1、Designation: D500 95 (Reapproved 2016)Standard Test Methods ofChemical Analysis of Sulfonated and Sulfated Oils1This standard is issued under the fixed designation D500; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of l
2、ast revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.1. Scope1.1 These test methods cover the chemical analysis ofsulfonated and sulfated oils. The analytical procedures appearin the f
3、ollowing order:SectionMoisture:Test Method A. Water by Distillation with Volatile Solvent 49Test Method B. Moisture and Volatile Matter by Hot-Plate Method 1014Organically Combined Sulfuric Anhydride:Test Method A. Titration Test 1519Test Method B. Extraction-Titration Test 2024Test Method C. Ash-Gr
4、avimetric Test (in the Presence of TrueSulfonates)2528Total Desulfated Fatty Matter 2932Total Active Ingredients 3336Unsaponifiable Nonvolatile Matter 3741Inorganic Salts 4246Total Alkalinity 4749Total Ammonia 5052Acidity as Free Fatty Acids or Acid Number:Test Method A. In the Absence of Ammonium o
5、r TriethanolamineSoaps5356Test Method B. In the Presence of Dark Colored Oils but in theAbsence of Ammonium or Triethanolamine Soaps (Brine Test)5760Test Method C. In the Presence of Ammonium or TriethanolamineSoaps6163Water-Immiscible Organic Solvents Volatile with Steam 64701.2 The values stated i
6、n inch-pound units are to be regardedas the standard. The metric equivalents of inch-pound unitsmay be approximate.1.3 This standard does not purport to address all of thesafety concerns, if any, associated with its use. It is theresponsibility of the user of this standard to establish appro-priate
7、safety and health practices and determine the applica-bility of regulatory limitations prior to use. Material SafetyData Sheets are available for reagents and materials. Reviewthem for hazards prior to usage.2. Referenced Documents2.1 ASTM Standards:2D1193 Specification for Reagent Water3. Purity of
8、 Reagents3.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended thatall reagents shall conform to the specifications of the Commit-tee on Analytical Reagents of the American Chemical Society,where such specifications are available.3Other g
9、rades may beused, provided it is first ascertained that the reagent is ofsufficiently high purity to permit its use without lessening theaccuracy of the determination.3.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water conformingto Specificatio
10、n D1193.MOISTUREMethod A. Water by Distillation with Volatile Solvent4. Scope4.1 This test method covers the determination of waterexisting in a sample of sulfonated or sulfated oil, or both, bydistilling the sample with a volatile solvent. The method isapplicable only to sulfonated and sulfated oil
11、s that do notcontain the following: mineral acids, free sulfonic acids, or freesulfuric acid esters; or alkali hydroxides, carbonates or ac-etates; or alcohol, glycerin, diethylene glycol, acetone, or otherwater-miscible volatile compounds.1These test methods are under the jurisdiction of ASTM Commi
12、ttee D12 onSoaps and Other Detergents and is the direct responsibility of Subcommittee D12.12on Analysis and Specifications of Soaps, Synthetics, Detergents and their Compo-nents.Current edition approved July 1, 2016. Published August 2016. Originallyapproved in 1937. Last previous edition approved
13、in 2009 as D500 95(2009).DOI: 10.1520/D0500-95R16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.3Reagent Ch
14、emicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of reagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand Natio
15、nal Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States15. Apparatus5.1 The apparatus required consists of a glass flask heatedby suitable means and provided with a reflu
16、x condenserdischarging into a trap and connected to the flask. Theconnections between the trap and the condenser and flask shallbe interchangeable ground joints. The trap serves to collect andmeasure the condensed water and to return the solvent to theflask. A suitable assembly of the apparatus is i
17、llustrated in Fig.1.5.1.1 Flask, 500-mL, of either the short-neck, round-bottomtype or the Erlenmeyer type.5.1.2 Heat SourceThe source of heat may be either an oilbath (stearic acid, paraffin wax, etc.), or an electric heaterprovided with a sliding rheostat or other means of heat control.5.1.3 Conde
18、nserA water-cooled glass reflux condenser(Fig. 1), having a jacket approximately 400 mm (1534 in.) inlength with an inner tube 9.5 to 12.7 mm (38 to12 in.) inoutside diameter. The end of the condenser to be inserted in thetrap shall be ground off at an angle of 30 from the vertical axisof the conden
