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8.

2 Analyzer Sampling: Process Samples AR

W. M. BARROWS (1972) P. FOUNDOS (1982) (K. A. Perrotta and R. Strauss on filters)

B. G. LIPTK (1995, 2003) AT

Sampling

Flow Sheet Symbol

Costs: Compressed air filters cost about $60; stainless steel bypass filters, $300 to $600;
continuous-flow ultrasonic homogenizers, $3000; sludge centrifuge, $600; interval
sampling pump only, $750; automatic liquid sampler system, $1500 and up; complete
sampling system for single-process gas stream, $3000 to $6000; complete sampling
system for single-process liquid stream, $3500 to $7000. The per-stream cost in a
multistream sampling system drops as the number of streams increase.

Partial List of Suppliers: ABB Automation Analytical Div. (www.abb.com/usa)


Advantech Automation (www.advantech.com)
Air Dimensions Inc. (corrosion-resistant sampling pumps) (www.airdimensions.com)
Air Instruments & Measurements (www.aimanalysis.com)
Ametek Process Instruments (www.ametekpi.com)
Applied Chemometrics (www.chemometrics.com)
Bristol Equipment Co. (liquid samplers) (www.bristolequipment.com)
Cole-Parmer Instrument Co. (homogenizers, composite samplers) (www.coleparmer.com)
Collins Instrument Co. (sampling systems, bypass filters) (www.collinsinst.com)
Draeger Safety (www.draeger.com)
Fluid Metering Inc. (www.fmipump.com)
GLI International (www.gliint.com)
Hach Co. (www.hach.com)
Horiba Instruments (www.horiba.com)
Kahn Instruments (www.kahn.com)
King Engineering Corp. (filters) (www.king-gage.com)
KNF Neuberber (www.knf.com)
Kurz Instruments Inc. (stack sampling) (www.kurz-instruments.com)
Markland Specialty Engineering (www.sludgecontrols.com)
MIE Inc. (www.mieinc.com)
Neutronics Inc. (www.neutronicsinc.com)
OnTrak Control Systems (www.ontrak.com)
Orbital Sciences (www.orbital-ait.com)
Orena ControlNet (www.orena.com)
Parker Filtration (www.parker.com/balston.com)
Perma Pure (www.permapure.com)
PGI International (www.pgiint.com)
Roseomunt Analytical Process Analytic (www.processanalytic.com)
Sensidyne (www.sensidyne.com)
Servomex Applied Automation (www.servomex.com)
Siemens Applied Automation (www.aai-us.com)
Siemens Energy & Automation, Process & Analytical Div. (process samplers)
(www.sea.siemens.com)
TBI-Bailey Controls (probe protector from coating) (www.tbi-bailey.com)
Teledyne Analytical Instruments (process sampling systems) (www.teledyne-aicom)

1170
2003 by Bla Liptk
8.2 Analyzer Sampling: Process Samples 1171

Thermo Onix (www.thermoonix.com)


Thermo Ramsey (www.thermoramsey.com)
Tyco Valves & Controls (www.tycovalves.com)
Y2 Systems (www.y2systems.com)
Zellweger Analytics (www.zelana.com)

INTRODUCTION 1. Will the sample be adversely affected by sample


transport and conditioning?
This section starts with a discussion of the general consider- 2. From what stage in the process will the sample be
ations that the designer needs to evaluate before starting the taken?
actual hardware selection for a sampling system. Next, the 3. How can the sample be transported to the analyzer?
various sample system components are described. The sec- 4. Is the sample a solid, liquid, gas, or mixture?
tion is concluded by a detailed evaluation of the various 5. In what phase must the sample be for analysis?
sampling applications, considering gas, liquid, solids, stack, 6. Must the sample be altered (filtered)?
reactor, slurry, trace, and other types of process samples. 7. Is sufficient sample available?
Sampling is also discussed in the first section of this 8. What will be the time lag introduced by transporting
chapter and under the individual analyzer categories. The the sample?
subject of sampling stack particulate concentration is sepa- 9. Where is the excess sample returned?
rately discussed in Section 8.3. 10. Will the analyzer be shared by one or more samples?

