Location: Cotton Structure and Quality Research2016 Annual Report
Objective 1: Enable, from a technological standpoint, new rapid and accurate commercial methods to assess cotton fiber quality. Objective 2: Enable economical, accurate and real-time methods to assess product quality and process efficiencies in pre-mill operations. Objective 3: Enable new commercial methods to detect, quantify and remove undesirable non-lint materials such as various sugars, seed coat fragments, non-leaf plant trash, etc. from cotton. Objective 4: In collaboration with industry partners, determine the impact of fiber quality and fiber processing practices on yarn and fabric quality and processing efficiencies. Objective 5: In collaboration with industry partners, determine the expected impact of new germplasms, agronomic practices, and ginning practices upon fiber quality, textile processing efficiency, and final product quality.
The U.S. cotton and textile industries agree on the need to increase U.S. cotton’s value and global competitiveness. It is proposed that this need be met by enabling new technologies and methods for accurately assessing the quality and processing efficiencies of cotton fiber at various processing stages from field to fabric. The first objective addresses the need for new rapid and accurate fiber quality assessments in the laboratory. Comprehensive evaluations will be conducted to broaden the technical and commercial attractiveness of image analysis, spectroscopy, microscopy, and color technologies to discern new measurements, with initial emphasis on 3-dimensional color, maturity, fineness, fiber diameter, fiber structure, and the relationship of these properties to key fiber quality properties. The second objective addresses the need for economical, accurate and real-time methods to assess product quality and process efficiencies outside of the laboratory in pre-mill operations. Comprehensive evaluations with state of the art spectroscopy and imaging instrumentation will be conducted to develop new quality measurement and monitoring methods for pre-harvest and post-harvest applications and operations. The third objective addresses the need for new assessments of non-lint materials and contaminants to provide improved tools for measuring, controlling and removing these non-lint materials. The development of rapid, accurate and non-destructive image scanning of seed coat fragments (SCF) and seed coat neps (SCN) will be developed, and these techniques will be used to understand what the AFIS is sensing when measuring SCN in fiber. Comprehensive evaluations with advanced chemical imaging spectroscopy technologies will be conducted to establish rapid detection and trash type identification protocols. State-of-the-art elemental analysis, chromatography, and spectroscopy technologies will be used to develop chemical measurements of fiber surface species, to include metal ions, sugars, amino acids/proteins, pectins, and waxes. These properties will be correlated to properties impacting fiber processing efficiency (i.e., stickiness and fiber friction). The fourth objective addresses the need for determining fiber quality-processing practices relationships and their impacts on product quality and processing efficiencies. In-house traditional and non-traditional quality measurements and textile processing will be used to determine the efficacy of these tests to predict processing efficiency and yarn/fabric quality and to understand the impact of fiber properties and processing on textile quality and efficiencies. The fifth objective addresses the need for determining the fiber quality-processing efficiency-product quality relationships. Comprehensive evaluations will be conducted on new germplasms using fiber quality and miniature-scale ring spinning. Advanced spectroscopic technologies will be used to characterize developing cotton fibers and their fine structure, their cell walls and physical properties.
