projek penilaian dan pengesahan produk...bab 1 muka surat sekapur sirih 4 pengenalan 5 1.1 sejarah...
TRANSCRIPT
PROJEK PENILAIAN DAN PENGESAHAN PRODUK BERKAITAN INISIATIF BIOROSOT DAN BIOKOMPOS
JOHOR (BBJ)
MODUL PEMBELAJARAN PENGESAHAN PRODUK
BIOPLASTIK
Perbadanan Bioteknologi dan Biodiversiti Negeri Johor
Tingkat 2, Bio-XCell Malaysia
No.2, Jalan Bioteknologi 1,
Kawasan Perindustrian SiLC
79200 Iskandar Puteri,
Johor Darul Takzim
Tel: 07-532 8810
Fax: 07-532 8811
Laman web: www.jbiotech.gov.my
©Perbadanan Bioteknologi dan Biodiversiti Negeri Johor
Terbitan Pertama 2019
Hak cipta terpelihara. Setiap bahagian daripada terbitan ini tidak boleh diterbitkan
semula, disimpan untuk pengeluaran atau dipindahkan kepada bentuk lain, sama ada
dengan cara elektronik, mekanik, gambar, rakaman dan sebagainya tanpa izin pemilik
hak cipta terlebih dahulu.
Perpustakaan Negara Malaysia Data Pengkatalogan-dalam-Penerbitan
Projek Penilaian dan Pengesahan Produk Berkaitan Inisiatif Biorosot dan Biokompos
Johor (BBJ)
Modul Pembelajaran Pengesahan Produk Bioplastik
Mengandungi indeks
ISBN 978-983-44342-3-6
Dicetak oleh
Azuarina Creative Sdn Bhd
No 61, 63 & 65, Jalan Pulai 23, Taman Pulai Utama,
81300 Skudai, Johor Darul Takzim
Tel: 07-520 4185 Fax: 07-520 4186
E-mail: [email protected]
2
ISI KANDUNGAN
BAB 1 Muka Surat
Sekapur Sirih 4
Pengenalan 5
1.1 Sejarah terciptanya plastik 6
1.2 Plastik menjadi ancaman 9
1.3 Sinar baru untuk bioplastik 11
1.4 Pendekatan Malaysia menangani isu plastik 13
1.5 Bioplastik dan jenis-jenisnya 15
1.5.1 Kanji thermoplastic 17
1.5.2 Polylactide 18
1.5.3 Poly-3-hydroxybutyrate (PHB) 19
1.5.4 Polyamide 11 20
1.5.5 Polythylene (PE) 21
1.6 Inisiatif Biorosot dan Biokompos Negeri Johor
21
BAB 2 Rangka Kerja Penerbitan Modul Bagi Penilaian dan Pengesahan Produk Bioplastik
22
2.1 Pengenalan 22
2.2 Objektif dan Skop Kerja 23
2.3 Gerak Kerja Pembangunan Modul Pembelajaran Bagi Penilaian dan Pengesahan Produk Bioplastik
23
2.4 Garis masa Projek 25
BAB 3 Ujian Pengesahan Bagi Produk Biorosot dan Biokompos Negeri Johor
26
3.1 Latar belakang 26
3.2 Test Method – Biodegradability Testing – Ready Biodegradability
27
3.3 35
3
Test Method – Thermogravimetric Analysis
3.4 Test Method – Compostability Testing – Plant Growth Test
39
3.5 Test Method: Toxicity – Heavy Metal Testing 42
3.6 Test Method: Assessment of the Oxo-Biodegradation of Plastics
48
3.7 Test Method: Toxicity - Migration Test 57
3.8 Test Method: Halal – Porcine Testing 64
BAB 4 Makmal – Makmal Analisa Yang Menjalankan Pengesahan Produk Bioplastik di Malaysia
71
4.1 Makmal Yang Menawarkan Ujian Pengesahan Bioplastik di Malaysia
71
4.2 Cadangan ujian pengesahan bioplastik 72
Rujukan 73
Appendix I 82
4
HAJI AHMAD BIN HAJI MA’IN Ketua Pegawai Eksekutif Perbadanan Bioteknologi dan Biodiversiti Negeri Johor (J-Biotech)
Assalammualaikum Warahmatullahi Wabarakatuh dan Salam Sejahtera
Pertama sekali, saya ingin melahirkan rasa syukur ke hadrat Allah diatas
limpahan rahmat dan kurniaNya, Perbadanan Bioteknologi dan Biodiversiti Negeri
Johor (J-Biotech) telah berjaya membangunkan “Modul Pembelajaran
Pengesahan Produk Bioplastik” di bawah Projek Penilaian dan Pengesahan
Produk Berkaitan Inisiatif Biorosot dan Biokompos Johor (BBJ).
Memelihara alam sekitar melalui pendekatan sains dan teknologi adalah
merupakan salah satu aspirasi anak syarikat kerajaan negeri Johor ini. Aspirasi
ini disokong dengan mandat yang diberikan kepada J-Biotech oleh kerajaan
negeri Johor untuk menerajui Inisiatif Biorosot dan Biokompos Negeri Johor sejak
tahun 2016 lagi. Salah satu teras inisiatif lima tahun ini adalah menyebarluaskan
pengetahuan kepada pelbagai lapisan masyarakat, khususnya pemain-pemain
industri biorosot dan biokompos tentang kepentingan menggunakan produk
mesra alam dalam usaha mengurangkan kebergantungan kepada plastik
konvensional demi memulihara dan memelihara alam sekitar di negeri Johor.
Modul yang dibangunkan ini adalah bertujuan untuk memberikan panduan
ringkas kepada pemain-pemain industri berkaitan dengan ujian-ujian pengesahan
biorosot dan biokompos yang ditawarkan oleh makmal-makmal di Johor, demi
membantu pemain industri menghasilkan produk mesra alam yang lebih berkualiti
dan kompetitif.
Akhir kata, saya berharap penerbitan modul pembelajaran ini dapat mencapai
matlamat kerajaan negeri Johor untuk mendorong lebih ramai lagi pemain
industri untuk sama-sama terlibat dalam merealisasikan pelaksanaan Inisiatif
Biorosot dan Biokompos Negeri Johor. Sekaligus menjadikan Johor sebagai
peneraju dalam teknologi hijau dan teknologi mesra alam di Malaysia, amnya.
Sekian, terima kasih.
5
BAB 1
PENGENALAN
Plastik merupakan sebuah gabungan bahan polimer yang terhasil dari
sumber organik mahupun sintetik yang boleh dibentuk. Antara contoh-contoh
bahan polimer yang terhasil daripada sumber organik adalah tar, syelek,
cengkerang kura-kura, tanduk binatang,, selulosa, getah tumbuhan dan lain-
lain. Manakala jenis-jenis bahan polimer sintetik pula adalah polyethylene,
polystyrene, polypropylene, polyvinyl chloride polytetrafluoroethylene dan lain-
lain.
Perkataan plastik tercipta daripada perkataan Greek iaitu plastikos
yang bermaksud mudah untuk dibentuk. Ini merujuk kepada kebolehcairan
dan keliatan bahan tersebut sewaktu proses pembuatan bagi memudahkan
ia untuk ditekan dan direka kepada pelbagai bentuk seperti kepingan,
seratan, bentuk rata, tiub, botol, kotak dan lain-lain.
Plastik digunakan dalam banyak sektor dan aplikasi kerana
kepelbagaian sifatnya. Plastik mempunyai isipadu yang rendah, ringan dan
mudah diuruskan. Plastik banyak digunakan dalam bidang pembungkusan,
pembinaan, pengangkutan, elektronik, pertanian, kesihatan, peralatan sukan
dan lain-lain. Plastik terbahagi kepada dua jenis iaitu thermoplastic dan
thermoset. Thermoplastic adalah plastik yang boleh dicairkan dan dibentuk
semula menggunakan melalui proses pendedahan kepada haba. Thermoset
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pula adalah plastik yang apabila telah dihasilkan, ia tidak boleh dicairkan dan
dibentukkan semula kepada bentuk yang asal.
1.1 Sejarah Terciptanya Plastik
Plastik pada asalnya tercipta dari bahan organik seperti syelek dan juga gula
getah. Namun begitu, semakin pesat teknologi berkembang dan dengan
peningkatan teknologi pengubahsuaian kimia, plastik telah mengalami evolusi
sejajar dengan perkembangan teknologi terkini. Pelbagai jenis unsur plastik
telah terhasil melalui pengubahsuaian kimia iaitu seperti getah, nitroselulosa,
kolagen dan galalite. Teknologi menghasilkan plastik sintetik telah wujud
sejak 100 tahun lalu. Antara plastik sintetik yang telah terhasil pada ketika itu
adalah parkesine / seluloid, polyvinyl chloride (PVC) dan akelite (Anon, 2019).
Unsur plastik sintetik yang pertama adalah parkesina iaitu hasil kajian
daripada ahli kimia Alexander Parkes pada tahun 1856. Kemudian pada
tahun 1869, John Wesley Hyatt menghasilkan seluloid. Kajian John (1869)
bermula apabila sebuah firma di New York menawarkan ganjaran sebanyak
$10,000.00 kepada sesiapa yang dapat mencipta bahan yang boleh dijadikan
sebagai pengganti kepada gading gajah yang digunakan untuk membuat bola
biliard. Populariti permainan billiard telah memberikesan kepada bekalan
gading gajah kerana ia digunakan dalam pembuatan bola billiard sejak tahun
1627 (Bellis, 2019). Sejajar dengan peningkatan permintaan bekalan gading
gajah memberi kesan peningkatan pemburuan gajah ini yang boleh
mengakibatkan populasi gajah terancam secara langsung
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John (1869) telah menghasilkan plastik sintetik ini dengan melalui
proses merawat serat selulosa kapas (nitroselulosa) menggunakan kapur
barus. Hasil kajian mendapati kesan tindakbalas ini mempunyai unsur yang
sama dengan cengkerang kura-kura, tanduk, linen dan gading (Bellis, 2019).
Oleh kerana itu, hasil kajian John (1869) ini dilihat sebagai pencetus revolusi
kerana ia bukan sahaja membantu pembangunan industri pembuatan malah
membantu mengekalkan kesejahteraan alam sekitar. Pada ketika itu, plastik
sintetik dijadikan sebagai penyelamat kepada gajah dan kura-kura kerana ia
mengurangkan penggunaan hasil daripada haiwan-haiwan tersebut bagi
mendapatkan sumber bahan mentah (Bellis,2019).
Inovasi tersebut telah menjadi pemangkin kepada peningkatan
penghasilan pelbagai jenis plastik. Antaranya ialah pempolimeran PVC
bermula dihasilkan pada tahun 1838-1872 (Freinkel, 2011). Manakala, plastik
jenis sepenuhnya sintetik yang pertama telah dibangunkan pada tahun 1907,
iaitu Bakelite yang dihasilkan oleh Leo Baekeland (Kettering, 1946).
Komposisi plastik sepenuhnya sintetik ini tidak mempunyai sebarang unsur
dari alam semulajadi. Bakelite terhasil dari tindakbalas antara phenol dan
formaldehyde dimana asid digunakan sebagai pemangkin (ACC, 2018)
Baekeland berjaya mencipta plastik sepenuhnya sintetik ini selepas
beliau melakukan pelbagai penyelidikan untuk menggantikan syelek. Syelek
adalah bahan popular yang dijadikan sebagai penebat arus elektrik pada
waktu itu kerana ia kerap digunakan untuk bekalan tenaga elektrik ke seluruh
Amerika Syarikat. Bakelite bukan sahaja sebagai penebat elektrik yang baik,
tetapi ia juga tahan lama dan tahan haba seperti Gambar 1. Ia juga mudah
dibentuk mengikut kepada keperluan penggunaan, dan ini menjadikan ia
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pengganti yang paling sesuai bagi syelek (Kettering, 1946; Anthony Raj,
2018).
Gambar 1: Plastik bakelite
Petrol merupakan bahan peralihan bahan semulajadi untuk
menghasilkan plastik. Proses penghasilan berlaku apabila stok petrol pada
ketika itu sangat banyak dan boleh didapati dengan harga yang murah.
