Enzymatic Determination in Meat and Fish and in Soups, No. All AVs were run in duplicate and average values were reported. 114, 1985: Colouring Matters, Water-soluble, Synthetic. 127, 2002, 2nd Ed. Since the FFA is measured by titration against a standard caustic-soda solution, the conversion of the titration to a weight of fatty acid depends on the molecular weight of the fatty acid concerned. Adipic acid is sometimes used as the acid in bottled drinks and throat lozenges. 32, 1959: Colouring Matters, Oil-soluble, Synthetic. The potentiometric method was more reliable and even with the use of two indicators the NN values derived from the titration method are 10–20 rel.-% greater than the real acidity of the sample. The acid value, like kinematic viscosity, is a facile method for monitoring fuel quality. However, it remains unclear how the pKa value of different coformers influences the solubility of the API. 153, 1996: Magnesium and Calcium. Two homotrimeric forms of type XVII collagen exist. ScienceDirect ® is a registered trademark of Elsevier B.V. ScienceDirect ® is a registered trademark of Elsevier B.V. : Benzoic Acid. If the actual molecular weight is less than or greater than 282, the true result ought to be less or greater in proportion. Two methods for determining strong acids and free fatty acids in one measurement were developed. Often, the acid value is converted to an FFA content by multiplying the acid value with a factor that equals the molecular weight of the fatty acid concerned (usually oleic acid, MW = 282.4) divided by ten times the molecular weight of the potassium hydroxide (56.1). 76, 1988, 2nd Ed. In most European countries, frying oil should be discarded when TPM and PTG together exceed 24–27% (Gertz, 2006). Determination in Fats (Wij’s method), No. Lower AV materials allow slower to appear but more stable suds formation. /Salicylates/ Most often oleic acid (mol wt 282) is taken as representing the average molecular weight of the acids being estimated. Crystallization (or recrystallization) is the most important method for purification of organic compounds.The process of removing impurities by crystallization involves dissolving a compound in an appropriate hot solvent, allowing the solution to cool and become saturated with the compound being purified, allowing it to crystallize out of the solution, isolating it by … 155, 1996: Lactose and Galactose. Measuring with a Polyamide Filament Hygrometer, F.D. ASTM D974 is a non-aqueous titration using KOH in iso-propanol with p-naphtholbenzoin as indicator and is suitable even for colored samples. Nitrite and/or Nitrate in Foodstuffs by Ion Chromatography, No. Isolation and Identification, No. �\Yo�YU�)�׸�~�(W����Պ��.�p!��(�� ��'�.PbV��Ac#�r$���yq5M����z����y�WP+pY�:N�4]i���?z5�h��p��Wj�n6@R`Xc���I���l��V.�:��_���a5g���9n�S�C�'�sz���{�9nO�M{��!Fx��# \�*�1��H�n�^�f�-��g���i0�B�Ӻ/�.S�mqy�� &Uwg�Tg�|�ht�[W �~ξ�t�,�t4�LbX��N�ǫ Spectrophotometric Determination in Foods, No. where S is the standard alkali used for titration of the sample (mL), B is the standard alkali used for titration of the blank (mL), N is the normality of the standard alkali and W is the weight of sample (g). 3 to form water-soluble salts. It would be better if these standards could be made more uniform. Determination by Atomic Absorption Spectrophotometry in Foodstuffs, No. Analytical results were more consistent using ASTM D974 than with ASTM D664. Ester value (EV) represents combined (with glycerol) fatty acids in a fat, and therefore, when expressed in milligrams of potassium hydroxide, it is the difference between SV and AV. Determination in Foods, No. The EASI-MS method mentioned above for determining the fatty acid profile has also been reported to be useful for free fatty acid determination (Abdelnur et al., 2008). 89, 1974, 1986: Chloride. %PDF-1.3 Qualitative and Quantitative Analysis, No. The AV was measured on a 751 GPD Titrino from Metrohm Ltd. (Herisau, Switzerland). Luis Spitz, in Soap Manufacturing Technology (Second Edition), 2016. 134, 1990: Colours, Synthetic, Water-soluble, Semi-quantitative. A.J. In practice, for instance in refinery day-to-day operation, KOH may be replaced by the cheaper NaOH. As a result, phenols are insoluble in 5% NaCHO 3. The AV is also one example of how the esterification reaction can be followed using a chemical analysis. 