Protein nitrogen combustion method collaborative study I. Comparison with smalley total Kjeldahl nitrogen and combustion results

During 1993–1994, a collaborative study of the determination of the nitrogen content of oilseed meals by the nitrogen combustion method was conducted among 24 laboratories in seven countries for the analysis of cottonseed, soybean (two samples), peanut, canola and safflower (two samples). These meals were also analyzed by the CuSO₄/TiO₂ Kjeldahl method (Official Methods and Recommended Practices of the American Oil Chemists' Society, 4th edn., 1989, Method Ba 4d-90) in the 1993–1994 Smalley Check Sample Program Oilseed Meal Series [Brown, J.,INFORM 5:640 (1994)]. Some participants used commercial nitrogen combustion instruments. In the Smalley Program, CuSO₄/TiO₂ Kjeldahl analysis gave nitrogen values that ranged from 0.05 to 0.13% lower than values obtained by the combustion method in the collaborative study. Nitrogen values obtained by the combustion method on an optional basis in the Smalley Program were generally lower by 0.01 to 0.03% than nitrogen values obtained by the combustion method in the collaborative study reported here.     

Comparison of kjeldahl and dumas methods for determining protein contents of soybean products

The Kjeldahl and Dumas methods for quantifying nitrogen content were compared using nine soybean products having protein contents ranging from 0.5 to 90%. In addition to comparing day-to-day variability of the Dumas method, differences between and variabilities of two Kjeldahl systems and Kjeldahl operators were also evaluated. The Kjeldahl method gave slightly, but significantly, lower values than did the Dumas method. Both the Kjeldahl and Dumas methods had equivalent variabilities (same SD about the means). The ratios between the means for the Kjeldahl and Dumas (K/D) protein values ranged from 0.66 to 1.03. The conversion equation y=−0.00536+0.97188x (R ²=0.9997) was developed and validated to convert from Dumas to kjeldahl protein concentrations.     

Low-field 1H nuclear magnetic resonance and chemometrics combined for simultaneous determination of water, oil, and protein contents in oilseeds

Prediction of the content of water, oil, and protein in rape and mustard seed was examined by a combination of low-field ¹H nuclear magnetic resonance (LF-NMR) and chemometrics, enabling utilization of the entire relaxation curves in the data evaluation. To increase the range of relative contents, the untreated seeds were wetted and dried; each treatment was followed by NMR analysis. The chemometric results are compared to traditional evoluation by multiexponential fitting of the relaxation curves. For this purpose a new jackKnife validation procedure was developed to evaluate the number of exponential components objectively. Classification of the two kinds of seeds was easily performed by LN-NMR. Partial least squares regression to oil content in untreated rape and mustard seed yielded models with correlation coefficients of r=0.88 and 0.89 with root mean square error of cross-validation (RMSECV) of 0.84 and 0.45, respectively. The rapeseed model was based on one component, wheres the mustard seed model was based on two components. If the seeds were dried, the predictive performance improved to r=0.98 and RMSECV=0.38 for rapeseed and to r=0.95 and RMSECV=0.38 for mustard seed. Upon drying, prediction of protein content in mustard seed improved, whereas the prediction of protein for rapeseed deteriorated. Global models, including the combination of untreated, wet, and dry seeds, all resulted in a robust and good predictive performance with RMSECV in the range 0.8–1.3% to water, oil, and protein content. It was demonstrated that drying the seeds to simultaneously determine water and oil content was not necessary when chemometrics was applied on the relaxation curves.     

半微量开氏法和红外热导法测试煤中氮的比较

为了提高煤中氮含量的测试效率,采用GB/T 19227—2008《煤中氮的测定方法》中的半微量开氏法和红外热导法测定煤中的氮,并对测试结果进行了分析对比。结果表明:2种测试方法测试结果准确,精密度不存在显著性差异,均能满足测试要求,但红外热导法测定煤中氮操作简便,自动化程度高,安全性好。     

Comparison of three whole seed near-infrared analyzers for measuring quality components of canola seed

