Vlave Stem Leack Tightness Method PDF

European Commission
Community Research
BCR Information
Project report
Applied Metrology
Valve Stem Leak-Tightness

Test Methodologies
—
-
COMPETITIVE A N D SUSTAINABLE GROWTH

European Commission
ber information
APPLIED METROLOGY
Valve Stem Leak-Tightness Test Methodologies
PROJECT COORDINATOR: BHR Group Limited
PARTNERS: CETIM
Neles Automation
Chesterton
European Sealing Association
Association Française des Industries de la Robinetterie
Elf Antar
Inficen
Alcatel CIT
Contract No. SMT4-CT97-2158
Research Directorate General _
2000 EUR 19772 EN

EUROPEAN COMMISSION
Community Research
DG Research/H - Competitive and Sustainable Growth Programme
Contact: "Growth Infodesk" - European Commission, ruédela Loi, 200 (M075 3/62), B-1049 Brussels
Fax: (32-2) 296.67.57- E-mail: growth(fb,cec. eu. int - Internet: http//www.cordis.lu/growth
Published by the EUROPEAN COMMISSION

Research Directorate General
LEGAL NOTICE: Neither the European Commission nor any person acting on behalf of the
Commission is responsible for the use which might be made of the following information.
A great deal of additional information on the European Union is available on the Internet.
It can be accessed through the Europa server (http://europa.eu.int).
Cataloguing data can be found at the end of this publication.
Luxembourg: Office for Official Publications of the European Communities, 2000
ISBN 92-894-0502-3
© European Communities, 2000
Reproduction is authorised provided the source is acknowledged.
Printed in Belgium
Contents
ABSTRACT 1
1. INTRODUCTION 2
2. ISSUES 5
3. AIMS 6
4. METHODOLOGY 7
4.1 Structure 7
4.2 Preliminary survey of measurement methods 7
4.3 Scope and approach of experimental programme 8
4.3.1 Evaluation of measurement methods 8
4.3.1.1 Sniffing 8
4.3.1.2 The flush method 9
4.3.2 Different gases at room temperature 10
4.3.3 Different gases at elevated temperatures 11
5. FLUSHING: EVALUATION 12
5.1 Characterisation 12
5.2 Initial evaluation tests 13
5.3 Confirmatory tests 13
6. RELATIONSHIP BETWEEN PPMV AND LEAK RATE (SAME GAS) 15
6.1 Sniffer evaluation tests 15
6.2 Discussion of sniffer evaluation tests 16
6.3 Power law correlation or "sniffing factor" approach? 18
7. RELATIONSHIP BETWEEN LEAK RATES OF DIFFERENT GASES 21
7.1 Correlation or prediction? 21
7.2 Room temperature experiments 22
7.2.1 Power law correlation approach 22
7.2.2 Theoretical predictive relationships _ 24
7.3 The effect of temperature 28

7.3.1 Hypothesis 28
7.3.2 Leakage mechanismforhelium 28
8. QUALIFICATION TEST MEASUREMENTS AND SITE PERFORMANCE 31
8.1 Helium leakage to VOC leakage 31
8.2 VOC leakage to VOC ppmv 31
8.3 Results 32
9. RELATIONSHIP OF OA TESTS TO QUALIFICATION TESTS 36
9.1 Relationship between ppmv of helium and leak rate thresholds 36
9.2 Establishment of appropriate threshold value 36
10. CONCLUSIONS 38
11. REFERENCES 40
APPENDIX 1 - GLOSSARY OF TERMS 42
APPENDIX 2 - UNITS 44
APPENDIX 3 - ADAPTATION OF EPA METHOD 21 FOR HELIUM SNIFFER

MEASUREMENTS 45
ABSTRACT
The emergence of standards on leak-tightness of industrial valves has given rìse to a set of
problems associated with the way in which leak-tightness is both measured and expressed.
Issues surround:
• The specified gas

End users prefer a leakage targets in gases representative of the duty. Valve manufacturers
and test houses prefer the use of helium as a safe, detectable, inert test gas, widely used
for leak testing in many other contexts.
• The measurement method

Many end users prefer a leak-tightness result expressed in terms of ppmv measured by
sniffing, since this is the format of Environmental Protection Agency (EPA) targets in the
USA and is widely used across the world for on-site leakage detection and repair (LDAR)
programmes.
Unfortunately, ppmv is a not a measure of leakage rate, but rather provides an indication of
leakage severity. Thus, the requirement is lor means of "translating" both between ppmv and
leak rate and between leakage of one gas and leakage of another under similar conditions.
"Translation" between ppmv and leakage is usually accomplished by means of empirical power
law correlations. However, due to the wide range of data sources on which they are based,
scatter in the data is very broad, rendering this approach, as it stands, unsuitable for valve
qualification and QA test standards.
"Translation" between leakage rates of different gases can either adopt a similar empirical
approach or, alternatively be based on predictive relationships derived from an understanding
of which leakage mechanism predominates. Until now, little directly relevant work has been
undertaken in this area.
The work reported here provides relevant technical data and analysis to help resolve these
issues by:
• investigating measurement methods and recommending means by which scatter in the

relationships between ppmv and leak rate can be dramatically reduced
·. evaluating measurements of leakage of different gases under similar conditions to identify

means of predicting leakage of various gases from measurements of helium leakage.
Experimental work was concentrated on valves representative of typical volatile organic

compound (VOC) duties over a range of sizes and types (but particularly 4" Class 300 gate
valves) with several different packing types (but mostly graphite) over a range of leakage rates
representative of this duty.
Conclusions are offered in Section 10.

1. Introduction
Increased concerns over environmental issues have lead to existing legislation in the USA and
current and forthcoming E.C. directives on air quality. These have focused attention on fugitive
emissions of Volatile Organic Compounds (VOC) from chemical and petrochemical plant, and
leakage from particular sources (1-5). Site surveys have indicated that the largest contribution
to plant VOC leakage comes from valves (6), and particularly from their stem seals (7). In an
attempt to: reduce product loss; comply with plant emission targets; and rationalise procurement,
plant operators are increasingly insisting on procuring valves demonstrating acceptable leakage
performance. For a given valve model, their particular concerns (8) are, to ensure:
1. adequate leakage performance after a representative number of mechanical and thermal

cycles with a particular valve;
2. an acceptably low percentage of installed valves exceeding the leak-tightness

classification threshold.
Consequently, relevant standards are currently under development (9,10) covering valve leak-
tightness qualification and quality assurance testing. These define (11):
• test methods and procedures
• leak-tightness criteria
• measurement methods
This work concerns measurement methods for qualification and QA tests.
The work described in this report was undertaken in a European collaborative project. The
financial support of the European Commission is gratefully acknowledged by the partners, who
were:
Coordinator: BHR Group Limited

Contacts: Simon Leefe, Mike Butcher
The Fluid Engineering Centre
Cranfield, Bedfordshire, MK43 OAJ
United Kingdom.
Tel. (Int+44) 1234 750422
Fax. (Int +44) 1234 750074
Email: [email protected], [email protected]
Web: www.bhrgroup.com
Contractors: CETIM
74 Route de la Joneliere
BP 82617, Nantes, 44326 Cedex 03
France
Fax. (Int + 33) (0)2 51 86 00 73
Contacts:
Yves Birembaut (Int +33) 2 40 37 35 82
E-Mail: [email protected]
Thierry Ledauphin (Int +33) 2 40 37 36 06
E-Mail: [email protected]
Emmanuel Sauger (Int +33) 2 40 37 35 90
E-Mail:[email protected]
Web: www.cetim.fr
Neles Automation, Field Control Division
Contact: Jari Tammela
Tulppatie 7A, PO Box 310, FIN-00811 Helsinki,
Finland
Tel. (Int +358) 20 483 5847
Fax. (Int +358) 20 483 5304
Email: [email protected]
Web: www.nelesautomation.com
Chesterton Industries BV
Contacts:
Ian Forsyth
32 Rue Joseph Hansen
L-1716 Luxembourg
Tel. (Int +352) 021 266836
Fax. (Int +352) 26202087
Hans Dekker
Tel. (Int+353) 87 4129853
Fax. (Int +353) 875 4129853
Web: www.chesterton.com

Contact: Brian Ellis
Bowerham House, The Grove, Lancaster, LA1 3AL
United Kingdom
Tel. and Fax. (Int +44) 1524 844222
Web: www.europeansealing.com
AFCP-AFIR
Contact: Georges Pichard
45 Rue Louis Blanc 924000, Courbevoie,
PARIS la Défense, 92038 Cedex
France
Tel. (Int+33) 147 17 62 98
Fax. (Int+33)1 47 17 63 00
Web: www.afcp-afir.org
Associated Elf Antar France

Contractors: Contact: Philippe Grosbois
Service Inspection, Raffinerie de Feyzin, BP6
69551 Feyzin Cedex
France
Tel. (Int +33) 4 72 09 51 69
Fax. (Int +33) 4 72 09 53 24
Infi con Ltd
Contact: Marc Wakelin
16 Waterside Way, Plough Lane, London, SW17 OHB
United Kingdom
Tel. (Int +44) 208 971 7050
Fax. (Int +44) 208 971 7005
Web: www.inficon.com
Alcatel CIT
Contact: Jean-Paul Johner
98av de Brogny BP2069, 74009 Annecy CEDEX
France
Tel. (Int+33) 5 56 58 72 88
Fax. (Int+33) 5 56 58 26 07
Issues
Historically (largely due to on-site leakage detection practice), the severity of valve stem leakage
has been assessed in terms of concentration near the leakage source, measured by a "sniffer"
device. Concentration is expressed in parts per million by volume or ppmv - often simply
designated ppm. Whilst this is not actually a measure of leakage, it is widely misunderstood to
be so, and many end-user valve test protocols specify it, because sniffing is relatively quick and
simple (hence low cost). Therefore, there are essentially two approaches to specifying leak-
tightness targets: ppmv and leakage rate (12). There are also two classes oftest gas: a safe
gas for testing purposes (helium is accepted as the most suitable) and VOCs representative of
the intended duty. Thus there are four possible combinations as the basis of any leak-tightness
test. The conflicting requirements in relation to these possibilities are represented in Fig. 1.
ppmv leak rate leak rate ppmv

Helium Helium VOC VOC
Most convenient Stipulation in Required for Preferred by many

for valve current draft of compliance end-users
manufacturers for ISO standard for with TA-Luft Compatible with
QA or type tests qualification tests EPA 21
Fig. 1 - Four possible combinations of test gas and leak-tightness specification:

conflicting requirements
For a standard to gain widespread acceptance, it must:
• be relevant to end-users' needs;
• adequately address regulatory authorities' concerns over VOC leakage;
• recognise legitimate issues over cost and safety of testing.
At present, no single combination of test gas and measurement method can satisfy all three
requirements. If there were a reliable means of translating between the basic measurements,
these conflicting requirements could be simply resolved by taking measurements in the most
convenient manner, and "converting" the results to any other desired form. For example, a
helium leak rate measurement might be taken to satisfy the ISO standard, and the result
"translated" to an equivalent ppmv of methane to satisfy an end-user's requirements.
Unfortunately, however, a straightforward conversion (as if between units, for example) is not
currently possible (13).
6
3. Aims
In view of the foregoing, the overall aims of the project were:
1. to establish measurement practices and procedures which improve accuracy and

repeatability and, crucially, which avoid ambiguity
2. to clarify why simple "conversions" are not possible between results using different
measurement approaches and test gases
3. to suggest, if possible, means of "translating" between the measurement possibilities

identified in Fig. 1 and evaluate associated error and scatter
4. Methodology
4.1 Structure
The programme of work described herein was broken down into three Work Packages. Each
involved a combination of theoretical, experimental and interpretative work. Based on a sensible
division of experimental content, they set out to examine, respectively:
• measurement methods
• relationships between results using different measurement approaches and different test
gases at room temperature
• the implications for these relationships at elevated temperatures
Since these Work Packages are closely related in their implications, a more interpretative
approach will be adopted here, to their reporting. Following a brief discussion of candidate
measurement methods, the scope and approach of the experimental programme are explained
in this Section. Then results are reported and analysed in subsequent Sections, organised
around a series of relevant issues, in some cases drawing on results from more than one Work
Package.
4.2 Preliminary survey of measurement methods

