FTIR and DSC of polymer films used for packaging: LLDPE, PP and PVDC

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1 FTIR and DS of polymer films used for packaging: LLDPE, PP and PVD John Petrovich SHAPE American High School Abstract: Polymers are compounds used in various materials. There are a plethora of methods used to analyze the composition and other properties of the material; these include Fourier Transform Infrared Spectroscopy (FTIR) and Differential Scanning alorimetry (DS). The profiles of the DS display varying melting peaks and glass transition regions for different samples. This indicates that DS can be used to determine different qualities of polymeric materials which include, but are not limited to, high density character, low density character, amorphousness, and semi crystallinity. We found from the DS profile that the melting point for various polyethylene samples range from approximately degrees. The DS profile for the polypropylene (PP) shows peaks at 163 and 156 degrees at the main and secondary melting peaks respectively. The DS profile for Stretch-Tite does not even have melting peaks. It instead has glass transition regions found at approximately 60 and 95 degrees. The lack of a melting peak in the polyvinylidene chloride (PVD) sample is indicative of an amorphous polymer. Introduction: Polymer films are extensively used commercial packaging. Species used in packaging include, but are not limited to polyester (PET), polyamide, polyvinyl chloride (PV), polystyrene (PS), polypropylene (PP) and polyethylene (PE). Polyethylene can form with different densities. These include low density (LDPE), linear low density (LLDPE), medium density (MDPE), high density (HDPE), and ultra-high density (UHDPE). It is possible for samples of LLDPE to take on characteristics of either LDPE or HDPE. Polymers can exist in two different morphologies while in a solid phase: o Amorphous: Molecules are randomly oriented within the polymer. These polymers can easily be altered in shape and generally exist in a rubbery state. o Semi crystalline: An arrangement of ordered molecules with some amorphous regions. These polymers are stiff and exist in a glassy state. This paper is focused on answering the following hypotheses: Hypothesis: an we utilize DS and FTIR data to determine why different LLDPE samples exhibit properties similar to either LDPE or HDPE? an one identify whether a polymer material is crystalline or amorphous based upon DS melting temperature data? 1

2 Samples: The pictures of the polymeric material samples that we used in this experiment are shown in figure 1. These samples are used in the physical state seen in the pictures. (a) (b) (c) (d) (e) (f) Figure 1: (a) Ziplock Sandwich Bags, (b) PE-LD bag with recycling code 4, (c) Glad wrap with adhesive side, (d) Act II popcorn bags, (e) Stretch-Tite Saran Wrap, (f) Walmart Bag Differential Scanning alorimetry (DS): DS is a method of analysis that allows the user to measure glass transition, melting temperature, and crystallization temperature while a polymeric material sample is being heated or cooled. Each polymer film tested had a specific melting and recrystallization point that was reflected in the DS as an endothermic and exothermic peak, respectively. During our research, we subjected various samples through a heating phase, a cooling phase, and another heating phase. We used a TA Instruments DS (Model Q2000) using low mass Aluminum sample pans and a sample weight with a mass of approximately 2-3 milligrams. The polyvinyl chloride sample was heated/cooled at a rate of 20 degrees centigrade per minute. All other samples were heated/cooled at a rate of 10 degrees centigrade per minute. For the data analysis of the DS profiles, TA Universal Analysis 2000 was used. Fourier Transform Infrared Spectroscopy (FTIR): FTIR is a spectroscopic method of analysis where IR rays are absorbed by bonds in a molecule. These IR ray s energy can be related to the vibrational energy of different bonds found within different functional groups in a compound. To provide a few examples, one might 2

