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This international standard was developed in accordance with intemationally recognized principles on standardiz,ation

established in the Decision on principles for the


Development of International Standards, Guides and Recommendations issuedly the'worki trade
organizaiion recrr"ical Barriers to Tlade (TBT) Conrmittee.

Desisnation: D4os2 - i6
4P
,ilfEn//t ftoNAL

Standard Test Method for


Density, Relative Density, and Apl Gravity of Liquids by
Digital Density Meterl
This standard is issued under the fixed designation D4052; the nunrber immediately following the designarion indicates the yea.
11f
original adoption or, in the case of revision, the year of last revision. A nunrber in parentheses indicates the year of last reapproval.
A
superscript epsilon (e) indicates an editorial change since the last revision or reapproval.

Tltis standard has been opproved for use by agencies of the n.s. Deparfinent of D,fense,

l. Scope* bubbles in the sarnple cell can be established with certainty.


l.lThis test method covers the determination of the density, For the determination of density in crude oil samples use Test
relative density, and API Gravity of petroleum distillates and Method l)5002.
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 siated otherwise. The accepted units of mea-
sample injection equipment. Its application is restricted to sure for density are gr-ams per millilitre (g/ml) or kilograms
liquids with total vapor pressures (see Test Method DslSl) 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 D7{}42) typically below about 15 000 mrn2/s at the tempera-
safetlt 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 and health practices and determine the applica-
no bubbles form in the U-shaped, oscillating tube, which can
bilitlt of regulatory limitations prior to use. For specific
affect the density determination. Some examples of products
warning statements, see 7.4, 7.5, and 10.3.
that may be tested by this procedure include: gasoline and
gasoline-oxygenate blends. diesel, jet, basestocks, waxes, and 2. Referenced Documents
lubricating oils.
1.1.1 Waxes and highly viscous samples were not included 2.1 ASTM Standards:z
D2B7 Test Method for API Gravity of Crude Petroleurn and
in the 1999 interlaboratory study (ILS) sample set that was
used to determine the current precision statements of the Petroleum Producrs (Hydrometer Method)
D445 Test h,lethod lbr Kinematic Viscosity of Transpar-ent.
method, since all samples evaluated at the time were analyzed
and Opaque l,iquids (and Calculation of l)ynamic Viscos-
at a test temperature of 15 "C. Wax and highly viscous samples
require a temperature cell operated at elevated temperatures itY)
necessary to ensure a liquid test specimen is introduced for
Dl li)3 Specification for Reagent \&'ater
D I25{i Guide for Use of the Petmleum Measurement Tables
analysis. Consult instrument manufacturer instructions for
appropriate guidance and precautions when attempting to D1298 Test N4ethod for Density, Relative Density, or ApI
analyze wax or highly viscous samples. Refer to the precision
Gravity of Cnrde Petroleum and Liqurid Petroleurn prod-
and Bias section of the method and Note I for more detailed ucts by Hydrometer N{ethod
D4057 Practice for Manual Sarnpling of Petroleum and
information about the 1999 ILS that was conducted.
Petroleum Products
1.2 In cases of dispute, the referee method is the one where D4177 Practice for Automatic Sampling of Petroleum and
samples are introduced manually as in 6.3 or 6.4, as appropri- Petroleum P:oducts
ate for sample type. D4377 Test Method l'or Water in CrLrde Oils by Potentiomet-
1.3 When testing opaque samples, and when not using ric Karl Fischer Titration
equipment that is capable of automatic bubble detection, D5002 Test Method for Density and Relarive Density of
proper procedure shall be established so that the absence of air Crude Oils by Digital Densit3, Analyzer
DS l9l Test Method lbr Vapor Pressure of Petroleum procl-
ucts (l\.{ini Method)
rThis test method is under the jurisdiction
of ASTM Comrnittee D02 on
Petroleum Prcduots, Liquid Fuels, and Luhricrmts and is the direct responsibility of
Subcommittee D02.04.0D on Physical and Chemical Metho<ts. 2
For referenced ASTM standards, visit the ASTIr{ wehsite, www.asrm.org, or
Current edition approved Dec. l, 2016. published January 2017. Originally contact AS'I'M Customer Service at service@rastm.org. For Arurual Book of ASTM
approved in 1981. Lasr prcvious edition approved in 2015 as D4052 _ 15. DOI: Stand.ards volume information, refer [o the standard's Document Sumnrary page on
10.1520/D4052-16. the ASTM u,ebsitc.

*A Summary of Changes section appears at the end of


this standard
Copyright OASTM lnternational, 1OO Barr Harbor Drive, PO Box C7OO, Wesl Conshohocken, pA .19428-2959.
United States
($p o+os2-lG
D7042 Test Method fbr Dynamic \riscnsity and Dernsity of constant to -F0.05 oC in the desired range. Temperature control
Liquids by Stahinger Viscometer (and the Calculation of can be maintained as part of the density analyzer instrument
Kinernatic Viscosity) package.