A preliminary survey of candidate measurement methods was conducted. This is reported
more fully in ref. 12, but is summarised in Table 1.
Method Summary
Sniffing • In demand from end-users(cte facto standard as site method)
• Quick and simple
• Not a measure of leak rate, but may correlate with leak rate
• Measurement prone to scatter
Vacuum method • Accurate
• Unambiguous
• Can be cumbersome to set up
• Possible problems with measurements from valves at elevated
temperature
• Rarely suitable for VOC measurements
Flushing • Un-tried as a localised technique
• Shows promise in theory
• Some practical issues to be evaluated
• Should be workable at elevated temperatures
• Suitable with VOCs (with appropriate flush gas)
Rate of increase of • Avoids the use of flush gas
concentration in bag • Should be suitable at elevated temperature
• Rigid "bag" results in nonlinear relationship between leak rate and rate
of increase in concentration, therefore not suitable
• Flexible bag unsuitable, because initially enclosed volume needs to be
known
Decay of pressure in • Conceivable as a method for a seal test fixture
test valve • Unsuitable for use on an industrial valve of typical size
• Cannot distinguish source of leakage (stem, bonnet, end flanges or test
fittings)
Bubble capture • Possible for room temperature QA testing on smaller items
• Not suitable at cryogenic temperatures
Table 1
8
4.3 Scope and approach of experimental programme
4.3.1 Evaluation of measurement methods
Following the survey of candidate methods (Table 1) it was decided to use the "vacuum method"
as a reference for the determination of leak rate, and to concentrate on the evaluation of
"sniffing" and the "flush method" (see Fig. 2)
Valve To detector
stem
b) vacuum method
To detector
c) flushing
Fig. 2 - Three measurement methods used
4.3.1.1 Sniffing
As already mentioned, sniffing does not provide a direct measure of leakage rate, but may be
correlated with it. Whilst some sniffers read out in flow rate units and others in concentration
units (see Section 6.2), results of the sniffing tests are expressed in terms of ppmv, to avoid any
possibility of confusing a sniffer reading with a leakage rate. The focus of the investigation was
the quantification of the scatter in the correlation between the sniffer reading and the leak rate.
A series of tests was conducted, in which the following factors were systematically varied:
• detector type
• stem diameter
• valve type
• working environment
• operator
• packing type
Each factor was investigated in a test series, in which a leak rate was set by gland and/or
pressure adjustment, then maintained constant. A number of repeat readings (typically 10
repeats) of the corresponding sniffer measurement were then taken. The leak rate was changed
and re-stabilised, then repeat readings of the corresponding new sniffer measurement were
taken. This procedure was repeated at different leak rates. Next, the factor that was being
investigated in the particular test series was changed, and the procedure repeated. The scope
oftest variables is summarised in Table 2.
9
Test gas Mostly Helium, (plus some methane in "Packing type" test series)
Leakage rate range ir/'toirratm.cnv'.s" 1
Valve types Rising stem and rotary (see note 1 )
Valve sizes 2", 3", 4", 6" nominal pipe size (see note 1)
Packing types PTFE and graphite (4 to 7rings),braided and V-ring, some with end rings
Detector types Helium mass spectrometer for "vacuum method" leak measurement
Helium sniffers: 3 models in "detector type" test series, but one more at a different
site in another test series;
Methane sniffers: 1
Wind speeds 0, 0.5,1.0 and 1.5 m.s'1
Operators 3 in "operator" test series, but 2 more at other sites for other test series
Note 1:4" Class 300 gate valveforall tests except "valve type" and "stem size" test series
Table 2 - Scope of evaluation tests for sniffing
4.3.1.2 The flush method

This is actually a class of measurement methods which are characterised by the leakage stream
being captured in an enclosure and carried to a detector by another gas which is blown or
sucked through the enclosure (see Fig. 3). In the "blow-through" variants, a pure flush gas is
forced through the system and the outlet stream concentration is sampled with a sniffer. In the
"suck-through" approach, the low is provided by the detector's suction pump.
Concentration, C
JL
Pressure
Flush gas regulator Detector
supply Flow rate Qp
measurement
Flow rate control
a) "Blow-through approach with pure flush gas
Qf + Q, = Qp
b) "Suck-through" approach with ambient airas flush gas
Fig. 3 - Basic variants of the flush method

10
In initial evaluation tests, variants of the flush method were tested for accuracy against
measurements taken by the vacuum method, as reference with no adjustment to the valve
between the two measurement methods. The impact of factors thought likely to affect accuracy
was also investigated. The scope of these tests is defined in Table 3. A very limited data set
was produced, but sufficient to indicate the most accurate variant for subsequent confirmatory
tests, in which a larger data set was produced. The scope of these tests is defined in Table 4.
Valve type 4" Class 300 gate valve

Test gas Helium
Flush gas Nitrogen
Leakage measured Stem/gland follower leakage only
Leak rate range lO^tolOâtm.cm^.s'1
Flush gas flow rate ("blow-through" variant) 10 to 70 ml.min'1 (0.17 to 1.17 atm.cnV.s"1)
Detector probe flow rate 40 ml.min"1 (0.67 atm.cm^.s"1)
Factors evaluated "blow-through" approach:
• exhaust line concentration measurement location:
- tee detector into exhaust line
- sniff exhaust line exit
• effect of poor seal between valve and leakage
encapsulation arrangement
"suck-through" approach
• feasibility of using bottled flush gas
• effect of flush inlet arrangement when flush gas is
surrounding air:
- clean air from outside laboratory
- local air near test valve
Table 3 - Scope of flush method preliminary evaluation tests

Test gas Helium
Flush gas Nitrogen
Leakage measured Total stem seal leakage
Leak rate range 1 χ 10'J to 6 χ 10"J atm.cnr'.s'1
Flush gas flow rate 350 to 1000 ml.min1 (5.8 to 16.7 atm.crrf.s'1)
Detector probe flow rate 70 ml.min'1 (1.17 atm.crrf.s'1)
Table 4 - Scope of flush method confirmatory tests
4.3.2 Different gases at room temperature

In order both to establish the quantitative relationship between leak rate of one gas and that of
another under the same nominal conditions, and to identify the leakage flow mechanism, the
following approach was adopted. Gland load was set such as to provide one of three leakage
levels. Helium was supplied at six increasing steps of pressure and the leakage measured at
each step. Subsequently, the same valve (with no adjustment of gland load) was supplied with
methane at the same set of pressure steps, and the leakage measured at each step. To
evaluate the influence packing stress level, the same sequence of measurements was repeated
on the same valve with the same two gases at a higher level of gland load. The whole
procedure was also conducted on a second valve with helium and ethane. The scope of these
tests is defined in Table 5. In order to provide additional confirmatory data on the relationship
between ppmv readings and leak rate (both in helium andjn VOCs), a sniffer-based
measurement was taken for each leakage measurement in this test sequence.
11

Stem seal Inconel-reinforced braided graphite
Gland load range (nominal packing stress) 16 to 42 M Pa
Test gases Helium, methane, ethane
Pressure range 2 to 46 bar gauge
Leakage measurement method Flush method (total stem seal leakage)
Flush gas Nitrogen (for helium)
Argon (for VOCs)
Flush gas flow rate 700 to 1000 ml.min'1 (11.7 to 16.7 atm.ernes'1)
Sniffer measurement methods EPA Method 21 (for VOCs)
Modified EPA Method 21 (for helium)
Helium detector probe flowrate (flushing and sniffing) 70 ml.min'1 (1.17 atm.cnv'.s"1)
VOC detector probe flowrate (flushing and sniffing) 1000 ml.min'1 (16.7 atm.cm .s"1)
Table 5 - Scope of room temperature tests on different gases
4.3.3 Different gases at elevated temperatures

Practical problems prevented the same test facility being used for both helium and hydrocarbons
at elevated temperature. This, together with the addition of temperature into the list of test
parameters necessitated a different approach to that adopted for room temperature tests. Here,
a matrix of gland load, temperature and pressure conditions formed the basis of tests in helium
in the laboratory, whilst selected conditions from this matrix were reproduced in an enclosed
area on site, with different VOCs, in the same valve. This way, comparisons could be made
between predicted and measured VOC leakage as a means of testing various proposed
correlation rules.
The test sequence for the helium tests involved: first setting a gland load and temperature whilst
stepping up through four pressures, measuring leakage rate at each step, then repeating this
sequence at each of four temperatures, then repeating the entire sequence at each of three
gland loads. The VOC tests, conducted for each of three different hydrocarbons, involved a
similar sequence, but at fewer combinations of pressure, temperature and gland load. The
scope of these tests is defined in Table 6. In order to test proposed relationships between VOC
leak rate and ppmv, a sniffer-based measurement was taken for each VOC leakage
measurement.

Packing type Inconel-reinforced braided graphite
Test gases Helium, methane, ethane, propylene
Temperature range 20 to 400 °C
Pressure range 9 to 30 bar gauge
Gland load range (nominal packing stress) 20 to 60 MPa
Helium measurement method Vacuum method
VOC measurement method Flushing
Flush gas Air
Flush gas flow rate 10 l.min'1
VOC sniffing method EPA Method 21
VOC detector probe nominal flow rate 1000 ml.min'1 (16.7 atm.cnf.s' 1 )
Table 6 - Scope of elevated temperature tests on different gases
12
5. Flushing: evaluation
5.1 Characterisation
The expected behaviour of the flush method was analysed (12). For best measurement
accuracy, detector probe flow rate must be several orders of magnitude greater than the
maximum anticipated leakage rate. If the "blow-through" approach is used, flush gas flow rate
should be substantially greater than the detector probe flow rate. Under these ideal conditions,
the following relationship:
Q I,indicate J ~ ^ Q f (1)
where
Q leakage rate
C measured concentration
Qf flush gas flow rate
For the "suck-through" approach, flush gas flow rate is determined by the rate at which the
detector pulls air through the system from the surroundings. This may be assumed equal to the
probe flow rate, Qp.
Predictable deviations from this relationship arise from air dilution when the flush gas flow rate
is less than the probe flow rate, and when the leakage flow rate becomes a significant fraction
of the probe flow rate. These deviations are shown in Fig. 4.
1.1
/ Q,/Qp = 10"3
/
Qi/Qp = 10'2
/ , /
SI 0.9 — Qi/Qp = 10' 1
Qi/Qp = 1
σ 0.8
0.7
~y^
0.6
Qf/QP
Fig. 4 - Expected behaviour of the flush method
Here, the horizontal axis is flush gas flow rate, normalised by probe flow rate. The vertical axis
is the leak rate as indicated by equation 1 normalised with respect to the actual leak rate. For
high accuracy, this value should equal 1. Therefore Fig. 4 shows that a well-designed flush
measurement set-up must use a flush gas flow rate greater than the detector probe flow rate.
13
It must also use a detector whose probe flow rate is at least two orders of magnitude greater
than the maximum anticipated leak rate.
5.2 Initial evaluation tests
The rationale and scope of these tests is outlined in Section 4.3.1 and Table 3. Results were
shown in ref. 12 in a format that makes a comparison with the expected behaviour of Fig. 4.
They are summarised in Table 7.
Method Accuracy Comment

