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CHEMICAL ANALYSIS of WOOD and WOOD PRODUCTS ( As Used at the U

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CHEMICAL ANALYSIS of WOOD and WOOD PRODUCTS ( As Used at the U PROCEDURES FOR THE CHEMICAL ANALYSIS OF WOOD AND WOOD PRODUCTS ( As used at the U. S. Forest Products Laboratory ) By Wayne E. Moore and David B. Johnson REVISED DECEMBER 1967 Forest Products Laboratory Forest Service U. S. Department of Agriculture The U. S. Forest Products Laboratory is maintained at Madison, Wis., in cooperation with the University of Wisconsin. PREFACE This manual is a compilation of procedures used at the U.S. Forest Products Laboratory for the chemical analysis of wood and wood products. It was assembled in order to bring together, in a single, readily available form, the analytical procedures in current use along with pertinent references and selected, representative, analytical data. Some of these procedures and many of the techniques and modifications included have not been available previously in the literature. All of the methods required for complete chemical characterization of wood are not included, but rather, only methods which the Forest Products Laboratory has had considerable experience with andfounduseful, accurate, and reliable. The manual is meant to be a working guide for the analytical chemist and technician involved in wood chemistry and is also, to a limited extent, meant to be a source book for information on the composition of wood and for supplementary information regarding the analytical techniques and apparatus used. Revisions of the manual will be issued as required by advances in technology. W. E. MOORE D. B. JOHNSON Analytical Development, Instrumenta- tion and Service Wood Chemistry Research Division U. S. Forest Products Laboratory CONTENTS Analytical Methods Acetyl and C- Methyl Groups Alcohol- Benzene Solubility of Wood and Pulp Alkoxyl Groups Ash in Pulp Ash in Wood Charcoal Analysis Ether Solubility of Wood and Pulp Ethyl Alcohol Extractives in Wood Formaldehyde in Paper and Wood Furfural Halides in Wood Holocellulose in Wood Hydr oxymethylf urfural Ion -Exchange Capacity of Pulp Itaconic Acid Lactic Acid Levulinic Acid Lignin in Pulp (Standard Hydrolysis) Lignin in Pulp (Modified Hydrolysis) Lignin in Wood (Standard Hydrolysis) Lignin in Wood (Modified Hydrolysis) Lignin in Wood (Spectrophotometric) Moisture in Wood and Pulp Nickel Nitrogen by the Kjeldahl Method (Total, Ammoniacal, and Urea Nitrogen) Pentosans in Pulp pH of Wood Polyethylene Glycol in Wood Propylene Glycol Pyroligneous Acids Sieve Analysis Silica in Organics Sodium in Fermentation Solutions Solids in Water Sugar Alcohols, Glycerol, and Glycols Sulfate in Cellulose Nitrate Total Organic Matter Uronic Acids Wood Sugars Appendix Definitions of Terms Related to Cellulose and Cellulose Derivatives Definitions of Terms Related to Precision and Accuracy Extractive -Free Wood (Preparation of) Minimum Sample Sizes Required for Analyses Spectrometry Nomenclature Index ANALYTICAL METHODS Acetyl and C-Methyl DETERMINATION OF ACETYL AND C -METHYL GROUPS Part I -- Acetyl Groups Principle The organic substance containing 0- acetyl or N- acetyl groups is hydro- lyzed in an acidic or alkaline medium. After hydrolysis, the volatile hydrolytic products are steam distilled out of the reaction mixture; the acetic acid in the distillate is determined by titration with standard sodium hydroxide solution. At the Forest Products Laboratory, the alkaline hydrolysis procedure is generally used (always for wood). The acidic hydrolysis is used for pure, stable compounds or when the sample is insoluble in alkali and can tolerate this more vigorous treatment (no components present that might be oxidized to acetic acid). Equations HOH(H+ or OH-)N. 1. CH3CO-OR ROH + CH3COOH (or CH3 C00-) R RlRi J 1 HOH(H+ or OH 1 2. CH3C0- HNN\ + CH3COOH (or CH3 C00-) N. R2 R2 3. CH3COOH + NaOH titration CH3COONa + H2O Apparatus 1 A Wiesenberger apparatus- (fig. 1) consisting of: 1. A heart -shaped, long -neck, ground -joint reaction flask, approxi- mately 7 in. high. and Acetyl Groups," "Based on The Microanalytical Determination of C- Methyl by E. Wiesenberger. Makrochem. 33: 51169 (1947). 67 -006 -1- Figure 1. -- Wiesenberger Acetyl Determination. Acetyl and C-Methyl 2. A ground -joint still -head, with two steam traps and removable plunger to permit addition of solutions to the reaction flask. 3. A ground -joint condenser approximately 15 in. long with a drip tip. 4. A 25 -ml. graduate. 5. An Erlenmeyer flask of 125 -ml. capacity. 6. Ground -joint (24:40) flasks of 500- and 750 -ml. capacity, for prepara- tion of reagents, steaming out the condenser, etc. 7. Pipets of appropriate sizes for delivery of reagents. Reagents Chromic Acid Method 1. 