3. Terminology 6.3 Syringes, for use primarily in manual injections, at least


2 mL in volume with a rip or an adapter tip that will fit the
3.1 De.finitious:
opening of the oscillating [ube.
3.1.7 density, n-mass per unit volume at a specified tem-
perature. 6.4 Flow-Through or Pressure Adapte4 for use as an alter-
native means of introducing the sample into the density
3.1 .2 relative density, n-the ratio of the density of a
analyzer either by a pump, by pressure, or by vacuum.
material at a stated temperature to the density of water at
stated temperature.
a Nnrn l-It is highly recommended that a vacuum not be applietl to
samples prone to light-end loss, as it can easily lead to the formation of
3.2 Definitions of Tbnns SpeciJic to This Standard: bubbles. It is recommended to fabricate a special cap or stopper for sample
containers so that air, such as from a squeeze pump, is used to displace a
3.2.1 adjustment, v-the operation of bringing the instru- test specimen to the Utube measuring cell by the flow{hrough method.
ment to a state of performance suitable for its use, by setting or
adjusting the density meter constants. 6.5 Autosample4 required for use in automated injection
3.2.1 .1 Discussion-On some digital density analyzer analyses. The autosampler shall be designed to ensure the
instruments, an adjustment may be made rather than calibrating integrity of the test specimen prior to and during the analysis
the instrument. The adjustment procedure uses air and freshly and be equipped to transfer a representative portion of test
boiled reagent water (Warning-Handling water at boiling or specimen to the digital density analyzer.
near boiling temperature can present a safety hazard. Wear 6.6 Tbmperature Sensing Device GSD), capable of monitor-
appropriate personal protective equipment.) as standards to ing the observed test temperature to within an accuracy of
establish the linearity of measurements over a range of +- 0.05 oC. If a liquid-in-glass thermometer is used
as the TSD,
operating tetnperatures. it shall be calibrated and graduated to 0.1 .C, and have a holder
3.2.2 calibration, v-set of operations that establishes the that can be attached to the instrument for setting and observing
relationship between the reference density of standards and the the test temperature. In calibrating the thermometer, the ice
corresponding density reading of the instrument. point and bore connections should be estimated to the nearest
0.05'C. For non-mercurial thermometers, the TSD device
4. Summary of Test Method shall be calibrated at least annually against a certified and
4. I
A small volume, approximately I mL to 2 mt , of liquid traceable standard.
sample is introduced into an oscillating sample tube and the 6.J Ultrasonic Bath, Unheated, (optional), of suitable di-
change in oscillating frequency caused by the change in the mensions to hold container(s) placed inside of bath, for use in
mass of the tube is used in conjunction with calibration data to efectively dissipating and removing air or gas bubbles that
determine the density, relative density, or ApI Gravity of the may be entrained in viscous sample types prior to analysis.
sample. Both manual and automated injection techniques are
described. 7. Reagents and Materials
7.1 Purity of Reagents-Reagent grade chemicals shall be
5. Significance and Use used in all tests. Unless otherwise indicated, it is intended that
5.1 Density is a fundamental physical property that can be all reagents shall conform to the specifications of the Commit-
used in conjunction with other properties to characterize both tee on Analytical Reagents of the American Chemical Society,
the light and heavy fractions of petroleum and petroleum where such specifications are available.3 Other grades may be
products. used, provided it is first ascertained that the reagent is of
sufficiently high purity to permit its use without lessening the
5.2 Determination of the density or relative density of
petroleum and its products is necessary for the conversion of accuracy of the determination.
measured volumes to volumes at the standard temperature of 7.2 Puritlt of Water-Unless otherwise indicated, references
l5 "c. to water shall be understood to mean reagent water as defined
by Type II of Specification l)l 193 or higher.
6. Apparatus
7.3 Wate4 reagent water, freshly boiled to remove dissolved
6.1 Digilal Analyzer-A digital analyzer consisting
Densit,v gasses,for use as primary calibration standard. (Warning-
of a U-shaped, oscillating sample tube and a system for Handling water at boiling or near boiling temperature can
electronic excitation, frequency counting, and display. The present a saf'ety hazard. Wear appropriate personal pratective
analyzer shall accommodate the accurate measurement of the equipment.)
sample temperature during measurement or shall control the
sample temperature as described in 6.2. The instrumenr shall be
:t
Reagent Chemit:als, Americnn Cltemical Society Specificatrcns, American
capable of meeting the precision requirements described in this
Chemical Society, Washington. DC. For suggestions on the festing of reagents not
test method. listed by the Ametican Cliemical Society, see Analar Stcndatds for l.nborator.y
Chenticals, BDH l,td., Poole, Dorset, U.K., and the llnied Strues pharnmcopeia
6.2 C i rc ulati n g C o nstant -Tempe rature B ath, (optiotal), ca- and National Formulary, U.S. Pharmaceutical Conventidh, Inc: (USpC), Rockville,
pable of maintaining the temperature of the circulating liquid tuD.
,($fp oaos2 - IG
7.4 Cleaning Solvent, such as petroleum naphthaa 9. Preparation of Apparatus
(Warning-Petroleum naphtha is extremely flammable), or
other materials that are capable of flushing and removing 9.1 Set up the density analyzer (including the constant
samples entirely from the sample tube. temperature bath and related attachments, if necessary) follow- "

