This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles

for the
Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Designation: D4052 − 22

Standard Test Method for

Density, Relative Density, and API Gravity of Liquids by
Digital Density Meter1
This standard is issued under the fixed designation D4052; the number immediately following the designation indicates the year of
original adoption or, in the case of revision, the year of last revision. A number in parentheses indicates the year of last reapproval. A
superscript 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* bubbles in the U-tube can be established with certainty. For the
1.1 This test method covers the determination of the density, determination of density in crude oil samples use Test Method
relative density, and API Gravity of petroleum distillates and D5002.
viscous oils that can be handled in a normal fashion as liquids 1.4 The values stated in SI units are regarded as the
at the temperature of test, utilizing either manual or automated standard, unless stated otherwise. The accepted units of mea-
sample injection equipment. Its application is restricted to sure for density are grams per millilitre (g/mL) or kilograms
liquids with total vapor pressures (see Test Method D5191) per cubic metre (kg/m3).
typically below 100 kPa and viscosities (see Test Method D445 1.5 This standard does not purport to address all of the
or D7042) typically below about 15 000 mm2/s at the tempera- safety concerns, if any, associated with its use. It is the
ture of test. The total vapor pressure limitation however can be responsibility of the user of this standard to establish appro-
extended to >100 kPa provided that it is first ascertained that priate safety, health, and environmental practices and deter-
no bubbles form in the U-tube, which can affect the density mine the applicability of regulatory limitations prior to use.
determination. Some examples of products that may be tested For specific warning statements, see 3.2.1, Section 7, 9.1, 10.2,
by this procedure include: gasoline and gasoline-oxygenate and Appendix X1.
blends, diesel, jet, basestocks, waxes, and lubricating oils. 1.6 This international standard was developed in accor-
1.1.1 Waxes and highly viscous samples were not included dance with internationally recognized principles on standard-
in the 1999 interlaboratory study (ILS) sample set that was ization established in the Decision on Principles for the
used to determine the current precision statements of the Development of International Standards, Guides and Recom-
method, since all samples evaluated at the time were analyzed mendations issued by the World Trade Organization Technical
at a test temperature of 15 °C. Wax and highly viscous samples Barriers to Trade (TBT) Committee.
require a temperature cell operated at elevated temperatures
necessary to ensure a liquid test specimen is introduced for 2. Referenced Documents
analysis. Consult instrument manufacturer instructions for 2.1 ASTM Standards:2
appropriate guidance and precautions when attempting to D287 Test Method for API Gravity of Crude Petroleum and
analyze wax or highly viscous samples. Refer to the Precision Petroleum Products (Hydrometer Method)
and Bias section of the method and Note 9 for more detailed D445 Test Method for Kinematic Viscosity of Transparent
information about the 1999 ILS that was conducted. and Opaque Liquids (and Calculation of Dynamic Viscos-
1.2 In cases of dispute, the referee method is the one where ity)
samples are introduced manually as in 6.2 or 6.3, as appropri- D1193 Specification for Reagent Water
ate for sample type. D1250 Guide for the Use of the Joint API and ASTM
Adjunct for Temperature and Pressure Volume Correction
1.3 When testing opaque samples, and when not using Factors for Generalized Crude Oils, Refined Products, and
equipment that is capable of automatic bubble detection, Lubricating Oils: API MPMS Chapter 11.1
proper procedure shall be established so that the absence of air D1298 Test Method for Density, Relative Density, or API
Gravity of Crude Petroleum and Liquid Petroleum Prod-
ucts by Hydrometer Method
1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products, Liquid Fuels, and Lubricants and is the direct responsibility of
2
Subcommittee D02.04.0D on Physical and Chemical Methods. For referenced ASTM standards, visit the ASTM website, www.astm.org, or
Current edition approved May 1, 2022. Published May 2022. Originally contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
approved in 1981. Last previous edition approved in 2018 as D4052 – 18a. DOI: Standards volume information, refer to the standard’s Document Summary page on
10.1520/D4052-22. the ASTM website.