19、ser. When inserted into the trap, the tip of thecondenser shall be about 7 mm (14 in.) above the surface of theliquid in the trap after the distillation conditions have beenestablished. Fig. 1 shows a conventional sealed-in type ofcondenser, but any other condenser fulfilling the detailedrequirement
20、s above may be used.5.1.4 TrapAtrap made of well-annealed glass constructedin accordance with Fig. 1 and graduated as shown to contain 5mL at 20C. It shall be subdivided into 0.1-mL divisions, witheach 1-mL line numbered (5 mL at top). The error in anyindicated capacity may not be greater than 0.05
21、mL.6. Reagents6.1 Oleic Acid, heated previous to use for 5 to 10 min overa free flame at a temperature of 130 to 135C.6.2 Xylene.7. Calibration7.1 To calibrate the apparatus add approximately1gofwater to a mixture of 80 g of xylene and 10 g of oleic acid.Conduct the distillation as described in 8.2
22、8.4. When all thewater has distilled, cool the apparatus, add another g of water,and repeat the distillation. Continue the calibration up to thecapacity of the receiving tube.8. Procedure8.1 Clean the condenser and the receiving tube thoroughlywith soap and warm water before using. Rinse well, then
23、treatwith hot cleaning solution (a mixture of 10 mL of saturatedpotassium dichromate (K2Cr2O7) and 990 mL of sulfuric acid(H2SO4, sp gr 1.84), and finally thoroughly wash and dry.8.2 Take enough of the sample to be tested for analysis toyield about 4 mL of water. Introduce the approximate quantityin
24、to a weighing bottle and make the weighings from the bottleinto the flask, taking care that after removal of the sample nodrops of oil are left on the outside of the weighing bottle. Add80 g of xylene and oleic acid equivalent to about two andone-half times the weight of the bone-dry sample to preve
25、ntfoaming and jellying of the contents of the flask. Introduceglass beads to prevent bumping and mix the contents of theflask thoroughly by swirling, taking care to avoid any loss ofmaterial. Fill the trap with xylene and immediately connect theflask with the distillation apparatus. Insert a loose c
26、otton plugin the top of the condenser tube to prevent condensation ofatmospheric moisture in the condenser tube.8.3 Heat the flask and regulate the heating so that thecondenser tube immediately below the water jacket is justbarely hot. In this way a minimum of water will condensefarther up the conde
27、nser where it may be difficult to volatilizeany moisture condensed on the walls.8.4 Continue the distillation at the specified rate untilpractically no water is visible on any part of the apparatusexcept within the graduations of the trap. This operationusually requires less than 1 h. Increase the r
28、ate of distillation inorder to remove all traces of condensed water in the condensertube, and continue the distillation until the water level in thetrap remains unchanged after a 10-min interval. Dislodge anydroplets adhering to the side of the receiver with a thin copperwire twisted into a loop. Im
29、merse the receiving tube in warmwater at about 40C for 15 min or until the xylene layerbecomes clear, then read and record the temperature and theexact volume of the water in the trap.9. Calibration9.1 The volume of condensed water measured in the trapmay be converted into its equivalent weight in g
30、rams by meansof Table 1. Calculate the percentage of water as follows:A =45to55mmB = 22 to 24 mm in inside diameterC = 9 to 11 mm in inside diameterD = 235 to 240 mmE = 146 to 156 mmF and G are interchangeable joints, standard taper 24/40.FIG. 1 Apparatus for Water Determination by Distillation with
31、Volatile Solvent, Method AD500 95 (2016)2Water, % 5 A/B! 3100 (1)where:A = weight of water, g, andB = weight of sample, g.Method B. Moisture and Volatile Matter by Hot-PlateMethod10. Scope10.1 This test method covers the determination of thepercentage of water and other compounds volatile at about10
32、0C existing in a sample of sulfonated or sulfated oil, orboth, by rapid evaporation. The test method is applicable onlyto sulfonated and sulfated oils that do not contain the follow-ing: mineral acids, free sulfonic acids or free sulfuric acidesters, ammonia, acetic acid or similar volatile acids, a
33、lkalihydroxides, carbonates, acetates or similar salts that may reactwith oleic acid at elevated temperatures liberating volatileacids, or glycerin, diethylene glycol, xylene, or other com-pounds of similar volatility.11. Apparatus11.1 The apparatus required consists of a glass-stopperedweighing fla
34、sk, a glass beaker, and a suitable thermometer.11.1.1 Weighing FlasksAny suitable glass-stopperedweighing flask of 10 to 15-mL capacity.11.1.2 BeakerA Griffin low-form glass beaker with anapproximate capacity of 150 mL and a diameter of about 5 cm.11.1.3 Heat SourceThe source of heat may be either a
