1、Designation: D4052 16Standard Test Method forDensity, Relative Density, and API Gravity of Liquids byDigital Density Meter1This standard is issued under the fixed designation D4052; the number immediately following the designation indicates the year oforiginal adoption or, in the case of revision, t
2、he year of last revision. A number in parentheses indicates the year of last reapproval. Asuperscript epsilon () indicates an editorial change since the last revision or reapproval.This standard has been approved for use by agencies of the U.S. Department of Defense.1. Scope*1.1 This test method cov
3、ers the determination of the density,relative density, and API Gravity of petroleum distillates andviscous oils that can be handled in a normal fashion as liquidsat the temperature of test, utilizing either manual or automatedsample injection equipment. Its application is restricted toliquids with t
4、otal vapor pressures (see Test Method D5191)typically below 100 kPa and viscosities (see Test Method D445or D7042) typically below about 15 000 mm2/s at the tempera-ture of test. The total vapor pressure limitation however can beextended to 100 kPa provided that it is first ascertained thatno bubble
5、s form in the U-shaped, oscillating tube, which canaffect the density determination. Some examples of productsthat may be tested by this procedure include: gasoline andgasoline-oxygenate blends, diesel, jet, basestocks, waxes, andlubricating oils.1.1.1 Waxes and highly viscous samples were not inclu
6、dedin the 1999 interlaboratory study (ILS) sample set that wasused to determine the current precision statements of themethod, since all samples evaluated at the time were analyzedat a test temperature of 15 C. Wax and highly viscous samplesrequire a temperature cell operated at elevated temperature
7、snecessary to ensure a liquid test specimen is introduced foranalysis. Consult instrument manufacturer instructions forappropriate guidance and precautions when attempting toanalyze wax or highly viscous samples. Refer to the Precisionand Bias section of the method and Note 8 for more detailedinform
8、ation about the 1999 ILS that was conducted.1.2 In cases of dispute, the referee method is the one wheresamples are introduced manually as in 6.3 or 6.4, as appropri-ate for sample type.1.3 When testing opaque samples, and when not usingequipment that is capable of automatic bubble detection,proper
9、procedure shall be established so that the absence of airbubbles in the sample cell can be established with certainty.For the determination of density in crude oil samples use TestMethod D5002.1.4 The values stated in SI units are regarded as thestandard, unless stated otherwise. The accepted units
10、of mea-sure for density are grams per millilitre (g/mL) or kilogramsper cubic metre (kg/m3).1.5 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 pract
11、ices and determine the applica-bility of regulatory limitations prior to use. For specificwarning statements, see 7.4, 7.5, and 10.3.2. Referenced Documents2.1 ASTM Standards:2D287 Test Method for API Gravity of Crude Petroleum andPetroleum Products (Hydrometer Method)D445 Test Method for Kinematic
12、Viscosity of Transparentand Opaque Liquids (and Calculation of Dynamic Viscos-ity)D1193 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
13、 MethodD4057 Practice for Manual Sampling of Petroleum andPetroleum ProductsD4177 Practice for Automatic Sampling of Petroleum andPetroleum ProductsD4377 Test Method for Water in Crude Oils by Potentiomet-ric Karl Fischer TitrationD5002 Test Method for Density and Relative Density ofCrude Oils by Di
14、gital Density AnalyzerD5191 Test Method for Vapor Pressure of Petroleum Prod-ucts (Mini Method)1This test method is under the jurisdiction of ASTM Committee D02 onPetroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility ofSubcommittee D02.04.0D on Physical and Chemical Metho
15、ds.Current edition approved Dec. 1, 2016. Published January 2017. Originallyapproved in 1981. Last previous edition approved in 2015 as D4052 15. DOI:10.1520/D4052-16.2For referenced ASTM standards, visit the ASTM website, www.astm.org, orcontact ASTM Customer Service at serviceastm.org. For Annual
16、Book of ASTMStandards volume information, refer to the standards Document Summary page onthe ASTM website.*A Summary of Changes section appears at the end of this standardCopyright ASTM International, 100 Barr Harbor Drive, PO Box C700, West Conshohocken, PA 19428-2959. United StatesThis internation
17、al standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for theDevelopment of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee
18、.1D7042 Test Method for Dynamic Viscosity and Density ofLiquids by Stabinger Viscometer (and the Calculation ofKinematic Viscosity)3. Terminology3.1 Definitions:3.1.1 density, nmass per unit volume at a specified tem-perature.3.1.2 relative density, nthe ratio of the density of amaterial at a stated
19、 temperature to the density of water at astated temperature.3.2 Definitions of Terms Specific to This Standard:3.2.1 adjustment, vthe operation of bringing the instru-ment to a state of performance suitable for its use, by setting oradjusting the density meter constants.3.2.1.1 DiscussionOn some dig
20、ital density analyzerinstruments, an adjustment may be made rather than calibratingthe instrument. The adjustment procedure uses air and freshlyboiled reagent water (WarningHandling water at boiling ornear boiling temperature can present a safety hazard. Wearappropriate personal protective equipment
21、.) as standards toestablish the linearity of measurements over a range ofoperating temperatures.3.2.2 calibration, vset of operations that establishes therelationship between the reference density of standards and thecorresponding density reading of the instrument.4. Summary of Test Method4.1 A smal
22、l volume, approximately 1 mL to 2 mL, of liquidsample is introduced into an oscillating sample tube and thechange in oscillating frequency caused by the change in themass of the tube is used in conjunction with calibration data todetermine the density, relative density, or API Gravity of thesample.
23、Both manual and automated injection techniques aredescribed.5. Significance and Use5.1 Density is a fundamental physical property that can beused in conjunction with other properties to characterize boththe light and heavy fractions of petroleum and petroleumproducts.5.2 Determination of the density
24、 or relative density ofpetroleum and its products is necessary for the conversion ofmeasured volumes to volumes at the standard temperature of15 C.6. Apparatus6.1 Digital Density AnalyzerA digital analyzer consistingof a U-shaped, oscillating sample tube and a system forelectronic excitation, freque
25、ncy counting, and display. Theanalyzer shall accommodate the accurate measurement of thesample temperature during measurement or shall control thesample temperature as described in 6.2.The instrument shall becapable of meeting the precision requirements described in thistest method.6.2 Circulating C
26、onstant-Temperature Bath, (optional), ca-pable of maintaining the temperature of the circulating liquidconstant to 60.05 C in the desired range. Temperature controlcan be maintained as part of the density analyzer instrumentpackage.6.3 Syringes, for use primarily in manual injections, at least2 mL i
27、n volume with a tip or an adapter tip that will fit theopening of the oscillating tube.6.4 Flow-Through or Pressure Adapter, for use as an alter-native means of introducing the sample into the densityanalyzer either by a pump, by pressure, or by vacuum.NOTE 1It is highly recommended that a vacuum no
28、t be applied tosamples prone to light-end loss, as it can easily lead to the formation ofbubbles. It is recommended to fabricate a special cap or stopper for samplecontainers so that air, such as from a squeeze pump, is used to displace atest specimen to the U-tube measuring cell by the flow-through
29、 method.6.5 Autosampler, required for use in automated injectionanalyses. The autosampler shall be designed to ensure theintegrity of the test specimen prior to and during the analysisand be equipped to transfer a representative portion of testspecimen to the digital density analyzer.6.6 Temperature
30、 Sensing Device (TSD), capable of monitor-ing the observed test temperature to within an accuracy of6 0.05 C. If a liquid-in-glass thermometer is used as the TSD,it shall be calibrated and graduated to 0.1 C, and have a holderthat can be attached to the instrument for setting and observingthe test t
31、emperature. In calibrating the thermometer, the icepoint and bore connections should be estimated to the nearest0.05 C. For non-mercurial thermometers, the TSD deviceshall be calibrated at least annually against a certified andtraceable standard.6.7 Ultrasonic Bath, Unheated, (optional), of suitable
32、 di-mensions to hold container(s) placed inside of bath, for use ineffectively dissipating and removing air or gas bubbles thatmay be entrained in viscous sample types prior to analysis.7. Reagents and Materials7.1 Purity of ReagentsReagent grade chemicals shall beused in all tests. Unless otherwise
33、 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 beused, provided it is first ascertained that the reagent is ofsufficiently high purity
34、to permit its use without lessening theaccuracy of the determination.7.2 Purity of WaterUnless otherwise indicated, referencesto water shall be understood to mean reagent water as definedby Type II of Specification D1193 or higher.7.3 Water, reagent water, freshly boiled to remove dissolvedgasses, f