These considerations are applicable both to the continu-


GENERAL CONSIDERATIONS ously flowing sample systems and to the less frequently used
grab samples. Grab sampling is limited by variations in
The sampling system is an integral and key part of an analyzer cleanliness of the sample containers, changes in the method
system and should be designed to obtain a representative of collecting the sample, delays in transporting the sample,
sample; transport the sample to the analyzer; condition the and deviations in withdrawing the sample from the sample
sample; accomplish sample stream switching, if necessary; container.
provide facilities for return and disposal of the sample; and The piped-in sample system usually includes the hard-
provide not only calibration facilities, but also preventive ware for calibrating the analysis system. It also provides a
maintenance features, and alarm functions for on-line reli- tap for obtaining samples for laboratory testing. Sample con-
ability and operator alerts. ditioning systems are usually costly to maintain.
If a sample has to be brought to an analyzer, a sample The installation price for the sampling system frequently
transportation delay and a potential for interference with the exceeds the cost of the analyzer, but its importance overrides
integrity of the sample will be introduced. If the measured this economic consideration because a second-class analyzer
composition is to be controlled, the transportation lag can can still furnish usable data if it operates with an efficient
seriously deteriorate the closed-loop control stability of the sample system, whereas a poor sample invalidates the entire
system. measurement.
Even more serious is the potential for interference with Therefore, the most important criterion is to keep the
the integrity of the sample, due to the effects of filtration, samples representative, both in time (short sample lines
condensation, leakage, evaporation, and so on, because these guarantee minimum transportation delays) and in composi-
operations can not only delay, but also change information tion. Whenever possible, the sample should not be tampered
that is to be measured: the composition of the process fluid. with because the steps of sample preparation (drying, vapor-
Consequently, the best solution is to eliminate all sam- izing, condensing, filtering, and diluting) always degrade the
pling systems and place the analyzer directly into the process. sample.
The in-pipe analyzer designs are becoming more and more
available. Particularly well suited for this design are the var- Sample Data Requirements
ious radiant energy and probe-type sensors.
A comprehensive listing of the characteristics of each sample
stream, including any abnormal conditions, should be pre-
Feasibility Evaluation pared before an analyzer sample system is designed. Data
are usually available from process conditions and laboratory
Sample systems are rarely duplicated, and thus each system analysis in existing plants and from design data for new
must be debugged as a new entity. In deciding the design of plants. Table 8.2a is a form to be used in summarizing the
a sampling system, the following questions should be raised: characteristics of a sample.

2003 by Bla Liptk


1172 Analytical Instrumentation

TABLE 8.2a
Sample Analyzer Data Form
Stream name or identification _________________________________________________________________________
STREAM COMPOSITION DATA
CONCENTRATION RANGE OF COMPONENT
COMPONENT IN MOL%, WT%, PPM TO BE MEASURED
OPERATING PROCESS DATA
Temperature _____________________________ Pressure __________________________________________________
Phase: Liquid _____________________________ Vapor ___________________________________________________
Corrosive components/solids __________________________________________________________________________
Stability (polymerize, decompose, etc.) _________________________________________________________________
Sample bubble point___________________________ Dew point ____________________________________________
SAMPLE CONDITIONS
Maximum distance: Tap to analyzer _____________________ Analyzer to return ______________________________
Speed loop required: Yes _______________________________ No __________________________________________
Sample return pressure point _________________________________________________________________________
Sample probe requirements: Connection size ______________________ Orientation ____________________________
Materials of construction: Stainless steel ________ Teflon ________ Viton ________ Glass ________ Other _________
Electrical areas classification _________________________________________________________________________
Power supply ______________________________________________________________________________________
Output signal ______________________________________________________________________________________
Utilities available: Stream __________________ Air ___________________ Cooling water_______________________

Process Vessel
or Pipe Wall Gate Valve

Pipe-to-Tubing
Connection

To
Sampling
System

Tubing

FIG. 8.2b
Sample probe assembly with process shutoff value.

Sample Takeoff Point practice to install a sampling probe (Figure 8.2b) for most
applications as a precautionary measure to prevent particu-
Sample conditioning begins with the location of a suitable lates from entering the sample transport system. Sampling
sample takeoff point. To obtain a representative sample, the processes that are still reacting chemically or pyrolysis gases
takeoff is usually located at the side of a process line, espe- may require reaction quenching, or fractionation, at the sam-
cially in the case of liquid samples where there is the possi- ple takeoff. This is done by cooling or back-flushing with an
bility of vapor on the top of a horizontal line and dirt or inert gas or liquid to keep the sample takeoff clean and
solids on the bottom of the line. For sampling vapors, the reliably active (Figure 8.2c), while drawing off a reproduc-
connection may be located in the side or top of the process ible sample for analysis.
line, but in both cases with due consideration to accessibility With the advent of in situ analyzer detectors, the sample
for maintenance. takeoff becomes the point of analysis and, for locating
Ideally, the sample at the appropriately selected takeoff in situ analyzers, the above considerations must be carefully
point will require little or no conditioning; however, it is good evaluated.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1173

Field Run At Analyzer Location

Sample to
Analyzer Analyzer Vent
Conditioning or
Coalescer System
Drain
Single-Line Transport
Vortex
Cooling
Vent
Tube Analyzer
Temperature or
System
Controller Cooling Drain
Section

By-Pass Stream
Instrument Vent, Drain
Warm
Air Supply Sample Return
Coolant
Exhaust Point or Sample
Analyzer Recovery System
Reflux
Action Filter System
Reflux
Section By-Pass Return Fast Loop
Sample Condensibles FIG. 8.2d
Sample transport methods.

