1、Designation: D 500 95 (Reapproved 2003)Standard Test Methods ofChemical Analysis of Sulfonated and Sulfated Oils1This standard is issued under the fixed designation D 500; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, the year of
2、 last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon (e) 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 th
3、e following order:SectionMoisture:Test Method A. Water by Distillation with Volatile Solvent 4-9Test Method B. Moisture and Volatile Matter by Hot-Plate Method 10-14Organically Combined Sulfuric Anhydride:Test Method A. Titration Test 15-19Test Method B. Extraction-Titration Test 20-24Test Method C.
4、 Ash-Gravimetric Test (in the Presence of TrueSulfonates)25-28Total Desulfated Fatty Matter 29-32Total Active Ingredients 33-36Unsaponifiable Nonvolatile Matter 37-41Inorganic Salts 42-46Total Alkalinity 47-49Total Ammonia 50-52Acidity as Free Fatty Acids or Acid Number:Test Method A. In the Absence
5、 of Ammonium or TriethanolamineSoaps53-56Test Method B. In the Presence of Dark Colored Oils but in theAbsence of Ammonium or Triethanolamine Soaps (Brine Test)57-60Test Method C. In the Presence of Ammonium or TriethanolamineSoaps61-63Water-Immiscible Organic Solvents Volatile with Steam 64-701.2 T
6、he values stated in 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 estab
7、lish appro-priate 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:D 1193 Specification for Reagent
8、 Water23. Purity of 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
9、 available.3Other grades 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 confor
10、mingto Specification D 1193.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 sulfona
11、ted and sulfated oils 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.5. Apparatus5.1 The apparatus required c
12、onsists of a glass flask heatedby suitable means and provided with a reflux 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
13、 return the solvent to theflask. A suitable assembly of the apparatus is illustrated in Fig.1.1These test methods are under the jurisdiction of ASTM Committee D12 onSoaps and Other Detergents and is the direct responsibility of Subcommittee D12.12on Analysis of Soaps and Synthetic Detergents.Current
14、 edition approved April 15, 1995. Published June 1995. Originallypublished as D 500 37. Last previous edition D 500 89.2Annual Book of ASTM Standards, Vol 11.01.3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on the testing of r
15、eagents notlisted by the American Chemical Society, see Analar Standards for LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, P
16、O Box C700, West Conshohocken, PA 19428-2959, United States.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
17、 other means of heat control.5.1.3 CondenserA 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 o
18、f 30 from the vertical axisof the condenser. 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 cond
19、enser fulfilling the detailedrequirements above may be used.5.1.4 TrapA trap 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 anyindicat
20、ed capacity may not be greater than 0.05 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.Cond
21、uct the distillation as described in 8.2-8.4. 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 w
22、arm water before using. Rinse well, then 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 wa
23、ter. Introduce the approximate quantityinto 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 t
24、he weight of the bone-dry sample to preventfoaming 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
25、 distillation apparatus. Insert a loose cotton 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 o
26、f water will condensefarther up the condenser 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 operationusual
27、ly requires less than 1 h. Increase the rate 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
28、a thin copperwire twisted into a loop. Immerse 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
29、converted into its equivalent weight in grams by meansof Table 1. Calculate the percentage of water as follows:Water, % 5 A/B! 3 100 (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 determin
30、ation of thepercentage of water and other compounds volatile at aboutA =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 withV
31、olatile Solvent, Method AD 500 95 (2003)2100C 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, ammoni
32、a, acetic acid or similar volatile acids, alkalihydroxides, 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 require
33、d consists of a glass-stopperedweighing flask, 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 He
34、at SourceThe source of heat may be either anelectric 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. Re
35、agents12.1 Desiccating AgentAny suitable desiccating agentmay be used.NOTE 1Recent investigations seem to indicate that calcium chlorideis unreliable as a laboratory desiccating agent.12.2 Oleic Acid.13. Procedure13.1 Weigh approximately5gofoleic acid into the beakerand insert the thermometer. Heat
36、the oleic acid gradually, whilestirring with 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 P
37、lace about6gofthesample in the weighing flask 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
38、 the moisture in the sample.14. Calculation14.1 Calculate the percentage of moisture and volatilematter in the sample as follows:Moisture and volatile matter, % 5 A/B! 3 100 (2)where:A = loss of weight, g, andB = weight of sample, g.ORGANICALLY COMBINED SULFURICANHYDRIDEMethod A. Titration Test (For
39、 Sulfated Oils)15. Scope15.1 This test method 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 t
40、heir combined SO3uponboiling with mineral acids 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 connect
41、ionbetween the flask and the condenser shall 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 requir
42、ed consists of aglass tube, 915 mm (36 in.) in length, and 8 mm (516 in.) inTABLE 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 0.9910744 0.9906645 0.99025AThis table is taken from Smithsonian Ta
43、bles, compiled from various authors.FIG. 2 Apparatus for Determination of Organically CombinedSulfuric Anhydride, Method AD 500 95 (2003)3outside 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 ofch
44、emically-resistant glass, approximately 4 mm (532 in.) indiameter. Before using, the glass beads shall be boiled thor-oughly in several portions of water or until the wash waterreacts neutral to methyl orange indicator.17. Reagents17.1 Ethyl Ether.17.2 Methyl Orange Indicator Solution (1 g/L)Dissolv
45、e0.1 g of methyl orange in 100 mL of water.17.3 Sodium Chloride (NaCl), solid.17.4 Sodium Hydroxide, Standard Solution (1 N)Accurately 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 NN
46、aOH solution is equivalent to 56.1 mg of KOH.17.5 Sodium Hydroxide, Standard Solution (0.5 N)Accurately prepare and standardize a 0.5 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 Aci
47、d, Standard (0.5 N)Accurately prepareand standardize a 0.5 N sulfuric acid (H2SO4) solution. Expressthe strength of the solution as 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,
48、sp gr 1.84) into 19 volumesof water while stirring.18. Procedure18.1 The procedure consists of two determinations: namely,(a) the alkalinity 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
49、 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 titration byadding first 0.5 N NaOH solution several drops at a time untilthe solution is alkaline and then the acid 1 or 2 drops at a timeuntil the end point is reached. Shake the solution