4N Chromic acid solution: 67 g. of chromic anhydride (Cr03) is dissolved in 500 ml. of boiled distilled water. After this solution has stood for 1 day, it is filtered through a fine sintered -glass suction filter. Then it is added with cooling to 125 ml. of concentrated sulfuric acid ( d. = 1.84) and is boiled an hour under reflux. .The ground -joint condenser and large ground -joint flask are used for this purpose. The heated solution is allowed to cool with the condenser attached. The flask is next attached to the distillation setup and the volatile acidic constituents are distilled over. This distillation is carried out at constant volume. Before it is .. started, 5 ml. water is added. This quantity is distilled off; then another 5 ml. is added and distilled. This operation is repeated until 25 ml. of distillate has been collected. The total is titrated with the standard sodium hydroxide. The distillation and titration steps are repeated with consecutive 25 -ml. portions of distillate until check titrations are obtained. 67 -006 -2- Acetyl and C- Methyl After the acid content of the distillate has become constant, the flask is cooled and the reagent is stored in a ground -glass stoppered bottle provided with a cap. This reagent decomposes slowly. It must be protected from dust and fumes, and should be kept in a cool, dark place. 2. Boiled distilled water. This should be freshly prepared, and should be tested for alkalinity or acidity, and be redistilled if necessary. 3. 0.01N Sodium hydroxide solution. 4. 0.O1N Hydrochloric acid solution. 5. 1% Alcoholic phenolphthalein indicator. Methyl Alcoholic 1N Sodium Hydroxide Method 1. Methyl alcoholic 1N sodium hydroxide. 40 g. sodium hydroxide is dissolved in a mixture of 500 ml. each of water and methyl alcohol. The methyl alcohol must be neutral; if necessary, it is distilled from potassium hydroxide. Store in alkali- resistant bottle for more constant blanks. 2. 1:2 Sulfuric acid. 3. Boiled distilled water (as in 2 of "Chromic Acid Method). 4. 0.O1N Sodium hydroxide solution. 5. 0.O1N Hydrochloric acid solution. 6. 1% Alcoholic phenolphthalein solution. For Analysis of Substances Containing Halogen 1. Silver chromate or silver sulfate, crystals. Procedures Care of the Apparatus To get accurate results, all parts of the apparatus must be thoroughly clean. All pieces are cleaned with chromic- sulfuric acid cleaning 67 -006 -3- Acetyl and C-Methyl solution and then rinsed repeatedly with tap water, special attention being paid to all ground surfaces; then they are rinsed several times with distilled water. Distillation flasks are dried in the oven; the other parts are merely allowed to drain. The distilling condenser is steamed out thoroughly at the . beginning of each day's work. If at any time the inner surface of any piece becomes filmed or noticeably contaminated, it must be cleaned as described. Chromic Acid Procedure A sample containing 0.02 mg. or more of acetyl (usually 3- to 5 -mg. sample) is weighed in a long -handled weighing tube (or a short capillary if the sample is a liquid) and deposited at the bottom of the reaction flask. (See notel). Two or three platinum tetrahedra are added. Then 2 ml. of the 4N chromic acid reagent is added from a pipet, washing down the sides of the flask. The flask is attached to one of the ground -joint condensers which has been clamped in a vertical position. The ground joint is sealed with a drop of distilled water, and held in place by the usual spring- and -hook device. The flask is immersed in a vessel of 85% phosphoric acid until the two liquid levels coincide. Heating with a Bunsen burner is begun. The . sample is refluxed at 1650 -170° C. for 1 to 1 -1/2 hr., or longer if necessary. When the refluxing period is ended, the flask is cooled and its exterior is washed thoroughly with tap water to remove the bath liquid. The condenser is washed down with 4 ml. distilled water. The flask is then disengaged from the condenser and the ground surfaces are washed with 2 ml. of water; then with 1 ml. 67 -006 -4- Acetyl and C- Methyl During the reflux period, the distillation condenser has been set up and connected with the still -head and one of the larger ground -joint flasks previously mentioned. This apparatus has been steamed out for about 20 -30 min. To distill the acetic acid, the larger boiling flask is replaced by the flask containing the refluxed solution. The flask is heated with a micro - burner, the flame being 2 -3 cm. from the bottom of the flask. The funnel at the top of the distillation head is filled with 2 ml. of distilled water. A clean 25 -ml. graduate is placed under the exit end of the condenser. The flask is heated until the vapors have begun to condense in the second steam trap. Then the flame is removed and the liquid allowed to be sucked back into the flask. This operation is repeated two or three times, until the parts of the apparatus are heated. In all, 7 ml. of water is used in washing the reflux condenser, and this amount, plus the 2 ml. of reagent originally used, adds up to a total volume of 9 ml.
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