Bypass-return fast loop is the most commonly used trans-


port loop for an analyzer mounted away from the sample
takeoff point. By circulating a continuous high velocity
Process Line across a device, to create a differential pressure, and drawing
off a bypass stream to the analyzer, a fast loop is obtained,
which is adjustable with no waste in the product. In most
FIG. 8.2c
cases, such devices as pumps, control valves, and process
Pyrolysis gas sample fractionation and conditioning unit.
equipment exist in the process for this purpose. Otherwise,
it may be necessary to install an orifice in the process line
Sample Transport
or a circulating sample pump. With a circulation sample
A representative sample extract from a process line must be pump, care must be taken to prevent cavitation by locating
continuously conditioned while in transport to avoid com- the pump close to the sample takeoff.
promising the sample integrity. Thus, provision must be made
to heat or cool the line as necessary for the specific condition.
The sample is normally transported in one of three ways Transport Lag
(Figure 8.2d).
After selecting the appropriate sample transport method for
Single-line transport is the most direct approach and is
each analyzer system, a calculation of the sample time lag
used when the sample line volume is small in relation to the
should be made, using conventional flow equations based on
analyzer sample consumption so that the transport time lag
the following:
is reasonably short. It is usually used when the analyzer is
field-mounted close to the sample point and sample exhaust
facilities are available. 1. Available differential pressures.
Bypass-stream transport is a commonly used method for 2. Total length of the fast loop from the sample takeoff
maintaining a high sample transport velocity that provides point to the analyzer location and back to the sample
minimum transportation lag. This method is used when sam- return point. Any restrictions on this loop should be
ples are vaporized at the tap and no facilities exist for return- excluded from available differential pressures.
ing the vapor to the process, or in similar situations. Consid- 3. Line sizes used.
eration must be given to the fact that the sample bypass must 4. Viscosity of the sample.
be piped to a drain or vent. This procedure may have a
negative impact on the environment, despite the fact that the Table 8.2e should be used as an aid in establishing vol-
cost of the sample being disposed of may economically jus- umes and pressure drops for some typical tubing and pipe
tify a sample recovery system. used in sample systems.

2003 by Bla Liptk


1174 Analytical Instrumentation

TABLE 8.2e
Dimensions and Volumes of Tubing and Pipe Used in Sample Systems
Nominal Internal Area
Volume per Inner
2
Diameter, in. Diameter, in. in. cc
1
316 stainless steel tubing /8 .0787 .0048 .9571
1
/4 0.1850 0.0268 5.3035
3
3 /8 /8 0.0253 0.0684 13.4417
1
/2 0.4055 0.1290 25.2984
1
Schedule 40 pipe /4 0.3642 0.1040 20.4521
3
/8 0.4921 0.1891 37.4904
1
/2 0.6220 0.3038 59.7408
3
/4 0.8268 0.5363 106.6800

Sample Disposal Quick Pressure


Disconnect PI
Gauge
Sample disposal is a critical area, both from the economic
point of view that would preserve any quantity of sample not
used and from the environmental side that would prevent the
Pressurized Liquid
emission of most hydrocarbons into the air. Cylinder
Nitrogen
When there is an economic justification for saving the or Other
sample, for example, liquids in boiling point and viscometer Inert Gases Flexible
analyzers, a sample collection and return systems must be Diaphragm
furnished to collect the sample at atmospheric pressures and
pump it back at high pressure into the process. For gases with Shut-Off
Valve
no sample return point, the sample can be pressurized back To Analyzer
into the process, or as is most frequently done, the sample Liquid Calibration Sample
can be vented into the flare system. However, except in rare
cases, venting is done directly into the atmosphere. When
Shut-Off Valves To
this is not possible, extreme caution should be taken to con- Analyzer
trol the back-pressure when venting the sample into a flare
or other collection system with varying pressures. Purge
Purge Connection
Ambient Considerations Connection
PI PI PI PI