3 be able to find a relatively large O-H peak at approximately cm-1. Another prominent example that can be seen in a plethora of polymer samples in the carbonyl functional group peak (=O) which occurs at about cm-1. s in lower energy areas on an FTIR graph are collectively known as the fingerprint region. Each region is unique for an individual compound and are thus extremely helpful in comparisons between different FTIR graphs. The exact model used in this research was the Perkin Elmer (Model Spectrum Two) for taking spectrum data in the wavelength range of cm-1. Samples were prepared by cutting 3 cm in diameter from each film and taping it to a Rensselaer Summer Program business card. Results: FTIR: The first portion of my research involved placing my samples into a FTIR spectrophotometer in hopes of revealing differences in functional groups between the various polymers. The following IR spectra are from those that I prepared with the assistance of various teacher s assistants: (a) Ziplock Bag (PE) (b) Bag PE-LD (PE) (c) Glad Wraps with Adhesive (PE) (d) Walmart Bag (PE) 3

4 (e) Act II Popcorn Wrapper (PP) (f) Stretch-Tite Wrap (PVD) FTIR spectra from previously published polymer chemistry literature is seen below. Due to a lack of HDPE or LDPE specific LLDPE FTIR spectra, comparison with the samples above was done with regular HDPE and LDPE spectra: Low Density Polyethylene: 4

5 High Density Polyethylene: Polypropylene: 5

6 Polyvinylidene hloride omparing my LLDPE-LDPE IR spectra with the example from previous literature, one might tell that the same functional groups are present, but their respective peaks are of slightly different proportions. One must recognize that the comparison is between LLDPE-LDPE and LDPE, and a differentiation in the amount of branching in both samples accounts for some of the different proportions in peaks. Another reason for this might be due to the fact that our experimental samples had color additives within them. This particular possible source of error can be seen when the peak is fatter than the established reference. Something similar occurs when comparing the experimental LLDPE-HDPE samples with the established reference from previous literature. This is particularly evident in the Walmart Bag sample. The aromatic -H peak approximately at 2900 cm-1 is particularly thick when compared to findings of the European ommission. This thickness is due to the grey color additives found in the Walmart bag. The experimentally determined IR spectrum for PP that we generated varied a great deal from the spectrum from the other literature. Most of the same functional groups are still present, but there are distinct curves in the profile that are not present from the spectrum generated by the European ommission. These curves are due to the sample that we used being of a relatively high thickness. It is also worth mentioning a strange fingerprint region not present in the reference spectrum. This could possibly be due to additives or contamination, a much less likely possibility considering the sample had been disinfected in a Suprasil ozone/uv oven. When one compares the LLDPE-HDPE and LLDPE-LDPE spectra, they lack any noticeable difference in structure. The only exception would be the inclusion of additional thickness/length to peaks due to additional branching in some samples. In a similar manner, FTIR didn t provide much information concerning levels of crystallinity of polypropylene and polyvinylidene chloride besides its structure. The FTIR 6

7 spectra generated in this experiment were similar to those determined by the European ommission except for the fact that the fingerprint regions are of slightly different proportions. This could be due to color additives, additional branching, or the reflection of IR light from the sample due to its thickness. DS: The second portion of my research involved putting my samples in a Differential Scanning alorimeter in order to determine melting temperature. Ziplock Bag (LDPE-like LLDPE) Tm() nd Ziplock Bag (LDPE-like LLDPE) Tm(ary) Degree 2 nd Degree

8 For this LDPE-like LLDPE DS profile, notice that both the Tm(main) and Tm(secondary) peaks are found around degrees. Also notice that both DS profiles have a distinct second peak. This peak exists due to differentiating densities throughout the polymeric sample. PD-LE Bag (LDPE-like LLDPE) Tm() PD-LE Bag (LDPE-like LLDPE) Tm(ary)

9 For this sample, both main and secondary temperature peaks fall around 120 degrees. Both DS profiles also have an additional peak due to a differentiation in density within the polymer sample. Glad ling Wrap (HDPE-like LLDPE) Tm() N/A Glad ling Wrap (HDPE-like LLDPE) Tm(ary) N/A

10 This HDPE-like LLDPE sample only has one noticeably melting peak in both DS profiles. This is a stark contrast with the two peaks experienced in the LDPE-like LLDPE samples. It is also worth mentioning that the melting peak is found at a higher temperature (~130 ). This is higher than the value determined for the LDPE-like LLDPE samples. Walmart Bag (HDPE-like LLDPE) Tm() N/A Walmart Bag (HDPE-like LLDPE) Tm(ary) N/A

