1、Designation: D 483 04An American National StandardStandard Test Method forUnsulfonated Residue of Petroleum Plant Spray Oils1This standard is issued under the fixed designation D 483; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision,
2、 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. Scope*1.1 This test method covers the determination of unsul-fonated residue in plant spray oils of petroleum ori
3、gin andapplies only to the petroleum oil content. It provides a measureof the degree of refinement of plant spray oils by determiningthe extent to which the oil is attacked by 98.61 % sulfuric acidunder closely standardized conditions. Since the relationshipbetween unsulfonated residue and the actua
4、l composition of theoil is not known, this test method should be applied only formeasuring the degree of refinement and not for the determina-tion of aromatics or olefins, or both.1.2 The values stated in SI units are to be regarded as thestandard.1.3 This standard does not purport to address all of
5、 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. Referenced Documents2.1 ASTM Standards:2D 1193 Specification for
6、 Reagent WaterD 1250 Guide for Petroleum Measurement TablesD 1298 Test Method for Density, Relative Density (SpecificGravity), or API Gravity of Crude Petroleum and LiquidPetroleum Products by Hydrometer MethodD 4052 Test Method for Density and Relative Density ofLiquids by Digital Density MeterD 40
7、57 Practice for Manual Sampling of Petroleum andPetroleum ProductsD 4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definition:3.1.1 unsulfonated residue, nin oils, that portion of an oilremaining unsulfonated after treatment with concentrated sul-furic acid.
8、4. Summary of Test Method4.1 A measured volume of sample is shaken with 98.61 %sulfuric acid at 100C in a Babcock bottle, shaking mechani-cally for 10 s at 10-min intervals. The volume not absorbed bythe acid is a measure of the unsulfonated residue in the sample.5. Significance and Use5.1 This test
9、 method is useful for distinguishing betweenoils that are adaptable to various types of spraying application,with a higher unsulfonated oil being required for leaf sprayingas compared to dormant vegetation application.6. Apparatus6.1 Sulfonation FlaskThe flask is shown in Fig. A1.1 anddescribed in A
10、nnex A1.6.2 Meniscus Viewing Lens, focusing type, consisting ofeyepiece and objective to facilitate reading the meniscus witha minimum of parallax, is recommended.6.3 Water BathsTwo water baths maintained at 25 60.5C and 99.5 to 100C, and conforming to the requirementsprescribed in Annex A1.6.4 Shak
11、ing MachineThe exact design described in theappendix is required for uniform control of shaking andprecision results. Hand shaking is permissible if technique isdeveloped to correlate results by machine shaking.6.5 CentrifugeA centrifuge as described in Annex A1 isrecommended.7. Reagents7.1 Purity o
12、f 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 grades may be1This tes
13、t method is under the jurisdiction of ASTM Committee D02 onPetroleum Products and Lubricants and is the direct responsibility of SubcommitteeD02.06 on Analysis of Lubricants.Current edition approved Dec. 1, 2004. Published December 2004. Originallyapproved in 1961. Last previous edition approved in
14、2000 as D 483 00.2For 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.3“Reagent Chemicals, American Chemical Socie
15、ty 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 Formulary, U.S. Pharmacopei
16、al Convention, Inc. (USPC), Rockville,MD.1*A Summary of Changes section appears at the end of this standard.Copyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959, United States.used, provided it is first ascertained that the reagent is ofsufficiently high
17、 purity to permit its use without lessening theaccuracy of the determination.7.1.1 Commercially prepared solutions may be used whenthey meet or exceed the specifications set in 7.1.7.2 Fuming Sulfuric Acid (approximately 15 % free SO3).(WarningSee 7.3 and 7.4.)7.3 Sulfuric Acid (98.61 %)Prepare by b
18、lending reagent-grade fuming and concentrated sulfuric acids to a concentrationof 98.61 6 0.1 % H2SO4as determined by titration.(WarningCorrosive. Health hazard. Oxidizer.) (WarningWhile preparing the reagent, protect the face with a safetymask and place the flask in a tray.)7.4 Sulfuric Acid (sp gr
19、 1.84, approximately 95 %)Concentrated sulfuric acid (H2SO4). (WarningCorrosive.Health hazard. Oxidizer.).8. Reference Spray Oil48.1 Test results for unsulfonated residue are highly depen-dent upon rate of shaking. A reference spray oil has beencalibrated for unsulfonated residue by a group of coope
