COS-ISO-00-OGN/OPS/CHEM/011

Rev. No.: 0 July 1999

OPERATION GUIDANCE NOTE

The Sampling of Steam and Water for

Chemical Monitoring and Analysis

OPERATION SERVICES DIVISION

National Thermal Power Corporation Ltd.

NATIONAL THERMAL POWER CORPORATION

OPERATION DIVISION FORMAL DOCUMENTATION SYSTEM
OPERATION GUIDANCE NOTE : COS-ISO-00-OGN/OPS/CHEM/011
Rev. No. : 0

Date : July 1999

The Sampling of Steam and Water for

Chemical Monitoring and Analysis

Approved for
Implementation by ..
Director (Operation)
Date: ..

Inquiries to: Head of Corp. Operation Services

The Sampling of Steam and Water

for Chemical Monitoring and Analysis
CONTENTS
S.No. Particulars

Page No.

1.0

SCOPE

2.0

SUPERSEDED DOCUMENTS

3.0

REFERENCES

4.0

DEFINITIONS

5.0

SAMPLING EQUIPMENT - TERMINOLOGY

6.0

WATER SAMPLING

6.1 General

6.2 Sampling Soluble Species

6.3 Sampling Particulate Species

6.4 Positioning & Installation of samplers

7.0

8.0

6.4.1 Samplers Type W1 & W2

6.4.2 Samplers Type W3 & W4

6.4.3 Boiler Water Sampling

Steam Sampling

7.1 General

7.2 Sampling Saturated Steam

7.3 Boiler Water Sampling

Use of Capillaries for Sampling

8.1 General

8.2 Methods of Preventing Blockage

Sample Abstraction for Manual Analysis

9.1 General

9.2 Sample Containers and Storage

9.3 Sampling Line Purging before Sample Abstraction

9.4 Liquid Samples (other than those taken from capillary lines)

9.5 Sampling Liquids for Particulates using samplers with

Capillary Lines

9.6 Sampling for Dissolved Gases

10.0

Further Information

11.0

Review

9.0

ANNEXURE

10

Calculation of Capillary Length

10

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The Sampling of Steam and Water for Chemical Monitoring and Analysis

THE SAMPLING OF STEAM AND WATER

FOR CHEMICAL MONITORING AND ANALYSIS
1.0 SCOPE
This document provides guidance on various aspects relating to the conditioning
and collection of samples of steam and water at power stations.
2.0 SUPERSEDED DOCUMENTS
Nil
3.0 REFERENCES
This Guidance Note makes reference to, or should be read in conjunction with the
following documents :
OD/OPS/CHEM/001 : Chemical Control of Water / Steam Circuits of Drum
Type Boilers
4.0

DEFINITIONS
For the purposes of this Guidance Note, the following definitions will apply :
Iso Kinetic Sampling
A technique in which the sample from a fluid stream passes into the orifice of a
sampling probe with a velocity equal to that of the stream in the immediate vicinity
of the probe (Isokinetic Sampling).
Sampler
A device used to obtain a sample of water or steam, either discretely or
continuously, for the purpose of examination of various defined characteristics.
Sampling Point
The precise position within a system from which a sample is taken.
Sampling Probe
That part of sample equipment, which is inserted into a body of steam or water
and into which the sample initially passes.
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The Sampling of Steam and Water for Chemical Monitoring and Analysis

Sampling Line
The conduit which leads from the sampling probe to the sample delivery point or
the analysing equipment.
Sampling Delivery Point
The end of a sampling line often remote from the sampling probe, from which a
sample is removed, either discretely or continuously, for examination.
5.0

SAMPLING EQUIPMENT - TERMINOLOGY

Historically, sampling equipment has fallen into two categories :
(i)

So-called fast sampling equipment in which the flow rate is controlled by the
use of one or more pressure regulating valves.

(ii)

Capillary sampling equipment in which the pressure and volume flow rates
are controlled solely by the length and bore of capillary tube which forms an
integral part of the sampler.

