Journal of Natural Resources and Environmental Management 11(4): 677-684. http://dx.doi.org/10.29244/jpsl.11.4.677-684 E-ISSN: 2460-5824 http://journal.ipb.ac.id/index.php/jpsl Production of bioplastics from organic waste with tapioca flour and glycerol Sri Widyastuti, Rhenny Ratnawati, Nurmasyta Sylviana Priyono Department of Environmental Engineering, Engineering Faculty, Universitas PGRI Adi Buana, Dukuh Menanggal XII Surabaya, 60234, Indonesia [+62 31-8281181] Article Info: Received: 06 - 10 - 2021 Accepted: 18 - 11 - 2021 Keywords: Bioplastics, glycerol, banana peel waste, rice waste, tapioca flour Corresponding Author: Rhenny Ratnawati Program Studi Teknik Lingkungan, Fakultas Teknik, Universitas PGRI Adi Buana Surabaya; Tel. +628563030395 Email: ratnawati@unipasby.ac.id Abstract. Bioplastic is plastic that can be decomposed because it can return to nature. This study investigates the optimal composition for the production of bioplastics with various compositions of raw material. In this study, two types of organic waste (banana peel and rice waste), tapioca flour, and glycerol, were used in different proportions for the production of bioplastics. Comparison of the composition of banana peel:tapioca flour:glycerol, respectively 1:10:7.5 (sample A) and 1:13:11.25 (sample B). The ratio of the composition of rice waste:tapioca flour:glycerol in sample C and D is 1:10:7.5 and 1:13:11.25, respectively. Bioplastics are processed using a composite of banana peel or rice waste which is dried to a moisture content of 70%. 30 mL of distilled water was added to the bioplastic and heated until thickened. The bioplastic is molded in a baking sheet while still hot and in an oven at 117˚C, then cooled at room temperature. The optimal composition of bioplastic is found in sample B with a biodegradation test value of 58%, and it contains bioplastics with functional groups O-H, C-H, C=O, C=C, C-O, and =C-H in the FTIR test results. The quality standard values for the tensile strength test and elongation test at break in sample B have values of 10.9 MPa and 29%, respectively. How to cite (CSE Style 8th Edition): Widyastuti S, Ratnawati R, Priyono NS. 2021. Production of bioplastics from organic waste with tapioca flour and glycerol. JPSL 11(4): 677-684. http://dx.doi.org/10.29244/jpsl.11.4.677-684. INTRODUCTION Bioplastics are plastics that can be decomposed by the microorganisms' activity quickly (Kelibay, 2020). Bioplastics can decompose without leaving toxic residues after being used up because of their nature that can return to nature. Production of bioplastics with high starch and tensile strength is a requirement in the manufacture of bioplastics (Kelibay, 2020). Inggaweni and Suyatno (2015) stated that high starch accelerates bioplastic's biodegradation because starch is a food source for microorganisms. Banana peel has a reasonably high starch value 59% (Melani et al., 2019). Widyaningsih et al. (2012) stated that banana peels contain 0.98% starch, 91.50% organic matter and affect tensile strength. Utami and Widiarti (2014) reported an addition of banana peel affected the tensile strength and elongation at break. Production of bioplastics using banana peel has been successfully investigated by Utami and Widiarti (2014), Munawaroh (2015), Agustin and Padmawijaya (2016), Melani et al. (2019). Rice waste obtained from leftover rice that has been consumed and is not suitable for consumption also has a reasonably high starch. Bahari and Cahyonugroho (2018) reported bioplastic production using rice waste makes the plastic easy to decompose. The results of the tensile strength and elongation at the break test are higher, the biodegradation time is more optimal. Bioplastic using rice waste research has also been carried out by Aini et al. (2015), Marichelvam et al. (2019) and Harimbi and Satria (2020). 