Sebagai contoh, Henry Ford, sebuah syarikat pengeluar kenderaan
menggunakan plastik berasaskan soya, namun begitu, kerana harga petrol
murah, syarikat ini telah beralih kepada bahan plastik berasaskan petrol untuk
komponen-komponen kenderaan keluarannya (Barrett, 2018).
Syarikat W.R. Grace juga telah menjalankan penyelidikan berkaitan
penghasilan bioplastik melalui tindakbalas mikrob, namun tidak berjaya
apabila mendapati kos untuk menghasilkan plastik dari sumber petrol adalah
lebih murah dan mudah didapati. Sejak itu penghasilan plastik berasaskan
sumber petrol ini semakin mendapat permintaan yang tinggi berbanding
bioplastik (Barrett, 2018).
Plastik semakin mendapat perhatian dalam banyak sektor pembuatan
di Amerika Syarikat ketika Perang Dunia ke-2 (Parker, 2019). Plastik banyak
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digunakan dalam pembuatan komponen-komponen peralatan perang (Beall,
2009). Sebagai contohnya, Nylon merupakan plastik yang digunakan dalam
penghasilan payung terjun, tali, perisai badan, topi keledar dan sebagainya
yang dihasilkan oleh ahli kimia Amerika iaitu Wallace Carothers (Anon,
undatedtahun). Pada ketika itu industri pembuatan plastik di Amerika Syarikat
telah meningkat sebanyak 300%. Selepas Perang Dunia ke-2, plastik kekal
mendapat perhatian dan telah digunakan dengan meluas dalam pelbagai
bidang. Plastik telah diangkat sebagai bahan yang mampu memberikan
penyelesaian kepada pelbagai masalah (Bellis, 2019; Anon, 2019). Beberapa
tahun kemudian, ahli kimia dari England, Rex Whinfield dan JamesTennat
Dickson menghasilkan polyethylene terephthalate yang mempunyai sifat yang
sama dengan Nylon dalam Perang Dunia ke-2. Namun, seorang jurutera
Amerika, Nathaniel Wyeth telah berjaya mengubah bahan ini menjadi bahan
plastik pembungkusan makanan pada tahun 1973 (Anon, undated). Beliau
juga telah mempatenkan proses penghasilan botol plastik menggunakan
bahan ini pada tahun 1977.
1.2 Plastik Menjadi Ancaman
Namun begitu, selepas beberapa tahun berlalunya Perang Dunia ke-2, plastik
mula dilihat sebagai sebuah ancaman (Beall, 2009; Parker, 2019). Ini terjadi
kerana sisa-sisa plastik menimbun dengan banyaknya di kawasan lautan dan
sungai sekitar tahun 1960-an (Parker, 2019). Keadaan ini telah
mengakibatkan pencemaran alam sekitar dan ia telah menarik perhatian
ramai aktivis yang aktif dalam melindungi dan mempertahankan alam sekitar.
10
Masalah mula timbul apabila plastik didapati sukar untuk dilupuskan dankekal
dimana ia dibuang (Anon, 2019). Masalah ini semakin teruk apabila
kesedaran mengenai kesan bahaya bahan aditif yang dilepaskan dari sisa
plastik tersebut, terutamanya daripada bisophenol-A (BPA) dan phatalates
semakin meningkat penggunaanya.
Kedua-dua bahan kimia ini dimasukkan ke dalam plastik ketika proses
pembuatan plastik (Warner & Flaws, 2018). Para saintis mendapati kedua-
dua bahan kimia tersebut mudah luntur dari plastik ke alam sekitar dan
secara tidak langsung masuk ke makanan, minuman dan badan manusia
(Teuten et al., 2009) Bahan-bahan kimia ini jugamemberikan kesan negatif
kepada sistem hormon badan manusia danmenimbulkankebimbangan
kepada orang awam (Warner & Flaws, 2018).
Sehingga ke hari ini, plastik telah menjadi ancaman kepada alam
sekitar seiring dengan perkembangan teknologi dan gaya hidup, terutamanya
di negara-negara yang mempunyai kepadatan penduduk yang tinggi seperti
Jepun (PWMI, 2014), Taiwan (Walther, 2015), United Kingdom (Howarth,
2013) dan Hong Kong (EPD, 2015). Selain itu, plastik memberi kesan yang
buruk kepada kesihatan manusia (Crinnion, 2010; Elliot et al.,1996),
pencemaran udara (Li et al., 1995), pencemaran tanah (Barnes et al., 2009),
pencemaran air (Howarth, 2013; Perkins, 2014), merosakkan rantaian
makanan (Rochman et al., 2014) dan mengancam biodiversiti (Derraik, 2002;
Gregory, 2009).
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1.3 Sinar Baru Untuk Bioplastik
Sekitar tahun 1970-an, pengusaha-pengusaha plastik telah mencadangkan
mekanisma kitar semula bagi mengurangkan kesan negatif terhadap plastik
ini. Namun cadangan ini tidak membawa sebarang penyelesaian yang
signifikan kerana peningkatan sisa plastik semakin bertambah dan tidak
pernah berkurang (Bradbury, 2017). Situasi ini telah menggalakkan lebih
ramai penyelidik-penyelidik mula menjalankan kajian penyelidikan bioplastik
yang teknologi tinggi pernah dibangunkan sebelum ini.
Dorongan penghasilan bioplastik ini ditingkatkan lagi kerana harga dan
produksi petrol yang tidak menentu disebabkan oleh Revolusi Iran dan
Perang Iran-Iraq. Pelbagai usaha telah dijalankan bagi menggalakkan
penghasilan bioplastik ini. Sebagai contoh, sebuah syarikat bernama Imperial
Chemical Industries yang terletak di United Kingdom (UK), dan syarikat
usahasamanya iaitu Malborough Teeside Management dari Malborough
Biopolymers telah menghasilkan bioplastik dari bakteria iaitu dinamakan
sebagai Biopol. Bahan bioplastik ini boleh dihasilkan dalam bentuk filamen,
cip dan serbuk (Feder, 1985). Teknologi penghasilan Biopol ini kemudiannya
telah digunakan oleh syarikat Monsanto bagi menggantikan penghasilan
plastic daripada mikrob dan bakteria. Syarikat Monsanto ini kemudiannya
dibeli oleh syarikat Metabolix Inc (Barber and Fisher, 2001).
Pada tahun 2010, seorang penyelidik dari France bernama Remy
Lucas telah berjaya menghasilkan bioplastik yang berasaskan alga. Teknologi
ini dikategorikan sebagai mesra alam kerana pemprosesan bahan mentah
untuk pembuatan bioplastik ini daripada alga, dan tidak menggunakan baja
12
dan racun perosak. Bioplastik yang dihasilkan dari teknologi ini juga adalah
sangat berpotensi kerana boleh terurai di dalam tanah dalam tempoh 12
minggu dan boleh terurai 5 jam di dalam air (Malet, tahun).
Pada tahun 2018, sekumpulan penyelidik Universiti Teknologi
Eindhoven telah berjaya menghasilkan sebuah kereta yang keseluruhannya
diperbuat daripadabioplastik. Kereta ini diberi nama Noah mempunyai berat
360kg dengan berat baterinya adalah60kg (Barrett, 2018). Bioplastik yang
digunakan untuk menghasilkan rangka kereta ini adalah berasaskan daripada
gula, manakala badannya diperbuat daripada asid poli-laktik dan kereta ini
tahan pada suhu persekitaran. Kereta ini mempunyai 2 buah enjin berkuasa
15 kilowatt dan mampu mencapai kelajuan maksimum 100 km per jam.
Kereta ini boleh dikitar semula dan ini merupakan teknologi yang sangat
berpotensi untuk mengurangkan kebergantungan kepada plastik
konvensional.
Sehingga kini, masih banyak penyelidikan dan aplikasi bioplastik
dijalankan di seluruh dunia. Kesedaran tentang pentingnya mengurangkan
penggunaan plastik konvensional semakin meningkat. Pelbagai pihak, telah
menjalankan peranan mereka untuk menggalakkan penggunaan bioplastik. Di
Malaysia, kesedaran menggunakan bioplastik juga semakin meningkat seiring
dengan penerimaan global berkaitan dengan teknologi ini. Banyak
pendekatan yang telah dilakukan oleh kerajaan Malaysia untuk meningkatkan
penerimaan penggunaan bioplastik di kalangan rakyat Malaysia itu sendiri.
13
1.4 Pendekatan Malaysia Menangani Isu Plastik
Malaysia mempunyai kesedaran untuk menangani isu sisa plastik dan
dijadikan sebagaisalah satu agenda utama negara. Malaysia dikategorikan
sebagai negara ke-8 yang menyumbang kepada isu sisa plastik global
(Balasegaram, 2018). Di Malaysia, terdapat lebih kurang 1,300 pengeluar
plastik dan pada tahun 2010, Malaysia telah menghasilkan hampir 1 juta sisa
plastik yang tidak diuruskan (Balasegaram, 2018). Sisa plastik ini dibiarkan
tidak terurus di tapak pelupusan sampah, kemudian masuk ke dalam sungai
dan laut. Sisa plastik sintetik ini adalah amat sukar untuk diuraikan.
Proses penguraian plastik mengambil masa sehingga ratusan
mahupun ribuan tahun dan ia menjadi masalah yang amat membimbangkan.
Jika ia dibiarkan berterusan, sisa plastik ini akan menimbun dan membentuk
seperti pulau sisa plastik yang dijumpai di Lautan Pasifik yang diberi nama
sebagai The Great Pacific Garbage Patch (Parker, 2018). Sisa plastik yang
terurai ini akan dimakan oleh haiwan marin yang akhirnya akan menjadi salah
satu komponen rantaian makanan kita. Tidak mustahil dalam tahun-tahun
yang mendatang, bilangan sisa plastik akan lebih meningkat (Kaplan, 2016).
Melihat kepada keburukan yang dibawa oleh plastik konvensional /
sintetik, Malaysia juga telah mula menggalakkan penggunaan bahan-bahan
alternatif sintetik plastik iaitu produk biorosot dan biokompos. Di peringkat
Kerajaan Persekutuan, Kementerian Tenaga, Sains, Teknologi, Alam Sekitar
Dan Perubahan Cuaca (MESTECC) telah melancarkan sebuah pelan halatuju
yang dipanggil “Roadmap Towards Zero Single-Use Plastics 2018-2030” bagi
menangani masalah isu sisa plastik. Pelan halatuju ini mempunyai tiga (3)
14
fasa. Fasa pertama adalah dari tahun 2018 sehingga 2021, fasa kedua
adalah dari tahun 2022 sehingga 2025, fasa ketiga dari tahun 2026 sehingga
2030 (Lee, 2019).
Fasa pertama adalah bertujuan untuk membangunkan pelan halatuju
ini, selain memberikan kesedaran kepada masyarakat tentang bahayanya
menggunakan single-use plastics dan mendapatkan kerjasama daripada
pelbagai pemegangtaruh terutamanya pihak-pihak berkuasa tempatan (PBT).
Dalam fasa ini juga, perlaksanaan bagi mengurangkan penggunaan single-
use plastic juga akan dilaksanakan. Sebagai permulaan, penggunaan
penyedut makanan di premis-premis makanan akan dikurangkan. Penyedut
makanan hanya akan diberikan apabila diminta oleh pelanggan tanpa
sebarang caj (MESTECC, 2018).
Fasa kedua pula melibatkan sasaran produk yang lebih luas untuk
penggunaan produk biorosot dan biokompos ini seperti pembungkus
makanan (food packaging), filem plastik, perkakas dapur, kotak penyimpan
makanan, kapas pengorek telinga, beg poli dan slow-release fertilizers. Dana
penyelidikan bagi melahirkan lebih banyak teknologi bioplastik yang lebih baik
juga akan dipertingkatkan dalam fasa ini (MESTECC, 2018).
Fasa ketiga atau fasa akhir adalah untuk memastikan jumlah
pengeluaran produk biorosot dan biokompos adalah tinggi selari dengan
peningkatan jumlah permintaannya. Selain itu, sasaran produk akan
diperluaskan kepada peranti perubatan, lampin dan lain-lain produk yang
menggunakan single-use plastics. Laporan akhir perlaksanaan biorosot dan
biokompos juga akan diterbitkan dalam fasa ini (MESTECC, 2018).
