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Polymers 2020, 12, 440 4 of 15 The C, O, and Ag content of the RCF and CANF0.04 surface was measured using XPS scanning (THERMO, Thermo Fisher Scientific, Tewksbury, MA, USA). The scanning method performed full scan of the samples (resolution: 1 eV), and accurately scan the C1s and Ag3d peak areas of the samples (resolution: 0.1 eV). The main residuals in the film samples obtained from the experiments were DMAc and Li element. The DMAC residues in RCF and CANF0.04 were studied by GC/MS (7890A-7000B, Agilent, Palo Alto, CA, USA) with Agilent 19091S-433 column and EI ion source. The test method was according to the SN standard SN / T 3587-2016. The safe residual dose of DMAc was based on OEKO-TEX certification Standard100. A 100 μg/mL DMAc standard solution was used as the threshold to determine whether the solvent content exceeded the standard. The Li residuals in RCF and CANF0.04 films were studied by ICP (Optima8300, Agilent, Palo Alto, CA, USA). One gram of RCF and CANF0.04 were digest it in 20 mL of 72% concentrated sulfuric acid, respectively. Added 20 mL of 64% nitric acid until the solution becomes clear, and set volume to 1 L with deionized water for measuring. According to the ISO 1924-2 (2008) standard, mechanical property tests were conducted at room temperature using a universal testing machine (IMT-202F, International Material Tester Co., Ltd., Dongguan, China). The cross-head speed was 10 mm/min. The dimensions of the test films were 100 mm × 10 mm × 0.02 mm to 0.04 mm. The initial separation of the grips was 50 mm. The light transmittance and haze of the RCF and CANF0.04 were measured using a light transmittance/haze meter (WGT-S, Thermo Fisher Scientific, Tewksbury, MA, USA). The light source was a standard light source C, and the films selected for testing were thickness of 0.03 mm. The thermal stability of RCF and CANF0.04 was measured by TGA using a TG analyzer (SDT Q600; TA instruments, New Castle, DE, USA) at a heating rate of 20 ◦C/min from 50 ◦C to 750 ◦C under a high purity air atmosphere. 2.6. Antibacterial Activities of Ag-NPs and Composite Films The antibacterial activity of Ag-NPs against E. coli and S. aureus was determined by MIC and MBC values. Both MIC and MBC were measured according to the Clinical and Laboratory Standards Institute standards CLSI M07-A10 (2015) and CLSI M26-A (1999). The antibacterial activity of composite films against two kinds of bacteria was qualitatively tested by the film inhibition zone; 0.5 mL of 106 CFU/mL fresh bacterial bacteria solution was evenly coated on the nutrient agar (NA) plate in the clean bench. Then, 13 mm diameter of round punched RCF to CANF0.08 was attached to the surface of the plate. The plates were incubated at 37 ◦C for 48 h, and the inhibition zone diameter of the films was simply measured with a vernier caliper. The contact sterilization ability of silver loaded cellulose films against the two types of bacteria was determined according to the ISO 22196 (2011) standard. Approximately 106 CFU/mL of fresh bacterial bacteria solution was coated on the surface of the blank plate (RCF and CANF0.04), and covered with polypropylene films. After incubation at 37 ◦C for 24 h, the plate, film, and cover film were washed carefully using 20 mL nutrient broth (NB)/H2O eluent with a volume ratio of 1:100 (v/v); 0.5 mL of the eluate was then coated on the NA plate and incubated for 48 h at 37 ◦C with a humidity of >95% before the growth of bacteria was observed. 3. Results and Discussion 3.1. Analysis of Ag-NPs Morphology and Chemical Structure DMAc possess low ionization energy and electron affinity, which has a weak ability to reduce silver ions, resulting in low rate of silver nanoparticles form to crystal nuclei, and thus the small size Ag-NPs can be prepared [33]. After one hour of reaction, the size of 90.79% of Ag-NPs was approximately 3 to 8 nm in the solution (Figure 1a,b). Smaller Ag-NPs formed into clusters quickly, but not agglomerated to large particles, demonstrating that PVP as a surfactant effectively prevent the rapid agglomeration of Ag-NPs. The size distribution of 82.29% Ag-NPs was 13 to 28 nm (Figure 1c,d),PDF Image | One-Pot Synthesis of Antibacterial Silver Nanoparticle
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