While "fast" sampling equipment is recognized as appropriate for the sampling of

water for soluble components, capillary sampler were originally developed for the
sampling of particulates, taking into account the desirability, firstly to sample
isokinetically and secondly, to minimize subsequent deposition of the particulates
in the sample line. As a consequence; the terms, 'isokinetic' and 'capillary' have
become almost synonymous when used in this context and the tendency has
arisen to associate only this type of sampler with the sampling of particulates whether in water or steam. However, in some power stations, 'fast' samplers
have been used successfully to abstract two-phase samples under essentially
isokinetic conditions and conversely, capillary systems have also been used for
sampling water for soluble components.
These designs allow for the sampling of both soluble and particulate matter in
water at pressure upto 300 bar and in steam at a maximum pressure of 200 bar.
Here, samplers are referred to as Types W1-W4 (for water) and S1-S2 (for
steam). Guidance on this use and application is provided by this Guidance
document.
6.0 WATER SAMPLING
6.1

General

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The Sampling of Steam and Water for Chemical Monitoring and Analysis
A pre-requisite of any sampling system is that it should extract a sample
representative of the fluid in the system for subsequent analysis. Problems are
most likely to arise when more than one phase is present.
6.2 Sampling soluble species
In instances where the subsequent analysis is for soluble species, a sampler of
type W1, W2 or W4 should be chosen, depending upon the pressure of the
system. With samplers W1 and W2 installed as recommended, i.e. with the inlet
slot facing away from the direction of flow, ingress of particulates is minimized and
thus deposition and the risk of blockage within the sample line reduced. The
need for this applies especially where long sample lines are used to route
samples to the on-line instrumentation.
6.3

Sampling Particulate Species

Representative sampling of particulates in water is important when analysing for
corrosion products of, for example, copper, iron or nickel. Such analysis may be
required, for example, to assess the extent of erosion or corrosion in the system,
or the efficiency of chemical conditioning. Ideally, sample abstraction should be
at, or near, isokinetic flow rates. Also, although sampling systems with control
valves are widely used, it is essential to avoid the problem of deposition of the
particulate material in valves or stagnant regions of the sampler itself. For this
reason, samplers have been developed which use the frictional drag of the
internal surfaces of a Stainless Steel capillary valve. Capillary samplers,
however, require a high level of attention, with respect to both their installation
and maintenance. They are, therefore, best regarded as scientific instruments
rather than station hardware and should be treated accordingly.
In some instances, a practical alternative to using capillary samplers is to use
samplers (as appropriate to the pressure) but with the inlet slot directed to face
into the flow. If this approach is adopted, it should be recognized that
experimental evidence suggests that the results from samples obtained in this
manner may be biased low compared with those obtained from capillary
samplers. This is probably due to a combination of factors, such as a departure
from isokinetic conditions and possible increased deposition in the sample lines.
For pressure upto 40 bar, a combined wide bore and capillary sampler is
available. By requiring only one entry point into the feed-line, installation is easier
and there is minimum interference with the mechanical integrity of the feed pipe
walls.
However, samplers are fitted with two identical capillaries, so that should one
become irreversibly blocked, the other may be used until such time as the unit
comes off load and a replacement can be fitted.
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The Sampling of Steam and Water for Chemical Monitoring and Analysis

6.4

Positioning and Installation of Samplers

There are numerous locations on power station where steam and water sampling
is required. Care should be taken in choosing the right type of sampler and
determining its proper positioning to suit the particular application. Generally,
sampling points should be chosen so as to avoid dead spaces and sections of the
plant, which are likely to be bypassed.

6.4.1 Type W1 and W2

There is no evidence that the siting of Types W1 and W2 for sampling of soluble
components is critical, other than to ensure that they are sufficiently downstream
of an injection point of a chemical or water stream for complete mixing to have
occurred. However, when Type W2 is used in conjunction with a Type W3
sampler (e.g. for assessing the overall efficiency of feed-water treatment), it
should be sited adjacent to, but downstream of this sampler.
6.4.2 Type W3 and W4
The principal use of samplers with capillary tubing is for the representative
sampling of suspended solids in water. When used for this purpose, it is
important that these samplers should be unaffected by disturbances in the main
flow. Ideally, Types W3 and W4 samplers should be located in vertical sections of
system pipe work with an ascending flow and at least five diameters before and
ten diameters after bends, valves and venturis, etc. However, in a modern power
station plant, it may be difficult to satisfy these conditions. Consequently, where
the ideal point cannot be found, the samplers should be sited two-thirds of the
way along the longest straight pipe in the relevant section of the system pipe
work.
6.4.3 Boiler Water Sampling
Boiler water sampling on some stations is achieved using a multi-tube sampling
arrangement mounted so as to obtain a representative sample along the length of
the drum. Whilst this may be adequate, an arrangement by which samples are
taken using the Type W2 sampler from a number of down comers and
subsequently combined by means of a manifold system, is much preferred. This
ensures that the sample taken for analysis is more representative of the water
reaching the evaporative surfaces of the boiler.
The W2 sampler should be positioned such that its inlet slot is away from the
direction of flow.