15
Walau bagaimanapun, pelaksanaan inisiatif ini adalah tertakluk kepada
undang-undang negeri masing-masing, walaupun pada peringkat kerajaan
Persekutuan pun telah ada inisiatif bagi menangani isu sisa plastik ini.
Sebagai contoh pihak berkuasa tempatan di wilayah-wilayah Persekutuan
dan negeri Melaka, telahpun menetapkan bahawa hanya produk biorosot dan
biokompos sahaja yang boleh digunakan di wilayah ini (Murali, 2015; Barrett,
2019). Johor juga telah melancarkan sebuah pelan yang dipanggil Pelan
Inisiatif Biorosot dan Biokompos Negeri Johor (Anon, 2016).
Antara usaha lain yang dapat dilihat adalah melalui penerimaan
Malaysia terhadap pelabur-pelabur dari luar negara yang telah lama
berkecimpung dalam industri bioplastik ini. Salah satu pelabur tersebut adalah
GlycosBio Malaysia Sdn. Bhd. Syarikat ini yang dicadangkan untuk dibina di
Johor, mempunyai platform penapaian bakteria yang mampu untuk
mengubahsuai pelbagai bahan semulajadi termasuklah gliserin dan sisa sawit
kepada bahan biokimia yang bernilai tinggi seperti monomer isoprene sintetik
(Bio-SIM) (Gibson, tahun). Negara luar memandang Malaysia sebagai sebuah
negara yang mempunyai banyak sumber alam semulajadi dan ini adalah
sangat bertepatan dengan strategi mereka bagi mendapatkan bahan mentah
untuk perusahaan bioplastik mereka.
1.5 Bioplastik dan Jenis-Jenisnya
Bioplastik adalah berasal dari perkataan Inggeris iaitu bioplastic.
Perkataan bioplastic ini adalah ringkasan dari biodegradable plastic yang
bermaksud sebagai plastik mudah urai. Bioplastik tidak seperti plastik
16
konvensional yang diperbuat dari bahan petroleum. Bioplastik adalah
dihasilkan daripada biomas (sisa-sisa) yang didapati dari bahan-bahan
semulajadi mesra alam yang boleh diperbaharui (Fridovich-Keil, 2018).
American Society of Testing and Materials (ASTM) menyatakan bahawa
bioplastik adalah plastik yang boleh diubahkan kepada biomas, air, karbon
dioksida, dan/atau methane melalui tindakbalas dari mikroorganisma
semulajadi seperti bakteria dan fungi, dalam jangkamasa dan keadaan
persekitaran yang bersesuaian (Hansen, 2019).
Definisi ini menunjukkan bahawa terdapat jangkamasa spesifik untuk
biodegradasi berlaku dan terpecah kepada beberapa cebisan. Definisi ini
adalah berbeza dengan definisi degradasi yang mana ia merupakan terma
yang lebih luas yang diberikan kepada polimer atau plastik yang boleh
dipecahkan dengan beberapa cara seperti disintegrasi fizikal dan kimia, dan
biodegradasi semulajadi. Selepas degradasi, plastik masih lagi boleh dijumpai
tapi dalam bentuk yang lebih ringkas dan cebisan.
Terma yang biasa dikaitkan dengan bioplastik adalah compostable.
ASTM menyatakan bahawa compostable dimaksudkan sebagai “plastik yang
melalui degradasi biologikal ketika proses composting (proses semulajadi
yang menukarkan sisa kepada aditif tanah yang kaya dengan pelbagai
nutrient) dan menghasilkan bahan-bahan seperti karbon dioksida, air,
sebatian bukan organik dan biomas pada kadar yang konsisten. Menurut
ASTM, terdapat standard yang spesifik untuk sejenis plastik dikategorikan
sebagai compostable iaitu ia perlu melalui proses biodegradasi, eko-toksik,
dan disintegrasi (penghancuran). Perbezaan antara plastik compostable
dengan bioplastik adalah terletak pada kadar tindakbalas ketiga-tiga proses
17
tadi. Ini menunjukkan bahawa semua plastik compostable adalah bioplastik
tetapi bukan semua bioplastik adalah compostable (Hansen, 2019).
Pada masa sekarang, bioplastik yang biasa digunakan adalah
diperbuat daripada selulosa (Isroi et al.,2017), kanji (Wahyuningtias &
Suryanto, 2017), glukosa (Bruder, 2019) dan minyak (Johansson, 2019).
Banyak teknik yang telah menukarkan bahan-bahan tadi kepada bioplastik
seperti kanji termoplastik (Blohm & Heinze, 2019), polylactide (PLA)
(Vatansevr et al.,2019), poly-3-hydroxybutyrate (Khattab & Dahman,2019),
polyamide 11 (Jariyavidyanont et al.,2019) dan biopolythylene (Brito et al.,
2011).
1.5.1 Kanji thermoplastik
Kini, kanji termoplastik merupakan penyumbang terbesar kepada
pasaran bioplastik dunia, di mana ia meliputi sekitar 50% sehingga 80%
daripada pasaran tersebut. Penghasilan bioplastik ini melibatkan proses
pemplastik (plasticizer) dan juga penstabil seperti sorbitol dan gliserin. Bagi
bioplastik jenis ini, ia terdiri daripada dua komponen utama iaitu kanji
thermoplastik itu sendiri dan juga polimer boleh urai semulajadi dan bersifat
kalis air seperti polyester, polyesteramids, polyesterurethanes dan
polyvinylalcohols. Proses yang terlibat dalam mencampurkan komponen-
komponen ini adalah dinamakan proses pencairan. Sewaktu proses
pencairan dilakukan, bahan yang mudah larut dalam air seperti kanji dan
bahan tidak larut air seperti plastik, digaul bersama untuk menghasilkan
plastik kanji kalis air (Jeffrey, 2013).
18
Plastik jenis ini banyak digunakan sebagai beg, bekas makanan, pasu,
peralatan dapur, cerek dan kadbod. Sumber kanji untuk menghasilkan
bioplastik ini berasal dari kentang dan jagung(Nafchi et al., 2013; Khan et
al.,2016; Altayan et al.,2019).
1.5.2 Polylactide
Polylactide merupakan salah satu bioplastik yang mempunyai potensi
yang bagus kerana mempunyai sifat yang sama dengan plastik konvensional
yang diperbuat dari sumber petroleum. Bioplastik ini mudah diproses kerana
proses pembuatannya adalah sama dengan proses pembuatan plastik
konvensional. Ini sebenarnya akan memudahkan pengusaha-pengusaha
plastik konvensional untuk beralih kepada menghasilkan plastik jenis ini
kerana mereka boleh menggunakan peralatan / mesin yang sama dengan
peralatan yang mereka gunakan untuk hasilkan plastik konvensional
(Anon,2010).
Bioplastik ini dihasilkan daripada kanji melalui proses penapaian
bersumberkan dari jagung (Royte, 2006), gandum (Heath, 2007) dan tebu.
Proses penapaian bahan-bahan organik tersebut menghasilkan asid laktik
(Gotro, 2012) yang kemudiannya melalui pelbagai proses pempolimeran dan
akhirnya menghasilkan plastik polylactide. Bioplastik jenis ini biasa
digunakan dalam penghasilan komponen komputer, peranti perubatan boleh
urai, tin, cawan, botol dan juga pembungkusan (Anon,2010).
Bioplastik ini juga digunakan dengan meluas dalam bidang
perubatan.Ia digunakan sebagai bahan dalam pembuatan komponen peranti
19
perubatan seperti skru, plat, dan implan kerana sifatnya yang mudah urai dan
boleh diserap oleh badan. Sebagai contoh, PLA sangat versatil kerana
sifatnya boleh berubah dengan mengubah komposisi bahannya
(Anon,2010).Kelemahan PLA adalah ia mempunyai takat kecairan yang
rendah iaitu 60°C, menjadikan ia tidak sesuai untuk digunakan sebagai
pembungkus makanan dan minuman panas. Walau bagaimanapun, sifat ini
boleh diperbaiki dengan memasukkan bahan tahan panas ke dalam adunan
plastik ini (Rogers, 2015).
Kelemahan lain PLA mungkin terletak pada proses pembuatannya
yang mempunyai elemen penapaian kanji untuk penghasilan asid laktik. Kos
untuk menghasilkan asid laktik tersebut boleh menelan sehingga € 1,300.00 /
tanberbanding dengan proses pengestrakan kanji dari bahan organik iaitu
€1,000.00 / tan (Anon,2010).
1.5.3 Poly-3-hydroxybutyrate (PHB)
Bioplastik ini dihasilkan dengan kehadiran bakteria yang
mempercepatkan proses glukosa dan kanji. Ia juga mempunyai sifat yang
lebih kurang sama dengan plastik polypropylene konvensional (Berwig et
al.,2016). PHB mempunyai takat lebur yang tinggi iaitu 175°C dan ia selalu
digunakan dalam pembuatan gam dan juga pembuatan getah mampat
(Mukopadhyay, 2010).
20
1.5.4 Polyamide 11
Polyamide 11 ada sejenis biopolimer yang diperbuat dari minyak
kacang kastor (Martino et al., 2014). Walaupun biopolimer ini diperbuat
daripada minyak organik, namun ia tidak boleh diuraikan. Ia banyak
digunakan dalam sektor yang memerlukan ketahanan yang tinggi seperti tiub
brek angin pneumatik, kasut sukan, peralatan elektrik dan pelbagai jenis salur
(catherers). Kekuatan dan kekurangan Polyamide 11 adalah seperti dalam
Jadual 1.
Jadual 1: Kelebihan dan kekurangan Polyamide (Sumber)
Kekuatan Kekurangan
Mempunyai tahap penyerapan air
yang rendah berbanding jenis
polyamide yang lain.
Kos penghasilan yang paling tinggi
Mempunyai kekuatan tahan yang
tinggi, walaupun ia dibekukan pada
suhu bawah takat beku.
Mempunyai tahap kekakuan dan
ketahanan haba yang rendah
berbanding polyamide lain
Tahan kepada bahan kimia seperti
gris, minyak, solven dan sebatian
garam
Mempunyai ketahanan yang rendah
terhadap air mendidih dan sinaran UV
Tahan kepada retakan, penuaan dan
kekasaran.
Memerlukan proses pengeringan
yang lengkap sebelum diproses.
Sumber: Omnexus (undated)
21
1.5.5 Polythylene (PE)
PE secara umumnya dikenali sebagai polimer yang berasaskan fosil.
Sifatnya tidak boleh diuraikan tetapi boleh dikitar semula.
1.6 Inisiatif Biorosot dan Biokompos Negeri Johor.
Inisiatif biorosot dan biokompos negeri Johor menjadi pemacu yang akan
memangkin komitmen sediaada kerajaan bagi memastikan pertumbuhan
ekonomi Johor dan gaya hidup orang awam tidak mengabaikan kepentingan
alam sekitar (Anon, 2016).
Objektif utama inisiatif ini adalah untuk mewujudkan situasi yang boleh
mendatangkan manfaat untuk alam sekitar, komuniti dan ekonomi Johor pada
jangkamasa panjang, selain mengurangkan kebergantungan kepada
polisterina dan plastik konvensional. Inisiatif ini terbahagi kepada beberapa
Fasa. Fasa pertama inisiatif ini bermula pada 1 Januari 2018, yang mana
pada fasa ini memberi penekanan untuk memupuk kesedaran kepada
pelbagai masyarakat tentang keburukan menggunakan plastik konvensional
yang tidak boleh terurai dan kepentingan menggunakan produk biorosot dan
biokompos sebagai alternatif.
22
BAB 2
RANGKA KERJA PENERBITAN MODUL BAGI PENILAIAN DAN
PENGESAHAN PRODUK BIOPLASTIK
2.1 Pengenalan
• Melalui inisiatif Biorosot dan Biokompos Johor (BBJ), Perbadanan
Bioteknologi dan Biodiversiti Negeri Johor (J-Biotech) telah diberikan
mandat bagi melaksanakan pelan tindakan untuk mengurangkan
kebergantungan produk berasaskan polisterin dan plastik konvensional
di seluruh negeri Johor.
