ Sci Technol 53(19):11467–11477CrossRef

76.

Yanagisawa H et al (2018) Simultaneous screening of major flame retardants and plasticizers in polymer materials using pyrolyzer/thermal desorption gas chromatography mass spectrometry (Py/TD–GC–MS). Molecules 23(4):728CrossRef

77.

Yanagisawa H, Maruyama F, Fujimaki S (2019) Verification of simultaneous screening for major restricted additives in polymer materials using pyrolyzer/thermal desorption gas–chromatography mass spectrometry (Py/TD-GC-MS). J Anal Appl Pyrolysis 137:37–42CrossRef

78.

Mallow O et al (2020) A new thermoanalytical method for the quantification of microplastics in industrial wastewater. Environ Pollut 259:113862CrossRef

79.

Wang L et al (2017) A simple method for quantifying polycarbonate and polyethylene terephthalate microplastics in environmental samples by liquid chromatography–tandem mass spectrometry. Environ Sci Technol Lett 4(12):530–534CrossRef

80.

Scherer C et al (2020) Comparative assessment of microplastics in water and sediment of a large European river. Sci Total Environ 738:139866CrossRef

81.

Mai L et al (2018) A review of methods for measuring microplastics in aquatic environments. Environ Sci Pollut Res 25(12):11319–11332CrossRef

82.

Bergmann M et al (2019) White and wonderful? Microplastics prevail in snow from the Alps to the Arctic. Sci Adv 5(8):eaax1157CrossRef

83.

Woodall LC et al (2014) The deep sea is a major sink for microplastic debris. R Soc Open Sci 1(4):140317CrossRef

84.

Witzig CS et al (2020) When good intentions go bad-false positive microplastic detection caused by disposable gloves. Environ Sci Technol 54(19):12164–12172CrossRef

85.

Klöckner P et al (2019) Tire and road wear particles in road environment – quantification and assessment of particle dynamics by Zn determination after density separation. Chemosphere 222:714–721CrossRef

86.

Primpke S et al (2020) EXPRESS: critical assessment of analytical methods for the harmonized and cost efficient analysis of microplastics. Appl Spectrosc:0003702820921465

Title: Analytical Methods for Plastic (Microplastic) Determination in Environmental Samples
Authors: G. Dierkes
T. Lauschke
C. Földi
Publisher: Springer International Publishing
Book: Plastics in the Aquatic Environment - Part I
Print ISBN: 978-3-030-84117-1

Electronic ISBN: 978-3-030-84118-8

Copyright Year: 2022
DOI: https://doi.org/10.1007/698_2021_744