*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

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 D4052 − 22
D4057 Practice for Manual Sampling of Petroleum and 3.2.4 sample aliquot, n—the fraction of the original labora-
Petroleum Products tory sample dedicated for this test.
D4175 Terminology Relating to Petroleum Products, Liquid
3.2.4.1 Discussion—The sample aliquot is typically residing
Fuels, and Lubricants
in syringes, sample vials, beakers, or containers for the purpose
D4177 Practice for Automatic Sampling of Petroleum and
of transferring a representative test specimen into the appara-
Petroleum Products
tus’ U-tube.
D4377 Test Method for Water in Crude Oils by Potentiomet-
ric Karl Fischer Titration (Withdrawn 2020)3 3.2.5 test specimen, n—the volume of the sample aliquot
D5002 Test Method for Density, Relative Density, and API residing in the U-tube during the measurement cycle.
Gravity of Crude Oils by Digital Density Analyzer 3.2.5.1 Discussion—Sample material residing in filling
D5191 Test Method for Vapor Pressure of Petroleum Prod- nozzles, tubing and valve manifolds is not considered “Test
ucts and Liquid Fuels (Mini Method) Specimen.” A test specimen can be measured only once.
D7042 Test Method for Dynamic Viscosity and Density of
Liquids by Stabinger Viscometer (and the Calculation of 4. Summary of Test Method
Kinematic Viscosity)
4.1 A volume of approximately 1 mL to 2 mL of liquid
sample is introduced into an oscillating U-tube and the change
3. Terminology
in oscillating frequency caused by the change in the mass of the
3.1 Definitions: U-tube is used in conjunction with calibration data to deter-
3.1.1 For definitions of terms used in this test method, refer mine the density, relative density, or API Gravity of the sample.
to Terminology D4175. Both manual and automated injection techniques are described.
3.1.2 density, n—mass per unit volume.
3.1.2.1 Discussion—The SI unit of density is kg/m3; the unit 5. Significance and Use
of measure g/cm3 is commonly used in industry. 5.1 Density is a fundamental physical property that can be
3.1.3 relative density, n—the ratio of the density of a used in conjunction with other properties to characterize both
material at a stated temperature to the density of water at a the light and heavy fractions of petroleum and petroleum
stated temperature. products.
3.1.3.1 Discussion—Relative density is also commonly 5.2 Determination of the density or relative density of
known as specific gravity. Commonly used stated temperatures petroleum and its products is necessary for the conversion of
are 20 °C ⁄20 °C, 15 °C ⁄15 °C, 20 °C ⁄4 °C and 60 °F ⁄60 °F. measured volumes to volumes at the standard temperature of
“Relative density” was historically known as the deprecated 15 °C.
term “specific gravity.”
3.2 Definitions of Terms Specific to This Standard: 6. Apparatus
3.2.1 adjustment, v—the operation of bringing the instru- 6.1 Digital Density Analyzer—A digital analyzer consisting
ment to a state of performance suitable for its use, by setting or of a U-shaped, oscillating tube, U-tube, and a system for
adjusting the density meter constants. electronic excitation, frequency counting, and display. The
3.2.1.1 Discussion—On some digital density analyzer analyzer shall accommodate the accurate measurement of the
instruments, an adjustment may be made rather than calibrating sample temperature during measurement or shall control and
the instrument. The adjustment procedure uses air and freshly keep the sample temperature constant to 60.05 °C. The instru-
boiled reagent water (Warning—Handling water at boiling or ment shall be capable of meeting the precision requirements
near boiling temperature can present a safety hazard. Wear described in this test method.
appropriate personal protective equipment.) as standards to
establish the linearity of measurements over a range of 6.2 Syringes, for use primarily in manual injections, at least
operating temperatures. 2 mL in volume with a tip or an adapter tip that will fit the
opening of the U-tube.
3.2.2 API gravity, n—a special function of relative density
60 °F ⁄60 °F, represented by: 6.3 Flow-Through or Pressure Adapter, for use as an alter-
native means of introducing the sample into the density
141.5 analyzer either by a pump, by pressure, or by vacuum.
°API= 2 131.5 (1)
relative density NOTE 1—It is highly recommended that a vacuum not be applied to
samples prone to light-end loss, as it can easily lead to the formation of
3.2.2.1 Discussion—No statement of reference temperature bubbles in the U-tube. It is recommended to fabricate a special cap or
is required since 60 °F is included in the definition. stopper for sample containers so that air, such as from a squeeze pump, is
3.2.3 calibration, v—set of operations that establishes the used to displace a test specimen to the U-tube measuring cell by the
relationship between the reference density of standards and the flow-through method.
corresponding density reading of the instrument. 6.4 Autosampler, required for use in automated injection
analyses. The autosampler shall be designed to ensure the
integrity of the test specimen prior to and during the analysis
3
The last approved version of this historical standard is referenced on and be equipped to transfer a representative portion of sample
www.astm.org. aliquot to the digital density analyzer.