677 Widyastuti S, Ratnawati R, Priyono NS The use of starch in the production of bioplastics can improve its biodegradable properties. On the other hand, the complex and robust properties that occur in bioplastics are due to the amount of starch that is too much. The high amount of solids also create cross-links between starch polymers which are tightly formed so that even greater forces are needed to suppress the bioplastic process (Suryanto et al., 2016). Tapioca flour is pure starch obtained by extraction from cassava milling, the amylopectin content will provide optimal stickiness (Azieyanti et al., 2019). Kumoro and Purbasari (2014) have successfully carried out bioplastics made from tapioca flour and aking rice (Haryanto and Saputri (2016); Haryanto and Titani (2017); Karim and Musta (2019). Starch as a primary material for bioplastics still has shortcomings, so additives are needed to improve its properties. A plasticizer is an additional material that serves to increase the elasticity properties. Research conducted by Suryanto et al. (2016) and Kelibay (2020) succeeded in the production of bioplastics addition glycerol. Kelibay (2020) states that glycerol is needed as a plasticizer that functions to increase the elasticity of bioplastics. Coniwanti et al. (2014) reported that glycerol could increase plastic films' flexibility and solubility, thereby increasing the biodegradability of starch-based plastic films. Suryanto et al. (2016) explained that glycerol has an essential role in manufacturing bioplastics because glycerol can reduce the hardness of bioplastics caused by too much tapioca flour content. Making bioplastics by utilizing waste banana peels and rice into more practical and environmentally friendly products supports the reduction of conventional plastic waste. This study aims to examine the optimal composition for the manufacture of bioplastics with various compositions of raw material for a banana peel or rice waste. MATERIALS AND METHODS This study was conducted at Solid Waste Laboratory, Department of Environmental Engineering, Engineering Faculty, Universitas PGRI Adi Buana Surabaya from February until August 2021. Banana Peels and Rice Waste Two types of organic waste for bioplastic production are banana peels and rice waste from household waste in Sidoarjo District, East Java Province, Indonesia. Eight experimental conditions were tested in duplicate using laboratory-scale reactors. The experimental design comprised two types of organic waste (banana peels and rice waste) and addition (tapioca flour and glycerol). Detailed experiment condition is given in Table 1. The experimental procedures were preparing banana peels and rice waste by mixing up with tapioca flour and glycerol. The banana peels and rice waste were air-dried for two days in the laboratory at room temperature before being used. The moisture content of banana peels and rice waste of 60-70%. Banana peels waste and rice waste are mashed and filtered through a sieve measuring 80 mesh particles. Sample Code A (1 BP:10 TF:7.5 G) B (1 BP:13 TF:11.25 G) C (1 RW:10 TF:7.5 G) D (1 RW:13 TF:11.25 G) Tabel 1 Experiment condition Raw Material Composition (weight, gram) Banana Peel Waste Rice Waste Tapioca Flour (TF) Glycerol (G) (BP) (RW) 1 10 7.50 1 13 11.25 1 10 7.50 1 13 11.25 Production of Bioplastics The production of bioplastics: 1 gram of banana peels and rice waste was placed in a beaker and weighted. Add tapioca flour (10 gram and 13 gram) and glycerol (7.5 gram and 11.25 gram) according to the variation. Add 30 mL of aqua dest in each variation of the composition, mix all the materials, and then put in hotplate 678 Jurnal Pengelolaan Sumber Daya Alam dan Lingkungan 11(4): 677-684 magnetic stirrer. The boiling took about 20 minutes and was observed by using a stopwatch. The mixture then was stretched and pressed on over paper and was dried in the oven at a temperature of 120oC. The mixture is then allowed to cool. Bioplastics Analysis The bioplastics analysis are tensile strength, elongation at break, biodegradability, and Fourier Transform Infra-Red Spectrophotometry (FTIR) according to ASTM or