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TECHNICAL BULLETIN V Standard Analytical Methods for Determining Pydraul: Specific Gravity Neut. No. (Acidity) Moisture TECHNICAL BULLETIN O/FF-17 Monsanto 0221899.02 TOWOLDMONOQ26524 Standard Analytical Methods for Determining Pydraur. Specific Gravity Neut. Mo. (Acidity) Moisture TECHNICAL BULLETIN O/FF-17 0221900 n im--immn w< or M*W MONSANTO MAAIS NO ANY f OL>LCTS MM (M 0 10 NAtliNtliS At 10 lH| f IIN{ St m rl'"l* uIiWkIwt itultl 0* Mi ftCHANTAIIltTY (im >lun(* (*n cm*. ten* --wt--wiMf--nAAl--n. fcKlmin Mi ImMjm * ** imiunIoun uiuit" Organic Chaaucab Division/*00 N. Lindborgh BM./SI louts. Missouri 63166 TOWOLDMONOQ26525 STANDARD ANALYTICAL METHOD Product: Pydraul and Therminol Fluids Test: Specific Gravity By Hydrometer SCOPE The specific gravity of Pydraul or Therminol fluids can be determined by spindle hydrometer. EQUIPMENT Steam-jacketed hydrometer jar, fabricated from 14" stainless steel plate to form a cylinder long by 2)4" diameter. Two pieces of s. s. tubing, I D. X 1", are welded 1" from each end. A hole is drilled in each of two No. 13 rubber stoppers to accommodate an ungraduated pyrex cylinder, 40 X 330 mm. One stopper is placed at the bottom of the cylinder, the metal jacket is fitted snugly over the stopper and the second stopper is placed at the top of the jacket. The assembly must be tight to prevent steam leaks. SAFETY Use normal caution to prevent thermal bums when handling the steamjacketed hydrometer jar. DETERMINATION 1. Determine the specific gravity with the following modifications: a. Use appropriate narrow range hydrometer. (Example: for Therminol-FR-1 a range of 1.3-1.5 -- Example: for Pydraul -- A-200 a range of 1.3 to 1.5). b. Adjust the sample to a temperature range of 50-105C by regulating the steam flow through the steam jacket. c. Use a temperature coefficient of 0.009/C. d. Correct the specific gravity to 25/15.5C. CALCULATION Sp. Gr. 25/15.5"C. X 1.002 = Sp. Gr. 25/25C. Report the specific gravity at the specified temperature to the nearest 0.001 units. Duplicate results should agree within 0.001 units. RESULTS If specific gravity value is below new fluid specifications -- example: by .05 -- then consult your MONSANTO fluid specialist. | ! j i | j I TOWOLDMONOQ26526 STANDARD ANALYTICAL METHOD Product: Pydraul and Therminol fluids Test: Acidity (mg-KOG/g) or Neutralization Number SCOPE This test for the acidity of the fluid is in accordance with the ASTM Standard Test D664-58, Standard Method of Test for Neutralization Number by Potentiometric Titration. The acid number is determined by dissolving a quantity of the fluid in a mixture of toluene and isopropyl alcohol containing a small amount of water and then titrating potentiometrically with alcoholic potassium hydroxide. A glass indicating electrode and a calomel reference electrode are used in titrating. End points are taken as pH 11. Equipment a. Meter -- Voltmeter or potentiometer with accuracy of plus or minus .005 v, sensitivity of .002 v, and a range of .5 v, such as Beckman Model 96A, Fisher Scientific Model 210, or equivalent. b. Glass Electrode -- Fisher Catalog No. 13-639-1, or equivalent. c. Calomel Electrode -- Sleeve type -- Fisher Catalog No. 13-639-60, or equivalent. d. Stirrer -- Variable -- speed mechanical stirrer of any suitable type. e. Buret -- Fisher Catalog No. 3-847, Size D, or equivalent. f. Beaker -- A 300 ml. beaker made with borosilicate glass. g. Stand -- A suitable stand to support stirrer, electrodes, and buret such that the beaker can be removed without disturbing the as sembly is desirable. Reagents a. Buffer, Nonaqueous Basic -- Add 10 ml of buffer stock solution A to 100 ml. of titration solvent. Use within 1 hour. b. m-Nitrophenol (mol. wt. 139.11), conforming to the following requirements: ' melting point -- 96 to 97C color -- pale yellow Store in brown glass bottle. , c. Buffer Stock Solution A can be made or purchased as desired. Purchased solution available from Fisher Scientific or Micro Essential Laboratory (Brooklyn, New York). A pH 11 buffer is suggested. To make the buffer solution proceed as follows: *2l902 TOWOLDMONOQ26527 