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The relationship between the
ur ilit
Go oor
ea
p
ac y
change in measurement output
P
od
y
and the change in measured
quantity is called sensitivity.
Ideally, this relationship is linear,
but in practice all measurements
involve some imperfections or
uncertainty. The agreement of
the measured value with the true
value is often called “accuracy”,
but this again is a somewhat vague
Repeatability
cc atab
y
Po
ea
ep
p
c u ta b
e
2
Another parameter related to inconsistencies present in manual or other contaminants into the
measurement performance is laboratory work. Examples of oil sample inevitably becomes
the lower detection limit (LDL), uncertainty sources in laboratory visible in the results as well. The
which is the lowest concentration analysis include: laboratory’s reproducibility – its
that the measurement instrument ability to repeat DGA results with
can reliably distinguish from • Sample preparation and GC- identical samples day after day
zero. Once again, “reliably” is a signal repeatability regardless of the operator – is an
somewhat vague term, which • Calibration and calibration excellent parameter to determine
can be determined, for example, sample preparation uncertainty the quality of the laboratory’s
as a 95% confidence level. processes.
• Partition coefficient uncertainty
There is a relationship between
(K)
measurement repeatability and It is recommended by IEC 60567
LDL – averaging reduces random • Vial volume uncertainty that every laboratory determines
variation in the measurement, • Sample mass uncertainty its own accuracy[2], meaning
improving repeatability and • Oil density uncertainty in practice its uncertainty. This
lowering LDL. In practice, the information should then be
LDL specification could be, for Oil sampling made available for users of the
example, twice the standard The biggest uncertainty source is laboratory’s services. Accredited
deviation of the measurement usually related to the quality of the laboratories must have this
readings at a 0-ppm gas level. As sample: how it was collected, the available as a requirement of
an example, if the measurement condition of the equipment used their accreditation. If official
device shows a higher value to collect it, how the sample was numbers for uncertainty are not
than that, there is about 2.5% stored, and how it was transported available, ask if the laboratory has
probability that the true value will all affect the quality. A participated in any international
would be 0 ppm. It is important to significant amount of gases like inter-laboratory comparison
note that it is very challenging to H2 and CO can escape from oil, tests – so-called round robin tests
create reference samples with very and humidity and ambient air (RRT) – and if their results are
low gas concentration, e.g. <1 ppm, gases like oxygen can contaminate available. This will give a good
making the LDL almost impossible the sample, resulting in erroneous rough indication of the expected
to measure in practice; it needs to laboratory analysis. This makes uncertainty level.
be defined theoretically based on it essential for the oil not to be in
the repeatability. contact with air at any point during The IEC 60567 standard gives
sample collection, and the sample examples of accuracies obtained
vessel must be completely filled when using its overall experimental
Laboratory DGA using the appropriate sampling procedure. These values are
When comparing the analysis procedure. The best working defined from IEC and CIGRE inter-
results of different methods, one solutions to achieve this are high- laboratory tests made on two
should be aware of uncertainties quality syringes and aluminum gas-in-oil standards and involving
relating to them both. The most bottles as they can tolerate 44 laboratories worldwide.
common uncertainty sources pressure variations during air Laboratory DGA uncertainty
are, for example, the oil-sampling cargo transportation, for example. depends on the gas extraction
method and quality, the gas- method used, the gas type, and
extraction method, used partition the gas concentration level. The
Laboratory analysis work
coefficients, differences in headspace (HS) method has
The uncertainty of laboratory
standards used, and so forth. It is higher uncertainty than vacuum
work also needs to be taken into
also important to understand that or stripping methods. If no other
account when evaluating DGA
a measurement cannot be more uncertainty data is available, you
results, or when comparing results
accurate than the reference used can use a ±15% average when
to data from an online monitor.
in calibration. evaluating laboratory DGA results
The first step in a laboratory is
and when comparing them to
to transfer a small amount of oil
an online monitor. The number
Laboratory DGA and related from the sampling vessel into a
for a specific laboratory may
uncertainties gas chromatography (GC) vial.
be significantly higher, but also
Laboratory DGA is affected This part of the process involves
somewhat lower for high-quality
by many factors, ranging from a human factor, because in many
analysis.
the quality of the oil sample to laboratories it is done completely,
the equipment, the standard or at least partially, manually.
used for analysis, and human Any human error that allows air
3
Variation due to standard method Table 1 Examples of accuracy levels for various extraction methods
in use according to IEC 60567 ed4-2011[2].