• Selain itu, ianya bertujuan untuk menyemai kesedaran tentang
kepentingan menggunakan produk mesra alam kepada masyarakat, J-
Biotech juga bertindak untuk mempromosikan dan menjual
pembungkus makanan BBJ dan beg bio-plastik bagi menyokong
pelaksanaan pelan tindakan tersebut.
• Sebagai memantapkan lagi pelaksanaan gerak kerja untuk
meningkatkan kesedaran awam tersebut, pembangunan modul ujian-
ujian pengesahan bioplastik yang ditawarkan oleh makmal-makmal di
Malaysia, terutamanya di Johor juga adalah perlu diketengahkan.
23
2.2 Objektif dan Skop Kerja
Mengenalpasti parameter-parameter ujian pengesahan produk
bioplastik yang ditawarkan oleh makmal-makmal analisa yang ada di
Malaysia, khasnya di negeri Johor.
Mengenalpasti makmal-makmal analisa yang menjalankan
pengesahan produk bioplastik di Malaysia, khasnya di negeri Johor.
Membangunkan Standard Operating Procedure (SOP) bagi ujian
pengesahan bioplastik yang telah dikenalpasti.
Mendapatkan validasi modul pembelajaran yang dibangunkan dari
pakar (pensyarah, pendidik bertauliah) di Institut Pengajian Tinggi
Awam / Swasta.
2.3 Gerak kerja Pembangunan Modul Pembelajaran Bagi Penilaian
dan Pengesahan Produk Bioplastik
Jadual 2: Gerak kerja pembangunan modul pembelajaran bagi penilaian dan
pengesahan produk bioplastik
Bil Perkara Penjelasan
1 Melaksanakan
‘market-intel’
berkaitan ujian
pengesahan
bioplastik
Mengadakan rujukan / survei bagi mendapatkan
maklumat untuk menjustifikasikan keperluan
untuk melaksanakan ujian pengesahan bioplastik
di makmal.
2 Melaksanakan ‘Market-intel’ ini juga bertujuan untuk
24
‘market-intel’ bagi
mengenalpasti
makmal-makmal
ujian pengesahan
bioplastik.
mengenalpasti makmal-makmal di Malaysia,
khasnya di Johor yang dapat menawarkan ujian-
ujian pengesahan bioplastik.
3 Membangunkan
SOP ujian
pengesahan
bioplastik yang telah
dikenalpasti dan
ditawarkan oleh
makmal-makmal.
SOP bagi setiap ujian pengesahan bioplastik
dibangunkan berdasarkan kepada standard-
standard yang dikenalpasti dari American Society
for Testing and Materials (ASTM), European
Standardization Committee (CEN) dan
International Standards Organization (ISO).
4 Menerbitkan modul
pembelajaran untuk
rujukan
pemegangtaruh
inisiatif BBJ
Membangunkan dan menerbitkan modul
pembelajaran supaya ia boleh dijadikan sebagai
garis panduan bagi pemegangtaruh-
pemegangtaruhseperti agensi-agensi kerajaan
dan swasta, pihak-pihak berkuasa tempatan
(PBT) dan institusi pengajian tinggi awam dan
swasta.
5 Mewujudkan kit
pendidikan dalam
bentuk pameran
berkaitan dengan
ujian pengesahan
bioplastik.
Membangunkan kit pendidikan yang
memaparkan info dan ujian pengesahan yang
boleh dijadikan rujukan orang awam dan juga
pemegangtaruh-pemegangtaruh untuk
disesuaikan dengan teras perniagaan / keperluan
mereka.
25
2.4 Garis Masa Projek
Seperti pada Apendix 1
26
BAB 3
UJIAN PENGESAHAN BAGI PRODUK BIOPLASTIK
3.1 Latar belakang
Ujian Pengesahan perlu dijalankan bagi produk bioplastik untuk
memastikan bahan dan produk plastik mematuhi piawaian Jabatan Standard
Malaysia serta memenuhi kriteria produk mesra alam. Johor merupakan salah
satu negeri di Malaysia yang menggerakkan inisiatif berkaitan biorosot dan
biokompos. Oleh kerana itu, Johor perlu mengadakan sistem pengesahannya
yang tersendiri bagi memastikan hanya produk yang berkualiti dan menepati
spesifikasi sahaja boleh digunakan di negeri ini. Terdapat beberapa ujian
pengesahan bioplastik sebagaimana yang ditetapkan dalam standard seperti:
Biodegradability Testing – Ready Biodegradability (OECD, 1992)
(Wajib)
Thermogravimetric Analysis (ASTM E 1131, 2004) (Pilihan)
Compostability Testing – Plant Growth Test (OECD, 2003) (Wajib)
Oxo-Biodegradation Analysis (BS 8472, 2011) (Wajib)
Toxicity – Heavy Metal Testing (HS1003, undated) (Wajib)
Toxicity – Migration Testing (BS EN 13130-1, 2004) (Pilihan)
Halal – Porcine Testing (MS 2672, 2017) (Wajib)
Terdapat beberapa lagi standard bagi pengesahan bioplastik, namun
begitu modul ini hanya menekankan tujuh (7) ujian pengesahan yang biasa
dilakukan dan ditawarkan oleh makmal-makmal seperti yang telah
27
diterangkan dalam Bab 4. SOP yang umum yang telah dibangunkan untuk
ujian pengesahan --bioplastik adalah seperti di bawah, namun ia boleh
berubah-ubah mengikut standard yang digunakan oleh sesebuah makmal itu.
SOP ini dibentangkan dalam Bahasa Inggeris kerana semua standard adalah
dalam Bahasa Inggeris.
3.2 TEST METHOD: BIODEGRADABILITY TESTING – READY
BIODEGRADABILITY
1.0 Introduction
A solution or suspension of the test in a mineral medium is inoculated and
incubated under aerobic conditions in the dark or diffuse light. The amount of
DOC in the test solution due to the inoculums should be kept as low as
possible compared with the amount of organic carbon due to the test
substance. In general, the degradation is followed by the determination of
parameters such as DOC, CO2 production and oxygen uptake and
measurements are taken at the sufficiently frequent intervals to allow the
identification of the beginning and the end of biodegradation. Usually, the test
will last for 28 days. The tests, however, maybe ended before 28 days, as
soon as the biodegradable curve has reached a plateau for at least three
determinations. The test may also be prolonged beyond 28 days when the
curve shows that biodegradation has started but that the plateau has not been
reached by day 28, but in such cases the chemical would not be classed as
readily biodegradable. The pass levels for readily biodegradable are 70%
removal of DOC and 60% of Theoretical Oxygen Demand (ThOD) or
28
Theoretical amount of evolved carbon dioxide (ThCO2) production for
respirometric methods. They are lower in the respirometric methods since, as
some of the carbon from the test chemical is incorporat into new cells, the
percentage of CO2 produced is lower than the percentage of carbon will be
used..
2.0 General Description
Water: H2O free from inhibitory concentrations of toxic substances (contain
<10% of the organic carbon content introduced by the test material). Oxygen
consumption of the water must be low (oxygen depletion <1.5mg DO/l)
Mineral Media: Prepared from stock solutions of appropriate concentrations
of mineral components (eg. Potassium and sodium phosphates plus
ammonium chloride, calcium chloride, magnesium sulphate, and iron (III)
chloride)
Methods of adding the test and reference substances:
Substances of adequate solubility (>1g/l) = prepare stock solutions at
appropriate concentrations and use aliquots to prepare the final test solution.
Dissolve less soluble substances in the mineral medium to avoid diluting the
buffer solution. Add substances that are even less soluble directly to the final
mineral medium.
Inoculum: Derived from various sources such as activated sludge, sewage
effluents (unchlorinated) surface waters and soils, or a mixture of these.
Pre-conditioning of Inoculum: Consists of aerating activated sludge (in
mineral medium) or secondary effluents for 5-7 days at the test temperature.
29
Abiotic Controls: Check for the possible abiotic degradation of the test
substances by determining the removal of DOC, oxygen uptake or CO2
evolution in sterile controls containing no inoculum.
The number of flasks and samples: At least two flasks or vessels
containing the test substances plus inoculums only should be used. Single
vessels suffice for reference compounds plus inoculum and, when required,
for toxicity, abiotic removal, and adsorption methods.
3.0 Instruments / Apparatus
i. BOD bottles with glass stoppers (250 – 300 ml / 100 – 125ml)
ii. Water bath and incubator
iii. Large glass bottles (2-5 liters)
iv. Oxygen electrode and meter
4.0 Chemicals
i. Water
ii. Potassium dihydrogen orthophosphate, KH2PO4
iii. Dipotassium hydrogen orthophosphate, K2HPO4
iv. Disodium hydrogen orthophosphate dehydrate, Na2HPO4.2H2O
v. Ammonium chloride, NH4Cl
vi. Calcium chloride, Anhydrous, CaCl2
vii. Calcium chloride, dihydrate, CaCl2.H2O
viii. Magnesium sulphate heptahydrate, MgSO4.7H2O
ix. Iron (III) chloride hexahydrate , FeCl3.6H2O
x. Concentrated hydrochloric acid, HCl
xi. Ethylene-diaminetetra-acetic acid (EDTA), disodium salt.
30
5.0 Preparation
5.1 Preparation of mineral medium
i. Prepare stock solutions as the following table. Each stock solution
needs to dissolve in water and makeup to 1L
Stock Solution A
1) KH2PO4 8.50g
2) K2HPO4 21.75g
3) NA2HPO4.2H2O 33.40g
4) NH4Cl 0.50g
PH = 7.4
Stock Solution B
1) CaCl2 27.50g
2) CaCl2.2h2O 36.40g
Stock Solution C
1) MgSO4.7H20 22.50g
Stock Solution D
1) FeCl3.6H2O 0.25g
i. In order to avoid having a problem, the solution will be prepare
immediately before use, add one drop of concentrated HCl or 0.4g
ethylene-diaminetetra-acetic acid (EDTA), disodium salt per liter.
ii. If precipitate forms in a stock solution, replace it with a freshly made
solution.
iii. Mix 1 mL of each stock solution with 800 mL water and make up to 1 L.
31
5.2 Preparation of stock solution of test substances
i. Dissolve 1-10g of test or reference substance in water and makeup
to 1L if the solubility exceeds 1g/L
ii. Otherwise, prepare stock solution in mineral medium or add the
chemical directly to the mineral medium, make sure that the
chemical dissolves.
5.3 Preparation of Inoculum
i. Collect a fresh sample and keep it aerobic during transport.
ii. Allow to settle for 1h or filter through a coarse filter paper and keep the
decanted effluent or filtrate aerobic until required.
iii. Up to 100 mL of this type of inoculum may be used per liter of medium.
5.4 Pre-conditioning of Inoculum
i. Inoculum may be pre-conditioned by aerating the secondary effluent for
5-7 days (if required)
5.5 Preparation of Bottle
i. Strongly aerate mineral medium for at least 20 minutes and allow to
stand. Generally, the medium is ready for use after standing for 20h at
the test temperature. Carry out each test series with a mineral medium
derived from the same batch. Determine the concentration of dissolved
oxygen for control purposes; the value should be about 9mg/L at 20°C.
Conduct all transfer and filing operations of the air-saturated medium
bubble-free, for example, by the use of siphons.
32
ii. Prepare parallel groups of BOD bottles for the determination of the test
and reference substances in simultaneous experimental series.
Assemble a sufficient number of BOD bottles, including inoculums
blanks, to allow at least duplicate measurement of oxygen consumption
to be made at the desired test intervals.
iii. Add fully-aerated mineral medium to large bottles so that they are
about one-third full. Then add sufficient of the stock solutions of the test
and reference substances to separate large bottles so that the final
concentration of the chemicals usually is greater than 10 mg/l. Add no
chemicals to the blank control medium contained in a further large
bottle.
iv. To ensure that the inoculum activity is not limited, the concentration of
dissolved oxygen must not fall below 0.5mg/l in the BOD bottles. This
limits the concentration of test substance in general to about 2 mg/l. An
idea of the highest concentration to be used can be obtained from the
ThOD (mg O2/mg chemical) of the test substance. For poorly,
degradable compounds and those with a low ThOD, 5-10 mg/l can be
used. In some cases, it would be advisable to run parallel series of test
substances at two different concentrations, for example, 2 and 5 mg/l.