Accurately weigh 27.8 0.1 g of m-nitrophenol and transfer to a 1-liter volumetric flask containing 100 ml. of isopropyl alcohol. Usings a 250 ml. graduated cylinder, add to the flask while con tinuously stirring its contents, 60/Nt + 1 ml. of 0.2 N alcoholic KOH solution (Nj being the exact normality of the KOH solution found by standardization). Dilute to the 100 ml. mark with iso propyl alcohol, and mix thoroughly. d. Potassium Chloride Electrolyte -- Prepare a saturated solution potassium chloride (KC1) in water. e. Potassium Hydroxide Solution, Standard Alcoholic (O/N). Add 6 g of potassium hydroxide (KOH) to approximately 1 liter of anhydrous isopropyl alcohol. Boil gently for 10 min. to effect solution. Allow solution to stand for two days and then filter the supematent liquid through a fine sintered -- glass funnel. Store the solution in chemically resistant bottle. Dispense in such a manner that the solution is protected from atmospheric carbon dioxide (C02) by means of a soda lime or soda asbestos guard tube, and such that it does not come into contact with cork, rubber, or saponified stop-cock grease. Standardize frequently enough to detect normality changes of 0.0005. f. Potassium Hydroxide Solution, Standard Alcoholic (0.2N) -- Prepare, store and standardize as directed in paragraph (e), but use 12 to 13 g of KOH to approximately 1 liter of isopropyl alcohol. g. Titration solvent -- add 500 ml of toluene and 5 ml. of water to 495 ml. of anhydrous isopropyl alcohol. The titration solvent should be made up in large quantities, and its blank value determined daily by titration prior to use. Preparation of Apparatus Use standard procedures for preparation and maintenance of electrode equipment. Procedure for Acid Number a. Into a 300 ml titration beaker, introduce a weighed quantity of Therminol or Pydraul of about 10 g 0.10 g, and add 125 ml of titration solvent. Make sure all surfaces of the electrode are wiped clean and wetted with electrolyte previous to titration. Place beaker on stand and adjust its position so that the electrodes are about half immersed. Start stirrer, and stir throughout titration at a rate sufficient to produce vigorous agitation without spattering or without stirring air into the solution. b. Fill buret with the 0.1 N alcoholic KOH solution and place the buret into the titrating assembly so that the tip is about 1 inch into the liquid. Record the initial buret and meter (cell potential) readings. Add suitable small portions stant potential has been established, record the buret and meter readings. In regions where 0.1 ml. of titration solution causes a change of 0.032 (corresponding OZ2V903 | TOWOLDMONOQ26528 to 0.5 pH units), add 0.05 ml. portions. In regions where changes are less radical, add portions large enough to produce a change equal to, but not greater than 0.032. Titrate in this manner to an end-point of pH 11. c. Blank -- For each set of samples, make a blank titration of 125 ml. of titration solvent, adding 0.01 N alcoholic KOH solution in 0.05 ml. increments to a meter of pH 11. Calculations a. Note the volumes of the titrating solution for both sample and blank used to reach end-point of pH 11. b. Calculate the acidity number as follows: Acid Number ^A-B>X^ X 561 w where: . A = millimeters of alcoholic KOH solution used to titrate the sample to its end point, B *= volume corresponding to A for the blank titration, N = normality of the alcoholic KOH solution, and W = grams of sample. Note: A colorimetric method, ASTM D 974-64, can be used, however, dark colored Therminol will sometimes interfere with the colorimetric end point. STANDARD ANALYTICAL METHOD Product: Pydraul & Therminol Fluids Test: Moisture (H20 content) SCOPE This test for moisture content of the Pydrauls and Therminols is in accordance with the ASTM Standard Test D1744-64, Standard Method of Test for Water by Karl Fischer Reagent. The water content is deter mined by titrating the fluid with standard Karl Fischer reagent to an electrometric end point. EQUIPMENT a. Buret -- Fisher Catalogue No. 3-847 Size D, or equivalent. b. Stirrer -- magnetic stirrer. c. Titration Flask -- Fisher