can be tested in laboratories that have implemented ISO/IEC 17025 (ASTM D882-12, 2002). The bioplastics product compared with bioplastics quality standards according to SNI 7188.7:2016 (Table 2). Tensile strength and elongation at break are physical reactions of bioplastics. The tensile test was done to carry out with the test object drawn from two directions so that the diameter shrinks and length increases. The amount of load and size increased during the test. Tensile strength is the maximum load accepted by the material ((Sofiah et al., 2019). Percent lengths can be calculated by comparing the film's size at break and the film's size before being pulled by the elongation at break. Tensile strength and elongation at break can be calculated using equations (1) and (2), respectively. Tensil Strength (MPa) = Elongation (%) = Load of break (Original width)(original thickness) (The final length of the test object−the initial length of the test object) x 100% The initial length of the test object (1) (2) The biodegradation by utilizing microorganisms to determine biological reactions. Biodegradation test by preparing a 2 cm x 6 cm sample and weighing. The sample is buried for one week, then dried and weighed. The biodegradation test can be calculated using equation (3). FTIR analysis uses infrared wavelengths to determine chemical compounds or functional groups in bioplastics (Suryati et al., 2017). Weight residual (%) = (The initial weight before biodegradation test−the final weight after biodegradation test) x 100% The initial weight before biodegradation test (3) Table 2 Bioplastics standard No. 1. 2. 3. Parameter Tensile strength Elongation at break Biodegradation Quality Standards* Minimum of 13.7 Mpa (139.74 N/mm²) Maximum of 5% Minimum 60% * Indonesia National Standards SNI 7188.7:2016 about product category easy plastic and bioplastic shopping bags decompose RESULTS AND DISCUSSION Tensile Strength Value The tensile strength of bioplastics in all treatments are shown in Figure 1 and Figure 2. Figure 1 shows that the addition of tapioca flour and glycerol give different tensile strengths in bioplastics. The tensile strength value using banana peel in samples A and B were 6.31 MPa and 10.9 MPa, respectively. In rice waste, samples C and D have tensile strength with a value was 5.57 MPa and 7.79 MPa, respectively. Tensile strength value tended that the sample using more addition tapioca flour and glycerol (13 gram and 11.25 gram) in samples B and D were higher than samples A and C using tapioca flour and glycerol (10 gram and 7.50 gram). Inggaweni and Suyatno (2015) reported bioplastic production from composites High Density Polyethylene (HDPE) and cassava peel starch have tensile strength of 19.44 MPa. Wattimena et al. (2016) stated addition glycerol also effects on the tensile strength of bioplastics. Kumoro and Purbasari (2014) 679 Widyastuti S, Ratnawati R, Priyono NS Tensile Strength value (MPa) reported bioplastic production using addition glycerol 15% has a tensile strength value of 20.65 MPa. Tensile strength in all treatments did not meet the bioplastic quality standard (SNI 7188.7:2016), where the tensile strength value should be a minimum of 13.7 MPa. Sample B is closest to the minimum bioplastic quality standard. 12 10 8 6 4 2 0 A B C D Sample Figure 1 Tensile strength of bioplastic product Elongation at Break Value Elongation at break value (%) Elongation at a break in all treatments showed different values (Figure 2). Sample A and B using banana peel have elongation at break was 33% and 29%, respectively. Sample C and D using rice waste have an elongation at break were 33% and 60%, respectively Sinaga et al. (2014) reported that the more tapioca flour and glycerol affect elongation at break bioplastic. Inggaweni and Suyatno (2015) stated the elongation at break increased along with the increase in the amount of starch. The increased elongation at the break due to the addition of the amount of starch caused interaction between the two polymers (Layuk et al., 2019). Elongation at a break in all treatments did not meet the bioplastic quality standard (SNI 7188.7:2016), where the elongation at break value should be maximum of 5%. 