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 D4052 − 22
6.5 Ultrasonic Bath, Unheated, (optional), of suitable di- D4377. Mixing at room temperature in an open container can
mensions to hold container(s) placed inside of bath, for use in result in the loss of volatile material from certain sample types
effectively dissipating and removing air or gas bubbles that (for example, gasoline samples), so mixing in closed, pressur-
may be entrained in viscous sample types prior to analysis. ized containers or at least 10 °C below ambient temperature is
required for such sample types where loss of volatile material
7. Reagents and Materials is a potential concern. For some sample types, such as viscous
7.1 Purity of Reagents—Reagent grade chemicals shall be lube oils that are prone to having entrained air or gas bubbles
used in all tests. Unless otherwise indicated, it is intended that present in the sample, the use of an ultrasonic bath (see 6.5)
all reagents shall conform to the specifications of the Commit- without the heater turned on (if so equipped), has been found
tee on Analytical Reagents of the American Chemical Society, effective in dissipating bubbles typically within 10 min.
where such specifications are available.4 Other grades may be
NOTE 2—When mixing samples with volatile components, consider the
used, provided it is first ascertained that the reagent is of sample properties in relation to both ambient temperature and pressure.
sufficiently high purity to permit its use without lessening the
accuracy of the determination. 8.3.2 For manual injections, draw the test specimen from a
properly mixed laboratory sample using an appropriate sy-
7.2 Purity of Water—Unless otherwise indicated, references ringe. If the proper density analyzer attachments and connect-
to water shall be understood to mean reagent water as defined ing tubes are used, as described in 6.3, then the test specimen
by Type II of Specification D1193 or higher. can be delivered directly to the analyzer’s U-tube from the
7.3 Water, reagent water, freshly boiled to remove dissolved mixing container. For automated injections, it is necessary to
gasses, for use as primary calibration standard. (Warning— first transfer a portion of sample by appropriate means from a
Handling water at boiling or near boiling temperature can properly mixed laboratory sample to the autosampler vials, and
present a safety hazard. Wear appropriate personal protective take the necessary steps to ensure the integrity of the test
equipment.) specimen prior to and during the analysis. Sample vials for the
7.4 Cleaning Solvent, such as petroleum naphtha5 or solvent autosampler shall be sealed immediately after filling up to
known to be miscible with the sample material without causing 80 % 6 5 % and shall be kept closed until the auto sampler
corrosion of the sample cell. Consult manufacturer’s informa- transfers the test specimen into the measuring cell. For highly
tion for details. (Warning—Petroleum naphtha is extremely volatile samples, cool the sample prior to measurement. Follow
flammable.) the manufacturer’s instructions.
7.5 Acetone, or other highly volatile solvent for flushing and NOTE 3—Overfilled sample vials can result in cross-contamination
drying the U-tube. (Warning—Extremely flammable.) between sample vials.

7.6 Dry Air, for drying the U-tube. 9. Preparation of Apparatus

8. Sampling, Test Specimens, and Test Units 9.1 Set up the density analyzer following the manufacturer’s
8.1 Sampling is defined as all the steps required to obtain an instructions. Set the internal temperature control so that the
aliquot of the contents of any pipe, tank, or other system, and desired test temperature is established and maintained in the
to place the sample into the laboratory test container. The U-tube of the analyzer. Verify the instrument’s calibration at
laboratory test container and sample volume shall be of the same temperature at which the density or relative density of
sufficient capacity to mix the sample and obtain a homoge- the sample is to be measured or perform an adjustment (see
neous sample for analysis. 3.2.1–Discussion) in preparation of analyzing samples.
(Warning—Precise setting and control of the test temperature
8.2 Laboratory Sample—Use only representative samples in the U-tube is extremely important. An error of 0.1 °C can
obtained as specified in Practices D4057 or D4177 for this test result in a change in density of one in the fourth decimal when
method. measuring in units of grams per millilitre.)
8.3 Test Specimen—A portion or volume of sample aliquot
obtained from the laboratory sample and delivered to the 10. Verification and Adjustment
density analyzer U-tube. The test specimen is obtained as
follows: 10.1 As a minimum requirement, calibration verification of
8.3.1 Mix the sample if required to homogenize, taking care the instrument is required when first set up and whenever the
to avoid the introduction of air bubbles. The mixing may be test temperature is changed. Whenever the apparatus fails a
accomplished as described in Practice D4177 or Test Method calibration verification without discernible cause, the apparatus
must be adjusted. See 3.2.1.

4
10.2 The adjustment routine for digital density meters
ACS Reagent Chemicals, Specifications and Procedures for Reagents and
Standard-Grade Reference Materials, American Chemical Society, Washington, involves using a minimum of two reference media. Typically,
DC. For suggestions on the testing of reagents not listed by the American Chemical this will be air and freshly boiled reagent water under atmo-
Society, see Analar Standards for Laboratory Chemicals, BDH Ltd., Poole, Dorset, spheric conditions. (Warning—Handling water at boiling or
U.K., and the United States Pharmacopeia and National Formulary, U.S. Pharma-
near boiling temperature can present a safety hazard. Wear
copeial Convention, Inc. (USPC), Rockville, MD.
5
Suitable solvent naphthas are marketed under various designations such as appropriate personal protective equipment.) Other materials
“Petroleum Ether,” “Ligroine,” or “Precipitation Naphtha.” such as n-nonane, n-tridecane, cyclohexane, and n-hexadecane