ing the manufacturer's instructions. Adjust the bath or intemal


7.5 Acetone, for flushing and drying the sample tube. tempemture control so that the desired test temperature is
(Warning-Extremely fl ammable.) established and maintained in the sample compartment of the
7.6 Dry Air, for drying the oscillator tube. analyzer. Calibrate the instrument at the same temperature at
which the density or relative density of the sample is to be
8. Sampling, Test Specimens, and Test Units measured or perform an adjustment (see 3.2.|-Discussion) in
8. I Sampling is defined as all the steps requirecl to obtain an preparation of analyzing samples. (Warning-precise setting
aliquot of the contents of any pipe, tank, or other system, and and control of the test temperature in the sample tube is
to place the sample into the laboratory test container. The extremely imporlant. An error of 0.1 .C can result in a change
laboratory test container and sample volume shall be of in density of one in the fourth decimal when measuring in units
sufficient capacity to mix the sample and obtain a homoge- of grams per millilitre.)
neous sample for analysis.
10. Calibration of Apparatus
8.2 Laboratory Sarnple-lJse only representative sarnples
obtained as specified in Practices D;t*s? or D4 I7T for this test 10.1 As a minimum requirement, calibration of the instru-
method. ment is required when first set up, whenever the test tempera-
ture is changed (unless the instrument is capable of performing
8.3 Test Specimen-Aporlion or volume of sample obtained
an adjustment; see 3"2. 1 Discussion), or as dictated by quality
from the laboratory sample and delivered to the density control (QC) sample results (see I l.l).
analyzer sample tube. The test specimen is obtained as follows:
8.3.1 Mix the sample if required to homogenize, taking care 10.2 When calibration of the instrument is required, it is
to avoid the introduction of air bubbles. The mixing may be necessffy to calculate the values of the constants A and B from
accomplished as described in practice D417? or Test Method the periods of oscillation (7) observed when the sample cell
l)1317. Mixing at room temperature in an open container can contains air and freshly boiled (Warning-Handling water at
result in the loss of volatile material fiom certain sample types boiling or near boiling temperature can present a safety hazard.
(for example, gasoline samples), so mixing in closed, preisur- Wear appropriate personal protective equipment.) reagent wa-
ized containers or at least l0 "C below ambient temperature is ter. Other calibrating materials such as n-nonane, n-tridecane,
required for such sample types where loss of volatile material cyclohexane, and n-hexadecane (for high temperature applica-
is a potential concern. For some sample types, such as viscous tions) can also be used as appropriate, provided the reference
lube oils that are prone to having entrained air or gas bubbles materials have density values that are certified and traceable to
present in the sample, the use of an ultrasonic bath (see {:.7) national standards.
without the heater turned on (if so equipped), has been found
Norn 4-On certain newer, cornmercially available instruments, a
effective in dissipating bubbles typically within l0 min. viscosity corection feature may be available and utilized in density
Nore 2-When mixing samples with volatile components, consider the determinations to minimize potential biases. Refer to inforrnation in the
sample properties in relation to both ambient temperature and pressure. Section l.l for more specifics.