Sample systems condition a sample suitable for introduction Shut-Off


into an analyzer while maintaining the integrity of the sample. Valve
As has been emphasized throughout this section, once a sam-
Two-Stage Two-Stage
ple is conditioned, it must be preserved in the conditioned Pressure
Pressure
state; therefore, provisions for heating, or in some cases cool- Regulator Regulator
ing, the sample lines and system must be furnished for the
integrity of the sample. Thus, the entire system must be pro-
Pressurized
tected from varying ambient temperatures, which could con- Cylinders
dense or flash the sample.
Gas Calibration Sample Manifold
Furthermore, as a general rule, the sample should be
located in enclosures that provide limited access to unautho- FIG. 8.2f
rized personnel and also protect the equipment from any Calibration provisions for liquid.
corrosive environment. It is accepted practice that systems
be completely preassembled and tested in conjunction with
ufacturer. Therefore, each system must include provisions for
analyzers prior to installation in the field.
testing and calibration. As is shown in Figure 8.2f, a means
of isolating the inlet is needed in order to allow a calibration
Test and Calibration
sample to be introduced manually or automatically.
The reliability of each analyzer is measured by its ability to Also necessary is a suitable calibration manifold with gas
check the analyzer calibration as recommended by the man- or liquid to furnish a reliable calibration sample to the analyzer.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1175

Storage of the test sample may be a consideration, especially The successful design of sample systems requires careful
for unstable liquids or gases with low dew points. Treatment analysis of the physical and chemical conditions of the
of the containers is very important for trace analysis samples. stream, as well as serious consideration of the ambient and
In all cases, the calibration provisions must be incorporated transport conditions, to ensure integrity of the sample. There-
into the systems and a sample provided that is compatible with fore, care should be taken in evaluating the above consider-
the desired stream composition and suitable for analysis by the ations with respect to a given stream and in applying the
analyzer used for the system. It is desirable, but not essential, correct analyzer to provide the desired measurement.
that the calibration sample be introduced automatically from Sample system design is based on experience, and when-
a remote location so that the instrument can be periodically ever possible, previous experience should be given prime
checked; however, in most systems the introduction of the consideration in the selection and application of components.
sample is done by manual switching at the analyzer. A successful sample system normally results in a successful
analyzer system. Therefore, no effort must be spared in
proper sample systems design, which requires a careful selec-
COMPONENTS OF SAMPLING SYSTEMS tion of the system components. These are discussed below,
starting with filters.
A number of devices are discussed here that are components
of analyzer sampling systems. These devices include gas and Filter Designs
liquid filters, bypass filters, liquid homogenizers, liquid grab
sample collectors, chemical reactor sampling systems, and Most analyzer sampling systems will include a filter with at
solids samplers. Later, under Applications, the various sam- least one wire mesh strainer (100 mesh or finer) to remove
pling probe packages and single-stream and multistream pro- larger particles that might cause plugging. Available filter
cess sampling systems are described. materials include cellulose, which should only be considered
The more components there are in a sampling system, in applications where it does not absorb components of inter-
the less reliable it is likely to be. The mean time between est. Sintered metallic filters can remove particles as fine as
failure and maintenance needs of the overall system will 2 microns; cellulose filters can remove down to 3 microns;
improve as the number of pumps, ejectors, regulating valves, and ceramic or porous metallic elements can trap particles
coolers, heaters, filters, coalescers, dryers, knockout traps, of 13 microns or larger. When the solids content is high, two
manifolds, timers, and other components that comprise the filters can be installed in parallel, with isolation valves on
system are reduced. each. Motorized self-cleaning filters are also available for
such services.
Selecting the System Components

Sampling systems require certain components, which are Separating Liquids from Gases Glass microfiber filter tubes
commercially available. One source is the analyzers manu- efficiently separate suspended liquids from gases. The filter
facturer, who through the years has developed systems com- tubes capture the fine droplets suspended in the gas and cause
patible with its analyzer, such as filter coalescers, condensers, the droplets to run together to form large drops within the
and washing and treating systems. depth of the filter tube. The large droplets are then forced by
A second source is the analyzer systems vendor, who had the gas flow to the downstream surface of the filter tube, from
designed special components, such as kinetic separators, fil- which the liquid drains by gravity. This process is called
1
ter probes, and the like, for use with analyzers for applications coalescing.
in rather hard service. The coalesced liquid drains from the tubes at the same
A third source is the specialty vendor, who has developed rate as liquid droplets enter the tubes. Therefore, the tubes
unique sampling components, such as pyrolysis gas sample have an unlimited life when coalescing liquids from relatively
conditioners; permeation devices for water removal systems; clean gases. The filters operate at their initial retention effi-
high-efficiency, self-cleaning filters; and so on. It is desirable ciency even when wet with liquid. The flow direction is inside
to check whether specialty items are available before trying to outside to permit the liquid to drip from the outside of the
to design new components. Most of the specialty components filter to the housing drain (Figure 8.2g).
have taken years of field testing to develop and modify for The filter tube grade should be selected for maximum
successful application. liquid drainage rate, rather than maximum filtration efficiency
When a large number of analyzers are used, the compo- rating, because a liquid drainage rate decreases with increas-
nents selected must be of the same type and manufacture for ing filtration efficiency rating. If liquid is carried into the
interchangeability and stocking of spare parts. Documenting filter in slugs rather than dispersed as droplets in the gas, a
a sample system with complete flow schematics, part identi- filter that is properly sized for steady-state conditions can be
fication, and manufacturing of various components is an flooded and permit liquid carryover. If slugging of liquid is
essential part of being able to properly start up a system and expected, a filter with a relatively large bowl should be selected
maintain it successfully over a long period. to provide adequate liquid-holding capacity, and provisions