The sophisticated Fourier transform infrared (FTIR) technique was examined as a simple and direct method to characterize cotton fiber growth and development, using sophisticated statistical tehniques. ARS scientists in New Orleans, LA, developed new FTIR techniques to characterize cotton fiber growth and development. The results indicated that the FTIR method has the potential for rapid, routine, non-destructive, and direct assessments of fiber development for cotton physiology and breeding applications, which could benefit cotton genomics researcher who at times produce only limited amount of fibers. Commercial cottons contain some degree of non-lint related contaminants (or trash) that reduces cotton market value and may require further cleaning steps. There is an interest in the relationship between High Volume Instrument (HVI) leaf grade and gravimetric trash content (weight and percentage of trash in the sample). ARS scientists in New Orleans, LA, determined the correlations between three Shirley Analyzer gravimetric trash content measurements (mass percentage; SAvisible, SAinvisible, and SAtotal) and the leaf grade categories determined by near infrared (NIR) spectroscopy. A general trend was observed of increasing SAvisible and SAtotal content with increasing leaf grade. Excessive seed meats and oils within a cotton sample cause processing problems for textile mills and can mimic a more harmful condition that is due to excessive insect deposits. ARS scientists in New Orleans, LA, have made progress in the implementation and refinement of a method to rapidly screen for the presence of seed meat materials in cotton samples by use of a sophisticated Fourier transform infrared (FTIR) method. This technique allows end users to appropriately respond to processing issues by identifying a cause of the issues. Quality measurements that can be performed both in and outside the laboratory (at-line, field, etc.) are desired by the industry. ARS scientists in New Orleans, LA, developed improved near infrared (NIR) spectroscopy methods, using micro NIR instruments, to measure micronaire and its components, maturity (cell wall development) and fineness (linear density or size) on ginned fiber and seed cotton (pre-ginning), both in and outside the laboratory (greenhouse). Method agreements between methods were very good, and techniques were developed to minimize the effects of different cotton varieties, the cotton seed itself, and temperature-humidity changes on the NIR results. Typically, laboratory fiber moisture content (MC) is measured on ginned fiber using an oven to dry the fiber. Laboratory fiber MC by microwave, using the microwave instrument, was established by ARS scientists in New Orleans, LA, for ginned cotton fiber. The program was expanded for the measurement of seed cotton at the gin (cotton prior to ginning). ARS scientists in New Orleans, LA, developed preliminary, rapid laboratory microwave MC measurement methods for seed cotton. Method agreement between the microwave MC and oven drying reference method was good. Additional samples to improve calibration robustness are being obtained. The Cottonscope instrument measures fiber maturity, fineness, and ribbon width. Cottonscope measurements were made on over 850 cottons from 3 crop years and from several states by ARS scientists in New Orleans, LA, to evaluate overall agreements between the Cottonscope and Advanced Fiber Information System (AFIS; a standard measurement) maturity and fineness results. The Cottonscope maturity and fineness range and variability indicated that the AFIS was less responsive to changes in MR and fineness compared to the Cottonscope. Seed-coat neps are seed-coat fragments with attached fiber that remain with the fiber during processing into fabrics, and are detrimental to yarn and fabric quality. ARS scientists in New Orleans, LA, developed a new technique to evaluate the impurity levels sensed by the existing instrument. Various sizes, shapes, types, and samples from various parts of the seed surface were measured, one spiked fragment at a time added and ‘fixed’ in different cotton fiber variety carrier slivers (strands of fibers). Instrumental results demonstrated that errors could occur in seed-coat nep counts. Seed-coat fragments were also weighed prior to and after testing, with significant weight losses noted. The preliminary study also showed cotton variety influences instrumental response and recovery of spiked seed-coat fragments. ARS scientists in New Orleans, LA, previously developed the American Society for Testing and Materials (ASTM) International standard test method for water in lint cotton by Karl Fischer Titration (D7785). The test specimen is sealed in a glass vial with an aluminum crimp cap. The ARS scientists demonstrated the sealed vials leak water vapor over a five day period. If sample integrity could be maintained in the sealed container for several days, cotton researchers without the testing equipment could ship the samples to sites with the apparatus, providing reduced cost and industry wide access to this method. ARS scientists developed a practical means to manage the leak, in which the vials were placed in a closed aluminum foil envelope. The technique maintained the initial water level in the specimen for five days. Presently, a labor-intensive, time-consuming Soxhelet extraction method is used