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Senior Seminar Presentation
- 1. Internship at Glatfelter’s Corporate Analytical Services Gloria Chung CHEM 487 Senior Seminar DRAFT!
- 2. Introduction • What is Glatfelter? • History of Glatfelter • Known Products • Job Title • Papermaking Process • Routine Analyses (Kraft Chemical Process & Kraft Recovery Process) • Conclusion
- 3. What is Glatfelter? • Glatfelter is an increasingly global manufacturer of engineered papers and specialty papers. • Goal: To strive to expand in product development with the dedication to decreasing negative environmental impact. http://www.careersatglatfelter.com/portfolio-view/about-glatfelter/
- 5. History of Glatfelter • 1864: Founded as “P. H. Glatfelter Company.” • 1880: Glatfelter led the industry with the world’s largest paper machine. • Early 20th Century: Glatfelter became an industry leader in uncoated printing paper, used mainly in novels and trade books. • 2014: Glatfelter received a $5 million Economic Growth Initiative Grant and a $3 million Clean Energy Grant from Governor Tom Corbett to allow a conversion from coal to natural gas. Poindexter, Alysa. Corbett awards grants to York county manufacturer for natural gas conversion project. WPMT FOX43, 18 Sept.
- 8. Known Products Produced #1 Worldwide #1 North America Major Brands Tea Bags Postal Applications Keurig Single-Serve Coffee Playing Cards Swiffer Nonwoven Wallcovering Trade Book Publishing Post-It
- 9. Job Title • Analytical Chemist Co-Op / Intern • Tasks: • Qualitative and quantitative analyses • Chemical and physical analyses • Instrumentation • Sample preparation • Assisting senior chemists • Although we conduct analytical services for outside vendors and customers, most of our samples are for the company for weekly routine analyses.
- 10. Papermaking Process Sjöström, Eero, and Raimo Alén. Analytical Methods in Wood Chemistry, Pulping, and Papermaking. Berlin: Springer, 1999. Print.
- 11. Debarking • Log is brought to the debarking drum. • Wood is tumbled upon one another, so the bark is completely stripped off. http://www.loggingon.net/new-research-results-operator-impact-on-processor- productivity_news_op_view_id_411
- 12. Chipping • Cut debarked wood into 1” x 1” square wood chips. http://www.ohiovalleyveneer.com/OhioValleyChipping.aspx
- 13. Screening • Removes all bad woodchips (irregular chip samples based on size). • Uniformity of chips allows an increase in yield and quality. • Oversized chips are recycled by sending them back to cut to the desirable size or made into sawdust. • Sawdust is used to power the boiler and utilized as biofuel to generate electricity. • ~40% of the electricity in Glatfelter mills are produced by recycled/re- used biofuels in order to reduce dependency on fossil fuels. http://fox43.com/2014/09/17/corbett-awards-grants-to-york-county-manufacturer-for-natural-gas-conversion-project/
- 14. Kraft Chemical Process • Main Purpose: Convert woodchips to individual fibers (pulp). • Digester: Digest the lignin that holds the cellulose fibers together. • Washing: Pulp is washed with black liquor, washing away any undigested woods like knots. • Oxygen delignification: Oxygen is used to remove any remaining lignin, extracting any color from the pulp. • Bleaching: Brightens fibers from initial brownish color to white. Glatfelter CAS Image Pulp
- 15. Extractable of Pulp Samples • Two Types of Pulp: • Softwood (SWD): Long fibers ~3-7mm in length. • Provide the flexibility of the paper. • Hardwood (HWD): Short fibers ~1-2mm in length. • Provide the strength to the paper. • Both types can be used combined in several ways to make various specialty papers.
- 16. HWD (Hardwood) Pine, SWD (Softwood)
- 17. Experimental Procedure • Solvent Used: Dichloromethane (DCM) • Apparatus: Condenser, extraction thimble, round-bottom flask, chiller, hot plate. • Time: 5 hours to allow the extraction to occur for at least 20 times. • Purpose: To maintain product development and assist in quality control of purchased wood.