2003 by Bla Liptk


1176 Analytical Instrumentation

Gas Out
Gas Out
Out In

Inner Foam Sleeve

Filtering Media

Outer Foam Sleeve Beads

Metal
Perforated Cylinder

Gas In Gas In

Packed Tower
Sparger
Scrubber
Liquid Drain
FIG. 8.2i
FIG. 8.2g Removal of corrosive gases or of condensable vapors.
2

Coalescing gas filter serves to remove liquid entrainment. (Courtesy


of Parker Filtration, formerly Balston Inc.)
all the liquid that is expected to be collected during any period
of unattended operation. To drain liquid while the filter is
Gas Out
operating at pressure or vacuum conditions, the reservoir inlet
valve is closed and the outlet valve is opened.
If the filter is under vacuum, the external reservoir is a
practical method of collecting coalesced liquid for periodic
Gas In manual draining. Alternatively, if an external vacuum source
is available, such as an aspirator, the liquid may be drained
continuously from the housing drain port.

Spargers, Packed Towers, and Strippers In some analyzer


Glass Wool
or Other applications it is necessary to remove corrosive gases or
Packing condensable vapors from the sample. This removal can be
done by bubbling the sample stream through a liquid solution.
In the case of a sparger (Figure 8.2i), the gas enters below
the scrubbing medium through a sintered disc, which breaks
it into small bubbles. This increases the liquidgas contact
surface area and thereby provides improved scrubbing effi-
Ball Float
Trap
ciency. At the same time, the small bubbles also increase the
tendency for foaming and liquid carryover, and therefore the
Drain sample flow velocities should be kept low.
Packed towers (Figure 8.2i) can also be used as scrub-
FIG. 8.2h
2 bers. In these designs the gas sample bubbles up through a
Entrained liquid separator with ball float trap.
nonreactive packing of beads that are wetted by a liquid
solution. Foaming and liquid carryover are problems in
should be made to drain the liquid automatically from the packed towers, as in a sparger.
bowl of the housing as it accumulates. When the impurities in the process gas stream are both
An automatic float drain can be used if the pressure is in solids and liquids, such as in particulate matter and mist
the 10- to 400-psig (28 bars) range. Above 400 psig, which carryover problems in chlorine plantsthe fiber mist elim-
3
is the upper limit for commercially available float drains inator (Figure 8.2j) should be considered. The liquid particles
(Figure 8.2h), the possibilities are 1) a constant bleed drain, form a film on the fiber surface, and the drag of the gas moves
2) a valve with an automatic timed actuator, or 3) an external this film and the dissolved solids radially, while gravity
reservoir with manual valves. The external reservoir can be causes them to move downward, resulting in a self-cleaning
constructed of pipe or tubing with sufficient volume to hold action.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1177

Clean
High Pressure PI PCV
Chlorene Gas
Polymerization To Analyzer
Fiber Product in Sampling
Liquid Phase System
Dirty
Chlorene
Gas

Draining Liquid Steam LC

Screens Jacket

Liquid
Seal Overflow Molten
Pot Polymer

FIG. 8.2j FIG. 8.2l


Fiber mist eliminator. Flash chamber makes the analysis of unreacted monomers possible.