8.3.2 For manual injections, draw the test specimen from a 10.2. I While monitoring the oscillator period, T, flush the
properly mixed laboratory sample using an appropriate sy- sample tube with cleaning solvent, followed with an acetone
ringe. If the proper density analyzer attachments and conneit- flush and dry with dry air. Contaminated or humid air can affect
ing tubes are used, as described in 6.4, then the test specimen the calibration. When these conditions exist in the laboratory,
can be delivered directly to the analyzer's sample tube from the pass the air used for calibration through a suitable purification
mixing container. For automated injections, it is necessary to and drying train. In addition, the inlet and outlet por-ts for the
first transfer a portion of sample by appropriate means from a U-tube must be plugged during measurement of the calibration
properly mixed laboratory sample to the autosampler vials, and air to prevent ingress of moist air.
take the necessary steps to ensure the integrity of the test 10.2.2 Allow the dry air in the U-tube to come to thermal
specimen prior to and during the analysis. Sample vials for the equilibrium with the test temperature and record the 7-value
autosampler shall be sealed immediately after filling up to for air.
8O Vo + 5 7o and shall be kept closed until the auto sampler 10.2.3 Introduce a smali volume, about I ruL to 2 mL, of
transfers the test specimen into the measuring cell. For highly fi:eshly boiled (Warning-Handling warer at boiling or near
volatile samples, cool the sample prior to measurement. Follow boiling temperature can present a safety hazard. Wear appro-
the manufacturer's instructions. priate personal protective equipment.) reagent water into the
sample tube using a suitable syringe or altemate, as described
Nors 3-Overfilled sample vials can result il cross-contamination
in 6.4 and 6.5. The test portion must be homogeneous and free
between sample vials.
of even the smallest air or gas bubbles. Allow the display to
reach a steady reading and record the l-value for water.
o
Suitable solvent naphthas are marketed under various designatiots such as 10.2.4 Calculate the density of air at the te'urpeiaturc of test
'Pctxrleunr Erher," "Ligroine." or "Precipitation Naphtha.,'
using the lollowing equation:
{ffi o+os2-16
TABLE 1 Density of WaterA l{}.2.1 li}.2.7, but subsritute 1.000 fbr d,, in perfomring the
N<rrp l-Several metrological entities have issued water density tables calculations described in I{}.2.6.
and alternative water density data is referenced in publications extemal to
ASTM and this test method. Using water density data from an alternative 10.3 On some density meter analyzers, weekly calibratibn
recognized source does not pose a conrpliance issue with this test method adjustments to constants A and B can be made if required,
as the variation in the data typically is limited ro the sixth decimal place. without repeating the calculation procedure. The need for a
Temperature, Density, Temperature, Density, Temperature, Density, change in calibration is generally attributable to deposits in the
'C g/ml 'C g/rnl "C g/ml sample tube that are not removed by the routine flushing
0.01 0.999844 21.O 0.997996 40.0 0.9922 6
1
procedure. Although this condition can be compensated for by
3.0 0.999967 22.O 0.997773 45.0 0.990213
4.O 0.99997s 23.0 0.997541 50.0 0.988035
adjtrsting A and B, it is good practice to clean the tube with a
5.0 0.999967 24.0 0.997299 55.0 0.985693 strong oxidizing acid (Warning-Causes severe burns) OI
10.0 0.999703 25.0 0.997048 60.0 0.9831 96 surfactant cleaning fluids whenever a major adjustment is
't5.0 0.9991 03 26.0 0.996786 65.0 0.98055'1
15.56 0.999016 27.0 0.996516 70.0 o.977765 required.
16.0 0.998946 28.0 0.996236 75.0 o.974843 10.3.1 Flush and dry the sample tube as described in l{}.2.1
17.0 0.998778 29.0 0.995947 80.0 0.971 790
and allow the display to reach a steady reading. If the display
18.0 0.998599 30.0 0.995650 85.0 0.9686 11
19.0 0.998408 35.0 0.994033 90.0 0.9653 10 does not exhibit the correct density for air at the temperature of
20.0 0.994207 37.78 0.993046 ooo 0.958421 test, repeat the cleaning procedure or adjust the value of
r Densities contorming to the lnternational Temperature Scale l9g0 (lTS g0) were constant B commencing with the last decimal place until the
extracted from Lemmon, E. W., Mclinden, M. O., and Friend, D. G., ,"1'hermo-
physical Properties of Fluid Systems,"N/Sf Ghemistry WebBaok, NIST Standard correct density is displayed.
Beference Database No. 68, Eds. P.J. Linstrom and WG. Mallard, National 10.3.2 If adjustment to constant B was necessary in 10.3.1
lnstitute of Slandards and Technology, Gaithersburg, MD, http://webbook.nist.gov.
then continue the recalibration by introducing freshly boiled
(retrieved July 24, 2013).
(Warning-Handling water at boiling or near boiling tempera-
ture can present a safety hazard. Wear appropriate personal
protective equipment.) reagent water into the sample tube as
described in l{}.2.3 and allow the display to reach a steady
d" : 0.001293[273.1s/Tllpn0l.325] g/ml- (t ) reading. If the instrurnent has been calibrated to display the
where: density, adjust the reading to the correct value for water at the
7 = temperature, K, and test temperature (Table I ) by changing the value of constant A,
P = barometric pressure, kPa. commencing with the last decimal place. If the instrument has
been calibrated to display the relative density. adjust the
10.2.5 Determine the density of water at the temperature of
reading to the value L0000.
test by reference to Tahle 1.
10.2.6 Using the observed l-values and the reference values Noru 5-If pefbrming a weekly calibration adjustment, it can be lbund
for water and air, calculate the values of the Constants A and B that more tian one value each for A and B, differing in the fourth decimal
using the following equations:
place, will yield the correct density reading for the density of air and
water. The setting chosen would then be dependent upon whether it was
t:fT., _ r",)tld" _ (1,1 e) approached from a higher or lower value. The setting selected by this
melhod could have the effect of altering the fourth place of the reading
B:7,2 _(exa") (3) obtained lbr a sample.