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The Sampling of Steam and Water for Chemical Monitoring and Analysis

7.0

STEAM SAMPLING

7.1

General
One of the principal problems with steam sampling, particularly saturated steam,
is that there are large density differences between the phases. There may also
be problems of solids deposition at the initial stages of steam condensation.

7.2

Sampling Saturated Steam

With the sampling of saturated steam, the additional problems of coalescence
and condensation militate against representative sampling. Nevertheless, there
are measures which can be taken to reduce errors. Firstly, it is best to sample
from a number of steam risers from the drum, combining the samples into one by
means of a manifold, before passing the combined sample to a cooler for
condensation and subsequent transport and/or collection. Secondly, it is
recommended that the Type S1 steam sampler be used for this purpose with
sample flows adjusted to give isokinetic sampling conditions at the sample inlet.
In this case, the sampler orifice should face the direction of flow.
The preference is for any valves to be mounted on the samplers but if the sampler
is mounted at a location which is not accessible in normal operation, then the
valves should be mounted along the sample line at the first accessible point.

7.3

Sampling Superheated Steam

There are two types of superheated steam samplers. Type S1 is more suitable for
insertion in small diameter pipes as part of a multipoint sampling system, in
which flows are combined to provide adequate samples for analysis and Type S2
is more appropriate where it is required to obtain a good, average sample from a
single penetration into one large bore pipe.
In both instances, a cooler should be installed immediately after the isolating
valves. Sample flow rates should be adjusted to give "isokinetic" sampling
conditions or, alternatively, by a length of capillary installed at the cooler outlet. In
the latter instance, the length of capillary required can be estimated, using the
procedure given in Annexure. The use of a capillary device is more suitable for
local manual sampling.
It should be remembered that the cooling water requirements for condensing and
cooling superheated steam samples are considerable and consequently, every
effort should be made to keep the sample volume flow rate to the minimum
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The Sampling of Steam and Water for Chemical Monitoring and Analysis
necessary for analytical demands. As a guide for 1 kg/min of sample, 57 KW of
heat need to be dissipated. With superheated steam at 160 bar and assuming a
cooling water inlet temperature of 20 deg. C, a cooling water rise of 15 deg.C and
counter current cooling, this corresponds to a cooling water flow rate of 54 kg/min.
8.0

USE OF CAPILLARIES FOR SAMPLING

8.1

General
Capillaries are a feature of water samplers and are used as a means of reducing
the sample pressure and controlling flow rate without the need for valves, which
helps avoid the problem of deposition. They require special and careful
treatment, however, in respect of both installation and use.

8.2

Methods of Preventing Blockage

Total blockage can best be prevented by ensuring that :
i. The sampling system is correctly installed with the minimum of horizontal
runs.
ii. Cooling water supplies are adequate and reliable.
iii. Regular flow rate checks are made to identify partial blockages.
Unless samples for the analysis of particulate matter are required during period of
heavy debris levels, i.e. start-up or commissioning, the capillary should be
blanked off using a suitable nipple and compression fitting.

9.0

SAMPLE ABSTRACTION FOR MANUAL ANALYSIS

9.1

General
The individual methods also describe suitable methods for cleaning sampling
vessels. Once cleaned, precautions should be taken to ensure that they remain
clean. In many cases, this can be done by enclosing the vessels in polyethylene
bags.

9.2

Sample containers and storage

The determination of trace impurities in high purity water imposes stringent
requirements on all aspects of the analytical process. Contamination can occur,
for example, from the atmosphere, from handling and by leaching from poorly
cleaned containers. On the other hand, trace constituents can be lost during
storage by volatilization, precipitation or absorption on to the container walls. The
latter phenomenon can occur, particularly with those species such as transition
metal ions, which will hydrolyse if the sample is not sufficiently acidic.