20、ratinglaboratories using both machine and hand shaking. Instructionsare given in Section 8 for using this reference oil as a guide toensure that the rate of shaking is correct.9. Calibration9.1 Machine Shaking RateA rate of 425 cycles/min wasused in the cooperative work to establish the unsulfonated
21、residue of the reference spray oil. There are small variations inseverity of shaking between individual machines, even whenthey are newly built and of the same make; and thesedifferences can increase with use. Consequently, each labora-tory shall run occasional tests on the reference spray oil. If a
22、nunsulfonated residue is found which differs by more than60.4 % from the established value, the rate of shaking shall beadjusted accordingly. A faster rate tends to give a lowerunsulfonated residue, and vice versa.9.2 Hand Shaking RateEach operator shall standardizehis technique of shaking so as to
23、obtain the established value(within 6 0.4 %) on the reference spray oil. A rate of 300cycles/min was used in the manual shaking tests in thecooperative program on the reference oil; however, an indi-vidual operators calibrated rate can differ appreciably from300 cycles/min.10. Sampling10.1 Obtain a
24、sample for this test method using PracticesD 4057 or D 4177.11. Procedure11.1 Adjust the temperature of the boiling water bath to 99.5to 100C and keep it in this temperature range throughout thetest. Adjust the shaker rate and check it before and after eachtest to make sure that the rate does not de
25、viate more than 610cycles/min from the rate established by calibration.(WarningWhen hand shaking, protect the face with a safetymask and point the Babcock bottle away from other personnel.Protect hands by wearing suitable safety gloves.)NOTE 1If hand shaking is used, shake the sulfonation flask bygr
26、asping the neck between the thumb and index finger and swinging theflask through an arc of approximately 20 so that the bottom of the flaskpasses through a distance of 64 to 89 mm (2.5 to 3.5 in.). Shake at the rateestablished by calibration within a tolerance of 610 cycles/min.11.2 Using Test Metho
27、ds D 1298 or D 4052, determine thedensity at 25C in grams per millilitre by means of dataobtained from Vol VIII and Vol XI/XII of the PetroleumMeasurement Tables. (See Guide D 1250.)11.3 Weigh into a clean, dry sulfonation flask the equivalentof 4.9 to 5.1 mL of the sample at 25C, weighed to the nea
28、rest0.005 g, adding the oil to the flask by pipet, and taking care todeposit as little oil as possible on the neck of the flask. Fromthe weight of the sample, calculate its volume at 25C.11.4 Slowly introduce 20 6 0.5 mL of H2SO4(98.61 %)into the flask in such a way that oil adhering to the neck of
29、theflask will be washed down. Transfer the flask to the carrier, andsuspend the carrier in the boiling water bath, with the flaskimmersed to a point between the 0 and 10 marks, noting thetime when this is done. Close the cover of the bath, and directa gentle stream of air across the top of the flask
30、 to blow awayany steam arising from the opening.11.5 After the flask has been in the bath for 10 6 1 min,remove the carrier and install it, with minimum delay, on theshaker. While wearing a face shield, shake for 10 6 1sattherate established in the calibration with the reference spray oil.(WarningCe
31、rtain samples of low unsulfonated residue canfoam excessively when shaken. Stop the shaker when the foamrises in the neck of the flask, and shake intermittently but at thespecified rate. Substitute the counter for the timer and shake atotal number of cycles equal to one-sixth of the numberrepresenti
32、ng the established rate in cycles per minute, eventhough it requires more than 10 s for example, if the rate is 425cycles/min, shake 71 cycles.) After shaking, return the carrierto the bath as quickly as possible. Repeat the shaking at 10 61 min intervals for a total of six shaking periods, so that
33、anhour has elapsed between the time of placing the flask in thebath, and the removal for the final shaking.11.6 After the final shaking, cool to approximately roomtemperature, and add sufficient H2SO4(95 %) to raise the oilinto the neck of the flask nearly to the top graduation. Place theflask in th
34、e centrifuge, balancing as necessary, and centrifugefor 10 min at a speed calculated by the equation given inA1.1.6, or taken from Table 1 to give a relative centrifugalforce between 80 and 100 at the bottom of the flask. Transferthe flask to a water bath maintained at 25 6 0.5C for 10 6 1min, with