to determine the wax content on the surface of raw cotton fiber. In order to increase productivity and decrease analysis time, ARS scientists in New Orleans, LA, are developing an improved method, using Accelerated Solvent Extraction (ASE), for the extraction and quantitation of surface waxes. The ASE method greatly reduces the extraction time. Method optimization is underway (cycle time, temperature, etc.) on the ASE extracted material to reduce the time required to separate waxes from the rest of the extracted material (sugars, pectic substances, etc.). The metal ions present on cotton may impact fiber properties and fabric dyeing. The sophisticated technique of Inductively Coupled Plasma-Optical Emission Spectroscopy (ICP-OES) is used to determine metal content. ARS scientists in New Orleans, LA, developed an ICP method to measure eight metal ions on cotton. For cotton varieties grown at the same location with two types of field irrigation (irrigated and rain fed), the concentrations of metals were compared and correlated with the High Volume Instrument (HVI) cotton quality parameters. Statistical analyses revealed that a cotton variety effect was the largest influence on the correlations between the HVI quality parameters, metal ions content, and the two irrigation levels. The structural arrangement of cotton and impact of fiber moisture are of interest to cotton breeders and geneticists. ARS scientists in New Orleans, LA, developed Fourier transform infrared (FTIR) spectroscopy techniques to measure fiber cell wall growth and development. Cotton fiber bundles were exchanged with heavy water (deuterium oxide) to examine differences in their FTIR spectra. The organization of the cellulose in the cotton fibers was similar regardless of the relative humidity or the cell wall development of the fiber. What differed was the amount of cellulose, not its structural arrangement. It was observed that fibers with higher water content demonstrated higher fiber strength and elongation. Cotton breeders and geneticists are interested in rapid and accurate assessments of cotton fiber chemical changes that occur during fiber growth and development, to include cell wall development. ARS scientists in New Orleans, LA, have developed FTIR micro-spectroscopy and chemical imaging techniques (single fibers) to examine the cell wall development of cotton fibers. FTIR spectra and the chemical images can show differences between immature and fully developed mature fibers that show promise in future fiber maturity determinations. Macro-sampling of cotton fiber bundles (multiple cotton fibers) was also performed utilizing a high resolution detector. Miniature-scale processing was further refined by ARS scientists in New Orleans, LA. Intended to replicate commercial processing using 30 grams of fiber instead of bale (106kg) quantities, it allows additional information to be gathered on the true quality of cotton fiber which is not necessarily reflected using existing laboratory testing methods. Samples of the National Cotton Variety Trials (NCVT) breeder trials (ARS and university cotton breeders) and additional samples from ARS researchers were processed through the refined miniature-scale processing (over 1,500 samples). Miniature-scale processing provides crucial information in assisting breeders in making variety selections for improved cotton varieties, and provides feedback on the efficacy of newly developed laboratory fiber quality tests. Changes to cotton production practices (irrigation, harvesting and ginning practices, etc.) impact cotton fiber quality. Small-scale processing trials, utilizing less than bale quantity (106kg)of cotton fiber on full-scale processing equipment, was utilized by ARS scientists in New Orleans, LA, on over 300 samples. These trials provided commercial quality results for the impact of production practices on cotton textile processing quality and efficiency. The data from small-scale processing trials has provided critical feedback to production practice research for ARS scientists at multiple ARS locations and have also been used to assist the U.S. textile industry in addressing production challenges to aid the domestic industry in remaining competitive with global competitors.
1. Cotton fiber maturity and crystallinity determination. Fiber maturity and crystallinity are important fiber characteristics, and they are determined by two separate measurements. A number of methods have been developed to determine cotton chemical structure (e.g., maturity and crystallinity), but their accuracy and suitability are subject to debate. In addition, the standard crystallinity measurement using X-ray diffraction techniques is very labor intensive and time consuming. Much interest has been expressed, primarily by cotton breeders and geneticists, for rapid, simultaneous measurements of maturity and crystallinity. ARS researchers at New Orleans, Louisiana, developed sophisticated Fourier transform infrared (FTIR) techniques to directly determine the cotton maturity and crystallinity simultaneously. The FTIR method yields accurate results and takes less than 5 minutes for the simultaneous measurement of maturity and crystallinity with a very small sample mass (as little as 0.5 milligrams). This method benefits and is used by cotton breeders and geneticists who at times produce only limited amount of fibers.