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Commercially available plastic containers have been found adequate for storage
of high purity water for periods of upto 8 days although contact time with any
container material should be kept to a minimum. Plastic containers are necessary
for the determination of ionic species such as sodium and potassium in stored
grab samples, but unsuitable for dissolved gas and total organic carbon analysis.
Suggested plastic container materials include polystyrene, polypropylene and
polyethylene.
Boro silicate glass containers are recommended for storage of water samples for
total organic carbon (TOC) determinations. They may be cleaned and sterilized
in accordance with ASTM D -3694.
Sample bottle cleaning is essential to achieve reliable grab sample analysis.
A suitable procedure is as follows :
Flush the container with demineralised water at least three times, then fill
completely, cap and allow to soak for at least 1 day, but not more than 5 days. If
5 days storage is exceeded before use, the container should be refilled with fresh,
high purity water. The high purity water is left in the container until sampling. It is
advisable that plastic gloves be worn throughout the cleaning, sampling and
transfer of the sample to the analytical instrumentation to avoid contamination
from the hands. This is particularly the case for sodium and chloride analysis.
9.3

Sampling Line Purging before Sample Abstraction

Although samplers with capillary sampling lines are continuously running, this
may not be the case with other types of sampler. Therefore, if the sample line is
closed off by a stop valve, the line must be purged for sufficient time before a
sample is collected. This is to ensure that a representative sample is obtained.
A sample flow rate of about 500 ml/min., cooled to less than 40 deg. C, should be
maintained.
Whenever samples are being collected, it is essential, especially for particulates
that there are no mechanical or pressure shocks to the system which could cause
excessive amounts of solid material to be transferred to the sample container.

9.4

Liquid Samples (Other than those taken from capillary lines)

The sampling procedure for liquid samples should be as follows :
Empty the soak water from the sample container and rinse at least three times by
filling it to about one-quarter capacity with sample water; shake, then empty the
container. When sampling for dissolved solids, the sample should be collected
with the end of the sample tubing at the mouth of, but not touching the sample
bottle. The sample should not come in contact with the outside of the sample
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tube. When sampling for organics or for atmospheric constituents, the grab
sample should be collected by an upward displacement through a tube extending
to the bottom of the container. Allow the container to overflow at least five
volumes, then close the container with a cap which has been rinsed with the
sample water.
9.5

Sampling Liquids for Particulates using samplers with capillary lines

The sampling vessel should consist of a polyethylene bottle with polyethylene cap
previously cleaned as described in the method (e.g. for nickel, iron or copper). A
hole should be drilled in the polyethylene cap and a length of PVC tubing shall be
tightly fitted through the cap with 25mm of tubing projecting into the bottle. The
I.D. and O.D. of the PVC tubing should be such that it will fit snugly over the end
of the capillary sampling line. The most suitable length of this sampling tube will
vary depending on local conditions at the sample delivery point, but about 13 mm
projecting out of the cap should be adequate. If necessary, this length can be
increased to about 100 mm. One 6 mm length of PVC tubing of I.D.
approximately that of the above PVC tubing is pushed over the PVC sampling
tube until it is flush with the external surface of the cap and another 6 mm length
pushed against the internal surface of the cap. These two 6 mm sleeves are
cemented to the inner sampling tube with PVC cement or cyclohexanone, thus
ensuring that it is held tightly in position. The bottle is calibrated for the desired
volume of sample and then the bottle and cap are cleaned according to the
instructions given with each method. After cleaning, the bottle is covered with a
polythene bag held in place by a rubber band.
To collect a sample, the correct amount of acid, as indicated in the method, is
added to the bottle and the polythene cap and the bag is replaced. A hole is
punctured in the bag by means of the capillary tip, previously washed with distilled
water and the capillary tip securely connected to the PVC tubing. It is essential
that the tip of the capillary be as smooth as possible to avoid cutting the plastic
tubing and thereby, possibly, blocking the capillary with small pieces of PVC. If
difficulties are encountered in making a connection, the end of the capillary can
be tapered or alternatively, the bore of the PVC tubing can be increased by
means of a hot wire. Loosen the bottle top to permit air displacement and collect
the required volume of sample. Disconnect the capillary and adjust the polythene
bag and rubber band so that the cap and sampling tube are protected against
contamination, i.e. so that contaminants cannot pass through the hold which has
been punctured in the polythene bag.