35、the graduated neck immersed to the upper oil level.NOTE 2The use of rubber cushions in the centrifuge carrier tubes toavoid breakage is recommended.11.7 Transfer the flask to the shelf in the 25C bath. Usinga suitable light source, and the aid of a viewing lens, record thereading on the graduated ne
36、ck at the top and bottom of the oilcolumn, estimating to one fifth of the smallest division. The4The reference spray oil may be obtained from R. E. Carroll, Inc., P.O. Box5806, 1570 North Olden Ave., Trenton, NJ 08638. If you are aware of alternativesuppliers, please provide this information to ASTM
37、 International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee1, which you may attend.D483042bottom reading is generally sharp and straight across, andoffers no problem. In reading the top, hold a black strip (about10 by 50 mm) at the
38、back of the neck, and about 5 mm belowthe top of the oil column, which makes the lowest meniscusappear as a black curve. Install the viewing lens at a right angleto the neck of the flask at the proper height, focus it, and readthe lowest black meniscus. The upper and lower levels on theoil layer are
39、 represented by points A and B in Fig. 1. Point Adenotes the lowest portion of the boundary between the clearoil and the darkest part of the air-liquid interface, and point Brefers to the lowest portion of the interface between the clearoil and sulfonation acid.11.8 Repeat the centrifuging and tempe
40、rature equilibration(11.6 and 11.7), until constant readings have been obtained.12. Calculation and Report12.1 Correct the readings at the upper and lower oil surfacesin accordance with the calibration error.12.2 Calculate the unsulfonated residue as follows:Unsulfonated residue, volume % 5 A 2 B!/V
41、 3 100 (1)where:A = corrected scale reading, at upper oil level, mL,B = corrected scale reading at lower oil level, mL, andV = volume of sample used, mL.12.3 Report all results to the nearest 0.2 %.13. Precision and Bias13.1 The precision of this test method as determined bystatistical examination o
42、f interlaboratory results is as follows:13.1.1 Repeatability The difference between two testresults, obtained by the same operator with the same apparatusunder constant operating conditions on identical test material,would in the long run, in the normal and correct operation ofthe test method, excee
43、d the following values only in one casein twenty:Range of UnsulfonatedResidue, %Repeatability (MachineShaking)79 to 97 0.513.1.2 ReproducibilityThe difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material would
44、, inthe long run, in the normal and correct operation of the testmethod, exceed the following values only in one case intwenty:Range of UnsulfonatedResidue, %Reproducibility (MachineShaking)79 to 97 2.013.2 The precision of this test method is not known to havebeen obtained in accordance with curren
45、tly accepted guide-lines.513.3 BiasThere being no criteria for measuring bias inthese test product combinations, no statement of bias can bemade.14. Keywords14.1 petroleum plant spray oils; unsulfonated residue5Supporting data have been filed at ASTM International Headquarters and maybe obtained by
46、requesting Research Report RR: D02-1007.TABLE 1 Rotation Speeds for Centrifuges of VariousDiameters of SwingDiameter of Swing,mm (in.)ARpm at 80 rcf Rpm at 100 rcf508 (20) 530 590533 (21) 520 580559 (22) 510 570584 (23) 500 550609 (24) 490 540AMeasured in millimetres (inches) between bottoms of oppo
47、site flasks when inrotating position.FIG. 1 Method for Reading Volume of Unreacted OilD483043ANNEX(Mandatory Information)A1. APPARATUSA1.1 ApparatusA1.1.1 Sulfonation Flask, as shown in Fig. A1.1. This is astandard Babcock test bottle known as “50 %, 9 g, 9 in., in0.5 %, cream test bottle.”A1.1.2 To
48、 calibrate the graduated neck of the flask: first, fillexactly to the zero mark with water (see A1.1.2.2); thendetermine the true capacity to the 50 mark by adding waterfrom a standardized 10-mL buret. Calculate a volume calibra-tion factor.A1.1.2.1 The buret shall be subdivided to 0.01 or 0.02 mLan
49、d be provided with a tip delivering drops of approximately0.01 mL. Corrections to the nominal values of the buret shouldbe obtained in the laboratory and used in the calculation.A1.1.2.2 Water shall be reagent water conforming to Speci-fication D 1193, Type III.A1.1.3 Water Bath, maintained at 25 6 0.5C of sufficientdepth to permit immersion of the sulfonation flask to the topgraduation, and provided with a shelf at such a height that theflask, when placed on it, would be immersed to a point justbelow the bottom graduation.A1.1.4 Boiling-Water Bath
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