70 60 50 40 30 20 10 0 A B C D Sample Figure 2 Elongation at break of bioplastic Biodegradation Value Biodegradation value in all treatments is shown in Figure 3. Figure 3 shows that biodegradation values in all treatments have varying values with a range of 58-87%. The biodegradation value from the banana peel in samples A and B were 67% and 87%, respectively. Samples C and D containing rice waste have 58% and 79% biodegradation values, respectively. Both biodegradation values in samples B and D using tapioca flour and glycerol were 13 grams and 11.25 grams have higher biodegradation values than samples A and C. It means 680 Jurnal Pengelolaan Sumber Daya Alam dan Lingkungan 11(4): 677-684 Biodegaradation value (%) that the ability to absorb water is more elevated and optimal microbial work process so that degraded quickly of bioplastic (Sofiah et al., 2019). Haryanto and Saputri (2016) stated that the most essential property of bioplastics was decomposition. Melani et al. (2019) reported biodegradation value of bioplastic from the banana peel with a range of 46.00-59.40% in 8 days. Haryanto and Saputri (2016) reported the highest biodegradation using soil media in 2 days with a value of 50%. Biodegradation values in samples A, B, and D met the bioplastic quality standard (SNI 7188.7:2016), where the biodegradation value should be minimum of 60%. 100 80 60 40 20 0 A B C D Sample Figure 3 Biodegradation of bioplastic product FTIR Value FTIR value in all treatment shown obtained 11 kinds of compounds that had various peak values (Figure 4, 5, 6, and 7), containing dextrose monohydrate powder, where this compound is a white powder containing starch. Hydroxypropyl-beta-cyclodextrin is a compound that is difficult to dissolve in water. While the peak values for bioplastics in all treatments are about 400, which means that bioplastic products in all treatments are easily soluble in water because they have a higher value than the bioplastic quality standard. In addition to containing these two compounds, the bioplastic also contained allyl alcohol, 2-butene-1.4 diol, glucose, methyl-13c alcohol, propargyl alcohol, somaltose approx 99%, alpha-cyclodextrin hydrate, maltrotriose hydrate, and gamma-cyclodextrin hydrate. The functional group O-H, C-H, C=O, C=C, C-O, and =C-H in all treatments indicate the formation of banana peel and rice waste bioplastics has already occurred, which was confirmed by FTIR spectroscopy. No indication of heavy metal, Cd<0.5 ppm, Pb<50 ppm, Hg<0.5 ppm, Cr⁶⁺<50 ppm, and did not contain azo dyes. Kumoro and Purbasari (2014) reported production of bioplastic from tapioca flour and rice flour resulted in FTIR showing the presence of an amide I group (a protein containing C=O bonds) and a spectral energy band with a position of cm⁻¹ is a marker of the existence of amide III groups found at 1 200 and 1 350 cm⁻¹. Zaroh and Widyastuti (2019) reported bioplastic production from tapioca pulp to have FTIR results with functional O-H, C-H, C=O, C=C, C-O, and = C-H, it means that bioplastic can be graded because bioplastic material with 30% chitosan and temperature value of 95˚C. Bioplastic Product from Banana Peels and Rice Waste Production of bioplastics from banana peels and rice waste are shown in Figures 8, 9, 10, and 11. The bioplastic in samples A and B have a plastic thickness of ± 0,04 mm, brown in color, had was slightly sticky, easy to fold, and not easy to tear. The bioplastic in samples C and D have a plastic thickness of ± 0.07 mm, slightly cloudy white, has a very rubbery, sticky texture, is easy to fold, and is easily torn. Production of bioplastics from banana peels and rice waste can be alternative to existing conventional plastics, especially packaging applications. 