Whole seed near-infrared (NIR) analyzers are capable of high-speed compositional analysis of oilseed commodities. This study compared the PerCon Inframatic 8144 (Perten Instruments, North America Inc., Reno, NV), the Tecator Infratec 1225 (Tecator AB, Hoganas, Sweden) and the NIR-Systems 6500 (NIR Systems, Inc., Silver Spring, MD) analyzers for measurement of oil, protein, chlorophyll and glucosinolates in intact canola seed of composite samples from the Grain Research Laboratory's (Winnipeg, Manitoba, Canada) annual Western Canada Harvest Surveys (1985–1989) for assembly of calibration and prediction sets. No significant differences were found between the three instruments for oil [standard error of prediction (SEP 0.43–0.55%)], protein (SEP 0.35–0.42%) and glucosinolates (SEP 2.4–3.8 mM/g). Neither the Tecator nor the PerCon instruments were effective for determining chlorophyll. By combining oil content and fatty acid composition data to give an estimate of the total level of each fatty acid in the sample, high correlations were obtained for total saturates, linolenic acid, and linoleic acid although the RPD (ratio of the S.E. of prediction to the S.D. of the original data) values were not high enough to enable routine use of the method to predict results. Presented at the 84th AOCS Annual Meeting & Expo, April 27, 1993, Anaheim, California.     

Comparison of different methods for the determination of the oil content in oilseeds

The investigation and assessment of the oil content of oilseeds are important criteria, especially for the oil milling trade. Standard methods for the determination of the oil content of oilseeds are very time consuming, with extraction periods of 4 to 8 h. Three different oilseeds—rapeseed, sunflower, and soybean—are extracted by supercritical fluid extraction (SFE), accelerated solvent extraction, microwave-assisted extraction, solid fluid vortex extraction, and Soxtherm, and the results are compared with the result of the German Fat Science Society (DGF) standard method B-I 5 (87). Besides, the extracts are analyzed regarding the content of tocopherols as a parameter for mild extraction conditions and the content of diglycerides and free fatty acids as parameters for the content of more polar lipids. The results of the determination of the oil content under optimal conditions are comparable with the results of the DGF standard method B-I 5 (87). There are no significant differences between the different methods. The content of tocopherols is dependent upon the extraction method and the type of oilseed. The highest content is obtained by SFE. The content of diglycerides and free fatty acids varied according to the oilseed.     

煤粉无焰富氧燃烧的数值模拟方法进展

无焰富氧燃烧是煤粉清洁燃烧技术的前沿发展方向之一,可在捕集高浓度CO₂的同时显著降低NOx排放,并提升富氧燃烧稳定性和热力性能。计算流体力学(CFD)作为燃烧研究的重要手段之一,具有快捷、成本低和数据丰富等优点,有效促进了无焰富氧燃烧技术发展。基于笔者团队对煤粉富氧燃烧和无焰燃烧的多年研究积累,对近十几年来煤粉无焰富氧燃烧CFD模拟方法和模拟研究进展进行了总结:首先强调了煤粉无焰燃烧的试验和数学定义,其由于存在非均相反应而区别于气体燃料无焰燃烧;然后详述了煤粉无焰富氧燃烧CFD模拟方法进展,包括模拟流动、传热、燃烧和污染物生成方面的子模型和机理,其中考虑强烈烟气卷吸的可实现k-ε湍流模型、P1或DO辐射模型及针对富氧气氛修正的WSGG气体辐射模型、CPD挥发分析出模型、考虑湍流与化学反应交互的有限速率EDC均相燃烧模型、针对无焰及富氧燃烧开发验证的均相反应机理、考虑气化反应的多步表面焦炭非均相燃尽模型、含氮化学详细反应机理氮转化模拟、动态自适应反应机理加速算法等可显著提高煤粉无焰富氧燃烧的模拟精度和计算效率。总结了煤粉无焰富氧燃烧在基准对照试验、微观反应区域分析、宏观反应特征、污染物生成及大型化锅炉概念设计方面的模拟研究情况;最后以大涡模拟、燃烧模型、高精度反应机理及动态自适应反应机理、工业应用优化等角度展望了煤粉无焰富氧燃烧CFD研究的发展方向。     

Influence of nonprotein nitrogen on estimation of protein from total nitrogen in fleshy fruits

The protein content of pulps of 26 fleshy fruit species from east Mediterranean habitats in Israel were estimated using two different methods: (1) the Kjeldahl procedure in which the total recovered nitrogen is multiplied by 6.25 to estimate total proteins, and (2) amino acid analysis by amino acid analyzer. The average protein content obtained by the Kjeldahl procedure was 5.75% (dry weight) while it was only 3.90% when amino acids were analyzed. The higher value of protein content by the Kjeldahl procedure is most likely the result of a relatively high proportion of nonprotein nitrogen compounds (31%) in these pulps. Therefore the 6.25 factor is not valid and a 4.05 factor may be more accurate for assessing the true protein content of these fleshy fruits. The data also suggest that the more accurate estimate of true protein (Y) from Kjeldahl total nitrogen (X) should be based on the highly significant linear regression between these two variables:Y=4.885X–0.6.     

