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Diffusible hydrogen measurement in welding consumables using a new

proton-exchange-membrane based hydrogen sensor

Conference Paper · February 2009

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 National Welding Seminar 2009, , 4th-6th February, 2009, Mumbai, India

DIFFUSIBLE HYDROGEN MEASUREMENT IN WELDING

CONSUMABLES USING A NEW PROTON-EXCHANGE-MEMBRANE
BASED HYDROGEN SENSOR

Girsh Kumar Padhy, V.Ramasubbu*, N. Murugesan#, C. Remash#, S.K. Albert*

Homi Bhabha National Institute, Kalpakkam Campus
*Material Joining Section, Materials Technology Division,
#Radiochemistry Division
IGCAR, Kalpakkam, Tamilnadu-603102

Abstract

A new proton exchange membrane based hydrogen sensor (PEMHS) has been used for the
measurement of diffusible hydrogen in welding consumables. Hydrogen evolved from the specimen is
collected in a chamber filled with argon gas and concentration of hydrogen in the gas was measured
using the sensor. The PEMHS is a fuel cell based device and uses nafion as proton exchange membrane.
The sensing electrode is palladium black and the counter electrode is platinum black. The electrolyte is
sandwiched between the barriers and a diffusion barrier at the sensing electrode side limits the supply of
hydrogen to the sensing electrode. The sensing electrode is exposed to hydrogen in argon and the
counter electrode to air. The limiting current produced is linearly dependant on concentration of
hydrogen in argon and hence the sensor is an amperometric device. This sensor is very sensitive and can
accurately measure hydrogen in ppm level in the inert gas mixture. Hence in addition to the total
diffusible hydrogen evolved from the weld after 72 hours of exposure at ambient temperature, the sensor
can also detect hydrogen evolution from the sample as a function of time. The paper presents the
principles of hydrogen measurement using this sensor, its applications for diffusible hydrogen
measurements and the results obtained on diffusible hydrogen measurement of indigenously developed
modified 9Cr-1Mo electrodes.

Key Words:

Diffusible Hydrogen content, Hydrogen Diffusivity, Nafion Based Hydrogen Sensor, Polymer
Electrolyte Membrane, Diffusible Hydrogen Evolution