Normally, calculate the ThOD based on the formation of ammonium
salts but, if nitrification is expected of known to occur, calculate on the
basis of the formation of nitrate ThODNO3. However, if nitrification is
not complete but does occur, correct for the changes in concentration
of nitrite and nitrate, determined by analysis.
33
v. If the toxicity of the test substance is to be investigated (in the case, for
example, of a previous low biodegradability value having been found),
another series of bottles is necessary. Prepare another large bottle to
contain aerated mineral medium (to about one-third of its volume) plus
test substance and reference compound at final concentration normally
the same as those in the other large bottles.
vi. Inoculate the solutions in the large bottles with secondary effluent (one
drop, or about 0.05 ml, to 5 ml /l, see paragraph 8) or with another
source such as river water (see paragraph 9). Finally, make up the
solutions to volume with aerated mineral medium using a hose that
reaches down to the bottom of the bottle to achieve adequate mixing.
vii. In a typical, run the following number of bottles are used:
a. At least 10 containing test substance and inoculums (test
suspension)
b. At least 10 containing only inoculums (inoculum blank)
c. At least 10 containing reference compound and inoculums
(procedure control) and, when necessary,
d. 6 bottles containing test substance, reference compound and
inoculums (toxicity control)
viii. However, to ensure being able to identify the 10-d window about twice
as many bottles would be necessary.
6.0 Procedure
i. Dispense each prepared solution or suspension immediately into the
respective group of BOD bottles by hose from the lower quarter (not
the bottom) of the appropriate large bottle, so that all the BOD bottles
34
are completely filled. When testing poorly soluble substances, ensure
that the contents of the large bottles are well-mixed by stirring. Tap
gently to remove any air bubbles.
ii. Analyse the zero-time bottles immediately for dissolved oxygen by the
Winkler or electrode methods. The contents of the bottles can be
preserved for later analysis by the Winkler method by adding
manganese (II) sulphate and sodium hydroxide (the first Winkler
reagent). Store the carefully stoppered bottles, containing the oxygen-
fixed as a brown manganese (III) hydrated oxide, in the dark at 10-
20°C for no longer than 24h before proceeding with the remaining
steps of the Winkler method. Stopper the remaining replicate bottles
ensuring that no air bubbles are enclosed, and incubate at 20°C in the
dark.
iii. Each series must be accompanied by a complete parallel series for the
determination of the inoculated blank medium. Withdraw at least
duplicate bottles of all series for dissolved oxygen analysis at time
intervals (at least weekly) over the 28 days incubation. Weekly samples
should allow the assessment of percentage removal in a 14-d window,
whereas sampling every 3-4 days should allow the 10-d window to be
identified, and would require about twice as many bottles.
iv. For N-containing test substances, corrections for the uptake of oxygen
by any nitrification occurring should be made. To do this, use the 02-
electrode method for determining the concentration of dissolved
oxygen and then withdraw a sample from the BOD bottle for analysis
35
for nitrite and nitrate. From the increase in concentration of nitrite and
nitrate, calculate the oxygen used.
3.3 TEST METHOD: THERMOGRAVIMETRIC ANALYSIS
1.0 Introduction
Thermogravimetric analysis (TGA) measures weight changes in a material as
a function of temperature (or time) under a controlled atmosphere. A TGA
analysis is performed by gradually raising the temperature of a sample in a
furnace as its weight is measured on an analytical balance that remains
outside of the furnace. In TGA, mass loss is observed if a thermal event
involves the loss of a volatile component. Chemical reactions, such as
combustion, involve mass losses, whereas physical changes, such as
melting, do not. The weight of the sample is plotted against temperature or
time to illustrate thermal transitions in the material.
2.0 General Description
Principal uses of TGA include measurement of a material’s thermal stability
and its composition. Typical applications include:
Filler content of polymer resins
Residual solvent content
Carbon black content
Decomposition temperature
The moisture content of organic and inorganic materials.
Plasticizer content of polymers.
36
Oxidative stability.
Performance of stabilizers.
Low molecular weight monomers in polymers.
3.0 Instruments / Apparatus
i. Thermogravimetric analyzer
4.0 Preparation
i. The bioplastic samples are cut into pieces (10mg) and transferred to
the sample holder;
ii. The samples are heated from 30°C to 800°C with a heating rate of
10°C per min in the presence of air with a flow rate of 50ml/min.
iii. The thermogravimetric, derivative thermogravimetric can identify the
thermal decomposition that occurs in bioplastic through the loss of
weight.
5.0 Procedure
i. Switch on the TGA analyzer
ii. Switch on the gas supply (Protective gas: N2, Reactive gas: O2) and
the Julabo cryostat.
iii. Make sure the water is circulating by the monitor on its flow meter.
iv. Switch on the PC to establish communication between STAR software
and TGA analyzer
v. Log on with user ID on the Main Launch Bar
5.1 Adjusting the Gas Flow with GC 20
37
i. Enter the setup menu by pressing the SETUP key on the SmartSens
Terminal.
ii. Touch the Gas button to display the gas flow rate.
iii. Press the Toggle button to open gas valve 1
iv. Adjust the gas flow with the relevant knob on the gas controller.
a. Knob 1: Method gas – O2
b. Knob 2: Cell gas – N2
v. Adjust the knob clockwise slowly to reduce the flow rate.
vi. Press the Toggle button again to switch to gas valve 2
vii. Touch the done button when the gas flow rates are as desired.
5.2 Setting Up Method For Experiment
i. Click on the Routine Editor to open the Method window.
ii. Click the New button to create a temperature program.
iii. Click on the Add Dyn / Add Iso button to create a new segment.
iv. Select the desired gas and flow rate by clicking on Segment Gas.
v. Click the Save button to save the created method with proper naming.
vi. Deactivate the Auto Start function. Select Control => Configuration
vii. Uncheck the Autostart box. The Save Curve and Save Evaluation will
automatically select.
viii. Key in the sample name.
ix. Leave the text box for sample weight and crucible position empty.
x. Send the experiment by clicking on the Send Experiment button.
5.3 Automatic Weighing In Of Sample With Sample Robot.
i. Send the desired experiment on the Experiments-Pending.
38
ii. Right-click and select Edit Experiment.
iii. Key in the crucible position on the sample robot and click OK button.
iv. On the same module, select Weigh-in Auto.
v. Select Pan and start the weighing by pressing OK.
vi. The sample robot will take the empty crucible automatically for
weighting. Make sure the crucible position is critical in correctly.
vii. After the empty crucible is being weighted, it will be returned to the
turntable of the sample robot. Fill the crucible with the respective
sample.
viii. Activate the Auto-Start function by clicking Control/Configuration and
select the Autostart checkbox.
ix. Start the experiment by clicking the Control/Start Experiment.
5.4 Data Evaluation Window – Open Curve in Evaluation Window
i. On the Main Launch Bar, select Session /Evaluation Window.
ii. Click on the Open Curve icon to select the desired curve. The blank
and sample should select together.
iii. The selected TGA and DSC curves are displayed together. Users can
separate both curves by clicking the Arrange Coordinates icon.
5.5 Blank curve subtraction
i. Click on the sample curve first, then followed by the blank curve. Select
Math / Subtract Curves
ii. The blank subtracted curve is displayed. Remove the undesired curves
as shown in the above figure.
iii. Repeat the same steps for the DSC curves.
39
5.6 Displaying 1st Derivative Curve
i. Select Math/1st Derivative
ii. The dialog box of Smooth Settings is then pop up. By default, the
Order is 1 and Points is 13. Click OK to proceed.
5.7 Step Evaluation
i. Select TA / Step Horiz. Repeat the same procedure for the following
step.
ii. The mass loss value is displayed. Repeat the same procedure for the
following step.
iii. To display the residue value of the last step, click on the last step, then
select Settings/Optional Results
iv. The Optional Results dialog box will then pop up. Check the box for
Residue and click OK.
v. To save evaluation curve, select File / Save Evaluation.
vi. To open the evaluation curve, select Open Folder to open the list of
evaluated curves. Select the curve that you desired.
3.4 TEST METHOD: COMPOSTABILITY TESTING – PLANT GROWTH
TEST
1.0 Introduction
This method is to assess the potential effects of substances on seedling
emergence and growth. As such, it does not cover chronic effects or effects
on reproduction (i.e seed set, flower formation, fruit maturation). Conditions of
40
exposure and properties of substances to be tested must be considered to
ensure that appropriate test methods are used. Seeds are placed in contact
with soil treated with the test substances and evaluated for effects following
usually 14 to 21 days after 50% emergence of the seedlings in the control
group.
2.0 General Description
The validity of the test: the following performance criteria must be met in the
controls such as;
i. Seedling emergence >70%
ii. Seedlings do not exhibit visible phytotoxic effects and the plant exhibit
only normal variation in growth and morphology for that particular
species.
iii. The mean survival of emerged control seedlings is at least >90% for
the duration of the study.
iv. Environmental conditions for a particular species are identical and
growing media contain the same amount of soil matrix, support media
or substrate from the same source.
Reference substance: Maybe tested at regular time intervals, to verify that
performance of the test and the response of the particular test plants and the
test condition have not changed significantly over time.
3.0 Instruments / Apparatus
i. Pots – using a sandy loam or sandy clay loam that contains up to 1.5
% organic carbon.
ii. Non-porous plastic or glazed pots with tray or saucer under the pot.
41
4.0 Raw Materials / Chemicals
i. Natural soil / Artificial substrate
ii. Inert material – acid-washed quartz, sand, mineral wool, glass beads.
iii. Test Specimens – Seeds
iv. Test Substances – should be applied in an appropriate carrier.
5.0 Procedure
Test Design
i. Plant seeds of the same species in pots.
ii. The number of species planted per pot will depend upon the species,
pot size, and test duration.
iii. The number of plants per pot should provide adequate growth
conditions and avoid overcrowding for the duration of the test.
iv. Control groups are used to assure that effects observed are associated
with or attributed only to the test substance exposure. The appropriate
control group should be identical in every respect to the test group
except for exposure to the test substances. To prevent bias, random
assignment of test and control pots is required.
v. Avoid seed coated with insecticide or fungicide. If seeds-borne
pathogens are a concern, the seeds may be soaked briefly in a weak
5% hypochlorite solution, then rinsed extensively in running water and
dried. No remedial treatment with other crop protection is allowed.
vi. The emerging plants should be maintained under good horticultural
practices controlled environment chambers, phytotrons or
greenhouses.
42
vii. When using growth facilities these practices usually include control and
adequate frequent (daily) recording of temperature, humidity, carbon
dioxide concentration, light intensity, light period, watering, etc. to
assure good plant growth as judged by the control plants the selected
species.
Test Conditions
i. Temperature: 22°C ± 10°C
ii. Humidity : 70% ± 25%
iii. Photoperiod: Minimum 16h light.
iv. Light intensity : 350 ± 50µE/m2/s
3.5 TEST METHOD: TOXICITY – HEAVY METAL TESTING
1.0 Introduction
To outline the steps and procedures necessary for testing plastic samples in
order to ensure the content of heavy metal in the product is acceptable.
2.0 Instruments/ Apparatus
Inductively coupled plasma mass spectrometer (ICP-MS), analytical balance,
water bath volumetric flask 1000 ml and 250 ml, Micropipettes from 5.0µl to
20.0 µl with plastic tips, pipettes from 100 µl to 10 ml, glass or plastic,
measuring cylinder 250 ml, protective glass, oven in range of 70°C ± 2°C,
atomic absorption spectrometer with an appropriate detection system and
sensitivity.