2. Cotton micronaire (measure of fiber maturity and size or fineness) prediction. To acquire fiber quality data on thousands of fiber samples from one crop-year, cotton breeders must ship the samples to fiber quality laboratories where current-in-use systems (such as the High Volume Instrument or HVI) are available. It is both desirable and beneficial for cotton breeders if robust and cost-effective alternatives or complements (such as near infrared (NIR) spectroscopy) to these laboratory methods/systems are available. Previous studies by various researchers have indicated the potential of NIR technique to determine micronaire rapidly and accurately. ARS researchers at New Orleans, Louisiana, found that an NIR model developed from earlier crop-year cottons enabled the accurate and quantitative prediction of fiber micronaire in new crop-year cottons. Cotton samples from earlier crop-years were used to develop calibration models for micronaire, and these calibrations were used to predict micronaire on later crop-year cotton samples. Further, the results determine the similarity or dissimilarity of cotton fibers harvested at differing locations over consecutive crop-years by using sophisticated statistical techniques.
3. Fiber strength vs. yarn strength relationship. Cotton yarn production and quality is one of the most critical elements in assessing the end-use quality of raw cotton fibers. Since yarn manufacturing requires specific heavy equipment, is labor-intensive and time-consuming, and uses a large amount of cotton fibers, substantial research has been performed to optimize the methods of predicting yarn performance from available properties of raw fibers through sophisticated statistical techniques. Unlike earlier less sophisticated regression approaches, ARS researchers at New Orleans, Louisiana, proposed a relatively simple and semi-qualitative screening method for a rapid comparison of yarn strength or tenacity (strength/yarn size), either within or between the varieties, directly from fiber quality results that are obtained from the primary and routine High Volume Instrument (HVI) measurements. The relationships between HVI fiber quality components (length, short fiber, etc.) and fiber strength and yarn tenacity were examined. The results indicated that the short fiber content index (SFI) had a more significant effect on the correlation between corrected yarn tenacity and corrected fiber HVI strength than other HVI fiber quality measurements. These results allow cotton scientists, growers, and fiber processors to estimate the potential yarn strength property of their cotton crops without further fiber spinning process, directly from HVI fiber qualities.
4. Plant and insect sugar analyses. Analysis of plant and insect sugars has grown in importance to the fiber and textile industries (color development, stickiness, etc.). An improved sugar measurement was developed and implemented by ARS scientists in New Orleans, Louisiana, using an Ion Chromatography IC method. Previous research showed certain ratios of the insect sugars melezitose and trehalulose deposited on cotton surfaces are indicative of either whitefly or aphid insect contamination, which may cause problems during cotton processing. Since raffinose and sucrose are isomers of melezitose and trehalulose, respectively, it can be difficult to fully separate them from the entomological sugars using IC, especially when the analysis time is shortened. Obtaining reliable IC values for those surface sugars is paramount in detecting a contamination and for informing textile stakeholders of cotton surface characteristics. These findings serve as proof-of-concept that improving the separation may elucidate useful information about constituent sugars on cotton. Several stakeholders are using sugar results from the new IC method.
5. Precise measurement of fiber stickiness. Specific levels of the short chain sugars melezitose and trehalulose deposited on the surface of cotton fibers are indicators of whitefly or aphid insect contamination. These deposits can cause stickiness problems during cotton ginning and textile processing. Cotton stickiness is highly complex, but surface sugars may play the largest role in manifesting an issue. ARS scientists in New Orleans, Louisiana, developed an ion chromatography (IC) method to identify and quantify and create sugar profiles of nine sugars of interest present in cotton: inositol, trehalose, glucose, fructose, trehalulose, sucrose, melezitose, raffinose and maltose. This result indicates that the color change Benedict Test for reducing sugars, which has been used to correlate the reducing sugars to stickiness, may not be sufficient for conjecturing a stickiness issue. Several stakeholders, especially high-value Pima fiber stakeholders in the western U.S., are now using ARS stickiness results.
6. Cotton fiber maturity and fineness measurements in yarns. Fiber maturity and fineness are important characteristics of cotton fibers, as they can impact fiber processing and dye consistency and quality. The Cottonscope instrument measures fiber maturity, fineness, and ribbon width. Previously, yarns would have to be deconstructed to obtain fibers to measure on the instrument, a very labor and time intensive process. The direct measurement of greige (not bleached or dyed) yarns would be a major advantage and a new application for the instrument and technology. Yarns were prepared from a set of fiber samples with wide property ranges. Comparative evaluations were performed on the original fibers, fibers from the deconstructed yarns, and the processed yarns. Overall, very good agreement was observed for each property between the lint, deconstructed fiber, and yarn results. These results demonstrated that the Cottonscope has a high potential for yarn measurements of the fiber maturity, fineness, and ribbon width. The new information is expected to benefit textile manufacturers (e.g., spinning mills) as a better tool to use in quality assessments between fibers and yarns.