Catalogue No. 10-163,500 ml capacity. d. Meter System -- A micro-ammeter circuit can be assembled accord ing to the attached diagram and using the following components: Microammeter -- A dc meter having 0 to 50 micro amp range with internal resistance of 1500 ohms. 0221* ** TOWOLDMONOQ26529 Battery --1.5 volt dry cell. Electrodes -- a one inch long 0.01 to 0.03 inch diameter platinum wire sealed in soft glass tubing with tip extending approximately 0.6 inches. Fill glass tubing with mercury and seal wire lead into top of tubing with collodin. Potentiometer -- having resistance of 2000 ohms. A meter circuit can also be purchased. Example: Precision titration No. 68880 or equivalent would be suitable. Attachments can also be purchased to convert PH meters to indicate Karl Fischer end points. Interferences: Free alkali; oxidizing and reducing agents; Mercaptans, certain basic nitrogenous substances, or other materials that react with iodine, interfere. Reagents a. Karl Fischer Reagent, Stock Solution -- Can be purchased from Fischer Scientific Catalogue No. SO-K-2; or made as follows: For each liter of solution, dissolve 85 lg of iodine in 270 2 ml of pyridine in dry, glass-stoppered bottle. Add 670 2 ml of methanol (99.9 percent). Cool the mixture in an ice bath to below 8.9C. Bubble gaseous sulfur dioxide (S02) through concentrated sulfuric acid (HjS04, sp. gr. 1.84) into the cooled mixture. Continue the addition of S02 until the volume has increased 50 1 ml. Alternatively, add 50 1 ml freshly drawn liquid SO? in small increments to the precooled mixture in an ice bath. Mix well and set aside for at least 12 hours before using. b. Karl Fischer Reagent, Dilute Solution -- Can be purchased from Fischer Scientific Catalogue No. SO-K-5 or made from stock so lutions as follows: Adjust the strength of the stock solution to a water equivalence of 2 to 3 mg. of water per ml by dilution with pyridine. c. Sample Solvent -- Mix 1 volume methanol with 3 volumes of chloroform. Standardization cf Karl Fischer Reagent: a. Add 50 ml. of the sample solvent to a clean, dry titration flask. Insert the stopper and adjust stirrer to give a smooth stirring action. Turn on the indicating circuit and adjust potentiometer to give a reference point with approximately 1 j*a of current flowing. TOWOLDMON0026530 Add Karl Fischer reagent in suitable amounts to the solvent to cause the needle to deflect from the reference. The end point is reached when after the addition of a single drop of reagent, the needle remains defected at least 1 /,a from the reference point for at least 30 seconds. b. To the solution in the titration flask add carefully, from a weighing pipet previously weighed to the nearest 0.1 mg., 1 drop of distilled water. Stopper the flask and reweigh the weighing pipet. Titrate to the end point as described in the above paragraph. c. Calculate the water equivalence of the Karl Fischer reagent as follows: where: F * water equivalence of Karl Fischer reagent, in milligrams per milliliter, W = milligrams of water added, and T = milliliters of reagent required for the titration of the added water. Procedure: a. Add 50 ml. of solvent to the titration flask and titrate with the standardized Karl Fischer reagent to the end point as described in paragraph (a) of the previous section. Stopper the sample inlet tube as quickly as possible in order to prevent absorption of mois ture from the atmosphere. b. Weigh approximately 50 ml of the fluid and add to the titrating flask in any convenient manner. c. Titrate the fluid to the end point as described above. Record the milliliters of reagent used. Calculation: Calculate the water content of the fluid as follows: water, ppm CF x 1000 W where: C milliliters of reagent required for titration of the Thermino) or Pydraul, F = water equivalence in milligrams of water per milliliter, 1000 = factor for converting to parts per million, and W -- grams of sample used. 0Z21906 TOWOLDMONOQ26531 Test fob Water m Liquid Petroleum Products (D 1744) Xf"l4 TOWOLDMON0026532 E3scw*asrjin "X "S- :ryg,T-.rir DISTRICT SALES OFFICES ALL DIVISIONS AKRON. 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