A lipidomic approach for profiling and distinguishing seed oils of Hibiscus manihot L., flaxseed,and oil sunflower

As important oil crops in Inner Mongolia, sunflower, and flaxseed had distinct lipid profiles in seeds. As an emerging cash crop, Hibiscus manihot L. has strong potential market competitiveness. In this study, the lipidome, fatty acid composition and quality characteristics of flaxseed, H. manihot L., and sunflower seed oils were analyzed and compared. A total of 270 distinct lipids were identified and analyzed with an emerging detection approach—lipidomics, which illustrated the tremendous difference among the samples. triacylglycerol, diacylglycerol and polar lipids were the most abundant lipids in all samples. H. manihot L. seeds contained higher saturated and monounsaturated fatty acids and lower polyunsaturated fatty acids. H. manihot L. seed oil had the longest oxidative stability index time, high content of vitamin E and total phenolics, while flaxseed oil embodied the lowest oxidative stability. The peroxide value and acid value of the three oils were within the allowable range of Chinese national standards.     

Comparison of the composition and properties of canola and sunflower oil sediments with canola seed hull lipids

The phase transition behavior and chemical composition of sediments from Canadian and Australian canola oils, as well as from sunflower oil, were studied by differential scanning calorimetry, X-ray diffraction, polarized-light microscopy, and chromatographic techniques. Australian canola sediment was similar to Canadian canola sediment in both melting and crystallization behaviors and chemical composition. Compared to canola sediment, sunflower sediment underwent phase transformation (melting and crystallization) at lower temperatures, and the enthalpies associated with the phase changes were greater. The X-ray diffraction patterns for these materials were similar, indicating identical crystalline structures. Sunflower sediment contained mainly wax esters (99%), while canola sediment contained about 72–74% of waxes. Moreover, sunflower sediment consisted of shorter-chainlength fatty acids and alcohols than canola sediment. A hexane-insoluble fraction from Canadian canola hull lipids had fatty acid and alcohol profiles and X-ray diffraction pattern similar to the corresponding oil sediment.     

AOCS collaborative study on sensory and volatile compound analyses of vegetable oils

An AOCS collaborative study was conducted to determine the effectiveness of sensory analysis and gas chromatographic analyses of volatile compounds in measuring vegetable oils for levels of oxidation that ranged from none to high. Sixteen laboratories from industry, government, and academia in Canada and the United States participated in the study to evaluate the flavor quality and oxidative stability of aged soybean, corn, sunflower, and canola (low-erucic acid rapeseed) oils. Analytical methods included sensory analyses with both flavor intensity and flavor quality scales and gas-chromatographic volatiles by direct injection, static headspace, and dynamic headspace (purge and trap) techniques. Sensory and volatile compound data were used to rank each of the oils at four levels of oxidation—none, low, moderate, and high. For soybean, canola, and sunflower oils, 85–90% of laboratories correctly ranked the oils by either analysis. For corn oil, only 60% of the laboratories ranked the samples according to the correct levels of oxidation by either analysis. Variance component estimates for flavor scores showed that the variation between sensory panelists within laboratories was lowest for the unaged oils. As storage time increased, the variance also increased, indicating that differences among panelists were greater for more highly oxidized oils. Between-laboratory variance of sensory panel scores was significantly lower than within-laboratory variance.     