The two most commonly used
Accuracy in presentage of the nominal value
standards in laboratory DGA
worldwide are IEC 60567 and EXTRACTION MEDIUM LOW
PROCEDURE CONCENTRATION CONCENTRATION
ASTM D3612, and each have
subsections concerning specific TOEPLER 13 35
gas-extraction methods: vacuum,
PARTIAL DEGASSING 13 30
stripping, or HS. IEC, CIGRE,
ASTM, and the Institute for STRIPPING 18 23
Inter-Laboratory Studies in the
Netherlands have executed a HEADSPACE 18 37
number of RRTs to evaluate the
MERCURY-FREE TOEPLER 15 1 14 1
variation between the analysis
for different standard extraction MERCURY-FREE PARTIAL DEGASSING 11 1
methods. The differences between
the laboratory methods used SHAKE TEST 15 44
are shown in Table 3. The results 1)
Based on a limited number of analyses.
clearly show that it is more difficult
for laboratories to obtain accurate
results with the HS method. Table 2 Accuracy levels of an ISO 17025 accredited laboratory using HS
method vs IEC 60567:2011 at different gas concentration levels.
In the table, “average accuracy” ACCURACY (%) ACCURACY (%) ACCURACY (%)
means the average of accuracies IN LOW IN MEDIUM IN HIGH
for each gas in the measured CONCENTRATIONS CONCENTRATIONS CONCENTRATIONS
oil samples while “number of H2 15.6 9.5 5.9
inaccurate laboratories” means
the percentage of laboratories CH4 13.9 8.3 6.7
participating in the RRTs that did
C2H4 26.7 10.6 3.8
not meet the IEC requirements
for accuracy (e.g. ±15% above C2H6 26.2 22.3 6.3
100 ppm).
C2H2 33.6 18.8 8.3
It is important to note that ASTM
CO 26.5 14.1 8.9
and IEC standards calculate gas
volume at different temperatures, CO2 10.7 11.3 11
0°C and 20°C respectively[2, 3]. This
alone accounts for 8% difference LAB. AVERAGE 21.9 10.4
in defined concentrations for IEC 60567:2011
identical samples, which has 37 18
FOR HS
to be taken into account when
comparing DGA results from
a monitor and a laboratory. All Table 3 The accuracy of laboratories using gas extraction methods A
(partial degassing), B (stripping), and C (HS). The IEC specification is
measured ppm values should
shown on the bottom row[1].
first be converted to the same
condition, either 20°C (IEC) or 0°C AVERAGE ACCURACY OF NUMBER OF INACCURATE
(ASTM), depending on preference. LABORATORIES (%) LABORATORIES, % OF
PARTICIPANTS
METHOD > 100 ppm < 8 ppm > 100 ppm < 8 ppm
A 12 18 17 0
B 19 65 60 63
C 28 51 75 42
IEC SPECIFICATION 15 30
4
Partition coefficients and gas measured, the coefficients are column and the individual amounts
extraction needed to calculate the initial are defined by the strength of the
In dissolved gas analysis whether gas concentration in oil. The less detector signal as a function of
in laboratory or online, gases have gas is extracted, as with HS, the time (peak area).
to be extracted from the oil to more results are dependent on
take the measurement. The more calculations and thus coefficients. GC is not a fundamental analysis
complete the extraction, the less method where the retention
uncertainty there will be related The majority of analysis times or signal strength are
to concentration calculations. The laboratories and on-line DGA universal; it requires equipment-
extraction efficiency depends on devices use the HS method or a specific calibration. There are
the method used. For example, the derivative of it with a membrane or two different methods commonly
Toepler method has almost 100% tube, because it is less complicated used for GC calibration, traceable
efficiency, whereas in the worst and more cost efficient. However, reference gas mixtures and
cases HS can achieve less than very few take into account the gas-in-oil standards with known
30% efficiency. differences in partition coefficients gas concentrations. Calibration
between oils from different defines a unique retention time
In the HS method, the proportion sources, which can be a significant for each gas component, and
of gas extracted equals source of error. the peak areas from the detector
signal are proportioned to the gas
concentrations of the calibration
Gas chromatography
reference.