7. Rapid cotton fiber moisture content measurements by microwave technology. The moisture content of cotton fiber is an important fiber property, but it is often measured by a laborious, time-consuming laboratory oven drying method. ARS scientists in New Orleans, Louisiana, developed a laboratory microwave moisture measurement, using a microwave instrument, to perform rapid, precise and accurate fiber moisture measurements. The method agreements between the microwave instrument and two oven drying reference methods were very good, and the precision of the microwave moisture content measurements was very high. The impact of sample fiber weight was minor, and long-term stability was excellent. The microwave fiber moisture method was shown to be viable and applicable for daily quality control use. An extensive, multi-month on-site trial of the instrument was performed by the USDA-Agricultural Marketing Service, with favorable results. In addition, international interest has been expressed in potential applications of the Aqualab technique.
8. Laboratory measurements of fiber micronaire and its components by small portable instruments. Micronaire, an indication of the fiber's maturity and fineness, is a key cotton fiber quality assessment property, as it can impact fiber processing and fabric quality. Micronaire is a function of two fiber components—maturity (cell wall development) and fineness (linear density or size). International interest exists for measuring micronaire and its components using small, portable NIR instruments for both laboratory and outside the laboratory locations (e.g., field or greenhouse), with initial emphasis on the laboratory (proof of concept). ARS scientists in New Orleans, Louisiana, developed laboratory methods on three small, portable NIR instruments for micronaire, maturity and fineness. Very good spectral agreement was obtained between instruments. Rapid (less than 1 minute), easy to use, and accurate measurements were achieved. Improvements will be necessary for the accurate measurement of fineness. The universal nature of cotton micronaire and maturity measurements by portable NIR instruments was validated, and they complement current laboratory measurements. These positive laboratory results indicated a high potential for future outside the laboratory NIR measurements, an area of interest to breeders.
9. Minimizing the occurrence of seed-coat fragments in ginned cotton. One of the keys to keeping U.S. cottons competitive in the global market is to reduce the unwanted occurrence of seed-coat fragments, with and without attached fibers, in ginned lint (fiber removal from the cottonseed during the ginning process). Seedcoat neps are seed coat fragments with attached fibers. ARS scientists in New Orleans, Louisiana, developed sophisticated techniques to reveal selectivity and sensitivity information of the seed-coat neps tester used world-wide. Cottons known to be free of impurities, along with fibers that were purposely spiked with the seed-coat tissue, were analyzed by the tester and revealed a significant level of counts that varied with variety and species. This information will benefit cotton breeders who use the tester results to select varieties with reduced levels of seed-coat fragments. Selected cotton varieties should be confirmed by other tests.
10. Bias reduction between moisture and water content measurements. The moisture content of cotton fiber can impact fiber properties and fiber processing. However, moisture content is not the same as the actual water content present in the fiber. Moisture content is measured by the oven drying method as weight loss (and contains other components besides water, such as degradation products). Whereas water content is measured by the Karl Fischer Titration method (developed by ARS scientists in New Orleans, Louisiana) as the volume of reagent consumed in a reaction specific to water only. These two methods may give different results. To understand the source of the discrepancy, different oven drying procedures, with dissimilar drying ovens, oven room conditions, and amount of cotton in the oven were investigated. The research revealed that the bias is due to incomplete oven drying. By changing oven drying features, it was possible to suppress one bias over the other. After selection of oven drying specifications, the method correction factor can be derived to put moisture and water contents on the same level. The correction factor permits the determination of the actual water content of the fiber from the oven drying method throughout the industry.