43
3.0 Chemicals
Acetylene, Deionised water, Nitric acid (HNO3); concentrated 1:1,
concentrated sulphuric acid (H2SO4), stock solution of cadmium (100ppm),
Lead (100ppm), chromium (100ppm) and mercury (1000ppm), Hydrogen
peroxide H2O2, 30% Stannous ion (Sn2+) solution (7.0g Sn2+ / 100ml), Acetic
acid 5% (w/v) in aqueous solution.
4.0 Procedure
4.1 Preparation of hot acetic acid extract for articles in container form
4.1.1 Measure a sufficient volume of 5% acetic acid by measuring cylinder
and preheat in the oven at 70°C ± 2°C. Fill the test specimen with acetic
acid to a level within 0.5 cm of the top of the test specimen. Record the
volume of acetic acid that has been used.
4.1.2 Cover the test specimen with glass to prevent evaporation, in the
minimum time to prevent evaporation of acetic acid. Wrap the bottom
of the test specimen with aluminium foil to prevent leakage of solution.
Leave this preparation for 2h in a thermostatically controlled oven
maintained at 70°C ± 2°C.
4.1.3 Discharge the solution and wash the test specimen twice with acetic
acid. If it contains precipitate, filter the solution and washings. Filter
paper should pre-washed with distilled water to remove contaminant.
The total volume of acetic acid for washing should not exceed 5% of the
volume used for filling up the container.
44
4.1.4 Stabilize the acetic acid extract by the addition of concentrated nitric
acid in the ratio of 3.5 ml per 100 ml of sample. Mix the aqueous extract
well and take an aliquot portion for analysis
4.2 Preparation of hot acetic acid extract for articles in bag form.
4.2.1 Cut sample as taken into pieces approximately 1cm2 to 2 cm2. Wear
protective gloves to prevent contamination.
4.2.2 Weigh 10 ± 0.1g of the test pieces to the accuracy of 0.01g, put them
into the conical flask, add 200 mL of 5% acetic acid and stopper the
flask. Leave this preparation to stand for 2 hours in a water bath of 70°C
± 2°C, shake occasionally.
4.2.3 Discharge the solution and wash test pieces in the flask twice with a
fresh portion of 5% acetic acid of 70°C ± 2°C. If it contains precipitate,
filter the hot preparation. Transfer the extract and washings or the
filtrate to be marked 250 mL volumetric flask; cool to 23°C ± 2°C.
4.2.4 Stabilize the extract by addition of concentrated nitric acid in the ratio of
3.5 Ml per 100 mL of sample. Fill up to the mark with water. Use the
content of the flask for further analysis.
Note: If necessary, it can scale up the solution but not more than twice its
original volume.
45
4.3 Determination of Cadmium, Lead, Chromium, and Mercury
4.3.1 Suggested spectrometer settings and detection limit are as follows:-
Heavy metal Wavelength, nm Detection limit
Cadmium 228.8 0.5µg/L
Lead 217.0 or 283.3 2µg/L
Chromium 357.9 1µg/L
Mercury 253.7 0.5µg/L
4.4 Preparation of reference solutions
4.4.1 Prepare a series of the standard metal solution in the optimum
concentration range, by diluting the single stock element solutions with
water containing 1.5 mL concentrated nitric acid/litre. The
concentration to be selected will depend on the instrument used and
the expected concentrations in the extract. Prepare a calibration blank
using all the reagents except for the metal stock solutions.
4.4.2 Select at least three concentrations of each standard metal solution to
bracket the expected metal concentration of the sample. Aspirate the
system with the blank solution and standard solution alternatively and
run the next standard in the same manner.
4.4.3 Prepare a calibration curve by plotting the absorbance of standards
versus their concentrations.
46
4.5 Determination of the metal content
4.5.1 Follow the instructions given by the manufacturer of the spectrometer in
order to reduce interference and background noise. The details of the
measurement depending on the type of spectrometer. Follow the
instructions and record the peaks for each element.
4.5.2 Three parallel extractions should be carried out. From each extract, at
least two parallel determinations should be carried out. Determine the
concentration of each element by means of the calibration graph or
alternatively, by use of the method of standard addition.
4.5.3 Aspirate the sample prepared in 4.1 and 4.2 and calculate the
concentration of each element from the measured absorbance.
4.5.4 Submit the 5% acetic acid used for the extraction to the test procedure
to provide a blank value to be deducted from the extracted value.
4.5.5 When using an atomic absorption spectrometer to determine chromium,
mix 1 mL of 30% hydrogen peroxide with each 100 mL of standard
solution or sample before aspirating. Alternatively, use proportionally
smaller volumes. The calibration curve for chromium should be based
on an original standard concentration before addition of hydrogen
peroxide.
4.5.6 When using absorption spectrometer to determine mercury, stabilize the
extract by addition of potassium dichromate solution to content of
approximately 10 mg of potassium dichromate per 100 mL of extract.
47
Note: Organic mercury compounds will not respond to the flameless
technique unless they are decomposed into mercury (II) ions. Potassium
dichromate oxidizes these compounds. Add 4ml of hydroxyl ammonium
chloride solution per 100 ml of extract to inactive the surplus of potassium
dichromate
4.5.7 Follow the instructions given by the manufacturer of the spectrometer in
order to reduce the mercury (II) ions to mercury. The reducing agent to
be used is either tin (II) chloride or sodium tetra hydroborate and the
appropriate amount is specified in the instructions.
4.6 Determination of the metal content
4.6.1 Calculate the results with a computer or graphically. Correct, where
appropriate, for background absorption. Take the blank value into
consideration in the evaluation. Express the results in mg/L or µg/L of
the extract.
Note: Trace element determinations are sensitive to a number of sources of
error. Impure reagents of modifiers, contamination during handling of the
solutions, adsorption on the walls of vessels, inadequate background
correction or unmatched acid concentrations of sample and calibration
solutions can cause error. The detection limit should be established by
measuring a sufficient number of blanks to allow calculation of the standard
deviation of the blank. The detection limit is determined as three times his
standard deviation.
48
3.6 TEST METHOD: ASSESSMENT OF THE OXO-BIODEGRADATION
OF PLASTICS
Introduction
0.1 General
The methods described in this British Standard measure the
mineralization of the carbon chains of plastic under controlled laboratory
conditions, including the presence of soil micro-organisms and oxygen.
The partially mineralized products of the degradation and oxo-
biodegradation tests can then be assessed for their effect on seed
germination and plant growth.
0.2 Title of the standard
The term “oxo-biodegradation” is defined in 3.8 as it is defined in CEN/TR
15351:2006, 5.2 as “degradation identified as resulting from oxidative and
cell-mediated phenomena, either simultaneously or successively”. Oxo-
biodegradation is not restricted to man-made polymers. It was first
recognized in the biodegradation of natural rubber [1] and it occurs in
natural materials such as lignocelluloses, probably mediated by enzymes
that produce free radicals [1]. This is analogous to the redox reactions of
transition metal ions, where oxygen radicals such as.OH and.OOH is
certainly involved in the initiation step. Propagation of the chain reaction
occurs primarily on both natural and synthetic products through ROO. This
chemistry is readily understood by biochemists since it is widely discussed
in both materials and biological chemistry literature (see [1 to 4] and in
many textbooks). Further elaboration in this standard does not seem to be
49
appropriate. In the environmental exposure of plastics both mechanisms,
abiotic and biotic operate together and the micro-organisms rapidly
remove the biodegradable oxidation products in a synergistic process. It is
difficult and time-consuming to reproduce this in the laboratory and for
convenience the two processes corresponding to weathering, which is an
abiotic process, and biodegradation has to be carried out in separate
tests. ASTM also recognizes the two operations in ASTM D 6954-04. This
is oxo-biodegradation, although ASTM does not use this term.
0.3 Use of this standard
This standard defines a specific template to be used for the reporting of
results in order to standardize communication and avoid confusion. This
standard is not a specification. Testing, according to this standard does
not provide any recommendation about the suitability of the tested
products for any particular application.
1.0 Scope
This British Standard describes methods for determining:
a) degradation by oxidation (abiotic tests);
b) biodegradation (biotic test in soil); and
c) phytotoxicity (plant growth tests); of plastics materials and products
2.0 Normative references
The following referenced documents are indispensable for the application
of this document. For dated references, only the edition cited applies. For
50
undated references, the latest edition of the referenced document
(including any amendments) applies.
ASTM D 5510-94(2001), Standard Practice for Heat Aging of Oxidatively
Degradable Plastics
BS EN ISO 4892-3, Plastics – Methods of exposure to laboratory light
sources –Fluorescent UV lamps
BS EN ISO 17556, Plastics – Determination of the ultimate aerobic
biodegradability in soil by measuring the oxygen demand in a
respirometer or the amount of carbon dioxide evolved
OECD 208, OECD guidelines for the testing of chemicals – Terrestrial
plant test: seedling emergence and seedling growth test
3.0 Terms and definitions
For the purposes of this British Standard, the following terms and definitions
apply.
3.1 abiotic without the action of living organisms
3.2 biodegradation degradation of a polymeric item due to cell-mediated
phenomena NOTE Source: PD CEN/TR 15351:2006, 5.2.
3.3 biotic through the actions of living organisms
3.4 carbonyl index absorbance of the carbonyl band normalized to an
invariant absorbance of the polymer NOTE See Grassie and Scott [2].
3.5 degradation change in initial properties due to chemical cleavage of the
macromolecules forming a polymeric item, regardless of the mechanism
51
of cleavage 3.6 mineralization (aerobic) conversion to carbon dioxide,
water, and other inorganic chemicals
3.6 oxo-degradation degradation resulting from oxidative cleavage of
macromolecules NOTE 1 Similarly, prefixes like thermo (for the action of
heat), photo (for the action of light) are to be used whenever one wants
to indicate an identified mechanism of degradation. NOTE 2 Source: PD
CEN/TR 15351:2006, 5.2.
3.7 oxo-biodegradation degradation resulting from oxidative and cell-mediated
phenomena, either simultaneously or successively. NOTE 1 Similarly,
prefix like thermo (for the action of heat), photo (for the action of light) are
to be used separately or in combination whenever one wants to indicate
the involvement of various identified mechanisms of degradation. NOTE 2
Source: PD CEN/TR 15351:2006, 5.2.
4.0 Principle
Plastics specimens are subjected to some or all of the following tests (see
Figure 1).
a) An oxidation/abiotic test (see Clause 7) by photo-oxidation and/or by
thermal oxidation. Degradation to embrittlement is measured by flex test or
by friability test.
b) A biodegradation/biotic test (see Clause 8) on residue embrittled by
oxidation as per the test in Clause 7. Mineralization is measured as carbon
dioxide evolved as a percentage of the theoretical yield for complete
mineralization of total organic carbon content.
52
c) A phyto-toxicity/plant growth test (see Clause 9) on partially evolved
residue from the biodegradation test in Clause 8. Phyto-toxicity is
measured as seed germination and crop biomass compared to control soil.
5 Materials and apparatus NOTE Other equipment is required for
referenced test methods. 5.1 Accelerated weathering device, typically
utilizing a UV lamp 400 W emitting between 290 nm and 450 nm, capable
of alternating exposure to dry, light conditions and wet, dark conditions at
a minimum ratio of 5:1.
5.0 Materials and apparatus
NOTE Other equipment is required for referenced test methods.
5.1 Accelerated weathering device, typically utilizing a UV lamp 400 W
emitting between 290 nm and 450 nm, capable of alternating exposure to
dry, light conditions and wet, dark conditions at a minimum ratio of 5:1.
5.2 Forced-air ventilation oven, capable of maintaining the internal volume at
(50–70) °C ±2 °C, and not exceeding 80 °C in operation, capable of
exchanging the unoccupied volume of the oven once per hour, which
conforms to ASTM D 5510-94(2001).
6.0 Sample preparation
6.1 Select requirements for samples either from the product or based on the
anticipated product. In particular, specify samples of a given mass that
are either:
a) all or part of the product, including the thickest parts; or
53
b) a sample of the material to be used in a product, at the expected
maximum thickness.
6.2 Measure and/or cut out sufficient samples of sufficient size and mass for
the selected tests, from a single batch of material. NOTE It is
recommended that 4 g is prepared for the biodegradation test (8.1) and a
sample of 6 g is needed for input to the biodegradation process in 8.2 to
produce sufficient quantities at 50% mineralization for the phytotoxicity
tests (Clause 9). That is, 10 g in total.
