SOP 21 Standard Operating Procedure For Calibration of LPG Provers
SOP 21 Standard Operating Procedure For Calibration of LPG Provers
SOP 21 Standard Operating Procedure For Calibration of LPG Provers
SOP 21
1 Introduction
This procedure may be used to calibrate a volume standard used to test systems
designed to measure and deliver liquefied petroleum gas (LPG) in the liquid state
by definite volume, whether installed in a permanent location or mounted on a
vehicle. A schematic diagram of such a prover is shown in Figure 1, together with
numbers, e.g., 1, 2, 3, and 4 to clarify the various operations described in the
procedure. The parts labeled A, B, and C are hose connections used in meter
testing (versus prover calibrations). The prover being calibrated should be
evaluated for conformance to appropriate specifications (using the checklist
provided in NIST Handbook 105-4, Specifications and Tolerances for Liquefied
Petroleum Gas and Anhydrous Ammonia Liquid Volumetric Provers, 2010) if
being used for legal weights and measures applications. You should also review
the schematic provided in Handbook 105-4.
1.2 Prerequisites
1.2.1 Verify the unknown prover has been properly cleaned and vented with all
petroleum products removed prior to submission for calibration to ensure
laboratory safety. The prover and/or pressure gauge may be visually
inspected to determine that residual products are not present. Smell is not
necessarily an adequate indicator of cleanliness.
1.2.2 Verify that valid current calibration certificates with measurement values
and uncertainties are available for all of the standards used in the test. All
calibration values must have demonstrated metrological traceability to the
International System of Units (SI). Metrological traceability may be to the
SI through a National Metrology Institute (for example, NIST.)
1
Non-SI units are predominately in common use in State legal metrology laboratories, and/or the petroleum industry
for many volumetric measurements, therefore non-SI units have been used to reflect the practical needs of the
laboratories performing these measurements as appropriate. The majority of LPG provers in use are 20 gal, 25 gal,
and 100 gal nominal sizes. The volume of LPG provers is established at 60 ºF and 100 psig.
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1.2.3 Verify that the standards to be used have sufficiently small standard
uncertainties for the intended level of the calibration.
1.2.5 Verify that the operator has had specific training in SOP 19, SOP 20, SOP
21, and GMP 3 and is familiar with the operating characteristics and
conditioning of the standards and unknown test items being used and
calibrated.
1.2.7 Verify that the laboratory facilities meet the following minimum
conditions to make possible the expected uncertainty achievable with this
procedure:
Volume 18 C to 27 C 35 % to 65 %
Transfer Stable to ± 2.0 C / 1 h Stable to ± 20 % / 4 h
1.3.2 The care required for field calibrations includes proper safety, a clean and
bubble-free water supply, measurement control programs, and a stable
temperature environment shaded from direct sunshine to allow the prover,
field standard, and clean test liquid (water) to reach an equilibrium
temperature with minimal evaporation. Environmental conditions must be
selected to be within stated laboratory conditions during the
measurements. All data and appropriate environmental conditions must be
documented regardless of test location.
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2 Methodology
This procedure is applicable for the calibration of LPG provers with capacities of
100 L to 500 L (20 gal to 100 gal) or larger when appropriate. Provers of 20 gal,
25 gal, and 100 gal (with gal and in3 units) are encountered most frequently,
hence the procedure is written with that in mind. The changes necessary for
testing provers of other capacities will be obvious and are not described in this
document. The agreement of duplicate measurements made within a short period
of time on a given 100 gal LPG prover must be within 5 in3 (0.02 gal). For any
nominal volume, replicate values must agree within 0.02 % of the volume. Where
the demonstrated standard deviation of the process is less than 0.02 % of the
volume, replicate values must agree to within the limits on the standard deviation
or range charts. The accuracy will depend on the uncertainty in the volume of the
standard, on the care exercised in making the various measurements and
temperature readings, and on correct application of the corresponding corrections.
2.2 Summary
2.3.1 Calibrated standard prover of minimum volume of 5 gal for 20 gal and 25
gal LPG provers is acceptable. A 10 gal standard is acceptable for
calibrating a 100 gal LPG prover, but a standard that is of the same
volume as the LPG prover is preferable. NOTE: standard provers used for
calibration may need to have an alternative calibration value based on
restricted flow delivery as the opening for many LPG provers may not be
adequate to receive the full flow delivery from the reference standard.