11. Cotton fiber contamination visualized by chemical imaging. Non-lint contaminants (trash) present in cotton fiber include both botanical trash (parts of the plant, such as bark, leaf, seed-coat fragments) and field trash (non-plant contamination, such as plastic bags and covers for cotton bales). Currently, High Volume Instrument (HVI), Advanced Fiber Information System (AFIS),SA, and human “classers” are commonly used to measure cotton trash. However, the HVI, AFIS, and Shirley Analyzer are not capable of discriminating between types of trash, while the use of human classers is time consuming and costly. The detection and identification of trash components is an area of high interest to the industry. ARS scientists in New Orleans, Louisiana, developed techniques using Fourier transform infrared (FTIR) spectroscopy, combined with chemical imaging, to determine and identify botanical and field trash contaminants on cotton fibers. Common botanical and field trash was imaged with a high resolution Infrared (IR) detector to create visual images of cotton samples mixed with both types of trash. Isolation of the IR spectra allowed for the easy identification of a number of common trash components. This technique is being proposed as a complimentary method to the conventional methods currently used to characterize cotton trash.
12. Moisture arrangement in cotton fibers observed with infrared microscope. The organization and movement of moisture/water in cotton fiber plays an important role in the properties of the fiber. Fiber with higher moisture exhibit greater strength and elongation, for example. Using an infrared (IR) microscope with high resolution, ARS scientists in New Orleans, Louisiana, developed methods to observe the organization of moisture in individual cotton fibers. The high resolution allowed for the creation of chemical images of the samples that helped to identify key components of the fibers. Not surprisingly, areas of high moisture in the fibers coincided with areas with reduced surface waxes. The understanding of the movement and organization of water in cotton will assist industry in understanding how different properties result from different sample locations.
13. Impact of production practices on fiber end use. Fiber production practices impact fiber quality, as measured by traditional techniques, as well as processability, which is harder to measure via conventional techniques. Changes in pre-mill production, such as field irrigation, harvesting practices, and ginning practices (removing the fibers from the cottonseed) can have an impact on fiber quality and processability of fiber into textile products. ARS scientists in New Orleans, Louisiana have gathered over 1,000 fiber samples from commercial production for conventional fiber quality measurements and miniature-scale processing of a subset of these samples to determine the impact of production practices on end use. This work was conducted in partnership with stakeholders, whom also provided funding to support the initiative. The differences in harvesting, ginning and lint cleaning were shown to produce differences in fiber quality. Miniature-scale processing clearly demonstrated differences between samples, even where traditional fiber quality techniques did not indicate significant differences. This work will assist in assessing new fiber quality measurements as well as assessing the true impact of changes to germplasm or production practices.
14. Improvements to miniature-scale processing. The ability to process cotton fiber into textile goods using gram quantities (30 grams and up) was previously developed by ARS scientists in New Orleans, Louisiana. The methodology has been improved to better reflect real-world processing and to improve the resultant quality of the textile products produced using this method. This work is of interest to researchers and to commercial stakeholders to enable processing trials on extremely small samples and to handle large numbers of samples. Over 1500 samples have been processed in the past year for ARS breeders, agronomists, ginners (processors who remove the fiber from the cottonseed), and fiber scientists as well as industry stakeholders. Results have been compared to those produced using small-scale processing as well as commercial industry processing with favorable outcomes. The improvements have reduced the differences between prior miniature-scale processing results and commercial results.
15. Improvements to small-scale processing utilizing full-scale equipment. Small-scale processing of cotton fiber into textile goods using less than bale quantities (106kg) was previously developed by ARS scientists in New Orleans, Louisiana. Improvements have been made to the small-scale processing to better reflect current domestic and international textile industry practices. This work is of interest to ARS fiber quality and ginning researchers as well as to commercial stakeholders. Over 200 samples have been processed using the improvements which better follow industry practice. Improved results allow not only the fiber quality to textile product quality relationships to be studied, but also to better measure processing efficiency which is of significant economic importance to stakeholders. Samples that have been produced using new harvesting and ginning (fiber removal from the seed) practices have been processed using the improved techniques, and the impact of these practices on the efficient processing of the cotton into yarns and fabrics has been measured. Changes in practice that had no apparent impact on fiber quality via conventional methods have sometimes been shown to have an impact on the processing efficiency (both positive and negative) of the cotton; which is of paramount importance to the domestic textile mills.
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