Separating Two Liquid Phases Theoretically, glass micro-


Clean gas to fiber filter tubes can separate suspended droplets of a liquid
Analyzer
or Condenser
that are immiscible in another liquid using the same process
by which they separate droplets of liquid from a gas. The
liquid droplets suspended in the continuous liquid phase are
Fiberglass
trapped on the fibers and run together to form large drops,
which are then forced through the filter to the downstream
surface. The large drops separate from the continuous liquid
Screen
phase by gravity difference, settling if heavier than the con-
Spray Nozzle tinuous phase and rising if lighter. The coalescing action of
Crystal Clear
High-Boiling
glass microfiber filters is effective with aqueous droplets
Sample, Filtered Steam suspended in oil or other hydrocarbons, and also with oil-in-
to 0.5 Micron Jacket water suspensions.
By Bypass Filter In practice, however, liquidliquid separations are much
Upstream
more difficult to achieve than are liquidgas separations. The
specific gravity difference between two liquids is always less
FIG. 8.2k
When dissolved inorganic solids or polymer-forming compounds than that between a liquid and a gas and, therefore, a longer
are present, stripping the liquid sample may be the answer. phase separation time is needed. Either the filter housing must
be oversized or the flow rate greatly reduced to avoid carry-
over of the coalesced phase.
Dissolved solids or polymer-forming compounds in a As a rule of thumb, flow rate for liquidliquid separation
process stream would leave a residue and eventually plug the should be no more than one fifth the flow rate for solidliquid
liquid sample valve. The logical solution is to force the res- separation. Even at low flow rates, if the specific gravity
idue formation to take place in a controlled area, such as in difference between the two liquids is less than 0.1 U (for
the fiberglass filter of the spray-stripping chamber shown in example, if an oil suspended in water has a specific gravity
Figure 8.2k. between 0.9 and 1.1), the separation time for the coalesced
If polymers represent a substantial portion of the process phase may be too long to be practical. In that case, if there
stream, the need for filter replacements becomes excessive is only a small quantity of suspended liquid, the filter tube
and therefore impractical. A better technique is to vaporize can be used until saturated with suspended liquid and then
the unreacted monomers through pressure reduction while changed.
keeping the polymers in a molten state through heating. This Another practical problem with liquidliquid separation
technique (Figure 8.2l) not only discharges polymers contin- is that small quantities of impurities can act as surface-active
uously, but also provides a usable vapor sample. agents and interfere with the coalescing action. For this rea-
When it is necessary to clean the windows on the various son, it is not possible to predict accurately the performance
photometers operating on gas samples, a warm air purge can of a liquidliquid coalescing filter, and each system must be
be used, keeping the window compartment isolated from the tested on-site. Testing can be started with 25-micron filter
sample. tubes and with inside-out flows at very low flow rates. If the

2003 by Bla Liptk


1178 Analytical Instrumentation

Automatic Low
Gas Vent Filter Flowrate
High Flowrate

Inlet
Pressure
Reducing Analyzer
Liquid Out Process Valve
Stream
Bypass

Glass Wool High Flowrate


or Other
Packing

Liquid In FIG. 8.2n


Slipstream or bypass filtration.

Slipstream Coalescing Low


Filter Filter Flowrate
FIG. 8.2m Inlet
2
Entrained gas separator. High
Pressure
Flowrate
Reducing Analyzer
suspended liquid is lighter than the continuous phase, the
Valve
housing should be oriented so that the drain port is up.
Coalesced Liquid
Bypass Drain
Removing Gas Bubbles from Liquids Glass microfiber fil-
ter tubes readily remove suspended gas bubbles from liquid,
eliminating the need for deaeration tanks, baffles, or other
separation devices. Flow direction through the filter is outside
High Flowrate
to inside, and the separated gas bubbles rise to the top of the
housing and are vented through the drain port. If slipstream FIG. 8.2o
sampling is used, the separated bubbles are swept out of the Slipstream plus coalescing filtration.
housing with the bypassed liquid. Filter tubes rated at 25
microns are a good choice for gas bubble separation.
Columns with glass wool packing can also be used to If bubble removal from a liquid is a requirement, this
remove entrained bubbles (Figure 8.2m). Here the gas bub- function may be combined with slipstream filtration, since
bles collect and agglomerate on the packing and form large the recommended flow direction for bubble removal is out-
bubbles. These bubbles break away and rise to the top, where side to inside, and the separated bubbles will be swept out
they are separated from the liquid and vented. of the housing by the bypass stream. In this case, the liquid
feed should enter at the bottom of the housing and the bypass
Slipstream and Bypass Filters In order to minimize the liquid should exit at the top of the housing.
transportation lag, a relatively large slipstream is usually A special problem arises in slipstream sampling if the
taken from the process and brought near the analyzer. As the filter is to coalesce and continuously drain suspended liquid
actual sample flow to the analyzer is small, only a small from a gas stream or to coalesce liquid droplets from a liquid
portion of this slipstream is sent to the analyzer; the bulk is stream. The coalescing filter requires two outlet ports, one
returned to the process (Figure 8.2n). This arrangement per- for the dry gas and one for the liquid drain. To combine
mits the main volume of the filter to be swept continuously coalescing and slipstream filtration, a filter housing would
by the high-flow-rate system, thus minimizing lag time; at need four portstwo for inlet and bypass and two for filtered
the same time, only the low-flow stream to the analyzer is gas and coalesced liquidwhich is not a practical design.
filtered, thus maximizing filter life. Therefore, slipstreaming plus coalescing requires two
A slipstream filter requires that its inlet-to-outlet ports be stages of filtration (Figure 8.2o). The second (coalescing)
located at opposite ends of the filter element to allow the stage must be located in the sample line into the analyzer
high flow rate of the bypassed material to sweep the surface and should be as small as possible to minimize lag time. If
of the filter element. A third port connecting the low-flow- the quantity of suspended liquid is not large, a miniature
rate lines to the analyzer allows filtered samples to be with- inline disposable filter unit may be used as a trap for the
drawn from the filter reservoir. suspended liquid, to be replaced when saturated.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1179