11 Notice that the melting peaks for this HDPE-like sample is also close to 130 degrees. The fact that this sample along with the other HDPE-like sample above have melting peaks nearly ten degrees higher may indicate that these species are highly ordered with little branching. Act II Popcorn Wrapper (PP) Tm() Act II Popcorn Wrapper (PP) Tm(ary) N/A

12 In this polypropylene sample, we experienced an anomaly at the main melting peak during the initial heating. As seen in the first DS profile on the page, there is an additional melting peak not observed in the graph directly above. This is most likely due to residual reactants from its synthesis or contamination before analysis. The second peak at approx degrees can be attributed to this residue burning away. Stretch-Tite Wrap (PVD) Tm() 1 st Glass Transition 2 nd Glass Transition For this PVD sample, it is important to note that it lacks a melting peak. The lack of a distinctive melting point indicates that the sample has a greater amorphous character than it does crystalline. Instead of a melting peak, the polymer film has two glass transitions, the first occurring at approximately 61 degrees and the other occurring at approximately 95 degrees. ompared to the established literature, the glass transitions are extremely high for the agreedupon glass transition temperature for PVD falls around 16 degrees. This difference in glass transition temperature range can be accounted for if one considers the additives that could be present in the Stretch-Tite wrap. 12

13 onclusion: In this research project, we created various samples from polymeric materials and ran them through FTIR spectroscopy and Differential Scanning alorimetry. I did so with the intent of discovering whether or not one could determine why LLDPE could exhibit LDPE or HDPElike characteristics. I also carried out this research with a secondary intent of being able to determine whether or not a polymeric sample was amorphous or semi crystalline just from reading DS profiles. Seeing as FTIR analysis did not provide much insight as to why LLDPE exhibits HDPE or LDPE like characteristics past structure, I put the samples through DS. For the Ziplock bag and PE-LD bag (LDPE-like LLDPE samples), their DS profiles show two distinct melting peaks that occur at approximately 110 degrees and 120 degrees respectively. For the Glad adhesive wrap and the Walmart bag (HDPE-like LLDPE samples), the DS profiles show one distinct melting peak that occurs closer to the degree range. The fact that the HDPE-like LLDPE samples melting peaks occur a temperatures ten degrees higher than LDPElike LLDPE samples agrees with the idea that HDPE samples are more highly ordered with less branching. This piece of evidence supports the portion of my hypothesis where DS can effectively be used to determine why LLDPE can exhibit HDPE and LDPE character. The DS profile for the popcorn wrapper (PP) shows peaks at 163 and 156 degrees at the main and secondary melting peaks respectively. The DS profile for Stretch-Tite does not even have melting peaks. It instead has glass transition regions found at approximately 60 and 95 degrees. The lack of a melting peak in the PVD sample is indicative of an amorphous polymer, and thus confirms the hypothesis that DS melting temperature data can be used to confirm whether a sample is crystalline or amorphous. Further research that could conducted involves exposing the samples to thermogravimetric analysis to see the level of thermal degradation. This would be especially helpful in making firmer conclusions concerning the contamination found in the PVD sample. Acknowledgements: I would like to thank the Research in Polymers Program at Rensselaer Polytechnic Institute as well as the National Science Foundation (Award Number ). I would also like to thank Dr. Ryu, Dr. Ma, Sara Till, asey Wong, Miriam Shao, Ben Stovall, my fellow high school research classmates, the SHAPE American High School Science Department (particularly Todd Mitchell), and my family for their generous support. References: [1] M.A Peltzer and. Simoneau OL Identification of Polymeric Materials European ommission Joint Research enter, Institute for Health and onsumer Protection (ISBN ) Publication Office of the European Union (2013). [2] Thomas, L.. haracterization of Phenomena in Linear Low Density Polyethylene by Modulated DS. TA Instruments, Inc. 13

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