Standard Method of Test for Determination of Organic Matter in Soils by Wet Combustion AASHTO Designation: T 194-97 (2004) 1. SCOPE 1A. ‘The “Wet Combustion” method for the determination of soil organic matter is most applicable when itis desired to determine the humus-like, easily-oxidized organic material to provide information relating to the suitability of the soil for plant growth. The method provides a good ‘estimate of this type of organic matter, and, when the soil contains only this type, it can also provide a good estimate of the total organic content. However, the reagents used react only very slightly with fresh plant materials such as wood, roots, grass, and weed tops, ete, or with hydrocarbons, charcoal, lignite coal and the organic remains in ancient sediments. f such ‘materials are present, and the total organic matter is to be determined, the “Loss on Ignition” (1.267) method must be used. 12 ‘The following applies to all specified limits in this standard: For the purposes of determining conformance with these specifications, an observed value or a calculated value shall be rounded off “to the nearest unit” in the last right-hand place of figures used in expressing the limiting, value, in accordance with R 11, Indicating Which Places of Figures Are to Be Considered ‘Significant in Specified Limiting Values. 13. ‘The values stated in SI units are to be regarded as the standard, 14, Refer to R 16 for regulatory information for chemicals. REAGENTS 24. T Normal Potassium Dichromate—Dissolve 49.04 g of dry reagen(KsCr,O)in distilled or deionized water and dilute to 1 L. COD 22, 0.5 Normal Ferrous Sulfate—Dissolve 140 g of reagent grade€e8O)-7H,0 in distilled water, add 40 mL of concentrated sulfuric acid, cool, and dilute to 1 L. Standardize this reagent each day by a “blank” tration against exactly 10.5 mL. of | Normal potassium dichromate, as described inthe method given below, but without a soil sample. 23. Barium Diphenylamine-Sulfonato—Dissolve 0.16 g of reagent grade barium diphenylamine- sulfonate in 100 mL of distilled water. 24 Galfric Acid >Concentrated (not less than 9 percent), reagent grade. 26. Phosphoric Acid, 85 percent, reagent grade. TSia T1947 “AASHTO (© 2006 by the American Association of State Highway and Transportation Oficial. ‘Alights reserved. Dupicaon isa veation of appicable law.34, 32. 33. 34. 35. 36. 37. 38. 39. 3.10. ant 3.12 4. 44 APPARATUS: Balance—The balance shall conform to AASHTO M 231, Class B. Erlenmeyer flasks, 400 ml. Volumetrie flasks, 1000 mL. Transfer pipettes, 10 mL. and 20 mL. (or burettes). Heat resistant pad. Graduated cylinders, 250 mL and 25 mL. Dropping bottles for indicator solutions. For barium diphenylamine-sulfonate solution, add 0.80 mL which equals 15 drops from dropping bottle. Burettes, 50 ml. (two required). Burette holder and laboratory stan. ‘Washing bottle, for distilled water. Glass or polyethylene bottle, minimum capacity, 1 L, for storage of potassium dichromate and ferrous sulfate solutions (two required), Oven, capable of maintaining 110° 5*C (230° 9°). PROCEDURE Weigh 0.750 to 1.0 g (Note 1) of oven-dried soil passing the 0.425-mm sieve (No. 40), to the nearest 0.001 g, transfer quantitatively to @ 400-mL Erlenmeyer flask, and add from a burette or pipette exactly 10 mL of the potassium dichromate solution. Immediately add from a graduate cylinder or a pipette 20 mL. of concentrated sulfuric acid, directing the stream into the solution. [Immediately swirl the flask vigorously to mix thoroughly and then allow ito stand on a sheet of asbestos for about 30 minutes, (See Note 2.) Add 200 mL of distilled or deionized water from & graduated cylinder, 10 ml. of phosphoric acid from a graduated cylinder (Note 3), and 0.80 mL, (15 drops) of barium diphenylamine-sulfonate indicator and swirl the flask to ensure thorough mixing. While still swirling the flask, add ferrous sulfate solution quantitatively from a burette. ‘The solution will first tur purple then from dark blue to light blue, after which the ferrous sulfate should be added slowly until the color changes to brilliant green with litle warning. Add 0.5 mL. (10 drops) more of the dichromate solution to restore an excess of dichromate, wash down