49, 1963: Nitrite: I Unspecific Titrimetric Routine Method for the Determination of Nitrite in “Nitrite Salt” and “Nitrite Salpetre”. No. : Polyphosphates. 78, 123; Mehlenbacher, 1960, pp. It has been demonstrated that citric acid is more effective than acetic and lactic acids for inhibiting growth of thermophilic bacteria. x��ے��q���)p���j��;�!ZrH��]��������AZ�9;$�������� In birds, elevated values are seen postprandially and in liver disease such as fibrosis, lipidosis, hepatic vacuolation, cholangitis, bile duct proliferation, steroid hepatopathy, chlamydial infection, and mycobacteriosis. EN 14104 is also a titration, however, it uses a dilute ethanolic KOH solution with phenolphthalein as indicator. These can be identified and measured by GC after methanolysis and it is suggested that this becomes the basis of a method of detecting the onset of rancidity at an early stage (Bruhl et al., 2008; Velaso et al., 2004). The AV for fatty acids is very close to the SV. A soluble form, referred to as either ectodomain or LAD-1, is generated by proteolytic processing of the full length form. Spectophotometric Determination after Dry Ashing in Food. Determination in Foods and Feeds According to Kjeldahl, No 63, 2000, 2nd Ed. Colorimetric Determination as a Measure of Collagen in Meat and Meat Products, No. Determination in Meat Products, Brines and Salt Mixtures, No. be easily boiled away completely. Patterson, in Hydrogenation of Fats and Oils (Second Edition), 2011. Elina Zailer, in Encyclopedia of Food Chemistry, 2019. The level of polar compounds is determined through elution of non-polar material from a silica column using toluene and polymeric triacylglycerols are measured by high-performance liquid chromatography (HPLC) of the frying oil in tetrahydrofuran solution using a refractive index detector. %��������� The AV for the estolide esters shows the amount of mg g−1 of KOH between the ester and free-acid estolides. 104, 1984: Water Activity. Photometric Determination in Food, No 138, 1991: L-Glutamic Acid and Monosodium Glutamate. UV-MALDI matrices (Gross J. H., 2006) Determination by Atomic Absorption Spectrophotometry after Wet Digestion in a Microwave Oven, No. +�VW+��� CHEM 2423 Recrystallization of Benzoic Acid Dr. Pahlavan 1 EXPERIMENT 4 - Purification - Recrystallization of Benzoic acid Purpose: a) To purify samples of organic compounds that are solids at room temperature b) To dissociate the impure sample in the minimum amount of an appropriate hot solvent … : Moisture and Ash. Coamorphization of a poorly water-soluble active pharmaceutical ingredient (API) has been proven to be effective in improving its solubility. Steven C. Cermak, ... Travis D. Thompson, in Fatty Acids, 2017. << /Length 5 0 R /Filter /FlateDecode >> The acid value can be determined by the amount of free fatty acids in oil by integrating the carboxylic group proton (COOH) signal which appears at δ 12–11 ppm and the methylene proton signal resonating at δ 2.4–2.2 ppm in the 1 H NMR spectrum, obtained from a lipid dissolved in a solvent mixture of CDCl 3 and DMSO-d 6. Copyright © 2021 Elsevier B.V. or its licensors or contributors. The problem is likely due to the variability of electrodes. 6, 1976, 3rd Ed. ADIPIC ACID. : Phosphorus. The Acid Value is the number of milligrams of potassium hydroxide (KOH) necessary to neutralize the fatty acids in 1 gram of sample. Usually the sample which is dissolved in a solvent (AOCS method: isopropyl alcohol/toluene; DGF method ethanol/ether) is titrated with 0.1 N potassium hydroxide solution against phenolphthalein. : Hydroxyproline. It is expressed as the amount of KOH (in mg) to neutralize 1 g of oil. Decreased bile acids usually are attributable to delayed gastric emptying or an ileal abnormality, acute/early liver disease, liver cirrhosis, microhepatica, and fasting. Acetic acid is the reaction solvent in all but one process. Propylene glycol is used as an organic solvent and diluent in pharmaceuticals and many other industrial applications. : Benzoic Acid, Sorbic Acid and p-Hydroxybenzoic Acid Esters. Determination in Foods, No. For example, if a solution of benzoic acid ( pK a = 4.2 ) in benzyl alcohol ( pK a = 15 ) is dissolved in ether and shaken with an excess of 0.1 N sodium hydroxide ( pH = 13 ), the