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 D4052 − 22
(for high temperature applications) can also be used as appro- 11. Quality Control Checks
priate adjustment materials, provided the reference materials 11.1 Confirm the instrument is in statistical control at least
have density values that are certified and traceable to national once a week when it is in use, by analyzing a quality control
standards. (QC) sample that is representative of samples typically ana-
10.3 Follow the manufacturer’s instructions for the proper lyzed. Analysis of a single QC sample can be sufficient.
adjustment of the apparatus. If the apparatus is adjusted using Analysis of QC sample results can be carried out using control
air and reagent water, observe the proper entries of air and chart techniques.6 If the QC sample result determined causes
water density values. the laboratory to be in an out-of-control situation, such as
10.3.1 The density of air varies with pressure and relative exceeding the laboratory’s control limits, instrument adjust-
humidity (see Table 1). Therefore, it is important that the ment is required. An ample supply of QC sample material
dewpoint of ambient air is below the adjustment temperature of should be available for the intended period of use, and must be
the instrument as to avoid condensation of water in the U-tube. homogeneous and stable under the anticipated storage condi-
This can be achieved by flushing ambient air through a tions. Prior to monitoring the measurement process, the user of
desiccant container and into the U-tube. the method needs to determine the average and control limits of
10.3.2 The density of air varies with ambient pressure as a the QC sample. The QC sample precision should be checked
consequence of site elevation and atmospheric changes in against the method precision to ensure data quality.
pressure. The air density can be calculated using this formula: 11.2 Although not mandatory, it is recommended that peri-
ρ air 5 0.001293@ 273.15 ⁄ T #@ P/101.325# g/mL (2) odic analyses of certified density standards (that is, traceable to
national standards) that are separate from those that may be
where:
used in adjusting the instrument, be used to confirm testing
ρair = density of air, accuracy.
T = temperature, K, and
P = site atmospheric pressure at the time of adjustment, 12. Procedure
kPa.
NOTE 4—P should preferably be determined by direct measurement of 12.1 Manual Injection:
the barometric pressure at the site of calibration. If direct measurement is 12.1.1 Introduce a volume of about 1 mL to 2 mL, of sample
not available, and common sources providing weather data are consulted, into the clean, dry U-tube of the instrument using a suitable
the pressure reported is typically corrected to Sea Level, PSL. Therefore, syringe or alternative, as described in 6.3.
such pressure data must be corrected back to site pressure, P. For
correction of PSL to P: 12.1.2 The sample can also be introduced by siphoning.
Plug the external TFE-fluorocarbon capillary tube into the
P=P SL 2 @ Site Elevation ~meters!/82.3# (3) entry port of the U-tube. Immerse the other end of the capillary
NOTE 5—In the International Standard Atmosphere, ISA, the pressure
drops 1 kPa per 82.3 m of elevation.
in the sample and apply suction to the other port using a
syringe or vacuum line until the U-tube is properly filled (see
10.3.3 The water density values are given in Table 1. Water Note 1).
density values are considered constant with respect to pressure 12.1.3 Ensure that the U-tube is properly filled and that no
in the range of normally occurring atmospheric pressure. gas bubbles are present. The sample must be homogeneous and
free of even the smallest gas bubbles. Check the integrity of the
TABLE 1 Density of WaterA filled sample by using optical or physical methods to verify
NOTE 1—Several metrological entities have issued water density tables absence of gas bubbles. If gas bubbles are detected, empty and
and alternative water density data is referenced in publications external to refill the U-tube, and recheck for gas bubbles.
ASTM and this test method. Using water density data from an alternative
recognized source does not pose a compliance issue with this test method NOTE 6—If the sample is too dark in color to determine the absence of
as the variation in the data typically is limited to the sixth decimal place. bubbles with certainty, the density cannot be measured within the stated
Temperature, Density, g/mL Temperature, Density, Temperature, Density,
precision limits of Section 15.
°C °C g/mL °C g/mL 12.1.4 For most instrument models, it is recommended to
0.01 0.999844 21.0 0.997996 40.0 0.992216 turn the illumination light off with minimal delay after sample
3.0 0.999967 22.0 0.997773 45.0 0.990213
4.0 0.999975 23.0 0.997541 50.0 0.988035 introduction and checking for bubbles because the heat gener-
5.0 0.999967 24.0 0.997299 55.0 0.985693 ated can affect the measurement temperature. For some models
10.0 0.999703 25.0 0.997048 60.0 0.983196 however, the cell light may be left on without affecting results.
15.0 0.999103 26.0 0.996786 65.0 0.980551
15.56 0.999016 27.0 0.996516 70.0 0.977765 Refer to the manufacturer’s recommendations concerning
16.0 0.998946 28.0 0.996236 75.0 0.974843 whether to leave the illumination light off or on.
17.0 0.998778 29.0 0.995947 80.0 0.971790 12.1.5 After the instrument displays a steady reading to four
18.0 0.998599 30.0 0.995650 85.0 0.968611
19.0 0.998408 35.0 0.994033 90.0 0.965310 significant figures for density, relative density, or API Gravity,
20.0 0.998207 37.78 0.993046 99.9 0.958421 and five for T-values, indicating that temperature equilibrium
A
Densities conforming to the International Temperature Scale 1990 (ITS 90) were has been reached, record the density, relative density, API
extracted from Lemmon, E. W., McLinden, M. O., and Friend, D. G., “Thermo-
physical Properties of Fluid Systems,”NIST Chemistry WebBook, NIST Standard
Reference Database No. 68, Eds. P.J. Linstrom and W.G. Mallard, National
6
Institute of Standards and Technology, Gaithersburg, MD, http://webbook.nist.gov. ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,
(retrieved July 24, 2013). Section 3: Control Charts for Individuals, 6th ed., ASTM International, W.
Conshohocken, PA.