9.6

Sampling For Dissolved Gases

If water is passed through continuous lengths of metal or glass tubing, there
should be no errors in oxygen and carbon dioxide measurement from in-leakage
of air from the atmosphere. The main likelihood of contamination is where two
pieces of rigid tubing need to be joined by a flexible coupling, since unless the
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The Sampling of Steam and Water for Chemical Monitoring and Analysis
right connecting material is used, permeation of air into the sample stream can
occur. Thick-walled neoprene tubing as a suitable coupling material, but even
with this, it is advisable to keep the length of tubing as short as possible and use it
simply as a connecting sleeve to make butt joints between the two sections of
rigid tubing.
10.0

FURTHER INFORMATION
Further information on sampling procedures and practices may be obtained
through OS/Engineering.

11.0

REVIEW
The head of Corporate Operation Services will be responsible for reviewing this
document on a 3 yearly basis, or as and when required .

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ANNEXURE
CALCULATION OF CAPILLARY LENGTH
Before an estimate can be made of the length of capillary to be installed, it is
necessary to calculate the mass flow rate delivered by the sampler under isokinetic conditions. This is done by the following formula:
m/M = (d/D)2 x n
Where,

m = sample mass flow rate

M = system mass flow rate
d = probe orifice diameter
D = pipe internal diameter
n = no. of orifices

With a knowledge of pressure at the main header and pressure drop (P) the
length of the capillary required can be calculated.
Pressure drop (P) across the capillary per meter the line length is calculated
using Darcy-Weishback formula as follows (Datas are given on the next page)
P

= f v2 / 2gd
= f(4Q/ d2)2 / 2gd

Thus,

= 8.271 x 10-2 (fQ2/d5)

( g = 9.8 m/sec2)

= 2.647 x 10-3 (Q2/d5)

(assuming f = 0.032)

= 2.647 x 10-3 (Q2/d5) in meter of liquid column per unit

length of capillary
= 2.647 x 10-4 (Q2 / d5 ) in kg /cm2 if the liquid being
sampled is water at ambient temperature

Where,

P
f
g

= Pressure drop (kg/cm2) in meters of liquid column

across the capillary per meter length of capillary
= pipe friction factor determined from catalogues for
stainless steel
= Acceleration due to gravity (m/sec2)

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Q = flow of sample (m3/sec)

D

= Internal diameter (in meter) of capillary

= velocity of fluid in the capillary in m/sec

EX AMPLE OF CALCULATION OF LENGTH OF CAPILLARY

Feed pipe internal diameter (D)

= 305 m

Water flow rate (M)

= 9740 kg/min at 70% MCR

Capillary internal diameter (d)

= 0.51 mm

No. of orifices (n)

=1

Thus, we have,
= (d/D)2 x n

m/M

Since the capillary is to be fixed to the main header, the capillary tip is to be bored
out to be 0.66 mm diameter.
Thus, we get
m/9740

= (0.66/305)2 x 1 (Using d = 0.66 mm )

= 0.0456 kg/min
= 7.6 x 10-7 m3/sec (taking density of sampled
water as 1000 Kg/m3)

Pressure drop per meter of capillary can be calculated as follows :

Q

= m = 7.6x 10-7 m3/sec

P = 2.647 X 10-4 (Q2 / d5 )
= 2.647 X 10-4 (7.6 X 10-7)2 / (0.00051)5
= 4.43 kg/cm2 per meter of capillary

Since the main header pressure is 180 Kg/cm 2, the theoretical length of capillary
to give a flow of 0.0456 kg/minutes shall be
180/4.43 = 40.63 meters.
Because of variation in water temperature along the length of the capillary and
uncertainties in the variability of capillary bore and surface condition, it is
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necessary to increase the length of installed capillary by 30% above the
calculated figure.
Hence the length of the capillary to be installed will be 40.63 x 1.30 = 52.82
meters.

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