- 18. Prep Work
- 20. Weighing dish with both DCM and extractives. Weighing dish with just extractives. All the DCM evaporated
- 21. Kraft Recovery Process Glatfelter CAS Image
- 22. Kraft Recovery Process Green Liquor Na2CO3 Na2S Conc. Black Liquor Na2S Diluted Black Liquor Na2S White Liquor NaOH Na2S Wood Pulp
- 23. Black Liquor Feed • Composition: 14% - 18% solids. • 65% organic: sodium salts of lignin, resin and fatty acids. • 35% inorganic: sodium carbonate, sodium thiosulfate, sodium sulfide. • Removes and washes away undigested woods: knots, lignin, hemicellulose.
- 24. Black Liquor Feed • Purpose: To maintain concentrations of certain elements • Na • K • Ca • Al • Mg • Si • Soluble Ca
- 25. Experimental Procedure • Trial 1 (Na, K, Ca, Al, and Mg): HNO3 • Trial 2 (Si): HBF4, H3PO4, and HNO3 • Trial 3 (Soluble Ca): HNO3
- 26. Prep Work
- 27. Microwave Digestion • Digestion system that automates control of a single reaction chamber. • High Pressure & temperatures: 199 bar and 300°C respectively. “Milestone UltraWAVE microwave digestion system and Recirculating Chiller.” 2006. Web. 13 Dec. 2016.
- 29. ICP-OES • Inductively Coupled Plasma – Optical Emission Spectrometer • Detects metals at concentrations (ppm and ppb). • Benefits: • Can measure a range of elements in a single analysis cycle. • Automated, enhanced accuracy and precision.
- 30. ICP-OES
- 31. ICP-OES • Auto-sampler pumps sample to the nebulizer into a fine mist. • Portion of the sample goes down the drain.
- 32. ICP-OES • Nebulizer introduces sample to the torch with Ar- plasma at ~7,000 – 10,000°C. • Hot plasma excites the atoms to a higher state. • 99% of sample gets knocked out. • Only 1% of the sample gets ionized by the plasma.
- 33. ICP-OES • Excited atoms fall back down to the grown state emits a light which is characteristic to the metal. • Different wavelengths of light are separated by prisms and gratings. • Concentration of the element is measured by the intensity of the signal, which is proportional to the concentration of the metal.
- 34. Conclusion • Routine analyses are important in the paper industry. • Look for trends over time. • Kraft Recovery Process is economical. • Recycling used chemicals minimizes the addition of more chemicals. https://careers.smartrecruiters.com/Glatfelter1
- 35. Glatfelter Opportunities • Two co-op / intern positions available starting the summer. • Other co-op opportunities in both Spring Grove and York campuses: IT, law, OSHA, engineering, and much more! • Contact Korri Struble (HR): Korri.Struble@glatfelter.com • Deadline: Feb. 20th Glatfelter University: Real- world prep class (resume building, interview, networking, team collaborations, business finances, and meeting with the CEO of Glatfelter).
- 36. Acknowledgement • Dr. Kennedy • Dr. Rajaseelan • Dr. Mbindyo • Chemists at Glatfelter • Fellow Chemistry Students • Family and Friends
- 37. References "Apparatus for the Manufacture of Wood Pulp." Scientific American 12.299supp (1881): 4764-765. Web. ”Black Liquor" All the Methods & Services Provided by Econotechs Laboratories. N.p., n.d. Web. Jan. 2017. Buchanan, Michael. "Solvent Extractives of Wood and Pulp (Proposed Revision of T 204 Cm-97)." Chemical Properties (2007): n. pag. Web. Chandler, E. E. Apparatus for determining boiling points and freezing points of solvents. J. Chem. Educ., 1938, 15 (4), p 166. “Introduction to ICP-MS.” n.d. Web. “Milestone UltraWAVE microwave digestion system and Recirculating Chiller.” 2006. Web. 13 Dec. 2016. “Milestone UltraWAVE Microwave Digestion System and Recirculating Chiller | BridgePath Scientific." BridgePath Scientific RSS. N.p., n.d. Web. Feb. 2017. Poindexter, Alysa. Corbett awards grants to York county manufacturer for natural gas conversion project. WPMT FOX43, 18 Sept. 2014. Web. "Precipitated Calcium Carbonate (PCC)." Precipitated Calcium Carbonate (PCC). N.p., n.d. Web. Feb. 2017. Sjöström, Eero, and Raimo Alén. Analytical Methods in Wood Chemistry, Pulping, and Papermaking. Berlin: Springer, 1999. Print. Virtual Soil Science Learning Resources. Inductively Coupled Plasma-Optical Emission Spectrometer (ICP-OES). YouTube. April 6, 2014. Web. January, 2017. "What Is ICP-MS?... and More Importantly, What Can It Do?" Introduction to ICP-MS. N.p., n.d. Web. 06 Feb. 2017.