"Blow-through" with Tails off when flush Accuracy improved by sampling
flush gas from bottled gas flow rate drops below concentration in the flush exhaust line
supply probe flow rate. Good for rather than that emerging from its exit
higher values of flush gas flow Quality of seal between leakage
rate encapsulation enclosure and leakage
source does not significantly affect
accuracy unless flush gas flow rate is
around or below probe flow rate.
"Suck-through" with Method unworkable
flush gas from bottled
supply
"Suck-through" with air Better at lower leakage rates Air from near leakage source (despite
as flush gas but not as accurate as "blow- contamination with leakage gas) did
through" method not significantly affect accuracy.
Table 7
The relative paucity of data precluded quantification of accuracy and scatter with meaningful
statistical analysis. Comments on the results should therefore be treated with caution. For
example, recent discussions outside the SMT project have suggested that better results than
indicated here can be obtained by the "suck-through with air asflushgas" method (14).
5.3 Confirmatory tests
Since the vacuum method cannot be usedforVOCs, a reliable alternative had to be used for
VOC leak rate measurement elsewhere in the research project. "Blow-through" flushing with a
bottled flush gas was identified above as the most accurate alternative and therefore as
potentially suitable. Additional confirmatory tests were therefore conducted, in helium (as
detailed in Section 4.3.1 and Table 4), to enable quantification of error against the vacuum
method, as reference. The results are summarised in Fig. 5.
The mean error was approximately 25%, but this was heavily biased by larger errors at the
higher leak rates. Further investigation suggested instrument problems associated with the
vacuum method readings at the highest leak rates. For this reason, the median error from the
51 observations was thought to be a better indicator of accuracy. This was 10.4%, confirming
that the flush method is a safe method to use for the range of leak rates studied here.
14
error
Fig. 5 - Statistical distribution of error

15
6. Relationship between ppmv and leak rate (same gas)

6.1 Sniffer evaluation tests
Results of the sniffing evaluation tests are shown in graphical form in Figs. 6 through 11 and are
summarised in Table 8.
10000
1000000 J
Detector A
I 100000 Χ—""* * »0 m/s wind speed
1000
9- 10000 ■ Detector Β > *9^^ Ι ■ 0.5 m/s wind speed
E 1.0 m/s wind speed
•a α
Detector C α. 100
■o
I · 1.5 m/s wind speed
(Λ
M • - ISO Class D 1 ñ — 0 m/s (best fit)
0) (Λ 10
E re 1 ^-—j-· 0.5 m/s (best fit)
• · ISO Class C α
Ε
1 • "", · · 1.0 m/s (best fit)
1.0E-04 1.0E-03 1.0E-02 1.0E-01 • - 1 . 5 m/s (best fit)
leak rate (atm.cm .s )
•
s —
■
01 · ,
1.0E-03 1.0E-02 1.0E-01
Fig. 6 - Effect of detectortype: leak rate (atm.cm'.s 1 )
helium Fig. 7 - Effect of wind speed:

helium, detector A
♦ Die-formed braided 10000 ♦ 19-20 mm stem dia.
100000 graphite
■ 3+2 Graphite Rings 1 ■ 25-26 mm stem dia.
1000
ί*
|10000 Wedge Graphite Q.
D. 32-35 mm stem dia.
O.
α Ό
£ 1000 Ss
• Die Formed braided
PTFE
100 19-20 mm stem dia.
3
ΙΛ ι
— Die-formed braided
(Λ
ro best fit
ω
ψ
ro — 25-26 mm stem dia.
o graphite (best tit) 10
ν
E 100 Wedge graphite (best best fit
fit) — 32-35 mm stem dia.
10
— Die-formed braided 1 best fit
PTFE (best fit)
1.E-04 1.E-03 1.E-02 1.E-01 1.E+00
1.E-05 1.E-04 1.E-03 1.E-02 1.1 - Power (3+2 Graphite
leak rate (atm.cm3.s'1) Rings) leak rate (atm.cm3.s ')
Fig. 8 - Effect of packing type: Fig. 9 - Effect of stem diameter

helium, detector Β helium, detector D
10000 100000 η ♦ Operator 1
> I ' ♦ rotary stem (20- ■ Operator 2

E 1000 > 10000
35 mm dia.) E
α ■ rising stem (19- Q.
Q. Operator 3
a. 32 mm dia.)
£
•a 100 ■O
— rotary stem best £0) 1000

1Λ * — Operator 1
fit ΙΛ
ro (best fit)
ro »
Ξ
— rising stem best
fit
v
E 100 I - Operator 2
(best fit)
Operator 3
10 .—^J (best fit)
1.0E-04 1.0E-03 1.0E-02 1.0E-01
1 E-05 1.E-04 1.E-03 1.E-02 1.E-01
leak rate (atm.cm3.s 1)
leak rate (atm.cm3/s)
Fig. 10 - Effect of valve type:
Fig. 11 - Effect of different operators:
helium, detector D
helium, detector Β
16
Factor Effect on ppmv - leak rate Implication or comment

correlation
Stem No significant effect over range Consistent with localised leakage or high probe
diameter of sizes investigated uptake. Possibility of systematic effect at larger
stem sizes should not be ruled out.
Valve type Small systematic effect: rising Consistent with defined leakage paths along axial
stem gives higher ppmv values scratches. "Sniffing distance" (see Note 1, below)
for given leakage rate than is a valve constructional factor which may
rotary stem influence this result
Packing type Marked effect higher Cause demonstrated to be more localised leakage
measured ppmv values with with PTFE giving higher local peaksforthe same
PTFE packings compared with total leakage rate (The sniffer method protocol
graphite for the same level of stipulates the recording of the maximum
actual leakage measured ppmv value as the sniffer is moved
NOTE: this does NOT imply around the leakage source)
that PTFE leaks more than
graphite
Detector type Major first order systematic Dependence on probe flow is not simple or
effect related to probe flow rate deterministic. However, quoting probe flow rate
with any ppmv measurement should aid
interpretation. Introduction of empirical "sniffing
factor" could provide a rational basis for
conversion between ppmv and leak rate, but with
a significant margin of error (see Section 6)
Operator No significant effect observed But note: strict experimental procedures followed
and measurements taken by experienced
technicians in reputable laboratories
Working Major first order systematic For QA or qualification tests, air currents can be
environment effect relating to dilution by controlled to near zero. However, some
local air currents. Order of ventilation is required to prevent build-up of
magnitude impact on significant background concentration.
correlation results from local
air speed as low as 0.5 m/s
(below walking pace).
Note 1 : An additional factor determined by valve construction, but not originally proposed when this
project was conceived, was termed the "sniffing distance" and could prove to be significant. It is
the distance between the top of the outermost packing ring (where leakage emerges from the seal)
and the point of measurement at the gland follower interface. For the gland follower/stem
interface, this distance is simply the axial length of the gland follower. For the gland
follower/stuffing box interface, it depends on the depth of penetration of the gland follower into the
stuffing box. The idea is that if leakage through the seal is localised at a "hot spot", the greater the
sniffing distance, the more opportunity the concentration has to even out, by diffusion and
dispersion. This would result in a decreasing ppmv reading as sniffing distance increases for the
same actual value of localised leakage.
Table 8
6.2 Discussion of sniffer evaluation tests
it should be clear from these results that there is no general or universal correlation between
sniffed concentration (ppmv) and valve stem leak rate. However, much can be said about the
reasons why this is so. These lie in an appreciation of what a sniffer actually measures.
Consider the following:
1. Only a fraction of the valve leakage finds its way into the probe: this fraction is not known a
priori and is not a quantity that is easy to predict. This is equally true of sniffer-based
17
detectors that measure flow rate (such as a mass spectrometer in sniffer mode) and those
that measure concentration.
2. A concentration-based detector measures concentration of the test gas in the probe: for a
given flow rate oftest gas into the probe, the balance of the total flow is made up of ambient
air, which provides more or less dilution. The measured concentration is therefore also
dependent on the total gasflowrate drawn into the detector.
A flow rate-based sniffer detector will read out directly in units of flow rate such as atm.cm3.s'1.
The reading, however, is not a measure of the leak rate, but rather of the probe uptake, Qtp, of
the leaking gas. This will only be some fraction, η, of the test gas leakage rate, Q,,|. Thus:
&,=[-W (2)
W
gives leakage rate from test measurement.
The quantity η, we have provisionally denoted "sniffing factor". It is not a constant: in the tests
described in Section 6.1, above, the value of η was found to range between 0.1% and 35% over
three detectors and a range of packing types, valve types and sizes. It also appears to depend
significantly on the leakage rate being measured. These dependencies are the reason both for
the nonlinearity of correlations between ppmv and leak rate (which are usually expressed as a
best fit power law) and for their inherent unpredictability.
In a concentration-based sniffer detector, the expression relating concentration, C, to the flow

of test gas into the probe, Qt,p and the total probe flow rate, Qp, is (from continuity
considerations):
C =^ (3)
Rearranging and expressing concentration as ppmv:
Qlp=QpA0^.ppmv (4)
The quantity Qp is a constant for a given detector, and is directly measurable. This quantity is
responsible for the major dependence of measured ppmv on detector type for a given leakage
demonstrated in Fig. 6.
Combining this deterministic relationship with the empirical relationship of equation 2 gives:
f
α.,=ιο- Q^ ppmv (5)
7
Comparing equations 2 and 5, we can see that to obtain leakage rate from a concentration-
based sniffer detector, two factors (probe flow rate and sniffing factor) are required, whereas to
obtain leakage rate from a flow rate-based sniffer detector only the sniffing factor is required.
With the foregoing clearly understood, the effects of the factors investigated as possible causes
of scatter can be readily explained. As just discussed, the first order effect of "detector type" is
18
explained in relation to the probe flow rate. All the other factors considered have a greater or
lesser effect on the fraction of the leakage flow rate drawn into the sniffer probe.
Clearly, the ventilation of the working environment has a huge effect, because significant air
currents around the valve blow the leaking gas away and predominate over any probe suction
currents except those extremely close to the probe tip. Therefore only a tiny fraction is drawn into
the probe. This is illustrated in Fig. 12.
120%
wind speed [m.s ']
Fig. 12 - Impact of wind speed on sniffer readings from the

same leakage source
The "sniffing distance" effect mentioned in note 1 to Table 8 and arising from the "valve type"
factor, is explained in terms of the dispersion of test gas leaking from a local "hot spot". The
greater the "sniffing distance" the more test gas will escape to atmosphere and the smaller the
fraction reaching the probe.
The "packing type", we saw influenced whether leakage was localised or uniformly distributed.
Where it was more localised, a greater fraction is drawn into the probe.
6.3 Power law correlation or "sniffing factor" approach?
The conventional approach is the use of power law correlations to estimate a leak rate from a
measured ppmv value. Whilst a large body of empirical data is available to support such
correlations, the fact that it comes from such a wide range of gases, detector types and working
environments (most of it is site data), means that scatter is large. To illustrate this point, let us
consider the entire data set arising only from the experiments described in Section 6.1. This is
illustrated in Fig. 13. Fig. 14 shows the spread of data taken with just one detector at zero wind
speed over a range of packing type, valve type and size. Comparison shows that the 95%
confidence interval on the power law correlation can be reduced from a factor of 260 to a factor
of 3.4 above and below the line of best fit.
19
1000000 -r
> 100000
Ξ
a.
o.
■o
10000 -
π
o
E 1000 -
100
0.00001 0.0001 0.001 0.01 1.0E-04 1.0E-03 1.0E-O2 1.0E-01 1.0E+00
3 1
leak rate (atm.cm3.s ') leak rate (atm.cm .s )
Fig. 13 - En tire data set with 95%

confidence in terval in dicated Fig. 14 - all data for only detector
"A" at zero wind speed
Further data obtained from the tests described in Section 4.3.2 and Table 5 show that this can
be still further improved when just one valve type and size and packing type are involved (as,
for example, in a QA test). This is illustrated in Fig. 15, in which the 95% confidence interval
is reduced to a factor of 2.0. This probably represents the best achievable repeatability with a
correlation approach, but is obtained at the e>pense of generality.
Helium test data
Gland load 2 (2 valves)
Gland load 3 (2 valves)
"Relationship based on
126907X1 average sniffing factor
0.9545 '95% confidence upper
limit on power law
0.0001 0.001 0.01 01 correlation
'95% confidence lower limit
leak rate (atm.cm .s' ) on power law correlation
Fig.15 - Helium data for one valve type and size, one
packing type, one detector, zero wind speed
Note that the exponent of the power law correlation, indicated on Fig. 15, is very close to 1,
suggesting near proportionality between ppmv and leak rate. This supports the notion of
"sniffing factor" discussed above. Following this observation, an average "sniffing factor" was
calculated for all helium test data using this detector (12% in this case). Using this detector's
probe flow rate and the average "sniffing factor", the relationship between ppmv and leak rate
given by equation 5 is also plotted on Fig. 15. It is almost indistinguishable from the power law
correlation. This is to be expected, since it is derived from the same well-specified data set.
However, it illustrates the use of a relationship based on sniffing factor as an alternative to an
empirical correlation.
20
A better indication of the more general usefulness of the sniffing factor approach may be
obtained from the zero wind-speed data derived from the more wide-ranging experiments
described in Section 6.1.
By comparing measured leak rate with leakage calculated from the sniffer-based ppmv reading
and the sniffing factor averaged across all zero wind-speed data for that sniffer, a fuller picture
can be built up of the scatter associated with this approach. This is illustrated in Fig. 16. The
location of the mean value very close to 1 reflects the accuracy of the average data, but the wide
scatter band (95% confidence interval represents a factor of about 20 around the mean) is less
encouraging. However, this needs to be compared with the scatter about the "best fit" power law
correlation derived from the same data set. This is illustrated in Fig. 17, where the 95%
confidence interval is a factor of 74 either side of the power law curve. Thus, by explicitly
allowing for probe flow rate, the use of the sniffing factor approach has reduced the 95%
confidence interval by a factor of nearly 4.
1000
« detector 1
■ detector 2
jt 100 - * detector 3
ra • detector 4
m^•■yljfirfrfi
St
•Q
E 10
3
1Λ
ra
ω
S
2
JÉ 0.1 -
ra
_ω ■h
■o
O . _ 95% confidence
> 0.01 -
'C
ω interval
■α
0.001 1 1 1 1 1
1.0E-05 1.0E-04 1.0E-03 1.0E-02 1.0E-01 1.0E+00
leak rate (atm.cm 3 .s ')
Fig. 16 - Accuracy and scatter of leak rate derived from

sniffing factor averaged across sniffer evaluation test data
10000000-t
All zero wind

