Astm D 4052
Astm D 4052
Astm D 4052
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1. Scope*
1.1 This test method covers the determination of the density,
relative density, and API Gravity of petroleum distillates and
viscous oils that can be handled in a normal fashion as liquids
at the temperature of test, utilizing either manual or automated
sample injection equipment. Its application is restricted to
liquids with total vapor pressures (see Test Method D5191)
typically below 100 kPa and viscosities (see Test Method D445
or D7042) typically below about 15 000 mm2/s at the temperature of test. The total vapor pressure limitation however can be
extended to >100 kPa provided that it is first ascertained that no
bubbles form in the U-shaped, oscillating tube, which can
affect the density determination. Some examples of products
that may be tested by this procedure include: gasoline and
gasoline-oxygenate blends, diesel, jet, basestocks, waxes, and
lubricating oils.
1.1.1 Waxes and highly viscous samples were not included
in the 1999 interlaboratory study (ILS) sample set that was
used to determine the current precision statements of the
method, since all samples evaluated at the time were analyzed
at a test temperature of 15C. Wax and highly viscous samples
require a temperature cell operated at elevated temperatures
necessary to ensure a liquid test specimen is introduced for
analysis. Consult instrument manufacturer instructions for
appropriate guidance and precautions when attempting to
analyze wax or highly viscous samples. Refer to the Precision
and Bias section of the method and Note 8 for more detailed
information about the 1999 ILS that was conducted.
1.2 In cases of dispute, the referee method is the one where
samples are introduced manually as in 6.3 or 6.4, as appropriate for sample type.
1.3 This test method should not be applied to samples so
dark in color that the absence of air bubbles in the sample cell
cannot be established with certainty. For the determination of
density in crude oil samples use Test Method D5002.
2. Referenced Documents
2.1 ASTM Standards:2
D287 Test Method for API Gravity of Crude Petroleum and
Petroleum Products (Hydrometer Method)
D445 Test Method for Kinematic Viscosity of Transparent
and Opaque Liquids (and Calculation of Dynamic Viscosity)
D1193 Specification for Reagent Water
D1250 Guide for Use of the Petroleum Measurement Tables
D1298 Test Method for Density, Relative Density (Specific
Gravity), or API Gravity of Crude Petroleum and Liquid
Petroleum Products by Hydrometer Method
D4057 Practice for Manual Sampling of Petroleum and
Petroleum Products
D4177 Practice for Automatic Sampling of Petroleum and
Petroleum Products
D4377 Test Method for Water in Crude Oils by Potentiometric Karl Fischer Titration
D5002 Test Method for Density and Relative Density of
Crude Oils by Digital Density Analyzer
D5191 Test Method for Vapor Pressure of Petroleum Products (Mini Method)
D7042 Test Method for Dynamic Viscosity and Density of
Liquids by Stabinger Viscometer (and the Calculation of
Kinematic Viscosity)
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1
This test method is under the jurisdiction of ASTM Committee D02 on
Petroleum Products and Lubricants and is the direct responsibility of Subcommittee
D02.04.0D on Physical and Chemical Methods.
Current edition approved Oct. 15, 2011. Published December 2011. Originally
approved in 1981. Last previous edition approved in 2009 as D405209. DOI:
10.1520/D4052-11.
2
For referenced ASTM standards, visit the ASTM website, www.astm.org, or
contact ASTM Customer Service at service@astm.org. For Annual Book of ASTM
Standards volume information, refer to the standards Document Summary page on
the ASTM website.
1
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6.4 Flow-Through or Pressure Adapter, for use as an
alternative means of introducing the sample into the density
analyzer either by a pump, by pressure, or by vacuum.
3. Terminology
3.1 Definitions:
3.1.1 density, nmass per unit volume at a specified
temperature.
3.1.2 relative density, nthe ratio of the density of a
material at a stated temperature to the density of water at a
stated temperature.
3.2 Definitions of Terms Specific to This Standard:
3.2.1 adjustment, vthe operation of bringing the instrument to a state of performance suitable for its use, by setting or
adjusting the density meter constants.
3.2.1.1 DiscussionOn some digital density analyzer instruments, an adjustment may be made rather than calibrating
the instrument. The adjustment procedure uses air and redistilled, freshly boiled water (WarningHandling water at
boiling or near boiling temperature can present a safety hazard.
Wear appropriate personal protective equipment.) as standards
to establish the linearity of measurements over a range of
operating temperatures.
3.2.2 calibration, vset of operations that establishes the
relationship between the reference density of standards and the
corresponding density reading of the instrument.