Editor's Notes
- What is Glatfelter? Glatfelter is an increasingly global manufacturer of engineered papers and specialty papers headquartered in York, Pennsylvania. Glatfelter’s everyday goal is to strive to expand in product development with the dedication to decreasing negative environmental impact.
- Glatfelter’s headquarters is based in York, Pennsylvania, with major mills in Spring Grove, Pennsylvania and Chillicothe, Ohio. Other U.S based locations include Ohio and North Carolina. International locations include Germany, France, China, and the Philippines.
- Glatfelter was founded as “P.H Glatfelter Company” in 1864. By 1880, Glatfelter led the industry with the world’s largest paper machine. In the early 20th century, Glatfelter became an industry leader in uncoated printing paper, often used in novels and trade books. In 2014, Glatfelter received a $5 million Economic Growth Initiative Grant and a $3 million Clean Energy Grant from Governor Tom Corbett to allow a conversion from coal to natural gas.
- Here is an image of the paper mill from over 150 years ago.
- Do any of these products look familiar to you?
- 40% of the U.S population touches a Glatfelter product every day. We are #1 Worldwide in tea bags, single-serve coffee, and nonwoven wallcovering. #1 in North America in postal applications, playing cards, and trade book publishing. Major brands that utilize our products include Keurig, Swiffer, and Post-It notes. What is trade book publishing? – A trade book publishing are --. Top quality, hardcover books, textbooks, etcs.
- At Glatfelter’s Corporate Analytical Services, I have the opportunity to be a co-op/intern. Although we conduct analytical services for outside vendors and customers, most of our samples are for the company for weekly routine analyses.
- This image shows the papermaking process from the start to finish. For my presentation, we will be focusing on 1) Wood Yard, 2) Digesting and Pulping, and 3) Washing – screening / Bleaching.
- At the wood yard, logs are brought into the debarking drum where they are tumbled upon one another. This allows the bark to be stripped off from the log.
- Debarked wood is then cut into 1” x 1” inch square woodchips. The size of the woodchip is crucial for the next step – screening.
- During screening, all irregular chip samples are removed based on size. The uniformity of chips is important because it allows an increase in yield and quality of the finished product. Any oversized chips are then recycled by sending them back to cut to the desirable size or made into sawdust. The sawdust is then used to power the boiler and utilized as biofuel to generate electricity. ~40% of the electricity of Glatfelter mills are produced by recycled/re-used biofuels in order to reduce dependency on fossil fuels.
- From here, the wood chips go through the… Kraft Chemical Process, which is a process to convert woodchips to individual fibers. It starts in the… Digester: Steam and white liquor are both used to bring the temperature in the digestion process to ~170°C; therefore, increasing the pressure. This digests the lignin that holds the cellulose fibers together. Washing: The pulp is then washed with black liquor. Black liquor washes away any undigested woods like knots from the pulp. It is also recycled and re-used. Oxygen Delignification: Oxygen delignification is where oxygen is used to remove any remaining lignin. Oxygen delignification also extracts any color from the pulp, so less chemicals are needed during the bleaching process, making this a significant environmental improvement. Bleaching: Bleaching is what brightens fibers from its initial brownish color to white. This is what gives paper its clean, bright white color which can then be used to make colored paper. If the bleaching process did not exist, paper products would have a brownish color similar to brown paper grocery bags. Benefits of the Kraft Chemical Process include the adaptability to all wood species, efficient chemical recovery system, high quality pulp, and lower manufacturing cost.
- Softwood (SWD): Are long fibers usually ~3-7mm in length. They provide the flexibility of the paper. Hardwood (HWD): Are short fibers usually ~1-2mm in length. They provide the strength to the paper base, and are also less expensive. Both softwood and hardwood can be used in combination to make various specialty papers. The next couple of photos that you see in my presentation are what I took in the lab during work.
- Here are examples of how samples are received for analysis. Initially, the pulp samples are wet; therefore, we have to let the samples sit out for about three days to ensure that they are completely air-dried. As you can see, the softwood has longer fibers while the hardwood are more compact almost popcorn like.