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 D4052 − 22
Gravity or T-values, or both, as appropriate. For instruments tion of closeness of determinations, utilizing optical or physical
that can print out results from the display, the print out can be methods for air bubble detection, or both.
used to meet the recording requirements. 12.2.2.1 This test method does not offer precision and bias
12.1.6 Based on the 1999 ILS7 testing protocols (see Note values for opaque samples and because sample properties vary
9), precision determinations involving a single manual greatly, determinability criteria is not offered, but shall be
injection, as well as taking the average of two manual established by a series of tests determinations on representative
injections, was evaluated. See the Precision and Bias section sample material. Perform a minimum of three consecutive
for more details. If the laboratory performs a single manual determinations of different test specimens from the same
determination, the density, relative density, or API Gravity syringe or sample vial without removing the syringe from the
values recorded in 12.1.5, or a combination thereof, is to be apparatus and without any rinsing or cleaning between deter-
used for reporting purposes. In most cases, a single manual minations. Average the two determinations with the highest
injection determination is sufficient for sample analysis. density or lowest API number and report per 12.2.3.
12.1.6.1 If the laboratory decides to perform a second
12.2.3 Record the density, relative density, or API Gravity
manual injection determination for a given sample, repeat
12.1.1 – 12.1.5. If the two determinations do not differ by more results, or a combination thereof, determined by the analyses as
than 0.0002 g ⁄mL for density or 0.0002 for relative density, appropriate, such as by using the instrument print out of results
average the two determinations, otherwise, discard both deter- to meet the recording requirements.
minations and repeat the analysis using two new test specimens
until the acceptance criteria identified above is satisfied. With 13. Calculation
respect to API Gravity determinations of gasoline or RFG 13.1 Calculating Density Analyzers—The recorded or
samples, if the two determinations do not differ by more than printed value is the final result when a single determination is
0.05° API Gravity units, average the two determinations, conducted (or taking the average of two determinations as the
otherwise, discard both determinations and repeat the analysis final result as identified in Section 12), expressed either as
using two new test specimens until the acceptance criteria is density in g/mL, kg/m3 or as relative density. Note that kg/m3 =
satisfied. With respect to API Gravity determinations of 1000 × g/mL.
distillates, basestocks, and lubricating oils, follow the protocol
in the prior sentence except use 0.03° API Gravity units as the 13.2 If it is necessary to convert a result obtained using the
acceptance criteria. Averaged results meeting the criteria iden- density meter to API Gravity, or a density or relative density at
tified in this section is to be used for reporting purposes. another temperature, Guide D1250 can be used only if the glass
expansion factor has been excluded.
12.2 Automated Injection:
12.2.1 The use of an autosampler (see 6.4) is required when NOTE 8—Some digital density analyzers are equipped to automatically
calculate and report sample results in API gravity units (see Test Method
analyzing samples by automated injection. Follow manufactur- D287 or D1298), based on the density or relative density results, or a
er’s instructions for ensuring the integrity of the test specimen combination thereof, determined by this test method and using the
prior to analysis, as well as transferring a representative test appropriate conversion equation derived from Guide D1250 (which
specimen into the instrument for analysis. excludes the glass expansion factor), for the specific sample type being
12.2.1.1 If the laboratory decides to perform a second analyzed.
automated injection determination for a given distillate,
basestock, or lubricating oil (see Note 9 and the Precision and 14. Report
Bias section), use the same acceptance criteria in 12.1.6.1 for 14.1 In reporting density, state the test temperature and the
allowed differences between each determination for density units (for example: density at 20 °C = 0.8765 g ⁄mL or
(0.0002 g ⁄mL), relative density (0.0002) and API Gravity units 876.5 kg ⁄m3).
(0.03°) as for manually injected samples. Averaged results
meeting the necessary acceptance criteria are to be used for 14.2 In reporting relative density, state both the test tem-
reporting purposes. perature and the reference temperature, but no units (for
example: relative density, 20/20 °C = 0.xxxx).
NOTE 7—Density meters equipped with autosamplers allow for unat-
tended operation, and erroneous results rooted in filling problems may 14.3 Report the final result for density or relative density to
pass unnoticed. Performing duplicate determinations may uncover sample four significant figures and reference this test method.
filling issues regardless of the sample material being tested.
12.2.2 Opaque samples may be tested using either manual 14.4 If reporting sample results in API gravity units (see
injection method described in 12.1 or using an autosampler as Note 8), report the final results to the nearest 0.1° API.
described in 12.2. When testing opaque samples, proper 14.5 In some cases, it may be necessary to report if results
procedure shall be established by which the absence of air were based on a single determination or an average of two
bubbles in the measuring cell can be confirmed with certainty. determinations, as well as if results were determined by manual
Such procedures include multiple determinations and evalua- injection or automated injection to meet specific requirements,
such as data recipients wanting to know such information in
7
order to understand how to interpret results relative to the
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1734. Contact ASTM Customer published method precision values. In such cases, it is permis-
Service at service@astm.org. sible to report this information along with the test results.