7,, = observed period of oscillation for cell containing water, 10.4 Some analyzer models are designed to display the
FS' measured period of oscillation only (I-values) and their
T, = observed period of oscillation for cell containing aiq calibration requires the determination of an instrument constant
ps, K, which must be used to calculate the density or relative
d,, = density of water at test temperature, g/ml, and density from the observed data.
d, = density of air at test temperature, g/ml. 10.4.1 Flush and dry the sample tube as described in l$.2" I
10.2.6.1 Alternatively, use the T and d values for the other and allow the display to reach a steady reading. Record the
reference liquid if one is used. Z-value for air.
10.2.7 If the instrument is equipped to calculate density 10.4.2 lntroduce freshly boiled (Warning-Handling water
from the constants A and B and the observed T-value from the at boiling or near boiling temperature can present a safety
sample, then enter the constants in the instrument memory in hazard. Wear appropriate personal protective equipment.) re-
accordance with the rnanufacturer's instructions. Alternatively. agent water into the sample tube as described in Il).2.3, allow
if the instrument is equipped to do so, let it rnake the the display to reach a steady reading and record the 7-value for
appropriate corections in the calibration or adjustment con- water.
stants as part of the built in calibration or adjustment proce- 10.4.3 Using the observed I-values and the reference values
dure. for water and air (l{}.2.4 and I0.2.5), calculate the instrument
10.2.8 Check the calibration and adjust if needed by per- constant K using the following equations:
fbrming the routine calibration check described in t{}.3. For density:
10.2.9 To calibrate the instrument to display relative :ld*
density, that is, the density of the sample at a given temperatur-e
K, _ d.l/Lr", _ T",l $)
referred to the density of water at the same temperature, follorv For relativc density:
,($fp o+osz - 1G