- The experimental procedure done for pulp extractables consist of a simple extraction with the solvent dichloromethane. Dichloromethane extracts non-volatile materials in pulp like waxes, fats, resins, sterols, and non-volatile hydrocarbons. The apparatus consist of a condenser, extraction thimble, round-bottom flask, chiller, and a hotplate. The amount of time it takes to finish the extraction is about 5 hours to give us a total of 20 extractions. The purpose is to maintain product development as well as assist in quality control of manufactured pulp. During these extractions, we are looking for defoamers and pitch. High deposit of defoamer and pitch react with calcium carbonate to form fatty acid salts, which can cause issues. Pitch = binding agent from wood (resin, fatty acids) We are checking for a trend on whether the pitch is high or down, or whether we are using too much defoamer or not enough defoamer. If we don’t maintain a specific trend, it can cause issues such as debris and a change in flow rates, which can mean the equipment will not operate properly. ------- During these extractions, we are looking for defoamers and pitch which is often wood resins. High deposit of silicon defoamer and fatty acids salts from pitch are an issue because fatty acid in wood resins released by pulping reacts with calcium carbonate to form fatty acid salts.
- To accurately determine the % ext of the pulp, we determine the %solids for each sample by comparing the air dry and oven dry weight of the sample. ~7g of pulp sample is placed in the extraction thimble.
- ~150mL of DCM is placed in the round-bottom flask along with 5 glass beads. The hot plate heats the dichloromethane and an extraction occurs due to the apparatus. After about 20 extractions, which is about 5 hours, I remove the round bottom flask from the apparatus and let the DCM in the round bottom flask evaporate, leaving about 40mL of the solution left. I would place the 40mL of the DCM and extractives in a pre-weighed weighing dish and rinse the round-bottom flask with ~30mL of DCM and also place the rinse in the weighing dish. The weighing dish is left in the hood over night, letting the DCM fully evaporate leaving just the extractives behind. The weight of the extraction helps us determine the percent of extractables in the pulp sample. _________ Based on the many reaction runs and results, HWD has more %ext than SWD. DCM: CH2Cl2 In the past used other organic solvents: ethanol, acetone, and benzene.
- Top image: weighing dish with both DCM and ext. This is left in the hood over night, so the DCM can evaporate. Bottom image: After leaving the weighing dish overnight in the hood, you’re left with only the ext. The DCM evaporated.
- The Kraft Chemical Process, which is this part of the image, is utilized to produce pulp. Additionally to this process is a Kraft Chemical Recovery Process, which is denoted in the red dots. Within the Kraft Recovery Process is the importance of recycling the black liquor feed.
- So here is the chemistry behind the Kraft Recovery Process. The Kraft Recover Process is a continuous loop of… In the recovery boiler, all the lignosulfinates and other oxidizing forms of sulfur, such as thiosulfate, is converted to sodium sulfide by reduction. The organic is also burned to yield sodium carbonate. Both are the components of green liquor. In the causticizing plant, the green liquor is reacted with calcium oxide, which is lime. The sodium carbonate in green liquor generates calcium carbonate (aka lime mud) in the causticizing plant. The lime mud is then taken to the lime kiln, where... CaCO3 + heat CaO + CO2 Calcium oxide goes back to react with the green liquor to make white liquor and also more lime mud. Carbon dioxide is taken back to the precipitated calcium carbonate plant (PCC Plant), where it reacts with lime to make a highly shaped form of calcium carbonate. This highly shaped form of calcium carbonate is used in the paper machine often as a filler, where it is less expensive than fiber and also creates opacity in paper.
- Black Liquor’s composition is anywhere from 14% to 18% solids. Of the solids, 65% of it is organic in nature. Examples of this are sodium salts of lignin, resin and fatty acids, acids from carbohydrates. The remaining 35% of the liquor is inorganic, which is from chemicals in the white liquor. Examples of this are sodium carbonate, sodium thiosulfate, sodium sulfide, and sodium hydrosulfide. Black liquor is used in the Kraft Process to remove and wash away any undigested woods, such as knots, lignin, hemicellulose. Its purpose is to free the fibers in the cellulose.