> speed data
E
a. - Upper 95%
Q.
"O confidence limit
Φ
L·. - Lower 95%
3
ΙΛ confidence limit
03
O
— Power law
Ξ
correlation
1.E-05 1.E-04 1.E-03 1.E-02 1.E-01
leak rate (atm.cm 3 .s' 1 )
Fig. 17 -Sniffer evaluation test data, all zero

wind-speed helium data (four detectors)
21
7. Relatio
n ship between leak rates of different gases
7.1 Correlatio
n or prediction?
As with the relationship between measured ppmv and leakage rate, there are two approaches
to the relationship between leakage rates of different gases under the same conditions: empirical
correlation or theoretical prediction. Correlation (again, usually a power law relationship) has the
advantage of being based on real empirical data, but suffers from two main disadvantages in
comparison with predictive models:
1) As more data is obtained from different sources a multiplicity of correlations are published.
This risks no single relationship gaining widespread acceptance.
2) It does little to further any understanding of the physical processes underlying the correlation,
leaving the approach prone to wide scatter, whereas theoretical, predictive models, when
validated against real experimental evidence, can help suggests ways of improving
accuracy.
Previous work on gaskets and packings (15, 16, 17,18) suggests that, at the level of leakage
rate of interest in this study, the governing mechanism is either viscous laminar flow, molecular
flow or, in the intermediate or transitional regime, a mixure of the two.
A theoretical approach can be developed by considering the governing equations for either
laminar or molecular flow along a typical leakage channel of length L and "diameter" D. (In
practice there will be a statistical distribution of channel lengths and widths.) The flow behaviour
depends on the Knudsen number, Kn, which is the ratio of channel width, D, to molecular mean
free path, λ. When K n>100, the molecular mean free path is short compared with channel
dimensions, so gas molecules are more likely to collide with each other than with the channel
walls: viscous effects predominate and the flow regime is laminar. Here the volumetric flow rate,
Qiam of gas of viscosity, μ, is given by:
Q,am=^-iP.2-P^ (6)
25ο.Ζ,.μ
where Pi and P2 are the upstream and downstream absolute gas pressures, respectively.
When Kn<0.1, the channel dimension is short compared to the mean free path so that gas
molecules are more likely to collide with the channel walls than with each other. This
characterises the molecular flow regime, in which the volumetric flow rate Qm0i of a gas of
molecular weight M at absolute temperature Tis given by:
(2--=rJîS-ü)
~6Lt (7)
where R is the universal gas constant.
Considering the average behaviour over a large number of such leakage channels, where broad
22
Channels predominate, leakageflowwill be dominated by laminar behaviour, so that:
&_=(^}«'-Λ:) (8)
Where narrow channels dominate leakage behaviour, theflowis mainly molecular:
Qmol ~
V m)^
(at a given temperature).
If most leakage channel dimensions are such that 0.1<Kn<100 or if there is a wide distribution
of channel dimensions, the flow behaviour is intermediate and (assuming P2 is small in
comparison to Pi) the leak rate is given by an equation of the form:
Qmx = Atf + £,/» (10)
If either laminar flow or molecular flow can be shown to predominate in given circumstances,
then equations 8 and 9 provide a basis for predicting the leakage rate of one gas from that of
another under the same conditions, thus:
02 = .£, (laminar) (11)

Mi,
and
02 = 'IE? .Qx (molecular) (12)
If the flow is predominantly intermediate, a predictive relationship is possible, based on equation

10, but is less straightforward.
7.2 Room temperature experiments
The rationale for these tests is given in Section 4.3.2, and the scope is outlined in Table 5.
Results will be examined using the two approaches discussed above (power law correlation and
theoretical prediction).
7.2.1 Power law correlation approach
The basic data are plotted in Figs. 18 through 20, one diagram for each of three gland loads.
Most of these curves appear to display two distinct regions, with increasing gradient at higher
leak rate. It is not presently clear whether this gradient change is significant, or whether it
signals a change in the flow regime. It is also unclear whether this results from experimental
scatter. If a flow regime change is the cause, this may be due to the decrease in mean free path
(hence increase in Knudsen number) as pressure increases.
23
- Helium (valve A)
:
Methane (valve A)
10
Helium (valve B)
Ethane (valve B)
Methane (valve A)
Helium (valve B)
Ethane (valve B)
= 0 1
υ "Power (Ethane (valve B))
y = 0.0378X
S 'Power (Helium (valve A))
o R2 = 0.9688
'Power (Helium (valve B))
ξ ooi
y = 0.0014X " Power (Helium (valve B))
R2 = 0.9401 "Power (Methane (valve A))
0 . 0 ( 9 1 — — "Power (Methane (valve A))
jy=1E-04x "Power (Ethane (valve B))
I R 2 = 0.9168
O.OÜUI I
1
—r-
10
—1 '00
Pressure (bar)
Fig. 18 - leak rate vs pressure at low gland load
Methanejvalve A)1
Helium (valve B)1
Bhane(valveB)1
Helium(valve A)1
Helium(valve A)2
Methane(valve A)2
Helium(valve B)2
Bhane(varve B)2
Pow er (HeliurrXvalve A)1)
Pow er (Helium(valve A)2)
Power (Methane(valve A)1)
Pow er (Methane(valve A)2)
Pow er (Helium (valve B) 1 )
Pow er (Helium(valve B)2)
Pow er (Bhanefvalve B) 1 )
0.0001
Linear (Bhane(valve B)2)
10
Pressure (bar)
Fig. 19 - Leak rate vs pressure at intermediate gland load
0.01
Helium (valve A)
: Methane (valve A)
iO.001 o Helium (valve B)
2 A Ethane (valve B)
JÉ
y =0.0001x°,3M
R2 = 0 5004
ι.οσοτ
10
pressure (bar)
Fig. 20 - Leak rate vs pressure at high gland load
24
7.2.2 Theoretical predictive relationships
The discussion of Section 7.1, above, suggests several means to make statements about the
flow regime based on analysis of the test results:
1. C omparison of the test data points for a single gas and gland load with a "best fit" curve of
the form
Q = const.{p-p0) (13)
(where ρ is absolute sealed pressure and p0 is absolute atmospheric pressure), i.e. plot
leakage vs. gauge pressure and examine the extent to which it falls along a straight line
passing through the origin, indicating molecular flow. An example is given in Fig. 21, for
helium and methane in Valve A at the intermediate gland load.
2. C omparison of the test data points for a single gas and gland load with a "best fit" curve of
the form
Q = const.{p2-p¡) (14)
i.e. plot leakage vs. (p2 - p02) and examine the extent to which it falls along a straight line
passing through the origin, indicating laminar flow. An example is given in Fig. 22 for helium
and methane in Valve A at the intermediate gland load.
0.025 τ
• Helium
♦ Methane
—Helium (best fit

through origin) through origin
Methane (best fit Methane best fit
through origin) through origin
60
Fig 21 - Molecular flow best fit lines: Fig. 22 - Laminar flow "best fit" curves:
helium and methane in Valve A at helium and methane for Valve A at
intermediate gland load intermediate gland load
Comparing Figs. 21 and 22 suggests that the data are better fitted, in this particular case, by the
molecular flow relationship. This is supported by the superior values of the correlation
coefficients.
3. C omparison of VOC leakage data at a given gland load with values predicted using equation
12 from the "best fit" molecular flow relationship given by the analysis step 1, above. This
is shown in Fig. 23 for the same data set as the previous examples.
In this particular case there is reasonably good agreement between the actual best fit curve
and the relationship predicted from the helium data on the basis of equation 12.
25
0.025 Helium data Helium data
Methane data Methane data
— — Methane molecular flow Helium laminar flow

predicted from helium best fit
molecular flow best fit
Helium molecular flow Methane laminar flow
best fit to data best fit
Methane molecular flow — —Methane laminar flow
best fit to data 40 predicted from helium
pressure (bar gauge) gauge pressure (bar)
Fig. 23 - Methane molecular flow relationship Fig. 24 - Methane laminar flow predicted from
predicted from helium molecular flow best fit: helium laminar flow best fit: comparison with
comparison with methane data and best fit methane laminar flow best fit
4. C omparison of VOC leakage data at a given gland load with values predicted using
equation 11 from the "best fit" laminar flow relationship given by the analysis step 2,
above. This is shown in Fig. 24 for the same data set.
In this particular case, the predicted curve differs greatly from the actual methane data.
Furthermore if the flow regime were laminar, we would expect to see methane leak rates
greater than the helium leak rates, whereas the actual methane leak rates are less than
those of helium. Both observations suggest that in this case the laminar flow assumption
is wrong, whereas the observations from step 3 are consistent with a molecular flow
assumption.
Six data sets arising from the combinations of VOC (methane and ethane) and gland load (low,
intermediate and high) were analysed in this way.
Functional form of leakage rate -vs- pressure curve

Referring to Figs. 21 and 22 one can see that the quality of the curve fit to either form of
relationship (laminar or molecular flow) can be quantified in terms of the correlation coefficient
(the R2 value) on the proportional "best fit" curves. These results and their implications are
tabulated in Table 9.
Gland Valve He Methane Ethane

load
Indication
Curve fit correlation Curve fit correlation Indication Curve fit correlation Indication
coefficient (Laminar coefficient (Laminar coefficient (Laminar
or or or
Laminar Molecular Molecular) Laminar Molecular Molecular) Laminar Molecular Molecular)
flow flow flow flow flow flow
assumption assumption assumption assumption assumption assumption
Low A 0.827 0.99 Mol 0.969 0.945 Lam
Β 0.963 0.807 Lam 0.903 0.972 Mol
Medium A 0.919 0.974 Mol 0.372 0749 Mol
Β 0.936 0.972 Mol 0.819 0.934 Mol
High A 0.958 0918 Lam 0.922 0.88 Lam
Β 0.862 0.929 Mol N/A N/A ?
Tab e 9 - Ind ¡cation c if leakaç|e flow re gime on basis o f functioiial form

26
VOC leak rate: less than or greater than helium leak rate?
For laminar flow, since both VOCs are less viscous than helium we would expect the leakage
rate of VOCs to exceed that of helium under the same conditions. For molecular flow, since
helium molecular weight is less than both VOCs, we would expect the leakage rate of VOCs to
be less than that of helium. Examination of data against this criterion offers another indication
of leakage flow regime. The results are tabulated in Table 10 In ail cases, VOC leakage is less
than helium leakage, strongly supporting the molecular low hypothesis.
Test conditions Theoretical VOC leak rate Observed Conclusion