Introduction

Hydrogen Assisted Cracking (HAC) is a serious problem in ferritic and martensitic steel weld
metal and in the heat affected zone (HAZ) of the weld joints. The diffusible hydrogen content in welding
consumables is used extensively for predicting the susceptibility of weldment to HAC [1]. As the cracks
are not allowed in weld joints, formation of these cracks should be prevented. The main source of
hydrogen in welds is the moisture content present in the flux coating of the electrode [2]. Other sources
include shielding gas, the oil /grease on the surface to be welded and the surrounding atmosphere.
During welding, the high temperature generated in the welding arc causes dissociation of water molecule
into hydrogen and oxygen and dissolution/absorption of the atomic hydrogen in the weld pool from the
arc atmosphere. The solubility of hydrogen in ferritic steel is less than 2 ppm at room temperature. As
the cooling rate is rapid in welds, no equilibrium is attained and the supersaturated hydrogen in the weld
metal diffuses into the HAZ or out of the weld during solidification and subsequent cooling of the weld.
Most of it is trapped at various defects such as grain boundaries, lath boundaries, dislocations etc. in the
weld and in the HAZ. Not all the supersaturated hydrogen is free to diffuse. Diffusion of hydrogen is
possible only if it is released from the traps which in turn depend upon the binding energy of the traps.
Hence only a part of the total hydrogen tends to diffuse at or near room temperature which is referred as
diffusible hydrogen (HD). The diffusible hydrogen interacts with the defects in the weld causing HAC.
Hence, diffusible hydrogen content in the weld metal shall be controlled to decrease cracking in the weld
joints of steels. This in turn requires measurement of diffusible hydrogen in the weld metal by a suitable
technique. As one of the major sources of hydrogen is the consumables, high diffusible hydrogen
content indicates hydrogen introduced from the welding consumable into the weld metal is high. Hence,
diffusible hydrogen content (HD – ml of hydrogen in 100 g of weld metal) is used to classify the welding
consumables on the basis of their hydrogen content. HD content is also useful to predict the minimum
preheat temperature to be employed during welding of steels to avoid cracking [3,4]. The estimation of
HD content from a weld is carried out by allowing hydrogen from the weld to diffuse out for a given time
at a fixed temperature and measuring its volume. The standard methods recommended by ISO, AWS,
DIN, BIS etc. are gas chromatography method and mercury method [5,6,7,8,9]. With both of these
methods measurement of diffusible hydrogen is done at high accuracy. Both the methods have a 1:1
correlation with the results obtained for HD content in ml/100 g of weld [10]. However, these methods
are not without drawbacks. One of the limitations with the mercury method is that the handling of
mercury is hazardous. In this method, only that diffusible hydrogen is measured which is evolved within
72 h of the welding at ambient temperature is measured where as the continuation of diffusible
hydrogen evolution for over 21 days has been reported[11] Also this method uses 72 hours for hydrogen
evolution which is time consuming. The gas chromatography method consumes lesser time (typically
~6 h); but hydrogen evolution is conducted at high temperatures. Another method which was in use but
now being discarded is the glycerin method [12,13]. Determination of HD content by mass spectrometer
has been also reported [14,15].
Recently a sensor for quantitative measurement of hydrogen content in gas mixtures were
developed from a conducting polymer prepared from Polyvinyl Alcohol (PVA) and phosphoric acid as
electrolyte membrane in an Amperometric Hydrogen Sensor operated in the fuel cell mode [16].The
feasibility of PVA based amperometric hydrogen sensor for diffusible hydrogen measurement has been
demonstrated [ 17 , 18 ]. The performance of the sensor agrees well with that of the standard Gas
Chromatography method [17]. The advantages of using the PVA based sensor are, it is simple in
construction, compact, cheaper and can be used in field applications to measure HD in welds. The
chamber can also be designed for HD measurements at elevated temperatures. As the long term stability
of the PVA membrane was poor, a new proton exchange membrane in which Nafion is replaced with the
PVA has been developed and this sensor shows better stability than that based on PVA. The new sensor
operates in fuel cell mode with a mechanical barrier limiting the supply of hydrogen to the sensing side
electrode. The sensor is designed as a two electrode device for hydrogen measurement in a gas mixture
containing hydrogen. Either platinum or palladium was used at the sensing electrode side and platinum
at counter electrode side. [ 19 ]. The present paper discusses the diffusible hydrogen measurements
carried out on standard specimens, which were prepared using modified 9Cr-1Mo steel base plate and
electrode. The sensor directly displays the response corresponding to the current generated due to the
hydrogen using the stored calibration parameters on a display unit and the in situ data acquisition is
done.
Experimental
Materials required for the Measurement
Test specimen preparation
The diffusible hydrogen measurements were done with indigenously developed modified 9Cr-
1Mo steel. The chemical composition of this steel is given in Table 1.The 9Cr-1Mo steel is available as
12 mm thick plate from which test specimens of dimension 30 mm x 15 mm x10 mm are machined out
as prescribed by ISO 3690. Run-on and run-off pieces of dimension 44 mm x 15 mm x 10 mm are also
machined out. The dimensional tolerance of the triplicate pieces are within ± 0.25 mm and all surfaces
are finished at right angles to ensure good contact between adjacent pieces. The schematic diagram of
test piece assembly which is shown in Fig. 1.

Table. 1 Chemical composition in Wt% of modified 9Cr-IMo steel plate and an electrode
Material C Cr Mo Mn Ni S P V Nb Cu N AI
Base metal 0.10 9.50 1.00 0.39 0.14 0.009 0.021 0.250 0.10 ------- 0.065 0.024
Electrode 0.10 9.00 1.00 0.70 0.70 0.012 0.009 0.017 0.06 0.05 0.055 0.010

Fig.1 Specimen assembly

Welding fixture
A welding jig made of copper is shown in Fig. 2. It is designed to promote the proper alignment
and clamping of the test piece assembly by means of a single clamping unit which is used with a ring
spanner. The use of copper facilitates high rate of heat removal from the specimen.