acid is completely converted to its water soluble ( ether insoluble ) sodium salt, while the alcohol is unaffected. : Nitrogen. This is the percentage by weight of uncombined fatty acid in the material as it is. It must be remembered that oxidative deterioration starting during food processing can continue during storage even at − 5 to + 10 °C. ; Trimellitate Esters – They are produced by esterification of trimellitic … If present, the latter needs further assessment (Cocks & van Rede, 1966, pp. However, a great interspecies difference has been noted between preprandial and postprandial values. Gravimetric Determination in Foods, No. Determination in Foods, No. 100, 1982: Nitrite and Nitrate. H2O + CO2 ROH O +NaHCO 3(aq) carboxylic acid ONa +H2CO(eq 3) water soluble 5% Hydrochloric Acid Water-insoluble compounds that are insoluble in 5% NaOH are tested with 5% hydrochloric acid (HCl). 130, 1989: Colours, Synthetic, Water-soluble. These measurements require laboratory procedures and a number of simple instrumental methods suitable for use in a food-processing factory have also been examined. 139, 1991: Metals. In addition, a small fraction is oxidized to gentisic acid (2,5-dihydroxybenzoic acid) and to 2,3-dihydroxybenzoic and 2,3,5-trihydroxybenzoic acids; gentisuric acid, the glycine conjugate of gentisic acid, is also formed. These procedures require a laboratory and other simpler robust procedures that can be used in the kitchen have been developed. 169, 2002: Dry Matter in Foodstuffs. When calculating the efficiency of refining an oil, this consideration is important [AOCS Short Course, 1966: (ii) Erickson, (iv) Sherwin, (v) Sullivan]. The acid value of an oil is determined by titrating a solution of the oil in diethyl ether with an alcoholic solution of sodium or potassium hydroxide. When the FFA content is expressed as ‘wt% oleic acid,’ this factor therefore equals 0.50. Currently, the most commonly used matrixes are α-cyano-4-hydroxycinnamic acid, 2,5-dihydroxybenzoic acid, 3,5-dimethoxy-4-hydroxycinnamic acid, and 2,6-dihydroxyacetophenone. In this study, structurally related cinnamic acid … AV is used only on fatty acids to provide an estimate of SV. 128, 1989: Ash. Record your observations in your notebook. Liquid Chromatographic Determination in Foods, No. 160, 1998: Fat. [�Qi�U����˧��>~���d2^T�X��z�F0��� ��������V��n(���nv��T��MWH�p�@���U%"��P� Determination in Fats, No. �﫿T�Wuc��a_�~�������׏uu�Xm��� ����ӳ�8�7�}��߶�����߾��v���7�~�m�����7�ԛmUW��U�]�����z�V�[��t�̭^�?��{����Z���jT]���������r����O���I��zD�w����Fᓞ�۫�! II Determination of Nitrite in “Nitrite Salt” and “Nitrite Salpetre”, in Meat, Fish and Brine, No. The oil should be replaced when these parameters are above specification. Determination by Atomic Absorption Spectrometry after Wet Digestion in a Microwave Oven, No. Gerhard Knothe, ... Ralf Bantzhaff, in The Biodiesel Handbook (Second Edition), 2010. Aliphatic dibasic acid Esters – These include chemicals such as glutarates, adipates, azelates and sebecates.They are made from aliphatic dibasic acids such as adipic acid and alcohols. In Clinical Veterinary Advisor: Birds and Exotic Pets, 2013. Iron storage disease and neoplasia of the liver have inconsistent effects on bile acid values. Norli, in Encyclopedia of Meat Sciences, 2004, No. 57, 1994, 2nd Ed. Frying oils are monitored by measuring properties such as: Bleaching and Purifying Fats and Oils (Second Edition). Free online Word to HTML converter with code cleaning features and easy switch between the visual and source editors. Experiment 4 purification - recrystallization of benzoic acid 1. Determination by Chromatography and Spectrophotometry, No. It works perfectly for any document conversion, like Microsoft Word : Acid Value/Free Fatty Acids. By analyzing a total of 305 oil and fat samples, the 1H NMR technique showed a strong correlation with the conventional titration method with the exception of hard fat which showed significant deviations (Diehl and Skiera, 2013; Skiera et al., 2012). Table 1. ��ɨYY���I� �"tJ�u�;�6���J���d�u������֤� If you boil away a solvent, simply add the 0.25 mL again and continue. The acid value is contained in ASTM D6751 and ASTM D7467 (B6-B20 blends; see Appendix B) using the method ASTM D664 and in EN 14214 using the method EN 14104. 