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 D4052 − 22
15. Precision and Bias7 for the gasoline and RFG sample types are likely due to the volatile nature
of these materials, even though the ILS participants were provided
15.1 The precision of the method as obtained by statistical instructions for how to properly handle these materials to minimize or
examination of interlaboratory test results at a test temperature prevent sample losses. The subcommittee responsible for the method is
of 15 °C is as follows for the following sample types and planning to conduct a subsequent ILS for gasoline and RFG sample types
ranges: with additional scrutiny paid to sample handling issues as a means to try
and improve the precision statements for these materials.
15.1.1 Repeatability—The difference between successive NOTE 10—Four (4) of the samples analyzed in the ILS indicated in Note
test results obtained by the same operator with the same 9 were ASTM Interlaboratory Crosscheck samples (that is, Gaso-
apparatus under constant operating conditions on identical test line–MG9808 and MG9812, RFG–RFG9807, and RFG9809). The robust
material, would in the long run, in the normal and correct mean of the total vapor pressures reported by Test Method D5191 for
operation of the test method, exceed the following value only these samples ranged from a low of 7.77 psi (MG9808) to a high of
13.40 psi (RFG9809). This corresponds to an approximate total vapor
in one case in twenty: pressure range of 54 kPa to 92 kPa.
15.1.1.1 Density (g/mL) and Relative Density—See Table 2.
15.2 Bias—After suggestions of its existence from
15.1.1.2 API Gravity—See Table 3.
15.1.2 Reproducibility—The difference between two single literature,8 a study has been performed which has confirmed
the presence of a bias between known density values for
and independent results, obtained by different operators work-
reference materials and from values determined according to
ing in different laboratories on identical test material, would in
this test method on the same reference materials. The matrix
the long run, in the normal and correct operation of the test
for this bias study comprised 15 participants, each analyzing
method, exceed the following values only in one case in
four reference oils with certified density values, established by
twenty:
the Netherlands Meet Instituut (NMI), by pyknometry, cover-
15.1.2.1 Density (g/mL) and Relative Density—See Table 4.
15.1.2.2 API Gravity—See Table 5. ing densities in the range of 747 kg ⁄m3 to 927 kg/m3 at 20 °C,
NOTE 9—The ASTM Interlaboratory Study (ILS) conducted in Fall with viscosities between 1 mPa.s and 5000 mPa.s (also at
19997 involved 11 laboratories and 23 samples. The samples included 5 20 °C). This study is documented in ASTM Research Report
motor gasolines, 1 motor gasoline + ethanol, 4 reformulated gasolines RR:D02-1387.9 Method users should, therefore, be aware that
(RFG), 2 lube oils, 1 basestock oil, 4 Jet-A fuels, 1 JP8 fuel, and 5 diesel results obtained by this test method can be biased by as much
fuels. The ILS protocol required laboratories to perform a total of four as 0.6 kg ⁄m3 (0.0006 g ⁄mL).
measurements per sample, which included both manual and automated
NOTE 11—Newer instrumentation exists which purports to correct
injections, with the first two determinations representing the first analysis
density results due to the influence of viscosity. However, the responsible
set and the second two determinations representing the second analysis
ASTM Technical Committee has not yet performed a new interlaboratory
set. This protocol was used to evaluate if a precision effect existed
study to confirm the elimination of the bias described in ASTM Research
between taking the first determination from each analysis set (that is,
Report RR:D02-1387.9
single determination) versus taking the average of the two determinations
from each analysis set, as well as determining if there was a precision
effect between manual and automated injections. The repeatability and
16. Keywords
reproducibility statements determined by the statistician reflect the corre- 16.1 API Gravity; density; digital density analyzer; petro-
sponding precision values associated with testing conditions identified. It leum distillates; petroleum products; relative density
should be noted that the precision statements determined for the gasoline
and RFG sample types in the 1999 ILS were poorer than expected relative
to the precision statements determined for the distillates, basestocks, and 8
Fitzgerald, H. and D., “An Assessment of Laboratory Density Meters,”
lubricating oils as well as relative to the previously published method Petroleum Review, November 1992, pp. 544–549.
version precision statements (which were based on the analysis of just 9
Supporting data have been filed at ASTM International Headquarters and may
three pure compounds (benzene, toluene, and xylene) analyzed by 3 be obtained by requesting Research Report RR:D02-1387. Contact ASTM Customer
laboratories in duplicate). The poorer than expected precision statements Service at service@astm.org.