681 Widyastuti S, Ratnawati R, Priyono NS 1078.39 1019.92 20 10 -0 4000 3500 3000 2500 2000 1500 20 10 4000 500 3500 3000 2500 Wed May 05 13:03:21 2021 (GMT+07:00) FIND PEAKS: Spectrum: Sampel A Region: 4000.00 400.00 Absolute threshold: 99.675 Sensitivity: 50 Peak list: Position: 408.65 Intensity: Position: 421.79 Intensity: Position: 848.82 Intensity: Position: 923.50 Intensity: Position: 1019.92 Intensity: Position: 1078.39 Intensity: Position: 1150.30 Intensity: Position: 1231.42 Intensity: Position: 1647.17 Intensity: Position: 2930.89 Intensity: Position: 3284.55 Intensity: Region: Search type: Hit List: Index 1079 1078 122 1141 30.323 31.034 59.778 57.389 23.598 51.973 62.410 74.225 79.892 80.428 62.052 774 820 245 1126 320 5835 Spectrum: Collection time: Wed May 05 13:05:15 2021 (GMT+07:00) Sampel A 3495.26-455.13 Correlation Match 69.70 68.42 60.95 52.17 6 51.76 50.38 50.20 50.09 49.62 49.39 Compound name Pullulan P2000 Pullulan P800 DEXTROSE MONOHYDRATE POWDER Hydroxypropyl-beta-cyclodextrin, ms = 0. Library HR Hummel Polymer and Additives HR Hummel Polymer and Additives Georgia State Crime Lab Sample Library HR Aldrich FT-IR Collection Edition II Allyl alcohol, 99% 2-Butene-1,4-diol, 95% Allyl alcohol Glucose Methyl-13C alcohol Tetramethylene sulfoxide, 96% HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II HR Nicolet Sampler Library HR Hummel Polymer and Additives HR Nicolet Sampler Library HR Aldrich FT-IR Collection Edition II Wed May 05 13:05:50 2021 (GMT+07:00) FIND PEAKS: Spectrum: Sampel B Region: 4000.00 400.00 Absolute threshold: 94.748 Sensitivity: 50 Peak list: Position: 403.37 Intensity: Position: 417.39 Intensity: Position: 848.83 Intensity: Position: 922.87 Intensity: Position: 1021.50 Intensity: Position: 1078.62 Intensity: Position: 1150.50 Intensity: Position: 1207.08 Intensity: Position: 1635.17 Intensity: Position: 2931.44 Intensity: Position: 3289.04 Intensity: Figure 4 FTIR in sample A Title: Sampel C 2000 1500 1000 500 Wavenumbers (cm-1) Wavenumbers (cm-1) Spectrum: Collection time: Wed May 05 13:02:15 2021 (GMT+07:00) 848.83 40 -0 1000 922.87 50 30 421.79 408.65 30 60 417.39 403.37 40 70 1078.62 1021.50 848.82 50 923.50 1231.42 1150.30 1647.17 3284.55 60 1207.08 1150.50 80 1635.17 90 80 Wed May 05 13:06:04 2021 (GMT+07:00) 2931.44 90 %Transmittance 100 2930.89 110 100 70 %Transmittance Title: Sampel B Wed May 05 13:03:35 2021 (GMT+07:00) 110 3289.04 Title: Sampel A 29.475 28.897 59.108 57.222 23.082 51.529 63.429 73.371 80.636 78.688 59.453 Region: Search type: Hit List: Index 1079 1078 122 1141 820 774 15480 245 1213 5835 Sampel B 3495.26-455.13 Correlation Match 69.43 67.93 60.92 53.94 6 53.42 53.40 51.84 51.63 51.47 51.22 Compound name Pullulan P2000 Pullulan P800 DEXTROSE MONOHYDRATE POWDER Hydroxypropyl-beta-cyclodextrin, ms = 0. Library HR Hummel Polymer and Additives HR Hummel Polymer and Additives Georgia State Crime Lab Sample Library HR Aldrich FT-IR Collection Edition II 2-Butene-1,4-diol, 95% Allyl alcohol, 99% Propargyl alcohol, 99% Allyl alcohol Propargyl alcohol; 2-Propyn-1-ol Tetramethylene sulfoxide, 96% HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II HR Nicolet Sampler Library HR Hummel Polymer and Additives HR Aldrich FT-IR Collection Edition II Figure 5 FTIR in sample B Wed May 05 13:00:39 2021 (GMT+07:00) Title: Sampel D 110 Wed May 05 12:57:45 2021 (GMT+07:00) 110 100 100 90 0 3000 2500 2000 1500 1000 Spectrum: Collection time: Wed May 05 12:59:54 2021 (GMT+07:00) Wed May 05 13:00:24 2021 (GMT+07:00) FIND PEAKS: Spectrum: Sampel C Region: 4000.00 400.00 Absolute threshold: 97.944 Sensitivity: 50 Peak list: Position: 419.30 Intensity: 28.810 Position: 848.84 Intensity: 54.420 Position: 923.19 Intensity: 51.794 Position: 1020.24 Intensity: 20.558 Position: 1078.62 Intensity: 45.410 Position: 1151.00 Intensity: 55.533 Position: 1237.11 Intensity: 68.109 Position: 1681.63 Intensity: 74.593 Position: 2932.21 Intensity: 74.598 Position: 3279.40 Intensity: 54.430 Region: Search type: Hit List: Index 1079 1078 122 1141 