35、or use as primary calibration standard. (WarningHandling water at boiling or near boiling temperature canpresent a safety hazard. Wear appropriate personal protectiveequipment.)3Reagent Chemicals, American Chemical Society Specifications, AmericanChemical Society, Washington, DC. For suggestions on
36、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. Pharmaceutical Convention, Inc. (USPC), Rockville,MD.D4052 1627.4 Cleaning Solvent, such as
37、petroleum naphtha4(WarningPetroleum naphtha is extremely flammable), orother materials that are capable of flushing and removingsamples entirely from the sample tube.7.5 Acetone, for flushing and drying the sample tube.(WarningExtremely flammable.)7.6 Dry Air, for drying the oscillator tube.8. Sampl
38、ing, Test Specimens, and Test Units8.1 Sampling is defined as all the steps required to obtain analiquot of the contents of any pipe, tank, or other system, andto place the sample into the laboratory test container. Thelaboratory test container and sample volume shall be ofsufficient capacity to mix
39、 the sample and obtain a homoge-neous sample for analysis.8.2 Laboratory SampleUse only representative samplesobtained as specified in Practices D4057 or D4177 for this testmethod.8.3 Test SpecimenAportion or volume of sample obtainedfrom the laboratory sample and delivered to the densityanalyzer sa
40、mple tube. The test specimen is obtained as follows:8.3.1 Mix the sample if required to homogenize, taking careto avoid the introduction of air bubbles. The mixing may beaccomplished as described in Practice D4177 or Test MethodD4377. Mixing at room temperature in an open container canresult in the
41、loss of volatile material from certain sample types(for example, gasoline samples), so mixing in closed, pressur-ized containers or at least 10 C below ambient temperature isrequired for such sample types where loss of volatile materialis a potential concern. For some sample types, such as viscouslu
42、be oils that are prone to having entrained air or gas bubblespresent in the sample, the use of an ultrasonic bath (see 6.7)without the heater turned on (if so equipped), has been foundeffective in dissipating bubbles typically within 10 min.NOTE 2When mixing samples with volatile components, conside
43、r thesample properties in relation to both ambient temperature and pressure.8.3.2 For manual injections, draw the test specimen from aproperly mixed laboratory sample using an appropriate sy-ringe. If the proper density analyzer attachments and connect-ing tubes are used, as described in 6.4, then t
44、he test specimencan be delivered directly to the analyzers sample tube from themixing container. For automated injections, it is necessary tofirst transfer a portion of sample by appropriate means from aproperly mixed laboratory sample to the autosampler vials, andtake the necessary steps to ensure
45、the integrity of the testspecimen prior to and during the analysis. Sample vials for theautosampler shall be sealed immediately after filling up to80 % 6 5 % and shall be kept closed until the auto samplertransfers the test specimen into the measuring cell. For highlyvolatile samples, cool the sampl
46、e prior to measurement. Followthe manufacturers instructions.NOTE 3Overfilled sample vials can result in cross-contaminationbetween sample vials.9. Preparation of Apparatus9.1 Set up the density analyzer (including the constanttemperature bath and related attachments, if necessary) follow-ing the ma
47、nufacturers instructions. Adjust the bath or internaltemperature control so that the desired test temperature isestablished and maintained in the sample compartment of theanalyzer. Calibrate the instrument at the same temperature atwhich the density or relative density of the sample is to bemeasured
48、 or perform an adjustment (see 3.2.1Discussion) inpreparation of analyzing samples. (WarningPrecise settingand control of the test temperature in the sample tube isextremely important. An error of 0.1 C can result in a changein density of one in the fourth decimal when measuring in unitsof grams per
49、 millilitre.)10. Calibration of Apparatus10.1 As a minimum requirement, calibration of the instru-ment is required when first set up, whenever the test tempera-ture is changed (unless the instrument is capable of performingan adjustment; see 3.2.1 Discussion), or as dictated by qualitycontrol (QC) sample results (see 11.1).10.2 When calibration of the instrument is required, it isnecessary to calculate the values of the constants A and B fromthe periods of oscillation (T) observed when the sample cellcontains air and freshly boiled (WarningHandling wat