Evaluation of methods of measurement of nitrogen in poultry and animal manures

Kjeldahl nitrogen (N), total N and forms of inorganic N (ammoniacal (NH₄)-N, nitrate (NO₃)-N and nitrite (NO₂)-N) were measured in a range of animal manures. The manures include fresh samples of poultry manure, sheep manure, horse manure, dairy slurry and pig slurry and composted poultry manure. Kjeldahl N was measured by standard micro-Kjeldahl digestion. For total N measurements, NO₃-N and NO₂-N were recovered during Kjeldahl digestion by pretreatments with various oxidizing and reducing agents. Inorganic forms of N were measured by extraction with 2M KCl solution.Kjeldahl digestion alone allowed measurement only of organic N and NH₄-N. Amongst various modifications to the Kjeldahl, pretreatment with either acidified (H₂SO₄) Zn-CrK(SO₄)₂ or acidified (H₂SO₄) reduced Fe achieved complete recovery of NO₃-N. Nitrite N was only recovered by first oxidising the NO ₂ ^- to NO ₃ ^- with KMnO₄ followed by reduction to NH₄-N with acidified (H₂SO₄) reduced Fe.More than 95% of the total N in fresh animal manure was present as organic N and NH₄-N which were recovered by the standard Kjeldahl digestion. In the case of fresh manures there was no difference between the amount of total N measured by the Kjeldahl digestion and its modified methods. However composting of poultry manure or drying of poultry manure, pig slurry and dairy slurry resulted in an increase in NO₃-N which was not recovered during Kjeldahl digestion alone. Under these conditions the total N could be measured by pretreating the samples with KMnO₄ and reduced Fe prior to Kjeldahl digestion.Drying of animal manures caused a decrease in organic N and NH₄-N, especially in poultry, pig and dairy manures. There was a slight increase in NO₃-N; but most of the decrease in N content with drying was attributed to the volatilization loss of ammonia (NH₃). Amongst various drying methods examined air drying caused maximum loss of N as NH₃ whereas freeze drying caused minimum loss of N. This suggests that fresh animal manures can be freeze dried for analysis of N which causes minimum loss of N.     

Comparison of extraction methods for determining tocopherols in soybeans

We evaluated the usefulness of saponification, direct solvent extraction, and Soxhlet extraction as extraction methods to determine the amounts of tocopherols in soybeans. Soxhlet extraction yielded the highest analytical values for each tocopherol homolog and was the best method for quantifying tocopherols in soybeans. Coupling of simple Soxhlet extraction with HPLC provided a highly reproducible procedure to quantify tocopherols in soybeans. The percent mean recovery ± standard deviation (n = 5) was 103.2 ± 1.21, 109.8 ± 4.18, 93.8 ± 1.12, and 106.9 ± 1.54% for α‐, β‐, γ‐, and δ‐tocopherol, respectively. The linearity test for quantification was carried out over the ranges of 0.4–10.0, 0.2–4.0, 2.0–16.0, and 0.4–10.0 µg/mL for α‐, β‐, γ‐, and δ‐tocopherol, respectively. Regression analysis showed an excellent linear relationship (R² >0.998), and the results of the validation parameters were generally reliable and satisfactory.     

Multivariate model for the prediction of soluble condensed tannins in crude extracts of polyphenols from canola and rapeseed hulls

The feasibility of using ultraviolet spectrophotometry to develop multivariate models for prediction of soluble condensed tannins (SCT) content in crude polyphenols extracts from canola and rapeseed hulls was investigated. The polyphenols were extracted from hulls using 70% (vol/vol) aqueous acetone. Partial least squares regression was used to correlate the spectral data of the crude polyphenols in methanol between 265–295 nm with the SCT content in hulls. Both the proanthocyanidin (P) and the vanillin (V) assays were used to provide reference data for creating the models. The predictive ability of the models is good, as indicated by the RPD values [the ratio of the standard deviation of data to the standard error of calibration (SEC) of above 5. Additionally, the SEC values suggest that P is superior to V in predicting the SCT content of hulls using this method.     

Chemical Protein Analysis: A Comparison of Kjeldahl Crude Protein and Total Ninhydrin Protein from Wild, Tropical Vegetation

Various methods are available for measuring the protein content of vegetation. This paper reviews and tests some common methods in order to provide recommendations to wildlife ecologists and primatologists. The traditional Kjeldahl crude protein method, which requires the conversion factor of 6.25 (CP6.25), was compared to values obtained through total ninhydrin protein (NP) analysis and by calculating crude protein from a newly developed conversion factor of 4.3 (CP4.3). The NP analysis gave values that were not significantly different from the CP4.3 values, and both were significantly lower than the CP6.25 values. An additional method was compared (available CP), which is CP6.25 values corrected by subtracting the acid-detergent lignin-bound crude protein. Comparisons were also made between CP4.3 and the available CP. These two methods correct the protein values differently, and theoretically CP4.3 corrects more severely, as explained in the text, but in some situations they may be correcting for the same chemical category of unavailable nitrogen. For fruits and flowers these values were not significantly different. For leaves the results were not so clear-cut. The Ugandan leaves (N = 42), Indonesian mature leaves (N = 40), Zimbabwe leaves (N = 24), and northern USA leaves (N = 11) were significantly different, and the CP4.3 always corrected more severely. The rest of the leaf sets (Belize, N = 68; Zaire, N = 36; Sumatra, N = 10; St. Catherine's Island, Georgia, USA, N = 37; and southern USA, N = 18) did not give a significant difference between CP4.3 and available CP. The choice of which analysis method to use (NP or CP4.3 versus available CP) depends on whether it seems reasonable to severely penalize all nonprotein nitrogen, considering the animal species being studied, or whether removing only the lignin-bound nitrogenous compounds is sufficient. Overall, the traditional 6.25 conversion factor is too large a conversion value for most wild vegetation; crude protein corrected only for lignin-bound protein is probably more accurate.     