Gland load Valve VOC Laminar flow Molecular flow VOC leak rate
assumption assumption
Low A Methane greater than less than <He Molecular
Β Ethane Helium Helium <He Molecular
leakage leakage
Medium A Methane <He Molecular
Β Ethane <He Molecular
High A Methane <He Molecular
Β Ethane <He Molecular
Table 10 - Indication of leakage flowregimeon basis ofrelativemagnitude
Comparison of curve fit and "predicted" constants

If, for example, laminar flow is postulated and assumed to hold for both helium and the VOC
under the same conditions, then regressional analysis of the helium data can provide a constant,
say, kHe, for the relationship given by equation 14. Thus,
Q= kHe.(p2-pÌ) (15)
From this, and the relationship of equation 11, it follows that the corresponding relationship
predicted for VOC leakage is:
Q= kyoc.(p2-p20) (16)
where
k = 'JÊM,: .k He (17)
κ Mmc j
Comparison of the value of kVoc computed in this way from the helium data with a value derived
from regressional analysis on the VOC data gives indication of the error involved in this
approach. This is conveniently expressed as the ratio of the value predicted from the helium
data to the value found from the VOC data. The amplitude of the logarithm (positive or negative)
of this ratio gives a measure of the factor (above or below) by which the estimated value
disagrees with the data.
In an entirely analogous procedure to test the molecular flow assumption, regressional analysis
of the helium data gives a value of the constant, say, mHe, in the relationship given by equation
13, thus:
Q= r
"He{p-Po) (18)
whence the corresponding predictive relationship for VOC leakage is:

27
Q= mvoc.{p-p0) (19)
where
M He
m
voc — .m He (20)
^ V ™voc J
Again, the ratio of the value of mVoc computed from helium data to the value estimated from
regressional analysis of the VOC data gives a measure of the error involved in the use of this
predictive relationship.
Finally, comparison of the errors in the predictive relationships based on the molecular flow and
laminar flow assumptions gives another indication of the leakage mechanism. This is tabulated
in Table 11.
Gland Valve Methane Ethane

load laminar Indication molecular
laminar molecular Indication
best fit pred'n log(ratio) best fit pred'n log(ratio) (mol/lam) best fit pred'n log(ratio) best fit pred'n log(ratio) (mol/lam)
Low A 4.46E- 7.53E-
05 03
2.23 1.67E- 0.033
03 68
1.30 Molecular
¡mi 1.71 Molecular
B 1.5E- 1.20E- 2.90 0.000 0.028
"'-"■ ¿f ';
. ' · . - ■ " ' ■ '
05 02 564 678
Med A 3.4E- 2.17E- 0.81 0.000 0.000 0.24 Molecular
06 05 13 23
B 3.8E- 7.95E- 0.32 0.000 0.000 0.04 Molecular
05 05 465 512
High A 5.9E- 2.62E- 0.65 2.1 E- 2.7E- 0.10 Molecular
07 06 05 05
- * ■ , > ' - ' . '
■ "'■ . . · ■ - ' ; Á:. ..
B - ■ ■ · " - ■
6.1E- 2.51 E- 0.62 2.13E- 1.63E- -0.12 Molecular
07 06 05 05
Table 11 - Indication of leakage flow regime on basis of curve f t constants
Comparison and c onc lusions

The preceding three evaluations of leakage mechanism are brought together for comparison in
Table 12.
Gland Valve Gas

load Helium Methane Ethane
functional functional VOC leak Comparison functional VOC leak Comparison
form of form of less or of curve fit form of less or of curve fit
leakage leakage more than and leakage more than and predicted
versus versus He predicted versus He constants
pressure pressure constants pressure
Low A Molecular Laminar Molecular Molecular - . - · ' V· · ";i-V
B Laminar Molecular Molecular Molecular

Medium A Molecular Molecular Molecular Molecular '·ƒ,-·. ■■#&3&®&$
B Molecular Molecular Molecular Molecular
High A Laminar Laminar Molecular Molecular ■ : ' ν-τ- - v - p » í S ^ * í ; ^ W
B Molecular ? Molecular Molecular
Table 12 - Summary of indications of leakage mechanism
This table shows that it is only at the intermediate gland load where all the data are consistent,
and indicate molecular flow. Under other conditions, there are conflicting pieces of evidence.
Indications of laminar flow at the high gland load condition are particularly surprising. The
observation that VOC leak rate is consistently less than helium leak rate under the same
28
conditions is particularly significant. Not only is it strongly suggestive of molecular flow, but also
suggests a way forward for the specification of a Qualification Test leak-tightness criterion if it
does not prove possible to calculate VOC leak rate from measured helium leak rate. If the end-
user's "in the field" VOC leak rate target is met with helium, it should certainly be met with VOC.
Alternatively, the power law correlation approach remains a possibility.
7.3 The effect of temperature
7.3.1 Hypothesis
Returning to the governing equations for laminar and molecular flow (equations 6 and 7,
respectively), we may examine the anticipated effects on the leakage flow when temperature is
changed.
Equation 6, for laminar flow, shows that the principal anticipated effect is through the
temperature-dependence of viscosity (which can nearly double over the temperature range
selected here). There may be indirect effects caused by changes in the distribution of leakage
channel dimensions, but these are beyond our current predictive capability.
Equation 7, for molecular flow, shows that we can expect a direct effect of temperature: leakage
should vary with the square root of absolute temperature, with all other quantities held constant.
Again, unpredictable changes in the dimensions of leakage passages may also affect leakage
rate.
7.3.2 Leakage mechanism for helium
The experiments outlined in Section 4.3.3 and Table 6 enabled an investigation of the leakage
mechanism in helium, for which there was a larger test matrix, and some selected comparison
between the expected leakage behaviour of three VOCs and their actual leakage behaviour.
Evidence from the room temperature tests, whilst in some cases conflicting, tended to suggest
that the leakage was predominantly by molecular flow. Therefore, an analysis of the kind
described in Section 7.2, above, was conducted on the helium data from the elevated
temperature tests, with a straight line fitted through the data plotted as leakage rate vs pressure.
The resulting correlation coefficients are given in Table 13.
Gland load Test temp( degC)

20 100 200 300
Medium 1 0.997 0.999
2 0.996 0.860 0.996 0.989
3 0.978 0.995
4 0.994 0.997 0.885 0.993
High 1 0.990 0.994 0.934 0.994
2 0.988 0.999 0.928
3
4 0.995 0.997 1.000 0.989
Table 13 - conrelation coefficients for linear curve fit
to leak rate vs pressure data
These results indicate that the data correlate very strongly with a direct proportionality
relationship, characteristic of molecular flow.
29
Another check on the flow regime can be madefromexamining the temperature dependence
of the helium leak rate data. For molecular flow, we would expect a relationship at absolute
temperature, T, between leak rate, Or, and sealed pressure, Δρ, of the form:
QT =mT.Ap (21)
where mT is the constant of proportionality, related to the corresponding constant, m0l at

reference temperature, T0, by:
ΥΠγ = /røg . (22)
Thus, expected values of mT can be estimated for the elevated temperature data from
regressional analysis of the room temperature data. These estimated values can be compared
with values of mT found directly by regressional analysis of the elevated temperature data and
the error found. This error is tabulated in Table 14.
Gland Test Temp (deg C I

load 100 200 300
Medium 1 51%
2 26% -14% 6%
3 115%
4 69% 70% 127%
High 1 59% 840% 393%
2 17% 90% -..*>
3 : * " '■- ΐ
4 34% 56% 113%

Table 14 - Estimate of error in derived temperature
dependence relationship
In all but cases but one, the estimated temperature dependence is an over-estimate of the actual
temperature dependence. The results of Table 13 suggest that this error does not arise from
any departure from molecular flow. This implies that there must be some other factor affecting
the temperature dependence of the leak rate -vs- pressure relationship. As suggested in Section
7.3.1, possibly arises from changes to the internal leakage paths through the seal.
Since there are only limited data on VOC leakage at high temperature and pressure, it was not
possible to examine the functional form of the leak rate -vs- pressure relationship for these
gases. However, where measurements were taken, it was possible to estimate the accuracy of
predicted VOC leak rate using the molecular flow relationship. Given the error (just discussed)
associated with temperature, predictions were based on helium data at the same temperature
(rather than on room temperature helium data). The approach adopted makes use of equation
20. Thus, expected values of mVoc can be estimated for VOC data from regressional analysis
of the helium data at the same temperature and gland load. Ihe expected value of VOC leak
rate at a given pressure, p, can then be calculated from equation 19. Comparison of the
estimated leak rate with the measured value gives a measure of the accuracy of the prediction.
The results are given in Table 15 in terms of a ratio of measured to expected result.
The methane predictions at high gland load are reasonable in comparison, for example, with
errors incurred by sniffing rather than flushing or vacuum measurement, but could hardly be
30
considered accurate. Ethane predictions are poor, being about one decade in error. Propylene
predictions are very poor. It is quite possible that the heavier gases deviate from molecular flow,
but there are insufficient data at present to check this hypothesis.
Gland Temp Pressure Methane Ethane Propylene

load (°C) (bar) Testi Test4 Test2 Testo Test3 Teste
Medium 20 9 :
' . ; ■ · . >
10.9 29.0
20 5.1 11.5 15.0 7.3 ■ ·..-'-/.
*%M $*f?rSB
100 9 %^Á ?^mm 37.0
200 20 ;., 4.2 : -', ■ ·-'.-. ..-'Vi 'iX :':"ii\'4'£y/-
300 9 13.9 14.2

20 4.0 9.3 4.1 9.5 *■ . * ; · ' > V - ' * -
High 20 9 35.3 35.8

20 1.1 2.3 20.9 5.0 -v ·. m
100 20 6.0 -■ ' . ·.-". .'-■-¿~.
200 9 54.1
300 9 67.7 61.5
20 2.6 4.1 15.9 10.0 - , ' ' ■ ' *
Table 15 - Accuracy of VOC leakage predictions based on Molecular Weight

correction and helium measurements (ratio of predicted leak to measured leak)
It does not appear possible to obtain a reliable calculation of VOC leakage from measurements
in helium under the same conditions with the molecular flow assumption - despite very strong
indication that the leakage mechanism is molecular flow (see Table 13). However, the results
in Table 15 do show that in all cases the measured VOC leak rate is less than the predicted
valué. This suggests that calculated VOC based on helium data measured under the same
conditions and using equation 12 would offer a conservative leak-tightness test criterion: if the
calculated VOC leakage falls within a threshold value, one would expect actual VOC leak rate
to fall further below this value.
31
8. Qualification test measurements and site performance