r, : [r.oooo - d,]tLr*2 - T.1f (5) introduction and checking for bubbles because the heat gener-
where: ated can affect the measurement temperature. For some models
however, the cell light rnay be left on without affecting results.
7,, = observed period of oscillation for cell containing water,
Refer to the manufactureros recomrnendations concerning
FS,
whether to leave the illurnination light off or on.
7,, = observed period of oscillation for cell containing air,
12.1.5 After the instrument displays a steady reading to four
ps,
signilicant figures for density, relative density, or API Gravity,
dnu - density of water at test temperature, g/ml, and and five for Z-values, indicating that temperature equilibrium
do = density of air at test temperature, g/ml.
has been reached, record the density, relative density, API
Il. Quality Control Checkrs Gravity or l-values, or both, as appropriate. For instruments
that can print out results from the display, the print out can be
ll.1 Confirm the instrument is in statistical control at least used to meet the recording requirements.
once a week when it is in use, by analyzing a quality control
12.1.6 Based on the 1999 ILS6 testing protocols (see Nore
(QC) sample that is representative of samples typically ana-
8), precision determinations involving a single manual
lyzed. Analysis of a single QC sample can be sufficient.
Analysis of QC sample results can be carried out using control
injection, as well as taking the average of two manual
injections, was evaluated. See the Precision and Bias section
chart techniques.t If the QC sample result determined causes
the lab to be in an out-of-control situation, such as exceeding
for more details. If the lab performs a single manual
determination, the density, relative density, or API Gravity
the lab's control limits, instrument recalibration or adjustment
values recorded in 12. 1.-{, or a combination thereof, is to be,
is required. An ample supply of QC sample material should be
used for reporting puryoses. In most cases, a single manual
available for the intended period of use, and must be homoge-
injection determination is sufficient for sample analysis.
neous and stable under the anticipated storage conditions. Prior
to monitoring the measurement process, the user of the method
12.1.6.1 If the lab decides to perform a second manual
injection determination for a given sample, repeat 12.1.1 *
needs to determine the average and control limits of the eC
12.t.5. If the two determinations do not differ by more than
sample. The QC sample precision should be checked against
0.0002 g/mL for density or 0.0002 for relative density, average
the method precision to ensure data quality.
the two determinations, otherwise, discard both determinations
'11.2 Although not mandatory, it is recommended that peri- and repeat the analysis using two new test specimens until the
odic analyses of certified density standards (that is, traceable to acceptance criteria identified above is satisfled. With respect to
national standards) that are separate fiom those that may be API Gravity determinations of gasoline or RFG samples, if the
used in calibrating the instrument, be used to confirm testing two determinations do not differ by more than 0.05' API
accuracy. Gravity units, average the two determinations, otherwise,
discard both determinations and repeat the analysis using two
12. Procedure new test specimens until the acceptance criieria is satisfied.
l2.l Manttal Iniection: With respect to API Gravity determinations of distillates,
l2.l.l Introduce a small amount, about I mL to 2mL, of basestocks, and lubricating oils, follow the protocol in the prior
sample into the clean, dry sample tube of the instrument using sentence except use 0.03'API Gravity units as the acceptance
a suitable syringe or alternative, as described in 6.4. criteria. Averaged results meeting the criteria identified in this
.2 The sample can also be introduced by siphoning.
12.1 section is to be used for reporting purposes.
Plug the external TFE-fluorocarbon capillary tube into the 12.2 Automated Iniection:
entry port of the sample tube. Immerse the other end of the 12.2.1 The use of an autosampler (see 6.5) is required when
capillary in the sample and apply suction to the other port using rmalyzing samples by autonrated injection. Follow manufactur-
a syringe or vacuum line until the sample tube is properly filled er's instructions for ensuring the integrity of the test specimen
(see N<xe 1).
prior to analysis, as well as transferring a representative test
12.1.3 Ensure that the sample tube is properly filled and that specimen into the instrument for analysis.
no gas bubbles are present. The sample must be homogeneous 12.2.2 When using an autosampler, it is required, based on
and free of even t}re srnallest gas bubbles. Check the integrity the results obtained in the 1999 ILS6 to analyze gasoline or
of the filled sample by using optical or physical rnethods to RFG samples using two separate test specimens per sample, in
verify absence of gas bubbles. If gas bubbles are detected, order that errors due to potential sample handling of volatile
empty and refill the sample tube, and recheck for gas bubbles. materials and potential bubble tbrmation may be detected and
Norr 6-If the sample is too dark in color to determine the absence of the system performance monitored. For all other sample types,
bubbles with certainty, the density cannot be measured within the stated a single determination using an autosampler is sullicient.
precision limits of Section i.5. 12.2.2.1 If the lab decides to perform a second automated
12.1.4 For most instrument models, it is recommended to injection determination for a given distillate, basestock, or
tum the illurnination light off with minirnal delay after sample lubricating oil (see Note 8 and the Precision and Bias section),
use the same acceptance criteria in ]2"1.6"1 for allowed
s AS'l-1\,'l
MNL 7, hlanuat on Prcsentatiorr o.f Data Control Ch.arr Anolysis,
Section 3: Control Charts frx' Individuals, 6th ed.. ASTM International. W'. 6
Suppolting data have bcen filed at ASTM Inrertrational l.Ieadquartels and may
Conshohockcn. PA. lrc obtaincd by requesring Research Report RR:D02-1734.