All dimensions in millimeters

Fig.2 Test piece assembly (welding jig) for hydrogen sampling of weld deposit
Specimen Chamber

The specimen chamber [20,21] used to collect diffusible hydrogen is essentially a stainless steel
chamber having an inlet and an outlet connected to needle valves. The chamber can be opened or closed
using a plug and the leak tightness of the plug is ensured with the help of an O-ring. Further by
performing Helium Leak Test of the chamber it is ensured that the leak rate of the chamber is less than
10 -9 std cc/min. Fig.3 shows the schematic of the specimen chamber along with plug. The volume of the
chamber is measured by filling it with distilled water and draining the water completely into a measuring
jar and measuring the volume of water.

Fig.3 specimen chamber with plug

Gas sampling valve
An eight-port gas sampling valve with a sampling loop of known volume was used for sampling
the gas from the specimen chamber for analysis. The sampling valve operates in two modes as shown in
Fig.4. In mode 1 shown in Fig.4 (a), the inlet of the sampling loop is connected to the specimen chamber
and the outlet is open to atmosphere. In this mode only the carrier gas line is connected to the
detector/sensor. In mode 2 shown in Fig.4 (b) the inlet of the sampling loop was connected to the carrier
gas line and outlet to the detector/sensor. For analysis of the gas, initially the valve is operated at mode 1
and the gas from the specimen chamber which is filled at a higher pressure than the ambient pressure, is
used to flush and fill the sampling loop while the carrier gas flows into the sensor. Subsequently the
valve is switched over to mode 2 operation and the carrier gas flows through the sampling loop to the
sensor carrying the gas present in the loop along with it. The sensor detects hydrogen and gives a signal
corresponding to it’s concentration in the gas mixture.
 Hydrogen
Sensor

1
2
8

Sample
Gas 3 Exit
7

4
Sampling 6

loop 5

Sampling
loop

(a) Mode 1

Hydrogen
Sensor

1
2
8

Sample 3

Gas 7
Exit

4
Sampling 6
5
Loop

Carrier
Gas

(b) Mode 2
Fig.4 Operation of eight-port sampling valve
The hydrogen sensor
The main component of the sensor is a conducting polymer, nafion. The polymer was cast as a
film, coated with palladium black on the sensing side, with platinum on the counter side and electrical
leads were taken. The sensing side of the coated polymer was exposed to the hydrogen argon gas
mixture while the counter side was exposed to air. Thus the sensor consisted of hydrogen exposed inner
palladium film and air exposed outer platinum film with the conducting polymer nafion sandwiched
between them and this acted as a fuel cell. A schematic representation of the sensor with conducting
leads is shown in Fig.5. Hydrogen present in the Ar-H2 mixture gets adsorbed at the sensing electrode
and looses its electron to form H+ which conducts through the polymer to reach the counter electrode
where it reacts with oxygen to form H2O. The signal corresponding to the short circuit current thus
produced due to conduction of hydrogen ion through the polymer was measured which in turn is used to
measure the concentration of hydrogen in the sampling chamber.

A-Polymer Electrolyte Membrane

B-Sensing Electrode (Pd film)
C- Counter Electrode (Pt film)
Fig.5 Schematic representation of the reactions taking place in the sensor

Diffusible Hydrogen Measurement procedure

Preparation of specimen for the HD measurement
The modified 9Cr-1Mo steel test sample was weighed to the nearest 0.01g. Bead-on-plate welds
were made on the specimen blank clamped on to the copper jig using SMAW process and the welding
electrode for which HD measurement is conducted. A good contact between the triplicate set of test
assembly and the copper fixture shown in Fig.2 was ensured for easy removal heat from the specimen.
The electrode used was an indigenously developed welding consumable for modified 9Cr-1Mo steel.
The weld metal was deposited on the base plate specimen blank using baked and unbaked electrodes.
Prior to deposition some of the specimen blanks were subjected to degassing at 650º C for 1 h and they
were subsequently stored in desiccators while others were used without degassing heat treatment. The
electrode baking treatment was 300º C /2 h and they were subsequently stored in and oven maintained at
150º C [7]. The welding parameters employed are given in Table 2.
Table 2: Welding parameters for the preparation of specimen
 Current, (I) Voltage, (V) Speed, (mm/s) Heat input (J/mm)
91 27 2.85 862