Referring back to Fig. 1, we see that there are potentially two measurements of interest to end-
users. Where compliance with TA-Luft is required, VOC leak rate is required. Thus, to estimate
VOC performance from the results of the ISO test, a relationship between VOC leak rate and
helium leak rate is required. The approaches to this problem and their accuracy were discussed
in Section 7, above.
However, the majority of end-users are primarily interested in sniffer-based ppmv thresholds to
comply with the provisions of the Clean Air act in the US and to facilitate established site-based
LDAR practice. This means that a linkage needs to be established between helium leak rate
measurements from the ISO test and VOC ppmv values (particularly methane, as a popular
representative gas).
In practice, this means using a two-step procedure involving:
• Step 1: helium leakage to VOC leakage
• Step 2: VOC leakage to VOC ppmv
This Section considers an evaluation of the accuracy of this two-step procedure.
8.1 Helium leakage to VOC leakage
Basic research has just been presented considering approaches to the first of this relationship.
Using helium data and predictive relationships of the form of equations 8, 9 and 10, for laminar,
molecular and intermediate flow, respectively, predictions were made for VOC leakage under
the same temperature and pressure.
8.2 VOC leakage to VOC ppmv
Factors affecting the accuracy of leak rate - to - ppmv relationships were discussed in Section
6. However, this concentrated on helium at room temperature. Whilst many of the conclusions
concerning the underlying physics, are considered likely to hold true for hot hydrocarbons, that
work did not explicitly evaluate this question. However, a body of data exists, (albeit from a wide
range of sources, and employing a range of different instruments) and can be drawn upon.
For each VOC leak rate calculated in Step 1, one of three previously published power law
correlations was used to estimate a corresponding ppmv value. The ppmv value thus calculated
could be compared with actual values measured in this study using a particular instrument.
The correlations used were as follows.
CETIM relationship
A room temperature relationship between methane ppmv and the associated total leakage was
defined by project partner CETIM from the methane measurements taken in the "sniffer
evaluation tests" (see Section 4.3.1.3 and Table 2). These tests involved measurements:
- in ppmv using a TVA 1000 (Foxboro) with a probe flow rate of 1 litre per minute
32
- in atm.cm3.s"1 using flushing with the same TVA 1000 and high purity air as carrier gas
The resulting correlation (with leakage expressed as mass flow rate, Qm, in mg.s"1 of methane)
was :
^ ν =5.263χ10 5 .ρ:·" (23)

where:
Cppmv Methane Screening Value measured by EPA Method 21 (ref. 19)
Qm Methane room temperature total leakage in mg.s'1 (methane associated density
is 0.7174 kg.m"3)
BP relationship
Using 6" class 600 valves, BP defined a relationship between methane ppmv and associated
mass leakage (20) at different pressures and temperatures. Total methane leakage rates were
measured using the bagging method. A Foxboro OVA -108 was used for these measurements.
No information is given on the probe flow rate in this reference.
The resulting correlation was:
C P / W I V =2.113X10 5 .Ö:· 1 2 (24)
BHRG relationship
BHR Group took room temperature measurements in a previous, preliminary study (16) using
methane and a 4" class 300 valve. Methane measurements were taken by bagging using a
Foxboro Century OVA 128 with a probe flow rate of 2 litres per minute.
The resulting correlation was:
C _ ν =1.576χ10\ρ:· 971 (25)
8.3 Results
Results were compiled in the form of the ratio, z, of the measured to the theoretically predicted
values of sniffer concentration in ppmv, thus:
ζ s-sss. (26)
As an example, Fig. 25 shows the variation of the ζ parameter with the three VOC gases at
different test conditions of temperature, pressure and gland nut toque, calculated with the BP
relationship. The X-axis corresponds to the sniffing measurements.
33
100 ι ■
Gas :Methane
Pressure : 20 bar
10 . r- i - :
r Relation : BP
υ 20 °C
• laminar
1 1: φ
1 å
o __Ϊ. :_ Æ... ■ intermediate
II
Ν i 40 Nm " # 40 Nm «
A
:_20°C t 3 0 0 e C molecular
300 °C m -- - '
0.1 20 °C
10 100 1000 10000

0.01 C mes in p p m v
100 = - + - ~H
Γ ~ — i— ■ -- Gas :Ethane
Pressure : 20 bar
10 = 40 Nm . Relation ■ RP
, 20 °C ¡ 20 Nm
Ó"
» — ί -= = Ι • laminar
Ι 1 = ^PS^*=
υII 40 Nm
Ν 30 0 "C --* ■ intermedíate
: ;= ==^20NmLijr20Nm
200 c
300 °C A
molecular
0.1
0.01 10 100 1000 10000 100 OC)0

Cmes ¡ η p p m v
Gas :Propylen
Pressure : 9 bar
Relation : BP
É| 20 Nm |
™ 'q r 20 Nm · |am¡nar
I 1 40 Nm ; lt 300 °C
u ■ynn'r
■ intermediate
II
N
40 Nm
01 ?n τ. * molecular
i
0.01
10 100 1000 10000
C mes ¡n ppmv
Figure 25 - Variations in ζ versus measured ppmv of VOC

34
Firstly, note that ζ is higher in the case of the molecular flow assumption than for laminar. The
difference, Δζ, between these two regimes increases from methane through ethane to propylene
(Δζ methane< Δζ ethane < Δζ propylene). If the flow regime is not known for sure, Δζ can be
considered as a fixed error band. This means that the prediction obtained for propylene will be
more problematic than for methane.
Secondly, note that the location of the "intermediate" markers is closer to the "molecular"
markers than to the "laminar" markers. This is an additional indication that molecular flow
predominates.
From Fig. 26, it is possible to infer the influence of the three main sources of error.
Gas :(all)
Pressure : (all)
Temperature : (all
Gland load : (all)
BHRG Intermediate
BHRG Laminar
BHRG Molecular
BP Intermediate
BP Laminar
BP Molecular
CETIM Intermediate
CETIM Laminar
CETIM Molecular
0.01
10 100 1000 10000 100000
Cmeas ¡Π p p m v
Figure 26 - Variations in ζ versus ppmv measurements with the three

target gases and the three empirical relationships
Sniffing measurement scatter

This has a major influence on the variation of z. If there were no inherent scatter in the
sniffing measurement itself, then all plotting symbols of the same shape and colour would
lie along a smooth line.
Quality of the ppmv-vs-leak rate relationship

This is responsible for an offset parallel to the z-axis which can reach a decade (compare
plotting symbols of the same shape but different colours). In one case the leak rate is
underestimated (z>1), whereas in another case the calculation overestimates the leak rate
(z<1). This difference may be explained by differences in the detector probe flow rate or in
the sniffing factor (see Section 6.2).
• Test gas flow regime

For each assumed ppmv-to-leak rate correlation (CETIM, BP or BHR Group), the laminar
markers (lower limit) are linked by a dashed curve, whilst the molecular markers (upper limit)
35
are linked by another dashed curve of the same colour. The gap between these curves
indicates the range of uncertainty associated with the assumed flow regime. The error
incurred by the use of the molecularflowassumption was examined in Table 15, above.
Great care should be taken in the use of empirical relations. Ail steps in this approach must be
well controlled. For example, it is better to use the same detector to perform the measurements
for the establishment of the ppmv-vs-leak rate relationship andforthe prediction validation.
36
9. Relationship of QA tests to qualification tests

There are a number of issues concerning the relationship between QA tests and qualification
tests, to which this project can contribute relevant comments and findings.
9.1 Relationship between ppmv of helium and leak rate thresholds
It is most likely that ISO will specify the sniffer method, with helium as test gas, for QA tests on
valve stem leak-tightness. Comments on the repeatability of this approach were made in
Section 6. For a QA test on a particular product line, many repeat readings are taken in the
same environment with the same instrument on only one valve type and size, pressurized to the
same level with the same test gas. This tighter specification of test conditions should result in
further reduction of scatter. Checks against a limited number of vacuum readings for these
same conditions may result in a reasonably accurate correlation between leakage rate and the
measured ppmv. It should, however, be noted that any ppmv -vs- leak rate correlation would be
highly specific to the particular test conditions and detector, and notgenerally applicable.
9.2 Establishment of appropriate threshold value
It is of course desirable to leave a margin of error between any pass/fail QA sniffer threshold
value and the corresponding leakage limit derived from the ISO tightness class limit via an
appropriate correlation. Two further comments maybe made in this respect, however.
Firstly, unlike qualification tests, QA tests will be conducted at a pressure substantially less than
rated pressure. Since we need to know what is an acceptable leakage rate at QA test pressure,
this re-raises the question of the pressure dependence of leakage rate and underscores the
central importance of understanding the leakage mechanism.
Secondly, it was found in this project that initial gland load adjustment, together with the first few
stem operations have a significant effect on the leakage. In the valve qualification test, initial
gland load adjustment and a certain number of stem operations are permitted, whereas in a QA
environment, there is unlikely to be either.
To illustrate this point, results are presented, in Fig. 27, of a series of tests in which leak-
tightness was assessed as a function of thefirstfewstem cycles. Here, measured leakage or
ppmv, normalised for each valve by its corresponding value at the end of the test, is plotted
against number of cycles. Since, by definition, data will converge on the value 1, we can
examine leakage consistency for different tests, regardless of the level of leakage.
In all cases tested, leakage attained reasonable consistency by 80 stem operations. In nearly
all cases, deviation was within 50% within 40 operations. Looking at data from any individual
test, there does not appear to be any systematic tendency for the leakage trend either toriseor
to fall from an initial to a final value. However, there is often an increase over the first 10 cycles,
followed by a decrease to thefinalvalue (although this is not always so).
37
4 50 . -*~2" gate valve, medium leakrates (graphite

packings), leakrate measurement
2" gate valve, low leakrate (P TFE
4.00
packings), ppm measurement
4" gate valve, medium leakrate (graphite
%, 3 - 5 0 1 packing), ppm measurement
a
■o ——6" gate valve, high leakrate (graphite
300 I packings), ppm measurement
π
E ~ * ~ 6 " gate valve, low leakrate (P TFE
0 2.50 t- packings), ppm measurement
| -·~2" rotary valve, medium leakrate (graphite
α 2 oo v m packings), ppm measurement
•c -1—2" rotary valve, low leakrate (P TFE V-
= 1 so rl rings), ppm measurement
—
1 Wé£5( - 3" rotary valve, medium leakrate (graphite
E packings), ppm measurement
1.00
3" rotary valve, medium leakrate (graphite
a packings), leakrate measurement
χ
0.50
3" rotary valve, low leakrate (P TFE
0.00 4" rotary valve, medium leakrate (graphite
50 100 150 20] packings), ppm measurement
4
Stem operations " rotary valve, low leakrate (P TFE
Fig. 27 - Effect of stem operations on leakage consistency
The qualification test is designed to provide information about the longer-term response of the
sealing performance through thermal and mechanical cycling, but this does not address the
issue of the relationship between the type test and an "acceptable" leakage in a QA test. Clearly,
it is impractical to suggest conducting, say, 40 stem operations as part of a QA test procedure.
However, the deviation of early seal leakage readings from their "bedded-in" values, might
suggest the use, in a QA test, of an appropriate "safety factor" on a threshold leakage value
defined by the qualification test.
38
10. Conclusions
A major contribution has been made towards the clarification of a number of important issues
relating to valve stem leak-tightness measurement and interpretation. Significant conclusions
are:
• Sniffing does not measure leakage rate. It is a local measurement, based on probe uptake
of leakage gas.
• Test methods that measure valve stem leak rate must be "global", i.e. they must catch all of
the stem seal leakage. Results are expressed in massflowrate units such as mg.s'1 or in
atm.cm3.s"1 (or equivalent p-V throughput units) - see Appendix2.
• A sniffer detector that reads out in units of flow rate is not measuring leak rate, but the probe
uptake of leaking gas. Since only an unknown proportion of the leaking gas is drawn into the
probe, there is no simple universal relationship between these quantities.
• A sniffer detector that reads out in ppmv is measuring concentration of leakage gas drawn
into the probe. The ppmv reading is simply related to probe uptake of leakage gas and
probe flow rate, but since probe uptake is an unknown proportion of leak rate there is no
simple universal relationship between ppmv and leak rate.
• Both sniffer probe flow rate and factors that affect sniffer probe uptake influence the
relationship between ppmv and leak rate.
• The most significant factors affecting this relationship are sniffer probe flow rate and local
air currents. The use of a single detector type and elimination of significant local air currents
can dramatically reduce scatter in the accuracy of power law relationships between ppmv
and leakage rate (from 2 orders of magnitude to a factor of 2 or 3).
• Under well-controlled circumstances, the typical near-proportionality between leakage rate

