1、Designation: D483 04 (Reapproved 2014)Standard Test Method forUnsulfonated Residue of Petroleum Plant Spray Oils1This standard is issued under the fixed designation D483; 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 () indicates an editorial change since the last revision or reapproval.1. Scope1.1 This test method covers the determination of unsul-fonated residue in plant spray oils of petroleum origin andapplies
3、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 actual composition o
4、f 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 asstandard. No other units of measurement are included in thisstandard.1.3 This st
5、andard 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. Referenced Documents2.1
6、 ASTM Standards:2D1193 Specification for Reagent WaterD1250 Guide for Use of the Petroleum Measurement TablesD1298 Test Method for Density, Relative Density, or APIGravity of Crude Petroleum and Liquid Petroleum Prod-ucts by Hydrometer MethodD4052 Test Method for Density, Relative Density, and APIGr
7、avity of Liquids by Digital Density MeterD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum Products3. Terminology3.1 Definitions:3.1.1 unsulfonated residue, n in oils, that portion of an oilremaining unsulfonated afte
8、r treatment with concentrated sul-furic acid.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 th
9、e sample.5. Significance and Use5.1 This test 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
10、flask is shown in Fig. A1.1 anddescribed in Annex 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 Baths Two water baths maintained at 25 60.5C and 99.5 to 100C, and conforming to t
11、he requirementsprescribed in Annex A1.6.4 Shaking Machine The 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
12、 Annex A1 isrecommended.7. Reagents7.1 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,1This test method is u
13、nder the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricantsand is the direct responsibility ofSubcommittee D02.06 on Analysis of Lubricants.Current edition approved May 1, 2014. Published July 2014. Originally approvedin 1961. Last previous edition approved in 2009
14、 as D483 04 (2009)01. DOI:10.1520/D0483-04R14.2For 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.Copyright ASTM
15、International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United States1where such specifications are 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
16、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 and7.4.)7.3 Sulfuric Acid (98.61 %)Prepare by blending reagent-grade fuming and concentrated sulfuric acids to
17、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 1.84, approximately 95 %)Concentrated sulfuric acid (H2SO4). (W
18、arningCorrosive.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 cooperatinglaboratories using both machine and hand shaking. Instruct
19、ionsare 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 unsulfonatedresidue of the reference spray oil. There are small variations i
20、nseverity 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 anunsulfonated residue is found which differs by more than60.4 %
21、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 standardize histechnique of shaking so as to obtain the established value(within 6 0.4 %) on the reference sp
22、ray oil. A rate of300 cycles 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 sample for this test method using PracticesD4057 or D4177.11. Pr
23、ocedure11.1 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 deviate more than610 cycles min from the rate established by calibra
24、tion.(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 bygrasping the neck between the thumb and index finger and swinging th
25、eflask through an arc of approximately 20 so that the bottom of the flaskpasses through a distance of 64 to 89 mm. Shake at the rate established bycalibration within a tolerance of 610 cycles/min.11.2 Using Test Methods D1298 or D4052, determine thedensity at 25C in grams per millilitre by means of
26、dataobtained from Vol VIII and Vol XI/XII of the PetroleumMeasurement Tables. (See Guide D1250.)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 nearest0.005 g, adding the oil to the flask by pipet, and taking care todeposit as little
27、 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 theflask will be washed down. Transfer the flask to the carrier, andsuspend the carrie
28、r 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 to blow awayany steam arising from the opening.11.5 After the flask has been in the b
29、ath 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.(Warning Certain samples of low unsulfonated residue canfoam excessively when shaken. Stop the s
30、haker 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 numberrepresenting the established rate in cycles per minute, eventhough it requires more than 10 s f
31、or example, if the rate is425 cycles min, shake 71 cycles.) After shaking, return thecarrier to the bath as quickly as possible. Repeat the shaking at10 6 1 min intervals for a total of six shaking periods, so thatan hour has elapsed between the time of placing the flask in thebath, and the removal
32、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 the centrifuge, balancing as necessary, and centrifugefor 10 min at a speed calculated
33、by the equation given inA1.1.6, or taken from Table 1 to give a relative centrifugal3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For Suggestions on the testing of reagents notlisted by the American Chemical Society, see Annual Standards for
34、LaboratoryChemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeiaand National Formulary, U.S. Pharmacopeial Convention, Inc. (USPC), Rockville,MD.4The reference spray oil may be obtained from R. E. Carroll, Inc., P.O. Box5806, 1570 North Olden Ave., Trenton, NJ 08638. If you are
35、 aware of alternativesuppliers, please provide this information to ASTM International Headquarters.Your comments will receive careful consideration at a meeting of the responsibletechnical committee,1which you may attend.D483 04 (2014)2force between 80 and 100 at the bottom of the flask. Transferthe
36、 flask to a water bath maintained at 25 6 0.5C for10 6 1 min, with the graduated neck immersed to the upper oillevel.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, an
37、d the aid of a viewing lens, record thereading on the graduated neck at the top and bottom of the oilcolumn, estimating to one fifth of the smallest division. Thebottom reading is generally sharp and straight across, andoffers no problem. In reading the top, hold a black strip (about10 by 50 mm) at
38、the 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
39、 are 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 t
40、emperature 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
41、B!/V# 3100 (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 examinati
42、on of 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, e
43、xceed the following values only in one casein twenty:Range of UnsulfonatedResidue, %Repeatability (MachineShaking)79 to 97 0.513.1.2 Reproducibility The difference between two singleand independent results obtained by different operators work-ing in different laboratories on identical test material
44、would, 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 c
45、urrently accepted guide-lines.13.3 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 residueTABLE 1 Rotation Speeds for Centrifuges of VariousDiameters of SwingDiameter of Swing,
46、mmARpm at 80 rcf Rpm at 100 rcf508 530 590533 520 580559 510 570584 500 550609 490 540AMeasured in millimetres between bottoms of opposite flasks when in rotatingposition.FIG. 1 Method for Reading Volume of Unreacted OilD483 04 (2014)3ANNEX(Mandatory Information)A1. APPARATUSA1.1 ApparatusA1.1.1 Sul
47、fonation 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 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 a
48、dding 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 mLand 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
49、 in the calculation.A1.1.2.2 Water shall be reagent water conforming to Speci-fication D1193, 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, maintained at 99.5 to 100C,and of sufficient depth to permit immersion of the sulfonationflask to a point between the 0 and 10 marks. The top of the b
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