3
Reagent Chemicals, American Chemical Society Specifications, American
Chemical Society, Washington, DC. For suggestions on the testing of reagents not
listed by the American Chemical Society, see Analar Standards for Laboratory
Chemicals, BDH Ltd., Poole, Dorset, U.K., and the United States Pharmacopeia
and National Formulary, U.S. Pharmaceutical Convention, Inc. (USPC), Rockville,
MD.
4
Suitable solvent naphthas are marketed under various designations such as
Petroleum Ether, Ligroine, or Precipitation Naphtha.
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and control of the test temperature in the sample tube is
extremely important. An error of 0.1C can result in a change
in density of one in the fourth decimal when measuring in units
of g/mL.)
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9. Preparation of Apparatus
9.1 Set up the density analyzer (including the constant
temperature bath and related attachments, if necessary) following the manufacturers instructions. Adjust the bath or internal
temperature control so that the desired test temperature is
established and maintained in the sample compartment of the
analyzer. Calibrate the instrument at the same temperature at
which the density or relative density of the sample is to be
measured or perform an adjustment (see 3.2.1Discussion) in
preparation of analyzing samples. (WarningPrecise setting
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No reproduction or networking permitted without license from IHS
(1)
where:
T = temperature, K, and
P = barometric pressure, torr.
10.2.5 Determine the density of water at the temperature of
test by reference to Table 1.
10.2.6 Using the observed T-values and the reference values
for water and air, calculate the values of the Constants A and B
using the following equations:
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TABLE 1 Density of WaterA
Density,
g/mL
Temperature,
C
Density,
g/mL
Temperature,
C
Density,
g/mL
0.0
3.0
4.0
5.0
10.0
15.0
15.56
16.0
17.0
18.0
19.0
20.0
0.999840
0.999964
0.999972
0.999964
0.999699
0.999099
0.999012
0.998943
0.998774
0.998595
0.998404
0.998203
21.0
22.0
23.0
24.0
25.0
26.0
27.0
28.0
29.0
30.0
35.0
37.78
0.997991
0.997769
0.997537
0.997295
0.997043
0.996782
0.996511
0.996231
0.995943
0.995645
0.994029
0.993042
40.0
45.0
50.0
55.0
60.0
65.0
70.0
75.0
80.0
85.0
90.0
100
0.992212
0.990208
0.988030
0.985688
0.983191
0.980546
0.977759
0.974837
0.971785
0.968606
0.965305
0.958345
A
Densities conforming to the International Temperature Scale 1990 (ITS 90)
were extracted from Appendix G, Standard Methods for Analysis of Petroleum and
Related Products 1991, Institute of Petroleum, London.
(2)
B 5 Ta2 ~A 3 da!
(3)
(4)
(5)
where:
Tw = observed period of oscillation for cell containing
water,
Ta = observed period of oscillation for cell containing air,
dw = density of water at test temperature, and
da = density of air at test temperature.
11. Quality Control Checks
11.1 Confirm the instrument is in statistical control at least
once a week when it is in use, by analyzing a quality control
(QC) sample that is representative of samples typically analyzed. Analysis of a single QC sample can be sufficient.
Analysis of QC sample results can be carried out using control
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Temperature,
C
12. Procedure
12.1 Manual Injection:
12.1.1 Introduce a small amount (about 1 to 2 mL) of
sample into the clean, dry sample tube of the instrument using
a suitable syringe or alternative, as described in 6.4.
12.1.2 The sample can also be introduced by siphoning.
Plug the external TFE-fluorocarbon capillary tube into the
entry port of the sample tube. Immerse the other end of the
capillary in the sample and apply suction to the other port using
a syringe or vacuum line until the sample tube is properly filled
(see Note 1).
12.1.3 Ensure that the sample tube is properly filled and that
no gas bubbles are present. The sample must be homogeneous
and free of even the smallest gas bubbles. Check the integrity
of the filled sample by using optical or physical methods to
verify absence of gas bubbles. If gas bubbles are detected,
empty and refill the sample tube, and recheck for gas bubbles.
NOTE 6If the sample is too dark in color to determine the absence of
bubbles with certainty, the density cannot be measured within the stated
precision limits of Section 15.
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ASTM MNL 7, Manual on Presentation of Data Control Chart Analysis,
Section 3: Control Charts for Individuals, 6th ed., ASTM International, W.
Conshohocken, PA.
6
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1734.
5
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TABLE 2 Density (g/mL) and Relative Density (Repeatability)
Sample Types
0.800.88
0.00031
0.00016
0.00011
(6)
(7)
where:
Tw = observed period of oscillation for cell containing
water,
Ts = observed period of oscillation for cell containing
sample,
dw = density of water at test temperature,
K1 = instrument constant for density,
K2 = instrument constant for relative density, and
T = temperature of test, C.