GC is a traditional method to
identify gases and measure
where VOIL is the volume of oil and The challenge with gas-in-oil
how much of them are in a gas
VGAS is the volume of gas phase in standards is that they use a
mixture. A gas sample is injected
the GC vial and K is gas-specific specific oil and the question
from a sample vial into a thin GC
partition coefficient. remains how representative it
column and pushed through by a
is in regard to the gas solubility
helium (He) carrier gas. Different
In the standard HS method, values (partition coefficients)
gas components are separated
the volume ratio in a GC vial is of oil samples from various
in the column by their molecule
typically 10:12. transformers, especially when the
size, and because the retention
HS extraction method is used.
time is component specific the
The relationship in concentrations Reference gases in calibration have
small molecules come out first
(C) between oil and gas phase the same challenge that analysis
and larger ones later. After the
is dependent on the gas-to-oil results are dependent on the
column, the gases go to detectors.
volume ratio in an extraction vessel partition coefficients of different
Gas identification is based on
(VGAS/ VOIL). gases.
their retention times through the
5
On the right is an example of
the effect of using the gas-in-oil
standard for GC calibration if the
specific partition coefficients of 12 ml A
6
period with a live transformer, for Measurement ranges more demanding if gas mixtures
example six months. This would Commercial online monitors have with an extremely high level of
also give a first indication of the varying specifications for their explosive gases need to be tested.
stability of the measurement. measurement ranges. Whether the Such facilities would require extra
At least three to five oil samples widest ranges are necessary or not safety measures to be taken, for
should be drawn simultaneously, can be evaluated by considering example to have ATEX-approved
preferably for two independent the likely concentrations of equipment in the gas-in-oil
laboratories who can supply the gases and the explosive limits of preparation.
uncertainty values for their own flammable gases, for example.
processes. Samples should be It is also a question of safety as The 90-percentile values from
taken throughout the whole test to whether monitors can really various sources show relatively
period, for example once a month. be tested at extremely high low values compared to specified
concentrations of explosive gases. measurement ranges. However, in
Just as an example, if testing H2 some rare cases extremely high
concentration of 20,000 ppm in concentrations have been reported
oil, one should use a gas cylinder for methane, ethane, and ethylene
with 36% hydrogen which is well in the case of a T3 fault in oil[6].
above its lower explosive limit (LEL Those are typically in transformers
4%). The situation becomes even with a smaller volume of oil.
Table 4 90-percentile typical values found in transformers that are operating normally[6, 7, 8].
Table 5 Examples of gas concentrations in oil and the required concentration in gas phase to prepare a gas-in-oil
standard. The lower explosive limit of the gases is also presented.
GAS GAS-IN-OIL CONCENTRATION, PPM GAS-IN-GAS CONCENTRATION, PPM LEL PPM (IN AIR)
(K AT +70°C, IEC 60567)
7
Comparing online monitor is possible if the methods used brochure 783, DGA monitoring
and laboratory DGA follow different standards. Factors systems[1]. The procedure
affecting uncertainties include: also includes an evaluation of
When evaluating an online
laboratory performance. It may
monitor by comparing it to lab • Calibration methods not be an ideal test description,
references, the quality of the
• Gas extraction methods but it is definitely the most
samples and the uncertainty of
comprehensive onsite evaluation
laboratory procedures must be • Gas partition coefficients
criteria published for online
taken into account. Furthermore, • Oil sample quality monitors by an independent
it is important to remember that • Human factors organization.
every analysis method, whether
• Reference standard used
laboratory or online monitor, has
Below is another example of how
its own uncertainties. These should
Unfortunately, there is no standard to evaluate a monitor. Instead of
be considered when comparing
to help in testing and evaluating looking at the readings at just
results and making conclusions on
the performance of online one point, the monitoring data
monitor performance.
monitors in the field. However, is evaluated over a long period.
the recent CIGRE working group In this case, there is just one
In conclusion, due to various
D1/A2.47 has published a detailed gas, methane, as an example.
uncertainties related to dissolved
procedure describing how such Vaisala OPT100 DGA monitor
gas analysis, whether on-line or
tests could be executed: Procedure data is plotted over 2.5 years
off-line, one should expect some
for evaluating the accuracy of gas with an accuracy specification
differences in results even if the
monitors and laboratory results of ±10%. Since the uncertainty of
sample and the sampling method
in Appendix F of the technical the laboratory was not known,
were ideal[1]. A significant deviation
±15% was used, based on the
average lab accuracy examples
published in IEC 60567[2]. In
order to compare a lab to an
online DGA, it is more relevant
to compare the trends than the
actual measurements, while
also considering a possible bias
between the two. If the trends
are similar and the areas with
uncertainties are overlapping,
one can conclude that the two
different methods are in broad
agreement.
Figure 5 Methane (CH4) data over 2.5 years from Vaisala OPT100 monitor References:
1 CIGRE Technical Brochure 783
and laboratory references. Monitor specification 10% plotted grey and 15% 2 IEC 60567 4th ed., 2011
uncertainty for laboratory (average[2]). 3 ASTM D3612
4 IEC 60567 3rd ed., 2005
5 CIGRE Technical Brochure 409
6 CIGRE Technical Brochure 771
7 IEEE C57.104
8 IEC 60599 3rd ed., 2015