- It is important to test the black liquor on a weekly basis to maintain concentrations of certain elements. In the black liquor feed analysis, we test for concentration levels of these different metal elements Na – mainly used to determine balance for sodium to carbonate for following the inert deadload. The inert deadload is unnecessary because it costs money to heat and flow the weight. K – is often eutectic to form which makes the liquor stick to the recovery boiler. The liquor comes out in jets and get sprayed out to the pulp. We want to maintain a fine mist; however, stickiness of the liquor clogs the jets. Eutectic: relating to or denoting a mixture of substances (in fixed proportions) that melts and solidifies at a single temperature that is lower than the melting points of the separate constituents or of any other mixture of them.) Ca – used to determine calcium carbonate potential. Calcium carbonate causes scaling on evaporators and everywhere else in the system. It is a weird material because with heat it becomes less soluble. It will come down and plate on the evaporators making it less efficient with heating. Al & Si – determine clay and dirt Mg – comes in wood, but it can also form some carbonate salts; however, not as much as calcium. Soluble Ca – potential for scaling. It is waiting there ready to precipitate down. Difference between Ca (total) and Soluble Ca: Soluble: already formed Ca (total): the potential Shorten
- Black liquor samples are received weekly. We do three different test runs on each sample. The first test run determines Na, K, Ca, Al, and Mg. The second test run determines Si, and the last test run determines soluble Ca. Samples are prepped for digestion with different chemicals. Trial 1 (multi-element): Nitric acid Trial 2 (Si): Fluoroboric acid, phosphoric acid, and nitric acid Trial 3 (soluble Ca): Nitric acid
- Once the samples have been prepped, we utilize the Ultrawave microwave digester to digest the samples completely in a nitric-water bath. On the left: the samples have all the reagents. On the right: the samples after digestion.
- The Ultrawave microwave digester is designed to digest difficult samples, especially metals prep. The automatic digestion system offers a single reaction chamber made out of high-performance stainless steel for higher pressures and temperatures of up too 199 bar and 300C respectively.
- Samples are placed in a rack and lowered automatically into the microwave chamber, where a chamber clamp is placed to secure digestion process. Before the microwave energy is applied to the chamber, the chamber is pre-pressurized to prevent sample boiling with inert gas. The microwave energy is applied to all samples under the same pressure and temperature. At the end of the digestion, the samples are cooled. The digested samples are then filtered and necessary dilutions are made before placing the sample solutions into ICP tubes.
- The ICP-OES, inductively coupled plasma – optical emission spectrometer, detects metal at concentrations which we use ppm and ppb. One benefits of this spectrometer is that it can measure a range of element, even low levels on difficult metals like silicon and boron, in a single analysis cycle. Another benefit is that it can be automated with enhanced accuracy and precision throughout the analysis.
- For the ICP-OES… We utilize an auto-sampler Different types of nebulizers Glass vs. Teflon – we often use glass; however, when using reagents like fluoroboric, we utilize the teflon nebulizer because fluoroboric reacts with the glass. We also use teflon test tubes, volumetric flasks, and funnels when handling with HF during the digestion and dilution process. Standards are prepared monthly, with different samples for each analytical method.
- Using the auto-sampler, the sample gets pumped into the nebulizer, where it the sample gets turned into a fine mist. A portion of the sample goes down the drain, so it is important to have the tubing correctly placed on the motor.
- The nebulizer introduces the sample to the torch with Argon-plasma, which is ~7,000 – 10,000C. The hot plasma excites the atoms to a higher state. 99% of the sample gets knocked out by the plasma, and only less than 1% of the sample gets ionized with the plasma. -------
- When the excited atoms fall back down to the grown state, they emit a light which is characteristic to the metal. The wavelengths from different metals are emitted and it goes into the OES spectrometer. Different wavelengths of light are separated by prisms and gratings. It then goes onto the detector and the information is shown on the computer. The concentration of the element is then measured by the intensity of the light and wavelength. The intensity of the signal is proportional to the concentration of the metal, and this is compared to the standards. -----
- Season change impacts the industry Winter: frozen logs Summer: heat
- Dr. Kennedy & Dr. Rajaseelan – advisement and guidance throughout my years here at Millersville Dr. Mbindyo – advisement for both internships completed during my time here at Millersville. Helped me find this internship. Chemists at Glatfelter – teaching me great analytical lab skills and letting me utilize my knowledge in chemistry to real life work experience, as well as mentoring me throughout my last year at Millersville. Fellow Chemistry Students – for making this all enjoyable Family & Friends – for all there support