.(ff oaos2. 16
differences between each determination for density For density:
(0.0002 ChnL), relarive densiry (0.0002) and ApI Gravity uniti
(0.03') as for manually injected samples. Averaged iesults densiry. g/ml- (kg/m3) att : (1. + KJT", - 7,,,2) (6)
meeting the necessary acceptance criteria are to be used for For relative density:
reporting purposes.
relarive density, tlt : I+ Kr(T,, - 2,,,,) e)
12.2.3 For determining the density or rclative density of
gasoline or RFG mrnples analyzed by automated injection, where:
average the results of the two separate test specimens analyzed
in l?.22 if the two dererminations are within 0.0002 glmL of
T, = observed
T"
observed period of oscillation for cell containing water,
period of oscillation for cell containing
=
one another for density (or 0.0002 for relative density). If the sample,
two determinations fall outside this acceptance criteria, both d*. - density of water at test temperaturc,
determinations are to be discarded and 12"2.2 shall be repeated Kt = instrument coflstant for density,
until the acceptance criteria identified in the previous s"rter"e Kz = instrurnent constant for relative density, and
is satisfied. In cases where the acceptance criteria is not T = temperature of test, oC.
initially satisfled, the lab may need to investigate and take 13.3 If it is necessary to convert a result obtained usirig the
corrective actions befbre proceeding with subsequent analyses. density meter to API Gravity, or a density or relative density at
12.2.4 For determining the ApI Gravity of gasoline or RFG another temperature, Guide D I 250 can be used only if the glass
samples analyzed by automated injection, follow the same expansion factor has been excluded.
protocol defined in 12.2.3, except that the acceptance criteria
_Norr 7-Some digital density analyzers are equipped to automatically
for the results of the two determinations for ApI Gravity are to calculate and report sample results in ApI gravity units qsee Test Method
be within 0.05" API Gravity units before averaging l)287 or D1?9ti), based on the density or relative density results, or a
and cornbination thereof, determined by this test method and using the
reporting the results. appropriate conversion equation derived from Guide Dl25* (;hich
12.2.5 Opaque samples may be tested using either manual excludes the glass expansion factor),
for the specific sample type being
injection method described in 12. I or using an autosampler as analyzed.
described in 12.2. When testing opaque samples, proper 14. Report
procedure shall be established by which the absence of air
bubbles in the measuring cell can be confirmed with cefiainty. 14.1 In rcporting density, state the test temperature and the
Such procedures include multiple determinations and evalua_ units (for example: density at ZO "C = 0.8765 g/mL or
tion of closeness of determinations, utilizing optical or physical 876.5 kgln3).
methods for air bubble detection, or both. 14.2 In reporting relative density, state both the test tem-
12.2.5.1 This test method does not offer precision and bias perature and the reference temperature, but no units (for
values for opaque samples and because sample properties vary example: relative density, 20l2O"C = O.xxxx).
greatly, determinability criteria is not offered, but shafl bL
14.3 Report the final result for density or relative densify to
established by a series of tests determinations on representative
four significant figures.
sample material. Perform a minimum of three consecutive
determinations of different test specimens from the same 14.4 It reporling sample results in ApI gravity units (see
syringe or sample vial without removing the syringe from the Note 7), report the final results to the nearest 0.1. ApI.
apparatus and without any rinsing or cleaning between deter_ 14.5 In some cases, it may be necessary to report if results
minations. Average the two determinations with the highest were based on a single determination or an average of two
density or lowest API number and report per 12.2"{t. determinations, as well as if results were determined by manual
12.2.6 Record the density, relative density, or ApI Gravity injection or automated injection to meet specific requirements,
results, or a combination thereof, determined by the analyses as such as data recipients wanting to know such information in
appropriate, such as by using the instrument print out of results order to understand how to interpret results relative to the
to meet the recording requirements. published method precision values. In such cases, it is permis-
sible to report this information along with the test results.
13. Calculation
15. Precision and Bias6
l3.l Calculctting Density Analyzers-The recorded or
printed value is the final result when a single determination is l5.l The precision of the method as obtained by statistical
conducted (or taking the average of two determinations as the examination of interlaboratory test results at a test temperature
final result as identilied in Section l2), expressed either of l5'C is as follows for the following sample types and
as
density in g/ml. kg/m3 or as relative density. Note that kg/m3 ranges:
1000 x glml-.
= l5.l.l Repeatability--:111s difference between successive
test results obtained by the same operator with the same
13.2 Noncalculating Den.sity Analyz.er,s-tJsing the ob_ apparatus under constant operating conditions on identical test
served l-value for the sample and the 7-value for water and material. would in the long run, in the normal and correct
appropriate instrument constants determined in I{}.4.3, calcu_ operation of the test method, exceed the following value only
late the density or relative density using liq f.r **il T. Carry out in one case in twenty:
all calculations to six significant figures and round the final 15.1.1.1 Density (ghnL) and Relative..Densi4--See Tahle 2.
results to four. 15.1.1.2 API Gravity-See Tabl* 3.
.(flP oaosz - 10
TABLE 2 Density (g/ml) and Relative Density (Repeatability)
Range Sample Types Testing Condition Hepeatability
0.714.78 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 Oits (Manual or automated iniection)
Average of 2 Determinations 0.00011
(Manual or automated