Measurement of HD using the sensor

The specimen assembly for HD measurement was removed from the copper fixture immediately
after welding and quenched [22] in liquid nitrogen for 3-4 minutes and the test specimen was separated
from the run-on and run-off pieces with a hammer within 6 seconds. Then flux and ice condensed on the
specimen while taking out of liquid nitrogen were removed, the specimen was cleaned with acetone and
transferred to the specimen chamber. All these processes were completed within 30 seconds. The
specimen chamber was then closed, flushed and filled with argon gas at a positive pressure of 4 kg/mm2
and kept in an oven 45C for 72 hours. Hydrogen evolved from the specimen was collected inside the
chamber.
Prior to measurement the sensor was calibrated for different concentrations of H2-Ar mixtures.
The response obtained from the sensor is recorded with the help of a display unit and an x-t data
acquisition system. After calibration, the sampling loop inlet of the 8-port valve was connected to the
specimen chamber which is at a higher pressure. The loop is first flushed with the sample gas and then
sample gas from the chamber is injected into the sensor in the injection mode of the 8-port valve. A
response corresponding to the concentration of hydrogen in the chamber is recorded in the data
acquisition system. As the specimen chamber is at a higher pressure than the ambient, it was possible to
make two to three measurements using the gas mixture inside the chamber. After the measurement of
hydrogen concentration is completed, the weld specimen was taken out from the chamber, cleaned with
acetone, dried and weighed. From the volume of the chamber, hydrogen concentration measured from
the sensor, weight of the specimen, HD content / 100g of the weld metal was estimated.
In addition to standard measurement, hydrogen evolution from the specimen at different time
intervals (0-24, 24-48, 48-72, 72-120, 12-168 and 168-196 h) was also measured using the sensor. After
each measurement, the chamber was flushed for a minute and then pressurized again with argon gas.

Results and Discussion

Standard measurement
Figure 6 shows a typical output from the sensor obtained during calibration of the sensor with
different concentration of hydrogen in the Ar-H2 mixture. A linear relationship is obtained when the
peak height in the x-t data corresponding to the concentration of hydrogen passed through the sensor is
plotted against concentration of hydrogen which is shown in Fig.7.
Diffusible hydrogen was measured with the use of the following sample-electrode combinations
Set-1: Specimen blank without degassing-Unbaked electrode
Set-2: Degassed specimen blank- Baked electrode
Set-3: Degassed specimen blank-Unbaked electrode
A number of measurements were carried out for each set of sample-electrode combinations. For
set-1, the specimen blanks machined out from the steel plates in the normalized and tempered condition
was used directly without any degassing heat treatment and the electrodes removed from the packets
were used without any baking. The results of the measurements in all the three conditions are
summarized in Table 3.
 0 .0 8
H y d r o g e n s e n s o r c a lib a r a tio n
0 .0 7

0 .0 6
Sensor Signal (a.u.)

1010 ppm
0 .0 5

0 .0 4 757 ppm

0 .0 3
505 ppm
0 .0 2
252 ppm
0 .0 1

0 .0 0
0 500 1000 1500 2000
T im e ( s )

Fig.6 Response of the hydrogen sensor for different concentration of hydrogen in H 2-Ar mixture.

0 .0 5 0
L in e a r R e g re s s io n
Y = A + B * X
0 .0 4 5
P a ra m e te r V a lu e E rro r
------------------------------------------------------------
0 .0 4 0 A -0 .0 0 2 4 0 .0 0 1 4 5
B 4 .7 6 4 E -5 2 .1 1 9 2 5 E -6
------------------------------------------------------------
Peak Height in a.u.

0 .0 3 5
R SD N P
------------------------------------------------------------
0 .0 3 0 0 .9 9 8 0 3 0 .0 0 1 1 8 4 0 .0 0 1 9 7
------------------------------------------------------------

0 .0 2 5

0 .0 2 0

0 .0 1 5

0 .0 1 0

200 300 400 500 600 700 800 900 1000 1100
C o n c . o f H 2 in p p m

Fig.7 Calibration curve for hydrogen sensor obtained using standard Ar-H 2 mixtures