35、nelectric hot plate with or without asbestos paper or board cover,or an open flame under a suitable asbestos board and a wiregauze (to spread the heat).11.1.4 Thermometer, graduated from 90 to 150C, about 3in. in length, and substantially constructed.12. Reagents12.1 Desiccating AgentAny suitable de
36、siccating agentmay be used.NOTE 1Recent investigations seem to indicate that calcium chloride isunreliable as a laboratory desiccating agent.12.2 Oleic Acid.13. Procedure13.1 Weigh approximately5gofoleic acid into the beakerand insert the thermometer. Heat the oleic acid gradually, whilestirring wit
37、h the thermometer, until the temperature reaches130C. Place the beaker in an oven at 105 to 110C for 15 min,cool in a desiccator, and weigh. Repeat the heating over the hotplate and in the oven until two successive weighings differ byless than 1.5 mg.13.2 Place about6gofthesample in the weighing fla
38、sk anddetermine the weight accurately. Transfer the sample to thebeaker (containing the oleic acid and the thermometer) andweigh the flask again. Heat the mixture exactly as in the taringof the beaker as described in 13.1. The loss in weight isequivalent to the moisture in the sample.14. Calculation
39、14.1 Calculate the percentage of moisture and volatilematter in the sample as follows:Moisture and volatile matter, % 5 A/B! 3100 (2)where:A = loss of weight, g, andB = weight of sample, g.ORGANICALLY COMBINED SULFURICANHYDRIDEMethod A. Titration Test (For Sulfated Oils)15. Scope15.1 This test metho
40、d covers the determination of theorganically combined sulfuric anhydride existing in a sampleof sulfated oil by boiling the sample with sulfuric acid anddetermining the acidity of the reaction mixture. This method isapplicable only to oils that split off their combined SO3uponboiling with mineral ac
41、ids and that do not contain compoundsthat cannot be accurately titrated in water solution with methylorange as the indicator.16. Apparatus16.1 The apparatus required consists of a glass flask pro-vided with a glass stopper and an air condenser.The connectionbetween the flask and the condenser shall
42、be a ground joint.Perforated glass beads shall be used to prevent bumping.16.1.1 FlaskAn Erlenmeyer flask (Fig. 2) made of aborosilicate glass, having a capacity of approximately 300 mLand provided with a glass stopper.16.1.2 CondenserThe condenser required consists of aglass tube, 915 mm (36 in.) i
43、n length, and 8 mm (516 in.) inoutside diameter. The lower end of the tube shall be flared andground to fit the mouth of the Erlenmeyer flask.16.1.3 Glass BeadsPerforated glass beads, made ofchemically-resistant glass, approximately 4 mm (532 in.) indiameter. Before using, the glass beads shall be b
44、oiled thor-oughly in several portions of water or until the wash waterreacts neutral to methyl orange indicator.17. Reagents17.1 Ethyl Ether.TABLE 1 Specific Gravity of WaterATemperature, C Specific Gravity4 1.0000035 0.9940636 0.9937137 0.9933638 0.9929939 0.9926240 0.9922441 0.9918642 0.9914743 0.
45、9910744 0.9906645 0.99025AThis table is taken from Smithsonian Tables, compiled from various authors.D500 95 (2016)317.2 Methyl Orange Indicator Solution (1 g/L)Dissolve0.1 g of methyl orange in 100 mL of water.17.3 Sodium Chloride (NaCl), solid.17.4 Sodium Hydroxide, Standard Solution (1 N)Accurate
46、ly prepare and standardize a 1 N sodium hydroxide(NaOH) solution. Express the strength or concentration of thesolution as milligrams of KOH per millilitre; 1 mL of 1 NNaOH solution is equivalent to 56.1 mg of KOH.17.5 Sodium Hydroxide, Standard Solution (0.5 N)Accurately prepare and standardize a 0.
47、5 N NaOH solution.Express the strength of the solution as milligrams of KOH permillilitre; 1 mL of 0.5 N NaOH solution is equivalent to 28.05mg of KOH.17.6 Sulfuric Acid, Standard (0.5 N)Accurately prepareand standardize a 0.5 N sulfuric acid (H2SO4) solution. Expressthe strength of the solution as
48、milligrams of KOH per millilitre;1mLof0.5N H2SO4is equivalent to 28.05 mg of KOH.17.7 Sulfuric Acid (1 + 19)Carefully mix 1 volume ofconcentrated sulfuric acid (H2SO4, sp gr 1.84) into 19 volumesof water while stirring.18. Procedure18.1 The procedure consists of two determinations: namely,(a) the al
49、kalinity of the sample, designated as A, and (b) theincrease in acidity after boiling the sample with sulfuric acid,designated as F.18.1.1 Alkalinity, ADissolve 10 g of the sample in 100 mLof water in the 300-mL glass-stoppered Erlenmeyer flask,warming to obtain solution if necessary. After cooling, add 30g of NaCl, 25 mL of ether, and 5 drops of methyl orangeindicator solution; then add 0.5 N H2SO4with frequent butgentle shaking until the mixture is slightly acid. Shake thecontents of the flask vigorously, and complete the tit