TABLE 2 Density (g/mL) and Relative Density (Repeatability)

Range Sample Types Testing Condition Repeatability
0.71–0.78 Gasoline and RFG Single Determination 0.00045
(Manual injection)
Average of 2 Determinations 0.00031
(Manual or automated injections)
0.80–0.88 Distillates, Basestocks, and Single Determination 0.00016
Lubricating Oils (Manual or automated injection)
Average of 2 Determinations 0.00011
(Manual or automated injections)

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 D4052 − 22
TABLE 3 API Gravity (Repeatability)
Range Sample Types Testing Condition Repeatability
51–66 Gasoline and RFG Single Determination 0.090
(Manual injection)
Average of 2 Determinations 0.063
(Manual or automated injections)
29–45 Distillates, Basestocks, and Single Determination 0.032
Lubricating Oils (Manual or automated injection)
Average of 2 Determinations 0.022
(Manual or automated injections)

TABLE 4 Density (g/mL) and Relative Density (Reproducibility)

Range Sample Types Testing Condition Reproducibility
0.71–0.78 Gasoline and RFG Single Determination 0.00190–0.0344 (D–0.75)
(Manual injection)
Average of 2 Determinations 0.00195–0.0315 (D–0.75)
(Manual or automated injections)
0.80–0.88 Distillates, Basestocks, and Single Determination 0.00052
Lubricating Oils (Manual or automated injection)
Average of 2 Determinations 0.00050
(Manual or automated injections)
where: D = density or relative density value obtained

TABLE 5 API Gravity (Reproducibility)

Range Sample Types Testing Condition Reproducibility
51–66 Gasoline and RFG Single Determination 0.60 + 0.040 (G–60)
(Manual injection)
Average of 2 Determinations 0.60 + 0.037 (G–60)
(Manual or automated injections)
29–45 Distillates, Basestocks and Single Determination 0.133
Lubricating Oils (Manual or automated injection)
Average of 2 Determinations 0.128
(Manual or automated injections)
where: G = API Gravity value obtained

APPENDIXES

(Nonmandatory Information)

X1. ADJUSTMENT AND CALIBRATION PROCEDURE FOR NON-CALCULATING DENSITY METERS

X1.1 When calibration of the instrument is required, it is purification and drying train. In addition, the inlet and outlet
necessary to calculate the values of the constants A and B from ports for the U-tube must be plugged during measurement of
the periods of oscillation (T) observed when the sample cell the calibration air to prevent ingress of moist air.
contains air and freshly boiled reagent water. (Warning— X1.1.2 Allow the dry air in the U-tube to come to thermal
Handling water at boiling or near boiling temperature can equilibrium with the test temperature and record the T-value
present a safety hazard. Wear appropriate personal protective for air.
equipment.) Other calibrating materials such as n-nonane,
n-tridecane, cyclohexane, and n-hexadecane (for high tempera- X1.1.3 Introduce a small volume, about 1 mL to 2 mL, of
ture applications) can also be used as appropriate, provided the freshly boiled reagent water into the sample tube using a
reference materials have density values that are certified and suitable syringe or alternate, as described in 6.4 and 6.5.
traceable to national standards. (Warning—Handling water at boiling or near boiling tempera-
NOTE X1.1—On certain newer, commercially available instruments, a ture can present a safety hazard. Wear appropriate personal
viscosity correction feature may be available and utilized in density protective equipment.) The test portion must be homogeneous
determinations to minimize potential biases. Refer to information in the and free of even the smallest air or gas bubbles. Allow the
Section 15 for more specifics. display to reach a steady reading and record the T-value for
X1.1.1 While monitoring the oscillator period, T, flush the water.
sample tube with cleaning solvent, followed with an acetone
X1.2 Calculate the density of air at the temperature of test
flush, and dry with dry air. Contaminated or humid air can
using the following equation:
affect the calibration. When these conditions exist in the
laboratory, pass the air used for calibration through a suitable d a 5 0.001293@ 273.15 ⁄ T #@ P/101.325# g/mL (X1.1)