Table 3. Volume of HD/ 100 g of weld metal

Sample-Electrode Combinations Average HD content in weld metal
(ml/100 g )
Set-1 4.2  1
Set-2 2.2  1
Set-3 3.4  1
 These results clearly show that this new hydrogen sensor can be used for diffusible hydrogen
measurements in the weld joints. The electrodes used for this study are fully basic with HD content
specified to be below 4 ml/100g of weldmetal and this is the reason for low values of HD obtained in the
present study. Further, they also reveal the effect of baking of the electrodes and degassing of the
specimen blanks on HD measurement. In the absence of degassing of the specimen blanks, results of HD
measurement could be significantly higher than the actual.
In addition to the results presented in Table 3, a set of measurements were also carried out with
unbaked electrodes exposed to atmosphere for several days (few months). For this measurement, welds
were deposited on the specimen blank that were degassed and stored in desiccators. The HD content
obtained for these specimens were as high as 5.7 ml/ 100 g of weld at an average. This result clearly
shows the moisture absorption can significantly increase the HD content in the weld and its cracking
susceptibility and highlights the importance of proper storage and handling of the electrodes once
removed from the packet or the baking oven.

Variation of diffusible hydrogen as a function of time

It is reported that the evolution of HD from the specimen can last as long as 21 days even though
the measurements are seldom carried for duration longer than 72 h. Due to high sensitivity of the
hydrogen sensor it was possible to use this sensor to measure hydrogen concentration even at very low
levels (<100 ppm). Hence this sensor can be successfully employed to study evolution of hydrogen as a
function of time. In this study, hydrogen concentration in the chamber was measured for different
duration from set-2 specimens starting from 24 to 196 h. It was observed that evolution of hydrogen did
not stop even after 196 hours. Figure 8 shows the cumulative diffusible hydrogen content obtained after
different duration of the measurements as a function of time. Figure 9 shows the hydrogen evolved
between two successive measurements. It is clear that the hydrogen evolution is the maximum within the
first 24 hours then it decreases exponentially with time. Both the figures clearly show the hydrogen
evolution continues much beyond 72 h, the maximum recommended duration for standard methods HD
measurements. In the case of modified 9Cr-1Mo steel, the base metal and welding consumable chosen
for this study, the high alloy content and martensitic microstructure of both the weld metal and HAZ
significantly reduces the apparent diffusivity of hydrogen at ambient tempearature [23] and this could be
a contributing factor to the slow evolution of hydrogen from the weld joint of this steel.
2.5
Cumulative Hydrogen Content in ml/100 g of weld

_________ polynomial fit

2.0

Polynomial Regression
y = a + b1*x + b2*x^2 + b3*x^3 + b4*x^4 + b5*x^5
1.5
Parameter Value Error
------------------------------------------------------------
a -0.05923 0.0102
b1 0.04178 0.00122
1.0 b2 -3.95733E-4 3.9669E-5
b3 2.3496E-6 5.09042E-7
b4 -7.71073E-9 2.79501E-9
b5 1.03687E-11 5.49691E-12
------------------------------------------------------------
0.5
R-Square(COD) SD N P
------------------------------------------------------------
0.99999 0.00556 7 0.00498

0.0
0 50 100 150 200
Time in Hours

Fig 8. Cumulative hydrogen content from the weld sample as a function of time
 two successive measurement (ml/100g of weld metal)
0.035

Hydrogen evolved during the time period between

0.030

0.025

0.020

0.015

0.010

0.005

0.000

20 40 60 80 100 120 140 160 180 200

Time in hours

Fig. 9 Variation of hydrogen evolution from the specimen with time expired after welding.
Conclusion
Major conclusions from this study are the following
a) The proton-exchange-membrane based hydrogen sensor has been successfully
employed for measuring diffusible hydrogen content in the welding consumables and to
study evolution of hydrogen from the weld as a function of time.
b) Hydrogen evolution from the standard specimen for HD measurement is maximum during
initial hours and decreases exponentially with time. However, it is found that hydrogen
evolution continues even after 72h, the maximum duration for hydrogen evolution in most
of the tests.
Acknowledgements
Authors thank S/Shri. M. Arul and D. Manokaran of Materials Joining Section, IGCAR for the
help extended for the preparation of the weld specimen and Shri A.V. Vinod of Radiochemistry
Division, IGCAR for diffusible hydrogen measurement.
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