6.3 Measure and/or cut out test samples on a clean, dry grease-free surface.
6.4 Record the dimensions and masses of the prepared samples.
7.0 Oxidation tests
7.1 Introduction
Oxidation (abiotic) testing shall be by photo-oxidation/weathering (7.2) and/or
by thermal oxidation (7.3), using separate samples if both tests are
performed.
7.2 Photo-oxidation test
Expose the samples (6.1) to artificial weathering in the accelerated
weathering device (5.1) in general accordance with an exposure cycle in BS
EN ISO 4892-3.
7.3 Thermal oxidation test
54
Expose the samples (6.1) in the forced-air ventilation oven (5.2) either: at a
range of temperatures or at a single temperature between ambient and the
temperature at which chemical decomposition becomes significant.
7.4 Measurement of oxidation
At intervals appropriate to the material tested (chosen by trial and error)
measure the degree of oxidation by one of the following embrittlement tests of
the samples.
a) By bending the sample so that its opposite edges touch and assess
whether the sample fractures in a brittle manner.
NOTE 1 A more precise assessment of the degree of oxidation may be
obtained by measuring the flexural properties in accordance with BS EN ISO
178.
b) By rubbing the sample between the thumb and first finger (friability)
and assess whether the sample fragments. NOTE 2 A more precise
assessment of the degree of oxidation may be obtained by
measuring the impact-failure energy using a falling dart test in
accordance with BS 2782-3. NOTE 3 Care should be taken to
collect sufficient clean material, whether intact or fragmented, for
subsequent tests. NOTE 4 IR spectroscopy of the test residue to find
the carbonyl index is a useful method for confirming oxidation.
NOTE 5 Samples that are not embrittled under 7.4a) or 7.4b) may be returned
to the test chamber for further exposure.
7.5 Test termination
55
Terminate the test and record the time to embrittlement when:
a) samples break under the embrittlement test in 7.4a), or
b) samples fragment under the embrittlement test in 7.4b).
8.0 Biodegradation test
8.1 Test three samples recovered from the oxidation test (Clause 7) that have
reached condition 7.5a) or 7.5b) according to the biodegradation (biotic)
test in BS EN ISO 17556, with the possibility of terminating the test
beyond six months and recording the test duration.
8.2 Obtain samples for the plant growth test by: running the biodegradation
process in bulk using at least 6 g of oxidized material in 3 kg of soil (a
starting concentration double that recommended in BS EN ISO 17556)
and taking the sample as soon as practicable after the point where the
monitored test has reached 50% of theoretical mass of carbon dioxide
evolved. NOTE It may be necessary to use a higher concentration of the
sample to soil than recommended in BS EN ISO 17556. Care has to be
taken to maintain other experimental conditions.
9.0 Phyto-toxicity test
Measure the effect of the partly evolved plastics samples on plant germination
number and biomass, in accordance with OECD 208, using 0.5 kg per pot.
Use the test substance from 8.2 and use the negative control samples from
the biodegradation test. Use at least two plant species from two of the three
mentioned categories of OECD 208. Record the germination number and
biomass crop yield of plants, compared to the control soil.
56
10.0 Test report
A test report containing the following information as a minimum shall be
prepared following the template shown in Figure 2.
a) For all tests:
1) a reference to this standard, i.e. BS 8472:2011;
2) the material, its constituents and/or its unique manufacturer’s
identification code; and
3) initial sample size(s), thickness(es) and mass(es).
b) For photo-oxidation tests:
1) the type of UV lamp used as categorized in BS EN ISO 4892-3;
2) the total exposure time and the exposure cycle to which the samples
have been subjected; and
3) the relevant test criteria and results as required in 7.4 and 7.5.
c) For thermal oxidation tests:
1) the rate of airflow through the sample/total flow, the temperature due
to the forced-air ventilation oven, and the total time of exposure; and
2) the relevant test criteria and results as required in 7.4 and 7.5.
d) For biotic tests: the information required for a test report to BS EN
ISO 17556.
e) For phytotoxicity tests: the results required by OECD 208.
57
3.7 TEST METHOD: TOXICITY- MIGRATION TEST
1.0 Introduction
To outline the steps and procedures necessary for testing the migration of
specific substances into the foodstuffs.
2.0 Instruments / Apparatus
Cutting slab, 250 mm x 250 mm, Lint-free cloth or brush, tweezers, scalpel,
metal templates (100 mm ± 0.2 mm) x (100 mm ± 0.2 mm), ruler, 25mm ± 1
mm wide, analytical balance, cruciform specimen support, gauze mesh size of
1 mm, glass tube 35 mm ; length 100 mm to 200 mm, oven 40°C ± 1°C and
70°C ± 2°C, hot plate, glass beads, 2mm to 3mm in diameter, desiccator,
dishes (50mm to 90 mm; max weight: 100g), beakers, 2L, 250 ml, measuring
cylinder, 100 ml
3.0 Chemicals
Distilled water (stimulant A), acetic acid 3% (w/v) in aqueous solution
(stimulant B), ethanol 15% (v/v) in aqueous solution (stimulant C)
4.0 Procedure
4.1 Preparation of test specimen
4.1.1 Clean sample with a lint-free cloth or a soft brush from dust or any
contaminant.
4.1.2 The surface to volume ratio in the total immersion test is conventionally
1dm2 of food contact area to 100 ml of food stimulant.
4.1.3 Cut each test specimen into 25mm x 10 mm.
58
4.1.4 For those samples of irregular shape or thickness, the test specimens
should have a surface area of approximately 2 dm2. Calculate the
surface area of each test specimen to the nearest 0.05 dm2 Schlegel
Method.
4.1.5 Measure the dimensions of each test specimen to the nearest 1 mm
using the ruler.
For the Total Immersion Test, both the inside and outside surfaces of the test
specimen are in contact with food stimulants. Only 1 dm2 of the food contact
surface is taken into account in the calculation. Do not use the area of cut
edges that in contact with foodstuff since it will give higer result.
4.2 Exposure to food stimulant
4.2.1 Measure food stimulant into three glass tubes using measuring cylinder
100 ml ± 2 ml
4.2.2 If the evaporation method is to be used, measure food stimulants into
two additional tubes 120 ml ± 2 ml and label as blanks.
4.2.3 If the distillation method is to be used, measure food stimulant into two
additional tubes 100 ml ± 2 ml and label as blanks.
4.2.4 Place the five tubes that contained food stimulant in the thermostatically
controlled oven or incubator set at the test temperature (40°C or 70°C or
the selected temperature from Table 1) and leave until the test
temperature has been attained.
Table 1: Migration Test Conditions
59
Conditions of contact in actual use Test condition
Contact time, t
0.5 hr ≥ t
1 hr ≥ t > 0.5 hr
2 hr ≥ t > 1 hr
24hr ≥ t >2hr
t >24 hr
Test time
0.5 hr
1 hr
120 min
24 hr
240 hr
Contact temperature T
5°C ≥ T
20°C ≥ T > 5°C
40°C ≥ T > 20°C
70°C ≥ T > 40°C
T > 70°C
Test temperature
5°C
20°C
40°C
70°C
100°C or reflux
Contact conditions in actual use are known, select the corresponding test
conditions (exposure time and temperature) from Table 1 which is applicable
to the sample when it is in actual use. If the sample is intended for a food
contact application under two or more conditions, the migration test shall be
carried out at the most stringent test conditions (i.e. the longest time and/or
the highest test temperature). In case the contact conditions (temperature and
time) are not known, only 10-day test at 40°C and 2-hour test at 70°C is to be
carried out for food stimulants (A, B and C).
4.2.5 Take the tubes out of the oven or incubator. Place a test specimen into
each of the three tubes containing 100 ml.
60
4.2.6 Label the tubes for identification.
4.2.7 Ensure the test specimens are totally immersed in the stimulant. If they
are not, add either glass beads or rods to raise the level of the stimulant
until total immersion is achieved. This part of the operation should be
carried out in the minimum time to prevent undue heat loss from the
stimulant.
4.2.8 Mark the liquid level on the outside of each tube with a suitable marker.
4.2.9 Place all tubes in the oven or incubator, set at the test temperature and
observe the temperature, leave the tubes for a selected test period
(refer Table 1) after the air bath of the controlled oven or incubator has
reached a temperature within 1°C of the set temperature.
4.2.10 Take the tubes from the oven or incubator and check the level of
stimulant in each, if this has dropped to more than 10 mm below the
mark, or has been exposed to any part of the test pieces, repeat the
test using fresh samples.
4.2.11 If the level of stimulant in a tube is less than 10 mm below the mark,
remove the test specimen from the tube and allow the stimulant
adhering to the test specimen and support to drain back into the tube.
Recover at least 90% of the original volume of stimulants or simply
repeat the test.
4.2.12 Determine the number of residues in the stimulant, using the procedure
described in 4.3
4.3 Determination of migrating substances
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4.3.1 Preparation of dishes
4.3.1.1 Take five dishes, mark for identification, and place in the oven
that has been maintained at 105°C to 110°C for a period of 30
min ± 5 min to dry.
4.3.1.2 Remove the dishes from the oven, place in a desiccator and
allow cooling to ambient temperature. Weight and record the
individual masses of each dish.
4.3.1.3 Replace the dishes in the oven and repeat the cycle of
heating, cooling and weighing until individual consecutive
masses differ by not more than 0.5 mg, weight their masses.
4.3.1.4 Use the evaporation method or distillation method to obtain
the mass of the residue.
4.3.2 Evaporation method
4.3.2.1 Take the tube containing the stimulant and pour 40-50 ml
from each separate dish. Using a steam bath, hot plate or
another form of heating to evaporate the stimulant to a lower
volume (taking care to avoid loss, in particular, by
sputtering or overheating of the residues.
Note: the evaporation of acetic acid and ethanol should be carried out
in a fume cupboard.
4.3.2.2 When most of stimulant has evaporated, pour the remaining
stimulant from each the tubes into respective dishes and
continue the evaporation.
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4.3.2.3 Wash out each of the tubes which had contained test
specimens with two lots of 10 ml ± 1 ml of unused stimulant
and pour these washings into the respective dishes. Continue
evaporation. (A stream of nitrogen may facilitate
evaporation).
4.3.2.4 When the stimulant has almost completely evaporated, place
the dish in an oven maintained at 105°C to 110°C, for a
period of 30 min ± 5 min, to complete the evaporation and dry
the residue. Remove the dishes from the oven, place in a
desiccator and allow it cooling to ambient temperature.
4.3.2.5 Weigh and record the individual masses of a dish and
residue.
4.3.2.6 Replace the dishes in the oven and repeat the cycle of
heating, cooling and weighing until individual consecutive
masses differ by not more than 0.5 mg.
4.3.2.7 Determine the mass of the residue by subtracting the original
mass of the dish from the stable mass of the dish and
residue.
4.3.3 Distillation method
4.3.3.1 Transfer the stimulants to individual round bottom flasks (250
ml are suitable). Rinse each tube twice, including the blank
tubes, with 20 ml ± 2 ml of fresh stimulant, add these rinses to
the respective flasks.
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4.3.3.2 Place the flasks in an electric heating mantle and connect to a
sidearm distillation arrangement, or place them in a rotary
evaporator instead. Distill off the stimulants until
approximately 30 ml to 50 ml remains in the flask.
4.3.3.3 Transfer the remaining stimulant to an evaporating dish.
Rinse the flask with 10 ml ± 1 ml of fresh stimulant and add
the rinses to the appropriate dishes. Continue the
evaporation of the stimulant by using a steam bath hot plate
or other forms of heating described in the evaporation
method.