Comparison of four analytical methods for the determination of peroxide value in oxidized soybean oils

Previous work in our laboratory demonstrated that soybean oil oxidation, expressed as PV, can be determined using NIR transmission spectroscopy as an alternative to the official AOCS iodometric titration method. In the present study, a comparison of four peroxide analytical methods was conducted using oxidized soybean oil. The methods included the official AOCS iodometric titration, the newly developed NIR method, the PeroxySafe^™ kit, and a ferrous xylenol orange (FOX) method, the latter two being colorimetric methods based on oxidation of iron. Five different commercially available soybean oils were exposed to fluorescent light to obtain PV levels of 0–20 meq/kg; periodic sampling was done to ensure having representative samples throughout the designated range. A total of 46 oil samples were analyzed. Statistical analysis of the data showed that the correlation coefficient (r) and standard deviation of differences (SDD) between the standard titration and NIR methods were r=0.991, SDD=0.72 meq/kg; between titration and the PeroxySafe^™ kit were r=0.993, SDD=0.56 meq/kg; and between the standard titration and FOX method were r=0.975, SDD=2.3 meq/kg. The high correlations between the titration, NIR, and PeroxySafe^™ kit data indicated that these methods were equivalent.     

Antioxidant activity of evening primrose phenolics in sunflower and rapeseed oils

Crude ethanol/ethyl acetate extracts of industrial evening primrose (Oenothera biennis L.) seed meal were separated into six fractions using the Sephadex LH‐20 column chromatography and 96% aqueous ethanol as a mobile phase. Their antioxidant activities were tested in sunflower and rapeseed oils by using an Oxidograph apparatus at a temperature of 110 °C. Only the fractions III and IV displayed a pronounced antioxidant activity while the other fractions were either inactive or even pro‐oxidative. The active fractions contained phenolic acids and their esters; gallic acid, methyl and ethyl gallates, protocatechuic acid and its methyl ester were identified by GC/MS. Catechin was present, too, but exhibited only moderate antioxidant activity in sunflower oil.     

水泥行业用煤的燃烧特性评价及统计分析

本文通过热重分析检测煤炭燃烧特性,在已积累的大量数据基础上,对水泥行业用烟煤和无烟煤的煤烧特性各项指标统计分析,并对各项参数给出了参考数值：（1）烟煤着火温度范围在390～620℃,平均值在430℃左右;燃烧烈度范围0.3～2.7 mV/（mg·min）,平均值1.18 mV/（mg·min）;燃尽时间范围12～37 min,平均值18 min;(2)无烟煤着火温度范围在430～650℃,平均值558℃左右;燃烧烈度范围0.6～2.3mV/（mg·min）,平均值1.58mV/（mg·min）;燃尽时间范围10～30min,平均值13min。将燃烧特性参数进行赋分和排位,在数据库中求得分位值,绘制煤炭燃烧特性排位图,为生产用煤配煤提供技术指导和控制要求。     

Synthesis of GAGG:Ce3+ powder for ceramics using mechanochemical and solution combustion methods

Gadolinium aluminum gallium garnet doped with cerium (Gd_2.99Al_2.00Ga_3.00O_12.00:Ce_0.01, or GAGG:Ce) powders has been synthesized with high‐energy ball milling (HEBM) and solution combustion synthesis (SCS) techniques. The structures and morphologies of the powders were characterized through use of powder X‐ray diffraction (PXRD), photoluminescence (PL) measurements, dynamic light scattering (DLS), scanning electron microscopy (SEM), transmission electron microscopy (TEM), and UV‐decay time measurements. Changes in the mechanochemically produced powders were monitored over time, while the solution combustion synthesis of GAGG:Ce was conducted using various ratios and types of fuels. In both production methods, particle sizes on the order of microns gave evidence of agglomeration.