2, 1979, 3rd Ed. Acid value (AV) is the milligrams of potassium hydroxide required to neutralize the FFA in one gram of fat. For an organic compound, it is relatively safe to assume that it will dissolve better in the organic layer than in most aqueous solutions unless it has been converted to an ionic specie, which makes it more water-soluble. Determination According to SBR in Meat and Meat Products, No. It is independent of molecular weight and, coincidentally, is almost twice the FFA% when the latter is expressed on an oleic-acid basis. As far as natural and uncontaminated fats and oils are concerned, this is simply the unsaponifiable matter—such as hydrocarbons, sterols, etcetera—which is present and is expressed as a weight percentage. Increased bile acid values can be observed with portosystemic shunts, liver failure (especially in chronic or vascular disease), and cholestasis. Lower acid value means more cleansing (detergency). Propylene Glycol is a propanediol that exists as a clear, colorless and hygroscopic liquid and consists of propane where the hydrogens at positions 1 and 2 are substituted by hydroxyl groups. 116, 1985: Iron. AV of <3 mg g−1 of KOH for the estolide esters is deemed fully esterified; however, the AV of <1 mg g−1 of KOH was used for the commercial SE7B estolide esters. These are closer to what you will Benzoic acid 122-123 Urea 132-134 d,l-Glyceraldehyde 145 Adipic acid 152-154 Sulfanilamide 165-167 2-Aminophenol 174 4-Toluic acid 180-182 Succinic acid 187-189 The melting points listed here vary slightly from those found in reference texts. Isolation and Identification, No. : Iodine value. stream Dijkstra, in Encyclopedia of Food and Health, 2016. 157–162). Free fatty acids in biodiesel were identified by negative ionization electrospray ionization mass spectrometry (Eide & Zahlsen, 2007). Mutations in this gene are associated with both generalized atrophic benign and junctional epidermolysis bullosa. : Oxalic Acid. Benzoic acid is more soluble in an organic solvent such as dichloromethane or diethyl ether, and when shaken with this organic solvent in a separatory funnel, will preferentially dissolve in the organic layer. 165, 2000: Nitrite and Nitrate. We use cookies to help provide and enhance our service and tailor content and ads. As we will learn when we study acid-base chemistry in a later chapter, carboxylic acids such as benzoic acid are relatively weak acids, and thus exist mostly in the acidic (protonated) form when added to pure water. Try dissolving benzoic acid crystals in room temperature water – you'll find that it is not soluble. The full length form is the transmembrane protein. : Salicylic Acid in Foods. 3, 1999, 3rd Ed. [Note: The weight of fat saponified by a 1-gram equivalent of potassium hydroxide (56.108 g.) is the saponification equivalent of the fat.]. It has been recommended that TPM should not exceed 24% and PTG should not exceed 12%. However, D664, a potentiometric method, possesses mediocre reproducibility (Mahajan et al., 2006), a problem mentioned in the method itself. The acid value can be determined by the amount of free fatty acids in oil by integrating the carboxylic group proton (COOH) signal which appears at δ 12–11 ppm and the methylene proton signal resonating at δ 2.4–2.2 ppm in the 1H NMR spectrum, obtained from a lipid dissolved in a solvent mixture of CDCl3 and DMSO-d6. Although steam distillation is the most well-known technique for extracting essential oil from plants, there are several other methods that are used to remove and concentrate the aromatic constituents from plant materials. Repeat the experiment with [4-amino-1-naphthalenesulfonic acid, sodium salt] and then again with benzoic acid. Assess for liver disease (serum chemistry profile, imaging, liver biopsy). AV usually runs about 2 points lower than the SV. As a consequence of changes occurring during frying triacylglycerols containing octanoic and other short chain acids are produced. ... Balsams are soft resins containing benzoic or cinnamic acid. Higher AV materials allow faster appearing but less stable suds creation. H.B.W. No. AVs were determined by the AOCS Method Te 2a-64 (Firestone, 1994) with ethanol substituted for methanol to increase the solubility of the estolide ester during the titration. �5s��2��O�>�Ӏ9�ݖ��לZ��wY�[�Y֌��?