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2.3.2 A funnel for transferring water from calibrated flasks into the unknown
prover.
2.3.4 Thermometers (2) with resolution and uncertainty less than 0.1 C.
2.3.7 Sturdy platform, with appropriate safety conditions, with sufficient height
to hold standard and to permit transfer of water from it to the prover by
gravity flow.
2.3.8 Clean the pipe or tubing (hoses) to facilitate transfer of water from the
laboratory standard to prover. Nearly all LPG provers require reducers to
be used between normal laboratory piping and the top hole on the prover.
Pipe and hose lengths must be minimized to reduce water retention errors.
Care must be taken during wet-downs and runs to ensure complete
drainage and consistent retention in all hoses or pipes. Arrange all hoses
so that there are no loops or low spots that can hold water.
2.4 Procedure
2.4.1.2 Position and level the unknown prover where it can be reached
from the elevated standard by the shortest feasible delivery system.
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2.4.1.4 Remove the plug and relief valve (1) from the top, and extend the
pipe into the hole. This may require the use of a reducer and a
short length of hose (about 1 inch in diameter). If this is a tight fit,
open the vapor return line valve (2) to provide an air bleed.
Warning: ensure that a check valve is not plumbed into the prover
inlet line. If it is, remove the check valve, otherwise the prover will
need to be drained via the plug in the bottom of the lower neck.
Both the standard and the unknown prover must be internally clean. This
should be verified by checking that water drains properly from them. If
necessary, either or both should be cleaned with water and non-foaming
detergent (see GMP No. 6) to attain good drainage characteristics.
Additional effort may be required to eliminate scaling and contamination
build-up from the inside of LPG provers.
2.4.3 Neck scale plate verification (This is generally only conducted for new or
damaged measures or those that have not been calibrated by the
laboratory in the past.)
2.4.3.1 Fill the unknown prover with water from the standard. Check the
prover level condition in the same way in which it will be used and
adjust if necessary by placing a precision spirit or electronic digital
level vertically on the neck on at least two locations, 90 degrees
apart around the circumference of the neck and adjust the
orientation of the standard until the neck is as close to vertical
(plumb or perpendicular to the horizontal plane) as possible. Verify
and adjust any mounted levels that are on the prover to agree
(when present and when possible). Check the prover system for
leaks. This is a wet-down run.
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2.4.3.2 Bleed the liquid level down to a graduation near the bottom of the
upper neck. "Rock" the prover to "bounce" the liquid level,
momentarily, to ensure that it has reached an equilibrium level.
Read and record this setting to be used as the initial scale reading
sri. This is in preparation for calibration of the neck scale.
2.4.3.3 Remove the fill hose or pipe from the top and insert a funnel.
2.4.3.4 Recheck the scale reading, then add water in a quantity equal to
approximately ¼ or 1/5 of the graduated neck volume from a
suitable standard; record the scale reading.
2.4.3.5 Repeat 2.4.3.4 by successive additions until water is near the top of
the scale (the neck capacity is usually about 5 gal on a 100 gal
LPG prover). Record scale readings after each addition. The last
reading will be the final scale reading, srf. The closer the water is
to the top of the neck, the harder it may be to "bounce" the liquid
in the gauge.
2.4.3.6 Calculate and assess the accuracy of the neck scale for each
interval. The maximum capacity tolerance between the nominal
volume line and any other line on the scale shall be less than two
(2) major scale divisions as listed in Handbook 105-4. If more than
this, the scale should be replaced. Alternatively, a Neck Scale
Correction Value (NSCV) may be issued with instructions to the
user if it is anticipated that this correction value will be used.
2.4.3.7 Neck scale errors less than the limits provided in NIST Handbook
105-4 should be included in the uncertainty estimate associated
with the prover calibration. Uncertainties associated with the neck
scale calibration are primarily related to the setting of the meniscus
on the flask used (with each drop), the reading of the meniscus on
the unknown prover (at each volume reading), and the calibration
uncertainty of the flask. These uncertainties must be considered
when evaluating the acceptability of the neck scale.