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 D4052 − 22
where: test, repeat the cleaning procedure or adjust the value of
T = temperature, K, and constant B commencing with the last decimal place until the
P = barometric pressure, kPa. correct density is displayed.
X1.2.1 Determine the density of water at the temperature of X1.3.2 If adjustment to constant B was necessary in X1.3.1,
test by reference to Table 1. then continue the recalibration by introducing freshly boiled
(Warning—Handling water at boiling or near boiling tempera-
X1.2.2 Using the observed T-values and the reference
ture can present a safety hazard. Wear appropriate personal
values for water and air, calculate the values of the Constants
protective equipment.) reagent water into the sample tube as
A and B using the following equations:
described in X1.1.3and allow the display to reach a steady
A 5 @ T w2 2 T 2a # ⁄ @ d w 2 d a # (X1.2) reading. If the instrument has been calibrated to display the
2
B 5 T 2 ~ A 3 d a!
a (X1.3) density, adjust the reading to the correct value for water at the
test temperature (Table 1) by changing the value of constant A,
where: commencing with the last decimal place. If the instrument has
Tw = observed period of oscillation for cell containing water, been calibrated to display the relative density, adjust the
µs, reading to the value 1.0000.
Ta = observed period of oscillation for cell containing air, NOTE X1.2—If performing a weekly calibration adjustment, it can be
µs, found that more than one value each for A and B, differing in the fourth
dw = density of water at test temperature, g/mL, and decimal place, will yield the correct density reading for the density of air
da = density of air at test temperature, g/mL. and water. The setting chosen would then be dependent upon whether it
was approached from a higher or lower value. The setting selected by this
X1.2.2.1 Alternatively, use the T and d values for the other method could have the effect of altering the fourth place of the reading
reference liquid if one is used. obtained for a sample.

X1.2.3 If the instrument is equipped to calculate density X1.4 Some analyzer models are designed to display the
from the constants A and B and the observed T-value from the measured period of oscillation only (T-values) and their
sample, then enter the constants in the instrument memory in calibration requires the determination of an instrument constant
accordance with the manufacturer’s instructions. Alternatively, K, which must be used to calculate the density or relative
if the instrument is equipped to do so, let it make the density from the observed data.
appropriate corrections in the calibration or adjustment con- X1.4.1 Flush and dry the sample tube as described in X1.1
stants as part of the built in calibration or adjustment proce- and allow the display to reach a steady reading. Record the
dure. T-value for air.
X1.2.4 Check the calibration and adjust if needed by per- X1.4.2 Introduce freshly boiled reagent water into the
forming the routine calibration check described in X1.3. sample tube as described in X1.1.3, allow the display to reach
X1.2.5 To calibrate the instrument to display relative a steady reading and record the T-value for water. (Warning—
density, that is, the density of the sample at a given temperature Handling water at boiling or near boiling temperature can
referred to the density of water at the same temperature, follow present a safety hazard. Wear appropriate personal protective
X1.1 to X1.2.3, but substitute 1.000 for dw in performing the equipment.)
calculations described in X1.2.2. X1.4.3 Using the observed T-values and the reference
values for water and air (X1.2 and X1.2.1), calculate the
X1.3 On some density meter analyzers, weekly calibration instrument constant K using the following equations:
adjustments to constants A and B can be made if required, For density:
without repeating the calculation procedure. The need for a K 1 5 @ d w 2 d a # ⁄ @ T w2 2 T 2a # (X1.4)
change in calibration is generally attributable to deposits in the For relative density:
sample tube that are not removed by the routine flushing
K 2 5 @ 1.000 2 d a # ⁄ @ T w2 2 T 2a # (X1.5)
procedure. Although this condition can be compensated for by
adjusting A and B, it is good practice to clean the tube with a where:
strong oxidizing acid (Warning—Causes severe burns) or Tw = observed period of oscillation for cell containing water,
surfactant cleaning fluids whenever a major adjustment is µs,
required. Ta = observed period of oscillation for cell containing air,
X1.3.1 Flush and dry the sample tube as described in X1.1 µs,
and allow the display to reach a steady reading. If the display dw = density of water at test temperature, g/mL, and
does not exhibit the correct density for air at the temperature of da = density of air at test temperature, g/mL.

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 D4052 − 22

X2. CALCULATIONS

X2.1 Noncalculating Density Analyzers—Using the ob- For relative density:

served T-value for the sample and the T-value for water and relative density, t⁄t 5 11K 2 ~ T 2s 2 T w2 ! (X2.2)
appropriate instrument constants determined in X1.4.3, calcu-
where:
late the density or relative density using Eq X1.4 and Eq X1.5.
Carry out all calculations to six significant figures and round Tw = observed period of oscillation for cell containing water,
the final results to four.
Ts = observed period of oscillation for cell containing air,
For density:
dw = density of water at test temperature,
density, g/mL~ kg/m3 ! at t 5 d w 1K 1 ~ T 2s 2 T w2 ! (X2.1) K1 = instrument constant for density,
K2 = instrument constant for relative density, and
T = temperature of test, °C.

SUMMARY OF CHANGES

Subcommittee D02.04 has identified the location of selected changes to this standard since the last issue
(D4052 – 18a) that may impact the use of this standard. (Approved May 1, 2022.)

(1) Added Terminology D4175 to Sections 2 and 3. (3) Revised subsections 7.4 and 7.5.
(2) Revised definition for density in subsection 3.1.2.

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