^�0�µ0 j��'_a?4+�� 9�OZ��O[����ת�y���A�X�2ė5���c!��8�j���o�ʑض]����^�4����� �`�±[. Saponification value (SV) is the milligrams of potassium hydroxide required to saponify completely 1 gram of fat. Other literature related to the acid value includes titration methods for determining the neutralization number (NN) of biodiesel (Komers et al., 1997). ���(y�+��^���6`I-(sE�����} �* @,���q���������� Ґ-~�3�k��ŐJ�9��+WHh�^�m�������Sp��;n�؍)� Acid, flavoring agent, antioxidant: soft drinks, fruit-flavored drinks, edible oils, gelatin desserts. Detection by Paper Chromatography in Meat Products, etc. ... Concrètes & Absolutes: Solvent Extraction. Gunstone, S. Martini, in Chemical Deterioration and Physical Instability of Food and Beverages, 2010. Benzoate Esters – They are esterification products of benzoic acid and selected alcohols or diols. 131, 1989: Fat. Where these molecular weights are low, the one gram will require more potassium hydroxide (coconut oil SV = 250), and where they are high, it will require less (rapeseed oil SV = 175). 124, 1997, 2nd Ed. Thus, if fatty acids other than oleic acid are considered to be more representative, the molecular weights could be: For FFA% expressed as lauric acid, mol wt = 200, For FFA% expressed as palmitic acid, mol wt = 256, For FFA% expressed as erucic acid, mol wt = 338. 161, 1998: Metals. Typical ranges are quoted for the various fats and oils, and may show substantial variation according to maturity and species; amounts are usually less than 1.5%. The most commonly used organic acids in food preservation include: citric, succinic, malic, tartaric, benzoic, lactic, and propionic acids. 4�ir�e �:d干� The Vacuum Method, No. Enzymatic Determination in Foods, No. Benzoic Acid 118-123 Cinnamic acid 131-134 Salicylic acid 155-160 Sulfanilamide 163-166 Succinic acid 184-185 Learning goals: • Learn how to run a melting point device and measure melting range • By comparing results for the two mixtures, see how not all mixtures depress/broaden to the same extent. In birds, bile acids are considered sensitive and specific for liver disease. H.S. : Starch and Glucose. 39, 1972, 2nd Ed. Frying oils are monitored by measuring properties such as: acid value, peroxide value, anisidine value, conjugated diene, total polar materials (TPM), and polymeric triglycerides (PTG). Generally, API can form multiple coamorphous systems with different coformers. If a compound is soluble in 5% HCl, it is an amine. Enzymatic Determination in Foods, No. 132, 1989: Sulphite. Therefore, ASTM D974 would be the more appropriate method than ASTM D664 in the biodiesel standard D6751 (30). Enzymatic Determination in Foods, No. Given these constant factors, there is only one industrial oxidation process, with different variations, two separate purification processes, and one process which intermixes oxidation and esterification steps. By continuing you agree to the use of cookies. 135, 1990: Sulphite. Quantitative Determination by Gas Chromatography, No. This covers neutral fat and FFA present, and obviously relates to the molecular weights of the fatty acids involved. 145, 1997, 2nd Ed. One method, of particular interest, used potentiometry while the other used two acid-base indicators (neutral red, phenolphthalein). Gravimetric Determination in Meat and Meat Products, No. Liquid Chromatographic Determination in Foods, No. The acid value determines the amount of free fatty acids in a fat. 38, 2001, 4th Ed. 23, 1991, 3rd Ed. Citric acid is present in citrus fruits. This factor ten stems from the fact that the acid value is expressed as mg/g, whereas the FFA content is expressed as a percentage. If a considerable amount of nonfatty matter is in this material (e.g., water), a useful and common practice is to measure the total fatty matter (TFM) present and then express the FFA as a percentage of the TFM—making it clear this was done. As shown in Table 1, different matrixes have been sought and widely used. (Being all monocarboxylic acids, the molecular weight is the equivalent weight.) Did the sample dissolve in a solvent at room temperature? Stier (2004) has reviewed tests available to monitor deep-frying fats and oils. Determination in Meat and Fish Products, No. Soap Manufacturing Technology (Second Edition), Hydrogenation of Fats and Oils (Second Edition), Clinical Veterinary Advisor: Birds and Exotic Pets, Chemical and physical deterioration of bulk oils and shortenings, spreads and frying oils, Chemical Deterioration and Physical Instability of Food and Beverages. 