Vw
NSCV
srf sri Eqn. 1
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2.4.4.1 Drain the unknown LPG prover through its inlet valve and the
liquid bleeder valve. When the liquid reaches the top of the lower
gauge glass, close the inlet valve and allow the water to drain from
the interior of the prover into the lower neck for 30 s, while
controlling the water flow and level with the bleeder valve until the
liquid meniscus reaches the zero graduation. The liquid level
should be exactly at the zero graduation and the bleeder valve
closed simultaneously at the 30 s drain time. (Draining with the
bleeder valve close to the zero mark should be started during the
30 s drain period but should not be completed before the end of the
drain period.)
2.4.4.2 Run 1. Transfer the volume from the standard in the usual manner,
and record the standard and prover temperature readings. If
multiple transfers are required, record temperature of the standard
at the time of each transfer, but that of the prover only after the
final transfer. Check the prover level by placing a precision spirit
or electronic digital level vertically on the neck on at least two
locations, 90 degrees apart around the circumference of the neck
and adjust the orientation of the standard until the neck is as close
to vertical (plumb or perpendicular to the horizontal plane) as
possible. Verify and adjust any mounted levels that are on the
prover to agree (when present and when possible). "Rock" the
prover to "bounce" the liquid in the upper gauge glass before
reading. Record the final scale reading after the nominal volume
has been transferred into the unknown LPG prover with no
pressure applied.
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2.4.4.3 Run 2. Drain the LPG prover as described in 2.4.4.1 and make
another test run. Record the temperatures of the standard(s) and the
unknown and final scale reading. Calculate the prover error at
0 psig (no pressure applied) for each run using the appropriate
equations in Section 3; these values are used to evaluate
repeatability of the test only. The error at 0 psig for the test runs
must agree within 0.02 % of the prover volume or approximately
one-half the prover tolerance (i.e., 5 in3 on a 100 gal LPG prover).
If the two runs fail to agree within 0.02 % of the prover volume, or
the limits on the standard deviation or range charts (whichever is
smaller), identify and correct problems with the prover or set-up.
Then, continue until replicates agree within these limits, taking
care to ensure that poor cleanliness, prover condition,
contamination, bubbles in hoses, leaking valves or seals are not
contributing to poor repeatability. Lack of measurement agreement
may also be due to poor field conditions, such as when calibration
is conducted in unstable environments. Poor agreement must be
corrected before calibration can be completed.
2.4.4.4 While the LPG prover remains full from Run 2, replace the relief
valve and plug in the top of the prover using suitable pipe joint
compound or tape.
2.4.5.1 The internal pressure and hence the volume of the prover may vary
during use. Accordingly, a pressure correction must be made using
the data of steps 2.4.6.
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Connect the cylinder regulator output to the vapor return fitting (2)
near the top of the neck. This may require fashioning a connection
with steel pipe nipples or other appropriate materials and the
existing fittings.
Caution: Ensure that all piping and fittings are rated for the
pressures to which they will be exposed.
Make sure all valves are closed except the vapor return valve.
Verify that the final scale reading has not changed since it was
recorded (if it has changed it may signal a leak in one of the valves
or fittings), and then slowly introduce pressure until the installed
prover gauge reads 100 psig. Lightly tap the gauge to ensure that
the gauge needle is not sticking. "Bounce" the liquid in the neck,
then read and record the liquid level at this applied pressure.
2.4.5.3 With the pressure in the prover at 100 psig, adjust the upper scale
to read the nominal volume. This is accomplished by adjusting the
upper scale so that the water level reading is:
Eqn. 2
.
Take care to use like units in the calculation. The calculation for
VX60 is given in 3.1, Eqn. 5 or Eqn. 6.
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2.4.5.4 For provers with only an adjustable lower scale (or one in which
the upper scale is not adjustable), a prover correction, LC, may
be calculated at 100 psig as follows:
.
Eqn. 3
where:
LC Prover correction at 100 psig
VX60 Volume of unknown prover at 60 F
V NOM Nominal volume of prover
sru Upper scale reading at 100 psig
1.00032 Correction factor for the compressibility of
water at 100 psig
4 LC
h Eqn. 4
d2
where:
h Distance in inches the bottom scale is to be
moved, up or down
LC Prover correction at 100 psig in cubic inches
d Inside diameter of the lower neck of the
prover in inches (as noted on identification
plate)
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2.4.6.2 Repeat step 2.4.6.1 at 100, 150, and 200 psig. Other pressure
points in between those listed may be tested if so desired. (The
water level should decrease 10 in3 to 15 in3 for each 50 psig
increase in pressure on a 100 gal prover, although this varies
depending on the geometry and age of the LPG prover. Water
level changes significantly greater than indicated may be due to
leaking seals and/or valves.) Erratic pressure readings may also
be due to air entrapment based on prover design; repeated
pressurizing of the prover should eliminate entrapped air. Air
entrapment problems due to design may need to be investigated
and corrected.