Filtered Fluid
Filtering Element
(Can be Porous
Metal with 400 Quick
Mesh Size) Disconnect

Process Filtered Fluid


Stream Cleaned
to be Sample Particles
Analyzed
Sample to
Analyzer
No Cake Buildup
Dirty
Sample

Sample to
By-Pass
Analyzer
Filter
Restriction
Orifice Nitrogen FIG. 8.2r
or Slide or Steam Rotary disc filter.
Gate Valve Blow-Back

Another good filter design is the rotary disc filter (Figure


FIG. 8.2p
Self-cleaning bypass filter and its installation.
8.2r). Here the filtered liquid enters through the small pores
in the self-cleaning disc surfaces. The sample liquid is drawn
by the sample pump through the hollow shaft and is trans-
ported to the analyzer.
Cleaned Liquid For the removal of small amounts of polymer dust in vapor
or Vapor Sample
to Analyzer
samples, there are melt filters with removable, heated metallic
surfaces that melt and collect the polymer dust from the sample.
Liquid analyzer sample streams usually have a high sol-
ids content. In addition, the analyzers are often located in
remote areas of the plant and are infrequently serviced.
O-Ring Seal Cap Body Base Therefore, the sample filter system must have a long life
between filter tube changes even when solid loading is high.
Support Pad The recommendation for this type of application is a two-
stage filter system, a 75-micron prefilter followed by a 25-
micron final filter. The filters should be oversized as much
as possible without causing excessive lag time. Plastic filter
housings are usually a good choice.

Keeping Probes Clean


Liquid or Vapor
Bypass Stream Support Figure 8.1p illustrates one of the probe cleaner designs, and
Containing Solid In Filter Screen Table 8.1q lists the features and capabilities of a number of
Particles Out Element probe cleaners. There is yet another approach to keeping
probes clean, which grew out of the mining industry, where
FIG. 8.2q gypsum buildup on pH and oxidationreduction potential
Bypass filter with its cleaning action amplified by the swirling of
(ORP) probes was blinding these sensors.
the tangentially entering sample.
The Filterate Master (Figure 8.2s) consists of a filter cup
at the tip of a 2-in.-(50-mm)-diameter standpipe, which is
Self-Cleaning and Rotary Disc Filters If the material to be inserted into the process. The pH or other electrode is inside
removed is dust, the self-cleaning bypass filter (Figure 8.2p) this cup, which is made out of porous sintered stainless steel.
with automatic blow-back constitutes a potential solution. In A pump housed outside the process draws a vacuum inside
some instances, cyclone separators should be considered. In the cup, thereby drawing in the filtrate of the process fluid.
the latter device (Figure 8.2q), the process stream enters tan- The excess filtrate can be continuously returned by the pump,
gentially to provide a swirling action, and the cleaned sample while the filtered-out solids accumulate on the outside surface
is taken near the center. Transportation lag can be kept to less of the filter cup.
than 1 min, and the unit is applicable to both gas and liquid Operating experience shows that solids can build up to
samples. This type of centrifuge can also separate streams by over an inch (25 mm) thickness without blocking the filtrate
gravity into their aqueous and organic constituents. flow. The timer is set to periodically reverse the filtrate pump.

2003 by Bla Liptk


1180 Analytical Instrumentation

Backflush
Vibration
Filtrate Horn

Continuous-
Flow Cell
Signal
Wire Overflow
2"
(50 mm)

Inlet Orifice Plate

Orifice

Outlet

FIG. 8.2t
Ultrasonic homogenizer. (Courtesy of Cole-Parmer Instrument Co.)
Standpipe
Inserted
Into Process might otherwise plug the system, they also remove process
constituents and make the sample less representative.
The newer approach is to eliminate the potential for plug-
ging by reducing the size of solid particles (homogenization)
while maintaining the integrity of the sample. Thus, when a
pulverizer is used to replace the filter, the sample becomes
representative.
Homogenizers serve to disperse, disintegrate, and reduce
10 Porosity the particle size of solids and thereby reduce agglomerates
Sintered and liquefy the sample. Homogenizers can be mechanical,
Electrode