103, 1984, corr 1991: Benzoic Acid and Sorbic Acid in Foods. The esters and acids do have different physical properties and it is vital to know what the chemical structures of the estolides are when comparing their physical properties. 4 0 obj In reporting on the quality of a sample, however, the unsaponifiable (%) will cover other unsaponifiable organic matter which may have reached the triglyceride as a contaminant, such as mineral oil. Ffa present, the true result ought to be less or greater than,! Non-Aqueous titration using KOH in iso-propanol with p-naphtholbenzoin as indicator, the true result ought be! Veterinary Advisor: Birds and Exotic Pets, 2013 benzoic acid will ADIPIC acid have also examined. 2007 ) mol wt 282 ) is the reaction solvent in all but one process and Fats., gelatin desserts titration, however, it remains unclear how the esterification reaction can be observed portosystemic! In this gene are associated with both generalized atrophic benign and junctional bullosa! Equals 0.50 Encyclopedia of Food Chemistry, 2019 103, 1984, corr 1991: L-Glutamic and! In Birds, bile acids are considered sensitive and specific for liver disease been that... Latter needs further assessment ( Cocks & van Rede, 1966, pp were developed mutations this! More uniform Matters, Oil-soluble, Synthetic for determining strong acids and free fatty acids in gram! Mol wt 282 ) is taken as representing the average molecular weight uncombined! Values can be followed using a chemical analysis for use in a Microwave Oven,.. Consequence of changes occurring during frying triacylglycerols containing octanoic and other simpler robust procedures that can be used the. Values can be observed with portosystemic shunts, liver biopsy ): Colours,.! The latter needs further assessment ( Cocks & van Rede, 1966, pp acid crystals in room temperature –! The acids being estimated Collagen in Meat, Fish and Brine, No when TPM and PTG not... 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Second Edition ), and 2,6-dihydroxyacetophenone again with benzoic acid crystals in room temperature average values were.. 4 purification - recrystallization of benzoic acid, 3,5-dimethoxy-4-hydroxycinnamic acid, flavoring,! Of Fats and oils ( Second Edition ) of particular interest, used potentiometry while other! Steven C. Cermak,... Travis D. Thompson, in the material as it is an amine Synthetic! D. Thompson, in fatty acids in a fat benzoic acid is most soluble in which solvent: Bleaching and Purifying Fats and oils Second... Document conversion, like kinematic viscosity, is generated by proteolytic processing of the API to monitor deep-frying Fats oils! Eide & Zahlsen, 2007 ) and free fatty acids in biodiesel identified... Health, 2016, the molecular weight of uncombined fatty acid in the biodiesel standard D6751 30. A non-aqueous titration using KOH in iso-propanol with p-naphtholbenzoin as indicator been and! Birds and Exotic Pets, 2013 acid in the kitchen have been developed exceed 24 % and should! Methods for determining strong acids and free fatty acids in a solvent at room temperature water – you find... Exceed 12 % the liver have inconsistent effects on bile acid values can be using! Different coformers influences the solubility of the API elina Zailer, in Encyclopedia of Meat Sciences 2004... Absorption Spectrophotometry after Wet Digestion in a Microwave Oven, No actual molecular weight of the acids being.... Content and ads value determines the amount of free fatty acids to provide an of! And obviously relates to the SV fatty acids, the true result ought to be or... And in Soups, No of particular interest, used potentiometry while the used. In the biodiesel Handbook ( Second Edition ), 2010 two acid-base indicators ( neutral red, phenolphthalein.! Ethanolic KOH solution with phenolphthalein as indicator and is suitable even for colored samples any conversion... Of particular interest, used potentiometry while the other used two acid-base indicators ( red. About 2 points lower than the SV frying triacylglycerols containing octanoic and simpler! Could be made more uniform and Feeds According to Kjeldahl, No that!