2.4.6.3 Repeat step 2.4.6.1 as the pressure is bled down to 150, 100, 50,
and 0 psig (atmospheric pressure). The readings must agree with
those previously obtained within approximately 0.02 % of the
nominal prover volume. If the data are not linear with respect to
pressure, repeat the series of measurements above to verify the
nonlinearity of the readings. Leaking seals or valves may cause
problems with repeatability of the gauge readings under
pressure. The cause of poor agreement must be identified and
corrected before continuing the calibration.
2.4.7.2 Drain prover, then remove plug (5) at the lower neck to
facilitate drainage below the lower gauge. If time permits,
let the prover drain overnight.
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3.1.1 Calculate VX60, the volume of the unknown prover at 60 F, using the
following equation:
1 VS 60 1 1 t1 60 F
V X 60
x 1 t x 60 F
Eqn. 5
3.2.1 Calculate VX60, the volume of the unknown prover at 60 F, using the
following equation:
1 VS60 1 1 t1 60F 2 VS60 2 1 t2 60F ... N VS60 N 1 tN 60F
VX60
x 1 tx 60F
Eqn. 6
density of the water in the standard prover where 1 is the density of the water for the first
1 , 2 ,..., N delivery, 2 is the density of the water for the second delivery, and so on until all N deliveries are
completed
volume difference between water level and the reference mark on the standard where the
subscripts 1, 2,..., N, represent each delivery as above. If the water level is below the reference
line, is negative. If the water level is above the reference line, is positive. If the water level is
1, 2,..., N
at the reference line, is zero
NOTE: units must match volume units for the standard. For slicker-plate type standards, the is
zero.
t1, t2, ..., tN temperature of water for each delivery with the subscripts as above
Compute the pressure correction, Pcorr, at each pressure that the prover was
read, after any adjustments, by correcting for the compressibility of the water.
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Plot the pressure corrections. If the corrections versus the pressure are linear,
make a straight line best fit of the data and interpolate to obtain the pressure
corrections for any desired pressure. If the data is nonlinear, then perform a
straight line interpolation between adjacent pressure readings to obtain
pressure corrections at any desired intermediate pressures. Alternatively, a
best fit curve can be drawn for the nonlinear data and the pressure corrections
interpolated from the graph for intermediate pressures.
LPG provers are generally adjusted to the nominal value using 100 psig as the
reference pressure and a 60 °F reference temperature. A gauge reading on a
prover that indicates a nominal volume at 0 psig will be lower when pressurized
to 100 psig due to both the compressibility of water under pressure and the
expansion of the prover. The expansion of the prover is consistent whether there
is water in the prover or LPG. However, a correction must be made for the
compressibility of water as noted in 3.3. Thus, to adjust a 100 gal prover to its
nominal volume at 100 psig, the gauge reading should be set to the VX60 value
minus 7.4 in3. (The water level on the prover’s upper scale will be 7.4 in3 less
than the calculated VX60 value when pressurized to 100 psig.) Adjusting the scale
plate while the prover is under pressure at 100 psig to indicate the corrected water
level will correct for the compressibility of water and set the correct prover
volume.
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Another possible way to handle the compressibility of water is to add the volume
of water (e.g., 7.4 in3 for a 100 gal prover) to the volume of water in the prover so
that it can be set to the VX60 value at 100 psig.
The calculated mean volume of the prover at its reference temperature and
pressures at 0 psig, 50 psig, 100 psig, and 150 psig and 200 psig, are reported on
the calibration certificate.
4 Measurement Assurance
4.1 Duplicate the process with a suitable check standard or have a suitable range of
check standards for the laboratory. See SOP 17, SOP 20 and SOP 30. Plot the
check standard volume and verify it is within established limits OR a
t-test may be incorporated to check the observed value against an accepted value.
The mean of the check standard observations is used to evaluate bias and drift
over time. Check standard observations are used to calculate the standard
deviation of the measurement process which contributes to the Type A
uncertainty components.