4.3.3.4 Method of calculation for total immersion with aqueous food
stimulants. Express the overall migration as milligrams of
residue per decimeter of the surface of the sample which is
intended to come into contact with foodstuffs, calculated for
each test specimen using the following formula:
M = (ma – mb) S x 1000 (1)
Where,
M is the overall migration into the stimulant, in milligrams per
square decimeter of the surface area of a sample intended to
come into contact with foodstuffs;
ma is the mass of the residue from the test specimen after
evaporation of the stimulant in which it had been immersed, in
grams;
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S is the surface area of the test specimen intended to come
into contact with foodstuffs, in square decimeters. Note: only
one surface is counted
4.3.3.5 Calculate the result for each test specimen to the nearest 0.1
mg/dm2 and the mean of the individual test results, to the
nearest 0.1 mg/dm2.
4.3.4 Validity of result
The test results are considered to be valid only if the difference between the
test results in the same test satisfies the following conditions:
Table 2: Analytical Tolerance (Acceptable intra-test result difference) for
different stimulants.
Item Analytical Tolerance
All aqueous food stimulants ≤ 6mg/kg or 1mg/dm2
Item if more than two results are not within the analytical tolerance, then the
test should be repeated using fresh test specimens from the sample.
3.8 TEST METHOD: HALAL – PORCINE TESTING
1.0 Introduction
To outline the steps and procedures necessary for testing plastic samples in
order to ensure there is no contamination with porcine DNA in the product.
65
2.0 Instruments / Apparatus
Vortex, analytical balance, water bath, thermal cycler, electrophoresis, UV
transilluminator, Eppendorf tube, UV-visible spectrophotometer, puRe TaqTM
Ready-To-GoTM PCR Beads, Biofuge, water bath, micropipettes from 5.0µl to
20.0µl with plastic tips, pipettes from 100µl to 10 ml, glass or plastic,
measuring cylinder 250 ml, protective glass, oven in range of 70°C ± 2°C,
atomic absorption spectrometer with an appropriate detection system and
sensitivity.
3.0 Chemicals
Acetic acid 5% (w/v) in aqueous solution, concentrated nitric acid, deionized
water , ASL buffer, nuclease-free water, DNA easy kit, puRe TaqTM
polymerase, 10 mM Tris-HCl (pH 9.0 at room temperature), 50 mM KCl, 1.5
Mm MgCl2, 200 mM dATP, dCTP, dGTP and dTTP, BSA, 20 pmol forward
and reverse primer, 1.7% agarose gel of 1x TBE buffer, ethidium bromide.
4.0 Procedure
4.1 Preparation of hot acetic acid extract for articles in container form
4.1.1 Measure a sufficient volume of 5% acetic acid by measuring cylinder
and preheat in the oven at 70°C ± 2°C. Fill the test specimen with acetic
acid to a level within 0.5 cm of the top of the specimen. Record the
volume of acetic acid that has been used.
4.1.2 Cover the test specimen with an inert material to prevent evaporation,
e.g. glass. This part of the operation should be carried out in the
minimum time to prevent the evaporation of acetic acid. The bottom of
66
test specimen should be wrapped by aluminium foil to prevent leakage
solution. Leave this preparation for 2 hours in a thermostatically
controlled oven maintained at 70°C ± 2°C.
4.1.3 Decant the solution and wash the test specimen twice with acetic acid. If
it contains precipitate, filter the solution and washings. Filter paper
should be pre-washed with distilled water to remove artifacts. The total
volume of acetic acid for washing should not exceed 5% of the volume
used for filling up the container.
4.1.4 Stabilize the acetic acid extract by the addition of concentrated nitric
acid in the ratio of 3.5 ml per 100 ml of sample. Mix the aqueous extract
well and take an aliquot portion for investigation.
4.2 Preparation of hot acetic acid extract for articles in bag form
4.2.1 Tear or cut samples as taken into pieces approximately 1 cm2 to 2 cm2.
Wear protective gloves to prevent contamination.
4.2.2 Weigh 10 ± 0.1g of the test pieces to the accuracy of 0.01g, put them
into the conical flask, add 200 ml of 5% acetic acid and stopper the
flask. Leave this preparation to stand for 2 hr in a water bath of 70°C ±
2°C, shake occasionally.
4.2.3 Decant the solution and wash test pieces in the flask twice with a fresh
portion of 5% acetic acid of 70°C ± 2°C. If it contains precipitate, filter
the hot preparation. Transfer the extract and washings the filtrate to a
marked 250 ml volumetric flask; cool to 23°C ± 2°C.
67
4.2.4 Stabilize the extract by addition of concentrated nitric acid in the ration
of 3.5 ml per 100 ml of sample. Fill up to the mark with water. Use the
content of the flask for further investigation. Note: If necessary, it can
scale up the solution but not more than twice its original volume.
4.3 Porcine detection using Porcine Detection Kit
4.3.1 Add sample prepared in 4.1 and 4.2 into high-performance extraction
liquid
4.3.2 Shake it well.
4.3.3 Dip the porcine detection kit into the mixture. Leave it for 15 minutes.
4.3.4 Record the observation; Positive / Negative
4.3.5 Proceed for further testing if the result positive.
4.4 DNA Isolation
4.4.1 Transfer 0.03 ml of the prepared sample into a 1.5 ml Eppendorf tube.
4.4.2 Add 200µl ASL buffer (Qiagen) into the individual tubes containing the
sample material.
4.4.3 Vortex the mixtures for 5 minutes and incubated overnight for sufficient
lysis to maximize DNA extraction.
4.4.4 After incubation, vortex the samples for 2 minutes and centrifuge at full
speed (13,000 rpm) for 15 minutes using centrifuge (Biofuge) to
remove any solid particles.
4.4.5 Transfer 40µl of supernatant into a new Eppendorf tube and store at -
4°C for subsequent PCR application.
4.5 DNA Quantification
68
4.5.1 Measure the concentration and purity of the extracted DNA by
absorbance at 260nm using the UV-visible spectrophotometer.
4.5.2 Dilute 10µl of DNA sample in 990 µl of nuclease-free water for PCR.
Measure the DNA extraction with the Qiagen kit and the microwave
extraction in the range of 1000 – 1500 ng.
4.6 PCR Mix
4.6.1 Amplify the PCR Mix DNA (200 ng) using puRe TaqTM Ready-To-GoTM
PCR Beads.
4.6.2 In a final volume of 25µl, each reaction contain 2.5 units of puRe TaqTM
DNA polymerase, 10 mM Tris-HCl (pH 9.0 at room temperature), 50 Mm
KCl, 1.5 mM MgCl2, 200 mM DATP, DCTP,DGTP and DTTP and
stabilizer, including BSA.
4.6.3 Perform amplification using 20 pmol of each forward and reverse primer
on a thermal cycler. The forward primer is
5´ - TGCAGTCTCTCCTCCAAA- 3´ and the reverse primer is
5´ - CGATAATTGGATCACATTCTG- 3´.
4.6.4 Run the amplification using the following program : 94°C for 3 minutes to
denature the template DNA completely, followed by 35 cycles at 94°C
for 1 minute, 55°C for 1 minute and 72°C for 1 minute and close by the
extension step at 72°C for 7 minutes.
4.6.5 Determine the amplified DNA by gel electrophoresis in 1.7% agarose gel
of 1x TBE buffer and made visible by staining with ethidium bromide at
a constant voltage of 70 for 20 hr.
69
4.6.6 Observe the resulting fragments by using UV transillumination or any
other gel document systems.
4.6.7 The presence or absence of porcine DNA is confirmed by ultraviolet
fluorescence and documented.
4.6.8 The minimum level of detection (LOD) shall be 0.01 ng/µL. Generally,
the level of detection shall be in the range of 0.01 ng/µL to 0.05 ng/µL
depending on the primers used.
4.6.9 Real-Time PCR For positive presence of DNA the cycle threshold (Ct)
value shall be in the range of 32 to 40, that is, the LOD is 0.01 % (w/w).
5 Interpretation of Results
5.1 The results are expressed as follows:
Table 1: PCR results from the interpretation
Test
Sample
PCR Reagent Control
Extraction Blank
Control
Negative
Control
Positive
Control
Interpretation
of Results
+ - - - + Positive
- - - - + Negative
+ - + - + Inconclusive
+ + - - + Inconclusive
- - - - + Inconclusive
- - + - + Inconclusive
- + - - + Inconclusive
6. Test report
70
6.1 Both duplicate samples shall be positive in order to report as " porcine
DNA detected."
6.2 If only one of the duplicate samples is positive, the whole analytical
process (from extraction) shall be repeated.
6.3 If, after repeating, the same results are obtained, then the report shall
be "porcine DNA not detected”.
6.4 No ambiguous result shall be reported.
71
BAB 4
MAKMAL-MAKMAL ANALISA YANG MENJALANKAN PENGESAHAN
PRODUK BIOPLASTIK DI MALAYSIA
4.1 Makmal Yang Menawarkan Ujian Pengesahan Bioplastik di Malaysia
Melalui penyelidikan pasaran dan intel yang dilakukan, antara makmal-
makmal yang boleh menawarkan ujian pengesahan bioplastik seperti yang
dinyatakan dalam bab 3 adalah seperti dalam Jadual 3:
Jadual 3: Makmal-makmal yang menawarkan ujian pengesahan bioplastik
Bil Nama Makmal Lokasi Ujian ditawarkan
1
Environmental Technology Research Centre (SIRIM Berhad)
Blok 15, SIRIM Berhad 1, Persiaran
Dato’ Menteri, Seksyen 2, PO Box 7035, 40700 Shah
Alam Selangor
Biodegradability
Biocompostability
Oxo-Biodegradation Analysis
Thermogravimmetric Analysis
Heavy Metal
Analysis
2 Johor Toyyiban
Laboratories
Blok 1-2, 1-3 & 6-1, UTM-MTDC
Technology Centre
Halal – Porcine Analysis
Heavy Metal Analysis
3 Universiti Tun Hussein
Onn Malaysia TBA
Biodegradability
Biocompostability
Oxo-Biodegradation
Analysis
Thermogravimmetric
Analysis
72
4.2 Cadangan ujian pengesahan bioplastik
Biasanya, ujian-ujian asas yang diperlukan untuk pengesahan sifat-
sifat bioplastik adalah biodegradation, compostability dan heavy metal
analysis. Akan tetapi, seandainya bioplastik tersebut adalah berasaskan
biojisim (biomass), terdapat ujian tambahan yang periu dijalankan iaitu
ujian untuk racun perosak (pesticide), kulat (mould) dan yis (yeast). Jika
bioplastik tersebut digunakan sebagai pembungkus makanan, maka ujian
migrasi (migration test) adalah perlu dijalankan. Selain itu, Ujian
migration, disintegration dan photodegradation adalah ujian pilihan yang
perlu dijalankan bertujuan untuk memastikan tahap keselamatan produk
adalah memuaskan dan menjamin kesihatan manusia dan alam sekitar,
Akhir kata, pemilihan ujian pengesahan bioplastik sebenarnya tertakluk
kepada keperluan perniagaan sesebuah syarikat pengeluar bioplastik
yang berpandukan kepada sasaran pasarannya. Pihak industri
disarankan untuk berhubung dengan wakil makmal-makmal yang
dinyatakan di atas bagi mendapatkan keterangan teknikal yang lebih
lanjut bagi memenuhi keperluan syarikat dan juga pasaran masing-
masing.
73
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Appendix 1
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Modul ini mengandungi pengenalan tentang sejarah plastik, pendekatan dunia dan Malaysia amnya, dan Johor khususnya dalam menangani masalah plastik, sejarah terciptanya bioplastik dan juga jenis-jenis bioplastik. Modul ini juga diterbitkan bagi memberikan pendedahan kepada masyarakat tentang ujian-ujian pengesahan bioplastik yang boleh ditawarkan oleh makmal-makmal di Malaysia, khususnya di UTHM Johor, selaku rakan kerjasama tunggal yang beraspirasi untuk memberikan sokongan kepada kerajaan dalam menggalakkan penguatkuasaan penggunaan plastik boleh urai di bawah Inisiatif Biorosot dan Biokompos Negeri Johor.
Semoga modul ini dapat menambah pengetahuan masyarakat tentang bioplastik dan ujian-ujian yang berkaitan dengannya, disamping dapat dimanfaatkan sepenuhnya oleh pemain industri bioplastik sebagai panduan untuk mendapatkan bantuan teknikal bagi menambahbaik kualiti dan kebolehpasaran produk plastik mereka.