and ppmv suggests an alternative approach to the relationship between these quantities
based on an empirical "sniffing factor" (percentage of leaking gas taken up by the detector)
and known probe flow rate.
• The "sniffing factor" is not a constant, it is known to vary with leak rate, and is likely to
depend on other factors such as stem diameter, packing type, valve, etc. Therefore, if it is
averaged over a range of measurement conditions, the error band associated with its use
will be increased, and understanding of the underlying behaviour may be obscured.
• The probe flow rate is a function of the detector employed.
• By specifying "sniffing factor" and probe flow rate, ambiguity is avoided, whilst use of this
approach can reduce scatter. Further work is required for both helium and VOC detectors
across a wide range of temperatures, valve types and sizes, packing types, etc.
• Flushing represents a suitable, reasonably accurate alternative to sniffing over the range of
leakage rates for which it was evaluated and is a suitable technique for VOC leak rate
measurement. Lantern ring ports mayfacilitate the use of this technique.
• The vacuum method is suitable over a wide range of helium leakage rates. It may involve
minor modifications to a valve, however, to ensure a good vacuum seal. Again, a lantern
39
ring port may circumvent that problem.
Best practice guidelines have been produced for both sniffing and flushing, and results
forwarded to ISO/TC153/SC1/WG10.
Room temperature tests support the possibility of a predictive relation between the leak rate
of helium and that of light hydrocarbons (methane and ethane) on the basis of leakage flow
mechanism, at least under a limited range of conditions. More work is required to confirm,
generalise and determine confidence intervals.
Molecular flow appears to predominate at room temperature in many (not all) cases studied,
but some data are contradictory. An assumption of laminar leakage flow could not be
supported. Conclusions are not generally applicable to other valve types, sizes, packing
types and test gases. Further work is required.
An approach was developed to examine the quality of predicted VOC ppmv values from
measured helium leak rates under conditions of temperature and pressure representative
of site VOC duties (up to 30 bar and 300 deg C). This involves both predictive relationships
between leakage rates (based on molecular, laminar or intermediate flow) and empirical
correlations (gas-to-gas and leak rate-to-ppmv).
A significant data set was obtained for high temperature helium across a range of pressures
and under well-controlled conditions. This represents a useful database for future studies.
VOC ppmv measurements at elevated temperature confirmed the scatter involved in this
approach. This makes clear identification of leakage mechanism difficult. It also contributes
to a significant margin of error in any correlation from helium leak rate to VOC - typically a
decade or more.
Leakage measurements of methane, ethane and propylene byflushingdemonstrated the

feasibility of this approach for VOCs at elevated temperature. Results enabled selective
checks on the relationship between leak rates of helium and VOCs.
It did not appear possible to derive a reliable predictive relationship between leakage of
helium and that of VOCs based either on molecular or laminar flow assumptions, at elevated
temperature.
Since predicted VOC leakage based on helium measurements and a molecular flow
"correction" results in an over-prediction of VOC leakage, this represents a conservative
approach to specifying a leak-tightness criterion: actual VOC leakage is expected to be less
than the calculated value.
Leakage mechanisms at elevated temperature remain unclear: there is conficting

evidence and more work is required.
40
11. References
1. Colyer, R., Negotiated rule for equipment leaks, 1 st European Conference on Controlling
Fugitive Emissions from Valves, Pumps and Flanges, (ed. C. Lätty), BHR Group Limited (on
behalf of the ESA), 1995, pp. 9-34
2. Applicability of HON, Federal Register, Vol. 59, No. 78, Subpart F, §63.100, pp. 19454-
19468, April 1994
3. Technische Anleitung zur Reinhaltung der Luft - TA Luft (Technical instructions on air quality
control), Federal Ministry for Environment, Nature Conservation and Reactor Safety, Bonn
1986
4. Drechsler, W., Legal requirements for the reduction of fugitive emissions in Germany, 2nd
European Fugitive Emissions Conference - Controlling Fugitive Emissions from Valves,
Pumps and Flanges, VDI Verlag GmbH (on behalf of the ESA), 1998, pp. 13-19
5. Emissionsmenderung Mineralölraffinerien, VDI Guideline 2440, Verein Deutscher

Ingenieure, 1983 (Currently under revision)
6. Ellis, B.S., Emission legislation - development and progress, Papers presented at the
International Seal Forum at Achema '97, (Available from European Sealing Association,
Bowerham House, The Grove, Lancaster, LA3 1AL, U.K.)
7. Guidelines for controlling fugitive emissions with valve stem sealing systems, STLE Special
Publication SP-33, Society of Tribologists and Lubrication Engineers, October 1992.
8. Valve World Conference and Exhibition, Den Haag, November 1998, Workshop on
Standardisation. Convenor: Barrie Kirkman (BP Chemicals).
9. Standard method for the evaluation of external leakage of manual and automated on-off
valves, ISA-ds93.0.01, Committee Draft 14, Instrument Society of America, March 1998
10. ISO/WD 15848 Valve fugitive emissions

(Part 1) Classification system and qualification procedures for type tests of valve assemblies,
(proof of design test)
(Part 2) Production acceptance test of valve assemblies, (quality control)
In draft in ISO TC153/SC1/WG10
11. Leefe, S.E., SMT project on valve emission measurement methods 2nd European Fugitive
Emissions Conference - Controlling Fugitive Emissions from Valves, Pumps and Flanges,
VDI Verlag GmbH (on behalf of the ESA), 1998, pp. 237-249
12. Leefe, S.E., Valve stem leak-tightness: evaluation of measurement methods for qualification
and QA tests. Valve World, vol 4, no. 4, Aug 1999, pp. 48-57.
13. Leefe, S.E., Leakage measurement issues for industrial valve standards Valve World, vol.
5, no. 3, Jun 2000, pp.54-59
14. Private communication with M. Shaw of National Engineering Laboratory, East Kilbride,
Scotland, August 2000
41
15. Vignaud, J.C. and Massart, T., Mesure et calcul du débit de fuñe d'un joint en eau et vapeaur
d'eau - Cas d'un joint en graphite expansé matrice, Proceedings of the 3rd International
Conference of Fluid Sealing, Biarritz, France, 1993, pp. 521-532
16. Bazergui, A. and Louis, G., Predicting leakage for various gases in gasketed joints Society
of Experimental Mechanics, Spring Conference on Experimental Mechanics, SEM, Houston,
Texas, 1987
17. Chen, J., Kuo, J. and Miskell, C, A link between gasket tightness and fugitive emission leak
definition, Proceedings of the 6th Annual· Fluid Sealing Association Technical Symposium,
Houston, Texas, 1996
18. Kockelmann, H. and Gusko, A, On the tightness behaviour of graphite and fibre based sheet
gasket materials, Proceedings of the 3rd International Conference of Fluid Sealing, Biarritz,
France, 1993, pp. 335-352
19. Reference Method 21, Determination of volatile organic compound leak. Code of Federal
Regulations, Title 40, Part 60, Appendix A. Washington, D.O., U.S. Government Printing
Office. (Revised June 22, 1990)
20. Harrison, D., Smith, E., Billington, M.J. and Kirkman, B., "Evaluation of graphite valve
packings to reduce fugitive emissions on hydrocarbon duties", 1st European Fugitive
Emissions Conference on Controlling Fugitive Emissions from Valves, Pumps and Flanges
(ed. C. Lätty), BHR Group Limited (on behalf of the ESA), 1995, pp. 77-88
21. Leefe, S.E. and Davies, O.M., "Laboratory based test for valve stem leakage correlation
between test and working fluids", 1st European Fugitive Emissions Conference on
Controlling Fugitive Emissions from Valves, Pumps and Flanges (ed. C. Lätty), BHR Group
Limited (on behalf of the ESA), 1995, pp. 59-75
42
Appendix 1 - Glossary of Terms

Bag See "bagging"
Bagging The class of techniques for measuring the leak rate from a test object, in which the
test object, or the part of the test object from which leakage is occurring, is enclosed in a sealed
container known as a "bag". Various techniques fall into this category. The bag will be
connected via a pipe or tube to the detector and may also be connected to a source offlushgas
(see "flushing").
Calibration gas A mixture of known and certified concentration of the test gas in air, used for
the purpose of calibrating detectors.
Concentration or ppm methods The class of techniques for estimating the severity of a leak
based on a measure of the concentration of the test gas in the atmosphere close to the leakage
source.
Detector An instrument which is sensitive to the test gas and provides a quantitative indication
of its presence. This may be based on the concentration of test gas in the flow through the
instrument, or in a sample taken by the instrument. Alternatively, it may be based on a direct
measurement of flow of the test gas through the instrument.
Dilution probe A sniffer probe containing a T-branch through which the ambient atmosphere
is allowed to mix with the sample drawn in at the probe tip, thus diluting the concentration of test
gas reaching the detector instrument by a known factor. This is used to extend the range of a
detector to enable it to measure higher leakage concentration.
EPA 21 or EPA Method 21 A concentration method for the detection of VOCs, specified by the
American Environmental Protection Agency (see ref. 19).
Encapsulation cover/chamber/ring A rigid version of a bag, usually sealing against some

convenient surface of the test object.
Evacuated bagging/The vacuum method A variant of bagging in which the bag is evacuated
and any leakage fed directly to the detector (usually a mass spectrometer working at vacuum
conditions).
Flushing/Flush method A variant of bagging, in which the leakage into the bag is carried to
the detector in a stream of gas of known purity (the "flush gas") fed into the bag at a known
volumetric flow rate (the "flush gas flow rate"). The volumetric concentration of the test gas in
the flush gas reaching the detector then provides a direct measure of the test gas volumetric
leak rate. Knowing the temperature and pressure in the bag, we can then infer a leak rate of test
gas.
Flush gas See "Flushing"
Flush gas flow rate See "Flushing"
Global methods Leakage measurement methods that capture all ofthe test gas leaking into
an encapsulation chamber
Leakage Any test gas escaping from the test object

43
Leakage concentration The volumetric concentration oftest gas in the atmosphere adjacent
to the source of its leakage from the test object.
Leakage encapsulation cover/chamber/ring See "encapsulation cover".
Leak rate The flow rate (mass, molar, volumetric or pV-throughput - see Appendix 2) of test
gas leaking from the test object.
Mass leak rate The mass flow rate oftest gas leakingfromthe test object.
Modified EPA Method 21 A concentration method for the detection of helium, defined in this
project (see Appendix 3), but following a similar protocol to that laid out in EPA Method 21 (see
ref. 19).
ppmv or ppm A measure of volumetric test gas concentration in a given atmosphere,

expressed as parts per million by volume.
Probe A thin hollow hand-held tube whose tip is placed next to a leakage source to draw a
sample into a sniffer instrument.
Probe flow rate The flow rate (usually expressed as pV-throughput) at which gas is drawn into
a detector through the probe.
Probe tip The end of the probe placed next to the leakage source in sniffer methods
pV-throughput A measure offlowrateexpressed in terms of a product of a volumetricflowrate

and a pressure (see Appendix 2 for a fuller explanation).
Response time The time interval from a step change in test gas into a detector to the time at
which 90 percent of the corresponding final value is reached as displayed on the instrument
meter readout.
Sniffing/Sniffer method The use of a probe to draw a sample into a detector. This technique
is a local measurement used to indicate the presence of a leak and to provide a comparative
indication of its severity. It does not provide a quantitative measurement of leak rate.
Sniffer A detector equipped with a probe - alternatively, the probe itself.
Sniffer probe See "Probe"
Sniffer (or probe) flow rate The flow rate of gas (usually expressed as volumetric flow rate or
pV-throughput) into a sniffer.
Threshold value An upper limit on leak rate orppmv permitted by a regulation.
Test gas The species of gas whose leak rate out ofthe test object is being measured.
Test object The piece of equipment or part thereof whose leak-tightness is being measured.
Zero gas A gas (usually air) containing less than 10 ppmv of test gas, used in certain
detector evaluation procedures.
44
Appendix 2 - Units
Leakage can be expressed in several ways:
- volumetric leakage rate
- mass leakage rate
- molar leakage rate.
The first is convenient because it is easy to visualise. However, the rate at which a quantity of
the substance actually leaks is better expressed by the second and third, since the volume of
a given quantity of gas depends on its temperature and pressure, rendering the volumetric
leakage rate figure ambiguous.
One way around this is to refer to "standard" volumetric leak rate (e.g. in standard cm3s'1) in
which the volume is referred back to "standard" conditions (0°C and atmospheric pressure). The
other, roughly equivalent, approach is to quote leakage rate as "pV throughout". Here the
leakage rate is cited as the product of a pressure and volumetric flow rate. So that the mass or
molar flow rate can be calculated from this figure, the absolute temperature should also be
specified, but its omission is taken to mean "at 288.2 K" (which relates to the International
Standard Atmosphere at sea level). For example: 1 mbar litre/sec = 1 bar.ml/s, which is 1 ml/s
at 1 bar and 300K. In practice, the same flow rate could have resulted from 0.1 ml/s at 10 bar
or 10 ml/s at 0.1 bar, etc.
To assist conversion between units, refer to Table A2.1.
Conversion factors (n) for leakage rate units (1X= nY)