13.3 If it is necessary to convert a result obtained using the
density meter to API Gravity, or a density or relative density at
another temperature, Guide D1250 can be used only if the glass
expansion factor has been excluded.
NOTE 7Some digital density analyzers are equipped to automatically
calculate and report sample results in API gravity units (see Test Method
D287 or D1298), based on the density or relative density results, or a
combination thereof, determined by this test method and using the
appropriate conversion equation derived from Guide D1250 (which
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0.00045
14. Report
14.1 In reporting density, state the test temperature and the
units (for example: density at 20C = 0.8765 g/mL or 876.5 kg/
m3).
14.2 In reporting relative density, state both the test temperature and the reference temperature, but no units (for
example: relative density, 20/20C = 0.xxxx).
14.3 Report the final result for density or relative density to
four significant figures.
14.4 If reporting sample results in API gravity units (see
Note 7), report the final results to the nearest 0.1 API.
14.5 In some cases, it may be necessary to report if results
were based on a single determination or an average of two
determinations, as well as if results were determined by manual
injection or automated injection to meet specific requirements,
such as data recipients wanting to know such information in
order to understand how to interpret results relative to the
published method precision values. In such cases, it is permissible to report this information along with the test results.
Repeatability
excludes the glass expansion factor), for the specific sample type being
analyzed.
13. Calculation
13.1 Calculating Density AnalyzersThe recorded or
printed value is the final result when a single determination is
conducted (or taking the average of two determinations as the
final result as identified in Section 12), expressed either as
density in g/mL, kg/m3 or as relative density. Note that kg/m3 =
1000 3 g/mL.
13.2 Noncalculating Density AnalyzersUsing the observed T-value for the sample and the T-value for water and
appropriate instrument constants determined in 10.4.3, calculate the density or relative density using Eq 6 and 7. Carry out
all calculations to six significant figures and round the final
results to four.
For density:
density, g/mL ~kg/m3! at t 5 dw 1 K1~Ts2 Tw2!
Testing Condition
Single Determination
(Manual injection)
Average of 2 Determinations
(Manual or automated injections)
Single Determination
(Manual or automated injection)
Average of 2 Determinations
(Manual or automated injections)
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Range
0.710.78
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TABLE 3 API Gravity (Repeatability)
Range
5166
2945
Sample Types
Gasoline and RFG
Testing Condition
Repeatability
Single Determination
(Manual injection)
Average of 2 Determinations
(Manual or automated injections)
Single Determination
(Manual or automated injection)
Average of 2 Determinations
(Manual or automated injections)
0.090
0.063
0.032
0.022
0.800.88
Sample Types
Gasoline and RFG
Testing Condition
Reproducibility
Single Determination
(Manual injection)
Average of 2 Determinations
(Manual or automated injections)
Single Determination
(Manual or automated injection)
Average of 2 Determinations
(Manual or automated injections)
0.001900.0344 (D0.75)
0.001950.0315 (D0.75)
0.00052
0.00050
2945
Sample Types
Gasoline and RFG
Testing Condition
Reproducibility
Single Determination
(Manual injection)
Average of 2 Determinations
(Manual or automated injections)
Single Determination
(Manual or automated injection)
Average of 2 Determinations
(Manual or automated injections)
15.2 BiasAfter suggestions of its existence from literature,7 a study has been performed which has confirmed the
presence of a bias between known density values for reference
materials and from values determined according to this test
method on the same reference materials. The matrix for this
bias study comprised 15 participants, each analyzing four
reference oils with certified density values, established by the
Netherlands Meet Instituut (NMI), by pyknometry, covering
densities in the range of 747 to 927 kg/m3 at 20C, with
viscosities between 1 and 5000 mPa.s (also at 20C). This
study is documented in ASTM Research Report RR:D021387.8 Method users should, therefore, be aware that results
obtained by this test method can be biased by as much as 0.6
kg/m3 (0.0006 g/mL).
NOTE 10Newer instrumentation exists which purports to correct
density results due to the influence of viscosity. However, the responsible
ASTM Technical Committee has not yet performed a new interlaboratory
study to confirm the elimination of the bias described in ASTM Research
Report RR:D02-1387.8
7
Fitzgerald, H. and D., An Assessment of Laboratory Density Meters,
Petroleum Review, November 1992, pp. 544549.
8
Supporting data have been filed at ASTM International Headquarters and may
be obtained by requesting Research Report RR:D02-1387.
7
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Range
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16. Keywords
16.1 API Gravity; density; digital density analyzer; petroleum distillates; petroleum products; relative density
SUMMARY OF CHANGES
Subcommittee D02.04 has identified the location of selected changes to this standard since the last issue
(D405209) that may impact the use of this standard.
(1) Revised 8.3.1, 8.3.2, 12.1.3, and 12.1.4.
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