774 245 820 1126 91 1137 30 0 4000 3500 3000 2500 2000 1500 1000 500 Wavenumbers (cm-1) Spectrum: Collection time: Wed May 05 12:53:03 2021 (GMT+07:00) Compound name Pullulan P2000 Pullulan P800 DEXTROSE MONOHYDRATE POWDER Hydroxypropyl-beta-cyclodextrin, ms = 0. Library HR Hummel Polymer and Additives HR Hummel Polymer and Additives Georgia State Crime Lab Sample Library HR Aldrich FT-IR Collection Edition II Allyl alcohol, 99% Allyl alcohol 2-Butene-1,4-diol, 95% Glucose ISOMALTOSE APPROX 99% Hydroxyethyl-beta-cyclodextrin, ms = 1 HR Aldrich FT-IR Collection Edition II HR Nicolet Sampler Library HR Aldrich FT-IR Collection Edition II HR Hummel Polymer and Additives Sigma Biological Sample Library HR Aldrich FT-IR Collection Edition II Wed May 05 12:57:31 2021 (GMT+07:00) FIND PEAKS: Spectrum: Sampel D Region: 4000.00 400.00 Absolute threshold: 92.006 Sensitivity: 50 Peak list: Position: 433.29 Intensity: 54.471 Position: 572.06 Intensity: 52.820 Position: 717.06 Intensity: 55.200 Position: 849.01 Intensity: 73.007 Position: 925.47 Intensity: 71.103 Position: 1024.02 Intensity: 33.122 Position: 1079.04 Intensity: 57.106 Position: 1151.30 Intensity: 69.427 Position: 1464.02 Intensity: 75.868 Position: 1654.03 Intensity: 91.651 Position: 2848.43 Intensity: 66.222 Position: 2915.63 Intensity: 61.487 Position: 3284.69 Intensity: 58.382 Region: Search type: Hit List: Index 1079 1078 91 1133 1141 1125 1130 122 1146 1103 Sampel D 3495.26-455.13 Correlation Match 70.67 69.85 62.01 60.80 59.10 6 58.32 56.89 56.06 56.06 54.97 Compound name Pullulan P2000 Pullulan P800 ISOMALTOSE APPROX 99% alpha-Cyclodextrin hydrate Hydroxypropyl-beta-cyclodextrin, ms = 0. Library HR Hummel Polymer and Additives HR Hummel Polymer and Additives Sigma Biological Sample Library HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II Maltotriose hydrate, 95% Maltopentaose hydrate DEXTROSE MONOHYDRATE POWDER gamma-Cyclodextrin hydrate L-Glucose, 98%, mixture of anomers HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II Georgia State Crime Lab Sample Library HR Aldrich FT-IR Collection Edition II HR Aldrich FT-IR Collection Edition II Figure 6 FTIR in sample C Figure 7 FTIR in sample D Figure 8 Bioplastic product in sample A Figure 9 Bioplastic product in sample B. 433.29 572.06 40 500 Sampel C 3495.26-455.13 Correlation Match 73.31 72.26 62.84 56.23 6 52.61 51.48 50.94 50.43 49.43 48.29 849.01 717.06 1151.30 1464.02 2915.63 2848.43 3284.69 %Transmittance 419.30 50 10 3500 Wavenumbers (cm-1) 682 60 20 -10 4000 70 1079.04 1024.02 10 923.19 20 848.84 1151.00 1237.11 30 1078.62 40 1020.24 50 80 1681.63 2932.21 60 3279.40 %Transmittance 70 925.47 1654.03 90 80 Jurnal Pengelolaan Sumber Daya Alam dan Lingkungan 11(4): 677-684 Figure 10 Bioplastic product in sample C Figure 11 Bioplastic product in sample D CONCLUSION The optimum composition production of bioplastics occurred in sample B with banana peels:tapioca flour:glycerol was 1:13:11.25 (weight). Tensile strength and elongation at break of bioplastics were 10.9 MPa and 29%, respectively. The biodegradation value was 58%. Bioplastic content with functional group O-H, CH, C=O, C=C, C-O, and =C-H on FTIR test. Biodegradation value met the requirement of bioplastics quality according to Indonesia National Standards No. 7188.7:2016. Both parameters of tensile strength and elongation at the break did not meet the requirement of bioplastics quality. ACKNOWLEDGEMENT The authors gratefully acknowledge the Research and Public Service of the Universitas PGRI Adi Buana for the Adi Buana Research Grant, contract No. 104.1/LPPM/VII/2021. We also thank Ms. Annisa Rifka Alifia for her assistance in the writing process of the manuscript. REFERENCES [ASTM D 882-02] American Standard Testing and Material International. 2002. Standard Test Method for Tensile Properties of Thin Plastic Sheeting [Internet]. [downloaded 2021 Jun 14]. Available at: https://doi.org/10.1520/D0882-12.2. 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