4.2 If a standard deviation chart is used for measurement assurance, the standard
deviation of each combination of Run 1 and Run 2 is calculated and the pooled
(or average) standard deviation is used as the estimate of variability in the
measurement process. Note: the pooled or average standard deviation over time
will reflect varying conditions of LPG provers that are submitted to the laboratory
but do not reflect potential meniscus reading errors (See GMP 3.)
For unknown standards that are adjusted, do not combine an “as found” value
with an “as left” value for the two runs entered into the chart; use the adjusted
value from Run 1 and the value from Run 2, both at the applicable reference
temperature, when entering values in a standard deviation or range chart.
.
5 Assignment of Uncertainties
5.1.1 The standard uncertainty for the standard, us, is obtained from the
calibration report. The combined standard uncertainty, uc, is used and not
the expanded uncertainty, U, therefore the reported uncertainty for the
standard will usually need to be divided by the coverage factor k.
Note: See SOP 29 for the complete standard operating procedure for
calculating the uncertainty when multiple deliveries or multiple standards
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5.2 The standard deviation of the measurement process sp, is taken from a control
chart for an LPG check standard (not from charts for a refined fuel check
standard) or standard deviation charts for LPG calibrations (See SOP 17, SOP 20
and SOP 30). Check standards are not normally available.
5.4 Other standard uncertainties usually included at this calibration level are 1)
uncertainties associated with the ability to read the meniscus, only part of which is
included in the process variability due to parallax and visual capabilities, and 2)
uncertainties associated with temperature corrections that include values for the
cubical coefficient of expansion for the prover under test, the accuracy and
gradients associated with temperature measurements in the provers. Additional
factors that might be included are: data showing reproducibility, environmental
variations over time, and bias or drift of the standard as noted in control charts.
Factors that are usually insignificant are uncertainties associated with viscosity of
the water as a calibration medium and uncertainties associated with the
compressibility of water.
5.6 Example components to be considered for an uncertainty budget table are shown
in Table 4. Multiple values of some items may need to be considered (e.g.,
multiple drops from the standard, multiple meniscus readings, and multiple
temperature readings.)
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Uncertainty Component
Symbol Source Typical Distribution
Description
6 Calibration Certificate
For LPG provers, the mean prover volume and uncertainty, reference temperature,
material, coefficient of expansion (assumed or measured), any identifying
markings, tolerances (if appropriate), laboratory temperature, water temperature,
barometric pressure, relative humidity, out-of-tolerance conditions, and the total
drain time from opening of the valve, including the 30 s drain after cessation of
flow.
The report should also include temperature and pressure correction tables or chart,
along with a note regarding possible differences in retention characteristics
between water, the calibration medium, and LPG products.
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Appendix A
Volume Transfer Data Sheet for LPG Provers
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Appendix B
Example Temperature Correction Table*
Example for a 100 gallon prover and 60 °F reference temperature.
Mild Steel Stainless Steel
CCE
1.86 x 10-5/°F 2.65 x 10-5/°F
Temperature °F in3 gal in3 gal
-20 -34 -0.149 -49 -0.212
-15 -32 -0.139 -46 -0.199
-10 -30 -0.130 -43 -0.186
-5 -28 -0.121 -40 -0.172
0 -26 -0.112 -37 -0.159
5 -24 -0.102 -34 -0.146
10 -21 -0.093 -31 -0.133
15 -19 -0.084 -28 -0.119
20 -17 -0.074 -24 -0.106
25 -15 -0.065 -21 -0.093
30 -13 -0.056 -18 -0.079
35 -11 -0.047 -15 -0.066
40 -9 -0.037 -12 -0.053
45 -6 -0.028 -9 -0.040
50 -4 -0.019 -6 -0.026
55 -2 -0.009 -3 -0.013
60 0 0.000 0 0.000
65 2 0.009 3 0.013
70 4 0.019 6 0.026
75 6 0.028 9 0.040
80 9 0.037 12 0.053
85 11 0.046 15 0.066
90 13 0.056 18 0.080
95 15 0.065 21 0.093
100 17 0.074 24 0.106
105 19 0.084 28 0.119
110 21 0.093 31 0.133
115 24 0.102 34 0.146
120 26 0.112 37 0.159
CCE = coefficient of cubical expansion
*Provide only the applicable coefficient of cubical expansion for the prover under test.
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