the inside walls of the flask witha few mL. of water from a wash bottle, and complete the titration to a ‘one-drop, light green end-point by adding the ferrous sulfate drop by drop tothe swirling flask. If less than 5 mL of the ferrous sulfate solution has been used in the titration, repeat the determination with less soil. Make a standardizing “blank” run without a soil sample, but using exactly 10.5 ml. of dichromate and otherwise following the procedure given above. TSia T1942 ~ AASHTO (© 2006 by the American Associaton of Stale Highway and Transporation Offcils. ‘Alrighs reserved, Duplication is @ volabon of applicable aw.Note 1—For peat, use “Loss on Ignition” (T 267) method. It may be necessary to decrease the amount of soil below the minimum specified under Section 4.1, for sols greater than approximately 10-percent organic. “Loss on Ignition” (T 267) method must be used if soil sample is less than 0.200 g. Note 2—Because the action of chromic acid on organic matter is considerably affected by ‘temperature, the flask should be kept in a relatively draft-free place at room temperature, 20° to 30°C (68° to 86°F) for the 30-minute period. 5A. 62. 53. 54. 55. CALCULATIONS Determine the amount of dichromate solution that was reduced by the soil organic matter. This requires (1) standardization of the ferous sulfate solution so that the amount of dichromate equivalent tothe ferrous sulfate actually used in the tet may be determined and subtracted from the total dichromate used in the test; and (2) correction forthe small amount of dichromate reduced by impurities in the reagents used, Both ofthese requirements ar satisfied by the “blank” determination described inthe procedure, For example in a blank determination, 10.50 ml. of the dichromate solution might require 20.75 ml. of ferrous sulfate. Inthe test procedure for a hypothetical 1.000 g soil sample, 10.50 mL of dichromate would have been used; and the subsequent tration might require 6.80 ml of ferrous sulfate. The amount of dichromate actually reduced by the organic mater of this soil sample would therefore be 10.50 (1-6.80/20.75), or 7.06 mL; and since the dichromate is a Normal solution, this corresponds to 7.06 nilliequivalents of dichromate reduced A millioguivalent of carbon inthe oxidation reaction involved in this test method is 0.003 . The amount of carbon occurring in easily oxidized carbon would therefore be 7.06 x 0.003, or 0.021 and the percentage of easily oxidized carbon would be 0.021 x 100/1.000 = 2.1 percent. It is widely accepted that humus-like soil organic matter contains about $8 percent carbon. Therefore, to convert the percentage of easily-oxidized carbon to percentage of easily-oxidized ‘organi matter, multiply by 100/38 or 1.72. The percentage of easily oxidized organic matter in the ‘example soil would accordingly be 2.1 x 1.72 or 3.6 percent. thas been found for many agricultural soils that the amount of organic carbon indicated by the ‘Wet Combustion” method is about 77 percent of the total organic content, as determined by the “Loss on Ignition” method (T 267). Therefore, to approximate the total carbon or total organic matter percentage, the percentage of easily oxidized carbon or organic matter is multiplied by 100/77 or 1.3. In the example soil, the percentage of total carbon would be 2.1 x 1.3, 0r2.7, percent, and the percentage of total organic matter would be 3.6 « 1.3, or 4.7 percent. ‘The information given above in this section may be summarized inthe following equations: sly oxidized aon percent = 10 anoles a) x03-+massof soil (2) Total carbon, percent = Equation (1) «13. o Easily oxidized mater, percent = Equation (1) 172. @ Total organic matter, percent = Equation (I) x 13 x 1.72, or Equation (1)x2236 0 Note 3—It is possible that a color change during titration with ferrous sulfate solution may be impossible to observe with certain types and/or colors of soil If his occurs, filter the sample through No. 54 filter paper prior tothe addition of the barium diphenylamine-sulfonate and then ‘continue with the standard method. T1943 ‘AASHTO (© 2008 by the American Association of State Highway and Transportation Oficial ‘lights reserved. Duplication isa violation of applicable la.