ι
Y
1 1
Pa.nr'.s" mbar.l.s" atm.cnV.s'1 moles.s'1
or or
bar. cm3, s"1 std cm3.s"1
Pa.m3.s'1 1 10 9.87 4.403x10"4
1
mbar.l.s'
X or 0.1 1 0.987 4.403 x1o 5
3
bar.cm .s"
atm.cnr'.s'1 1.013 1
or 0.1013 4.61 x10' 5
3 1
std cm .s'
moles.s"1 2.271 x10 3 2.271 x104 2.24x104 1
Note: In the conversion from pV-throughput to a mass flow rate, for a
determined gas, thefollowingformula may be employed:
Qm = Qpv. M /(RT)
where:
Qm : mass flow rate in kg.s"1 QpV : throughput in Pa.nf.s'1
1
M : molar mass in kg.mole" R : universal gas constant in J.mole"1 K"1
Τ : temperature in Κ
Table A2.1 - Conversion between leak rate units

.
45
Appendix 3 - Adaptation of EPA Method 21 for helium sniffer

measurements
Proposed wording adapted directly from EPA Method 21 (see ref. 19) by BHR Group Limited.
1. APPLICABILITY AND PRINCIPLE
1.1 Applicability
This method applies to the determination of Helium leaks from valves, flanges and other
connections.
1.2 Principle
A portable instrument is used to detect leaks from individual sources. The instrument detector
type is not specified. This procedure is intended to locate and classify leaks only, and Is not be
used as a direct measure of emission rates from individual sources.
2. DEFINITIONS
2.1 Leak Definition Concentration

The local He concentration at the surface of a leak source that indicates that a leak is present.
2.2 Calibration Gas

The compound used to adjust the instrument meter reading to a known value. The calibration gas
is Helium at a concentration approximately equal to the leak definition concentration.
2.3 No Detectable Emission

Any He concentration at a potential leak source (adjusted for local He ambient concentration) that
is less than a value corresponding to the Instrument readability specification of section 3.1.1(c)
indicates that a leak is not present.
2.2 Calibration Precision

The degree of agreement between measurements of the same known value, expressed as the
relative percentage of the average difference between the meter readings and the known
concentration to the known concentration.
2.3 Response Time

The time interval from a step change in He concentration at the input of the sampling system to
the time at which 90 percent of the corresponding final value is reached as displayed on the
instrument readout mester.
3. APPARATUS
3.1 Monitoring Instrument
3.1.1 Specifications
a) The He instrument detector type may include, but is not limited to, mass spectrometry, infrared
absorption, and molecular screening.
b) Both the linear response range and the measurable range of the instrument shall encompass the
leak definition concentration specified in the regulation. A dilution probe assembly may be used
to bring the He concentration within this range, however, the specification for He sample probe
diameter shall still be met.
c) The scale of the instrument meter shall be readable to ±2.5 percent of the specified leak definition
concentration when performing a no detectable emission survey.
d) The instrument shall be equipped with an electrically driven pump to insure that a sample is
provided to the detector at a constant flow rate.
46
e) The instrument shall be equipped with a probe or probe extension for sampling not to exceed %
in. in outside diameter, with a single end opening for admission of sample.
3.1.2 Performance Criteria

a) The instrument pump, dilution probe (if any), sample probe and probe filter, that will be used
during testing, shall all be in place during the response time determination.
b) The calibration precision must be equal to or less than 10 percent of the calibration gas value.
c) The evaluation procedure for each parameter is given in Section 4.4.
3.1.3 Performance Evaluation Requirements

The calibration precision test must be completed prior to placing the analyser into service, and
at subsequent 3-month intervals or at the next use whichever is later.
3.2 Calibration Gases

The monitoring instrument is calibrated in tenns of parts per million by volume (ppmv) of helium
specified in the applicable regulation. The calibration gases required for monitoring and
instrument performance evaluation are a zero gas (air, less than 10 ppmv He) and a calibration
gas in air mixture approximately equal to the leak definition specified in the regulation. If cylinder
calibration gas mixtures are used, they must be analysed and certified by the manufacturer to be
within ±2 percent accuracy, and a shelf life must be specified. Cylinder standards must be either
reanalysed or replaced at the end of the specified shelf life. Alternatively, calibration gases may
be prepared by the user according to any accepted gaseous standards preparation procedure that
will yield a mixture accurate to within ±2 percent. Prepared standards must be replaced each day
of use unless it can be demonstrated that degradation does not occur during storage.
4. PROCEDURES
4.1 Pretest Preparations
Perform the instrument evaluation procedures given in Section 4.4 if the evaluation requirements
of Section 3.1.3 have not been met.
4.2 Calibration Procedures

Assemble and start up the He analyser according to the manufacturer's instructions. After the
appropriate warmup period and zero internal calibration procedure, introduce the calibration gas
into the instrument sample probe. Adjust the instrument meter readout to correspond to the
calibration gas value.
NOTE: If the meter readout cannot be adjusted to the proper value, a malfunction of the analyser
is indicated and corrective actions are necessary before use.
4.3 Individual Source Surveys

Determine the local ambient concentration around the source by moving the probe inlet randomly
upwind at a distance of one to two meters from the source, but in no case shall the distance be
less than 25 centimetres.
Place the probe inlet at the surface of the component interface where leakage could occur. Move
the probe along the interface periphery while observing the instrument readout. If an increased
meter reading is observed slowly sample the interface where leakage is indicated until the
maximum meter reading is obtained. Leave the probe inlet at this maximum reading location for
approximately two times the instrument response time. Subtract the local ambient concentration
from this reading.
Record and report the results as specified in the regulation reporting requirements. Examples
of the application of this general technique to specific locations are:
a) Valve Stem. The most common source of leaks from valves is at the seal between the stem and
housing. Place the probe at the interface where the stem exits the packing gland and sample the
stem circumference. Also, place the probe at the interface of the packing gland take-up flange
seat and sample the periphery.
b) Flanges
Place the probe at the outer edge of the flange-gasket interface and sample the circumference
of the flange.
47
4.4 Instrument Evaluation Procedures

At the beginning of the instrument performance evaluation test, assemble and start up the
instrument according to the manufacturer's instructions for recommended warmup period and
preliminary adjustments.
4.4.1 Calibration Precision

Make a total of three measurements by alternatively using zero gas and the specified calibration
gas. Record the meter readings. Calculate the average algebraic difference between the meter
readings and the known value. Divide this average difference by the known calibration value and
multiply by 100 to express the resulting calibration precision as a percentage.
4.4.2 Response Time

Introduce zero gas into the instrument sample probe. When the meter reading has stabilized,
switch quickly to the specified calibration gas. Measure the time from switching to when 90
percent of the final stable reading is attained. Perform this test sequence three times and record
the results. Calculate the average response time.
European Commission
EUR 19772 - Valve Stem Leak - Tightness Test Methodologies
Project Coordinator: BHR Group Limited

Partners: CETIM
Neles Automation
Chesterton
Association Française des Industries de ¡a Robinetterie
ElfAntar
Inficon
Alcatel CTT
Luxembourg: Office for Officiai Publications ofthe European Communities
2000 - 55pp., num. tab.
BCR information series
ISBN 92-894-0502-3
The emergence of standards on leak-tightness of industrial valves has given rise to a set of
problems associated with the way in which leak-tightness is both measured and expressed.
Issues surround:
• The specified gas

End users prefer a leakage targets in gases representative of the duty. Valve
manufacturers and test houses prefer the use of helium as a safe, detectable, inert test gas,
widely used for leak testing in many other contexts.
• The measurement method

Many end users prefer a leak-tightness result expressed in terms of ppmv measured by
sniffing, since this is the format of Environmental Protection Agency (EPA) targets in the
USA and is widely used across the world for on-site leakage detection and repair (LDAR)
programmes.
Unfortunately, ppmv is a not a measure of leakage rate, but rather provides an indication of
leakage severity. Thus, the requirement is for means of "translating" both between ppmv and
leak rate and between leakage of one gas and leakage of another under similar conditions.
"Translation" between ppmv and leakage is usually accomplished by means of empirical

power law correlations. However, due to the wide range of data sources on which they are
based, scatter in the data is very broad, rendering this approach, as it stands, unsuitable for
valve qualification and QA test standards.
"Translation" between leakage rates of different gases can either adopt a similar empirical
approach or, alternatively be based on predictive relationships derived from an understanding
of which leakage mechanism predominates. Until now, little directly relevant work has been
undertaken in this area.
The work reported here provides relevant technical data and analysis to help resolve these
issues by:
• investigating measurement methods and recommending means by which scatter in the

relationships between ppmv and leak rate can be dramatically reduced;
• evaluating measurements of leakage of different gases under similar conditions to identify

means of predicting leakage of various gases from measurements of helium leakage.
Experimental work was concentrated on valves representative of typical volatile organic

compound (VOC) duties over a range of sizes and types (but particularly 4" Class 300 gate
valves) with several different packing types (but mostly graphite) over a range of leakage
rates representative of this duty.
Conclusions are offered in Section 10.

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European Commission

Valve Stem Leak-Tightness

COMPETITIVE A N D SUSTAINABLE GROWTH

Valve Stem Leak-Tightness Test Methodologies

PROJECT COORDINATOR: BHR Group Limited

Contract No. SMT4-CT97-2158

Research Directorate General _

2000 EUR 19772 EN

Published by the EUROPEAN COMMISSION

Cataloguing data can be found at the end of this publication.

Luxembourg: Office for Official Publications of the European Communities, 2000

4.2 Preliminary survey of measurement methods 7

4.3 Scope and approach of experimental programme 8

4.3.1 Evaluation of measurement methods 8

4.3.1.2 The flush method 9

4.3.2 Different gases at room temperature 10

4.3.3 Different gases at elevated temperatures 11

5.2 Initial evaluation tests 13

5.3 Confirmatory tests 13

6. RELATIONSHIP BETWEEN PPMV AND LEAK RATE (SAME GAS) 15

6.1 Sniffer evaluation tests 15

6.2 Discussion of sniffer evaluation tests 16

6.3 Power law correlation or "sniffing factor" approach? 18

7. RELATIONSHIP BETWEEN LEAK RATES OF DIFFERENT GASES 21

7.1 Correlation or prediction? 21

7.2 Room temperature experiments 22

7.2.1 Power law correlation approach 22

7.2.2 Theoretical predictive relationships _ 24

7.3 The effect of temperature 28

7.3.2 Leakage mechanismforhelium 28

8. QUALIFICATION TEST MEASUREMENTS AND SITE PERFORMANCE 31

8.1 Helium leakage to VOC leakage 31

8.2 VOC leakage to VOC ppmv 31

9. RELATIONSHIP OF OA TESTS TO QUALIFICATION TESTS 36

9.1 Relationship between ppmv of helium and leak rate thresholds 36

9.2 Establishment of appropriate threshold value 36

APPENDIX 1 - GLOSSARY OF TERMS 42

APPENDIX 3 - ADAPTATION OF EPA METHOD 21 FOR HELIUM SNIFFER

• The specified gas

• The measurement method

• investigating measurement methods and recommending means by which scatter in the

·. evaluating measurements of leakage of different gases under similar conditions to identify

Experimental work was concentrated on valves representative of typical volatile organic

Conclusions are offered in Section 10.

1. adequate leakage performance after a representative number of mechanical and thermal

2. an acceptably low percentage of installed valves exceeding the leak-tightness

This work concerns measurement methods for qualification and QA tests.

Coordinator: BHR Group Limited

European Sealing Association

Associated Elf Antar France

ppmv leak rate leak rate ppmv

Most convenient Stipulation in Required for Preferred by many

Fig. 1 - Four possible combinations of test gas and leak-tightness specification:

1. to establish measurement practices and procedures which improve accuracy and

3. to suggest, if possible, means of "translating" between the measurement possibilities

4.2 Preliminary survey of measurement methods

4.3 Scope and approach of experimental programme

4.3.1 Evaluation of measurement methods

Fig. 2 - Three measurement methods used