1、Designation: D 5348 95 (Reapproved 2006)Standard Test Method forDetermination of the Moisture Content of Sulfonated andSulfated Oils by Distillation with Xylene1This standard is issued under the fixed designation D 5348; the number immediately following the designation indicates the year oforiginal
2、adoption or, in the case of revision, the year of 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 This test method covers the determination of waterexisting in a sam
3、ple of sulfonated or sulfated oil, or both, bydistilling the sample with a volatile solvent. The test method isapplicable only to sulfonated and sulfated oils that do notcontain the following: mineral acids, free sulfonic acids, or freesulfuric acid esters; or alkali hydroxides, carbonates or ac-eta
4、tes: or alcohol, glycerin, diethylene glycol, acetone, or otherwater-miscible volatile compounds. This test method wasderived from Test Methods D 500, Sections 4 through 9.1.2 The values stated in SI units are to be regarded as thestandard. The values given in parentheses are provided forinformation
5、 only.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 safety and health practices and determine the applica-bility of regulatory limitations prior to use.2. Refere
6、nced Documents2.1 ASTM Standards:2D 500 Test Methods of Chemical Analysis of Sulfonatedand Sulfated Oils3. Significance and Use3.1 This test method is intended to determine the moisturecontent of fats, oils, and fatliquors used in the softening andstuffing of leather. The moisture content is measure
7、d for thepurpose of quality assurance.4. Apparatus4.1 The apparatus required consists 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 g
8、round joints. The trap serves to collect andmeasure the condensed water and to return the solvent to theflask. A suitable assembly of the apparatus is illustrated in Fig.1.4.1.1 Flask, 500-mL, of either the short-neck, round-bottomtype or the Erlenmeyer type.4.1.2 Heat SourceThe source of heat may b
9、e either an oilbath (stearic acid, paraffin wax, etc.), or an electric heaterprovided with a sliding rheostat or other means of heat control.4.1.3 Condenser, a 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
10、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 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 distil
11、lation conditions have beenestablished. Fig. 1 shows a conventional sealed-in type ofcondenser, but any other condenser fulfilling the detailedrequirements above may be used.4.1.4 Trap, a trap made of well-annealed glass constructedin accordance with Fig. 1 and graduated as shown to contain 5mL at 2
12、0C. 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 mL.5. Purity of Reagents5.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise indicated, it is intended tha
13、tall reagents shall conform to the specifications of the Commit-tee onAnalytical Reagents of theAmerican Chemical Society.36. Reagents6.1 Oleic Acid, heated previous to use for 5 to 10 min overa free flame at a temperature of 130 to 135C.1This test method is under the jurisdiction of ASTM Committee
14、D31 on Leatherand is the direct responsibility of Subcommittee D31.08 on Fats and Oils. This testmethod was developed in cooperation with the American Leather Chemists Assn.(Method H 40-1957).Current edition approved April 1, 2006. Published April 2006. Originallyapproved in 1993. Last previous edit
15、ion approved in 2001 as D 5348 95(2001).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 Chemicals, A
16、merican 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 National Formul
17、ary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.1Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.6.2 Xylene.7. Calibration7.1 To calibrate the apparatus add approximately1gofwater to a mixture of 80 g of xylene and 10 g
18、of oleic acid.Conduct the distillation as described in 8.2, 8.3, and 8.4. Whenall the water has distilled, cool the apparatus, add another g ofwater, and repeat the distillation. Continue the calibration up tothe capacity of the receiving tube.8. Procedure8.1 Clean the condenser and the receiving tu
19、be thoroughlywith soap and warm 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 analy
20、sis toyield about 4 mL of water. 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 a
21、bout two andone-half times the 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 immediate
22、ly connect theflask with the 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
23、hot. In this way a minimum of 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 t
24、he trap. This operationusually 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 th
25、e side of the receiver with 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
26、 measured in the trapmay be 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.10. Precision and Bias10.1 Although this test method is widely used, precision
27、andbias information is not available at this time.11. Keywords11.1 distillation; leather; moisture; sulfonated and sulfatedoils; xyleneA =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
28、/40.FIG. 1 Apparatus for Water Determination by Distillation withVolatile Solvent, Method ATABLE 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
29、 Smithsonian Tables, compiled from various authors.D 5348 95 (2006)2ASTM International takes no position respecting the validity of any patent rights asserted in connection with any item mentionedin this standard. Users of this standard are expressly advised that determination of the validity of any
30、 such patent rights, and the riskof infringement of such rights, are entirely their own responsibility.This standard is subject to revision at any time by the responsible technical committee and must be reviewed every five years andif not revised, either reapproved or withdrawn. Your comments are in
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32、d a fair hearing you shouldmake your views known to the ASTM Committee on Standards, at the address shown below.This standard is copyrighted by ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959,United States. Individual reprints (single or multiple copies) of this standard may be obtained by contacting ASTM at the aboveaddress or at 610-832-9585 (phone), 610-832-9555 (fax), or serviceastm.org (e-mail); or through the ASTM website(www.astm.org).D 5348 95 (2006)3