TABLE 3 API Gravity (Repeatabitity)


Sample Types Testing Condition Repeatability
Gasoline and RFG Single Determination 0.090
(Manual injection)
Average of 2 Determinations 0.063
(Manual or automated injections)
Distillates, Basestocks, and Single Determination 0.032
Lubricating Oils (Manual or automated iniection)
Average of 2 Determinations o.o22
(Manual or automated injections)

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


Sample Types Testing Condition Reproducibility
o.714.78 Gasoline and RFG Single Determination 0.001 90--o.0344 (D-0.7s)
(Manual injection)
Average ot 2 Determinations 0.001 9s-0.03 r 5 (D-{.75)
(Manual or automated injections)
0.8H.88 Distillates,Basestocks,and Single Determination 0.00052
Lubricating Oils (Manual or automated injection)
Average ot 2 Determinations 0.00050
(Manual or automated injections)
where: D = density or relative density value obtained

TABLE 5 API Gravity (Reproducibility)


Bange Sample Types Testing Condition Reproducibility
51-66 Gasoline and RFG Single Determination 0.60 + 0.040 (G-60)
(Manual iniection)
Average of 2 Determinations 0.60 + 0.0s7 (G-60)
(Manual or automated injections)
2945 Distillates, Basestocks and Single Determination 0.133
Lubricating Oils (Manual or automated iniection)
Average of 2 Determinations o.128
(Manua' or automated injections)
where: G = API Gravity value obtained

15.1.2 Reproducibility--:lhe difference between two single taking the average of the two detenninations from each analysis set, as
and independent results, obtained by different operators work- well as determining if there was a precision effect between manual and
ing in different laboratories on identical test material, would in automated injections. The repeatability and reproducibility statements
the long run, in the normal and correct operation of the test determined by the statistician reflect the conesponding precision values
associated with testing conditions identified. It should be noted that the
method, exceed the following values only in one case in
precision statements determined for the gasoline and RFC sanrple types in
twenty: the 1999 ILS were poorer than expected relative to the precision
15.1.2.1 Densirv (g/mL) and Relative Density-See Table 4. staternents determined for the distiilates, basestocks, and lubricating oils
15.1.2.2 API Gravir;-*-See Tahle 5. as well as relative to the previously published method version precision
Nore 8-The ASTM Inrerlaboratory Srudy (ILS) conducred in Fall statemerts (rvhich were based on the analysis of just three pure com-
19996 involvecl I1 labs and 23 samples. The"samples included pounds (benzrne, toluene, and xylene) analyzed by 3 labs in duplicate).
-5 motclr
gasolines, 1 motor gasoline + ethanol. 4 relbrrnulated gasolines (RFG), 2 The poorer than expected precision statenrents fbr the gasoline and RFG
lube oils, I basestock oil, 4 Jet-A fuels, I JpS fuel, and 5 diesel fuels. The sanrple types are likely due to the volatile.nature of these materials, even
ILS protocol required labs to perform a total of lbur measurements per though the ILS participants were provided inslructions for how to properly
sample, which included both manual and automated injections, with the handle these naterials to minimize or prevent sample losses. The
first two determinations represcnting the first analysis set and the second subcommittee resptxrsible for the method is planning to conduct a
two determinations represen{ing the second analysis sel. This prolocol was sutrsequent ILS lor gasoline and RFG sample types .ivith.additional
used to evaluate if a precision efect existed between taking the first scrutiny paid to sample handling issues as a means to try and improve the
determination frorn each analysis st:t (that is, singlc: determination.l versus precision statements for these materials.
,dffi oaos2 - 16
9-Four (4) of the samples analyz.ed in the Il-S.indicated in :\ilte
NorE ing densities in the range of 7 47 kg/m3 to 927 kgtm3 at 2O "C,
li were ASTM Interlaboratory Crosscheck samples (that is, Gaso-
with viscosities between I mPa.s and 5000 mPa.s (also at
line-Mc9808 and MG98l2, RFC-RFG9807, and RFG9809). The robust
mean of the total vapor plessures reported by Test Method l)Stel for 20'C). This study is documenred in ASTM Research Bpport
these samples ranged from alow of 7.77 psi (MG9808) ro a high of 13.40 RR:D02-1387.8 Method users should, therefore, be awareihat
psi (RFG9809). This corresponds to an approximate total vapor pressure results obtained by this test method can be biased by as much
range of -54 to 92 kPa.
as 0.6 kgln3 (0.0006 g/mL).
15.2 Bias-After suggestions of its existence from Norr l0-Newer instrumentalion exists which purports to correct
literature,T a study has been performed which has confirmed density results due to the influence of viscosity. However, the responsible
ASTM Technical Committee has not yet performed a new interlaboratory
the presence of a bias between known density values for
study to confirm the elimination of the bias described in ASTM Research
reference materials and from values determined according to Report RR:D02-1387.8
this test method on the same reference materials. The matrix
for this bias study comprised 15 participants, each analyzing 16. Keywords
four reference oils with certified density values, established by 16.1 API Gravity; density; digital density analyzer; perro-
the Netherlands Meet Instituut (I.{MD, by pyknome.try, cover- leum distillates; petroleum products; relative density

7
Fitzgerald, H. and D., "An Assessment of Laboratory Density 8
Supporting data have been filed at ASTM Intemational Headquarters and may
P et ro le um Reylew, Novernb er 1992, pp. 544-549. be obtained by requesting Research Report RR:D02-1387.

SUMMARY OF CHANGES

Subcommittee D02.04 has identi{ied the location of selected changes to this standard since the last lSSUE
(D4052 - 15) that may impact the use of this standard. (Approved Dec. l, 2016.)

(1) Revised 1.3. Q) Added a new 12.2.5 and renumbered the original as i2.2.6.

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