Metal Filter
Cup
using rotor-stator-type disintegrator heads. In this design, the
rotor acts as a centrifugal pump, which is recirculating the
slurry while the shear, impact collision, and cavitation at the
Filtrate disintegrator head provide homogenization.
in Cup
In ultrasonic homogenizers, high-frequency mechanical
vibration is introduced into the probe (horn), which creates
1" pressure waves as it vibrates in front of an orifice (Figure 8.2t).
(25 mm)
As the horn moves away, it creates large numbers of micro-
FIG. 8.2s scopic bubbles (cavities), and when it moves forward, these
Electrode is protected from material buildup by back-flushed porous bubbles implode, producing powerful shearing action and agi-
filter cup. (Courtesy of TBI-Bailey Controls.) tation due to cavitation.
Such homogenizers are available with continuous-flow
When the flow direction is reversed, the filtrate flows back cells for flow rates up to 4 g/h (16 l/h) and can homogenize
into the filter cup and out through the porous filter. During liquids to less than 0.1-micron particles sizes. The flow cell
back-flush, the buildup is quickly removed and another fil- is made of stainless steel and can operate at sample pressures
tering cycle is initiated automatically. of up to 100 psig (7 bars).

Homogenizers Sample Conditioning

A frequent problem of sampling systems is plugging. There are The extracted sample begins conditioning at the takeoff point,
two ways to eliminate it. The older, more traditional approach continues through the transport, and finishes conditioning at the
is filtering. Unfortunately, as the filters remove materials that analyzer location prior to entering the analyzer (Figure 8.2u).

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1181

Field Analyzer Rack or House


Sample Conditioning
Shut-Off
250 To
Valve
Bypass
Lab HDR
Sample Analyzer
Open-Air Flow Indicator
Cooler Pressure With Adjusting
Shut-Off
Gauge Valve Set at
Y-Strainer Valve Dew Point FI Flow Indicator
0100 0-100 ~7100 cc/Min
Steam In at With Adjusting
FI
T = 1510F PI 45 PSIG PI 3-Way Valve Set at
Out
P = 460 PSIG 30 18F Solenoid 400 cc/Min
PSIG
F
In Shut-Off
Shut-Off Fine
Valve Valve 1/4 T
Pressure Reducing 1/4 T Filter
Kinetic 316
Station With Gauge 316
Separator
Liquid and Relief Valve Zero
Seal Trap Set at
Light Steam ~100# 2-Way Solenoid
Steam Out Trace for Cold
Span
Weather Protection
Conditioning System
Cooler and Field Pressure
Reduction Station

FIG. 8.2u
Typical sample conditioning system with remote preconditioning unit.

Analyzer
Cooling Water
Sample In Out Pressure Temperature
Gauge Flow
Out In Gauge
FI Indicator
PI T1 With
Control Flow Needle
Valve FI Indicator Valve
Self Calibration
Cleaning Sample
Filter
Sample Shut-Off
Cooler Coalescer Valves
Pressure
Shut-Off Regulator Lab Sample
Valves Pressure Take Off
Flow Relief Valve
Flow Indicator Pressure
FI FI Gauge
Indicator Check with
Valve Needle PI
Valve Check
Valve
Shut-Off
To Valve
Drain

FIG. 8.2v
Typical liquid product sample system for refinery applications.

All samples require some form of conditioning to make them of the components in the liquid used to wash the sample. The
suitable for the analyzer and to assure reliable on-stream oper- conditions of flow, temperatures, and pressures must be con-
ation. The conditioning is done at the appropriate location in trolled to maintain a relatively constant predetermined rela-
the sample system loop in order to maintain the integrity of the tionship of the composition. When washing, care must be
sample (Figure 8.2v). taken to keep the sample in the vapor phase by providing
Sample washing is usually limited to dirty, particle-laden heated transport lines or by making provisions for final mois-
streams whose composition will not be affected by the solubility ture removal as the analyzer may require.

2003 by Bla Liptk


1182 Analytical Instrumentation

1/4 NPT
Temperature Vapor Outlet
Adjusting Screw O Ring Seal
Temperature
Sensor

AC - IN
Heater

1/8 NPT
Liquid
Sample Inlet

FIG. 8.2w
Vaporizing regulator assembly (electrically heated).

Vaporizing Samples Vaporizing is frequently necessary for Low Pressure Wet


High Pressure Shell High Pressure
equilibrium liquids or when the analyzer requires it. The vapor- Purge Gas Outlet Dry Product
Wet Feed
ization is usually done by a vaporizer regulator (Figure 8.2w). Inlet Outlet
In such a regulator the sample is vaporized simply by pressure
reduction across a capillary or, more often, by using a heater
as well. Care must be exercised to avoid partial vaporization
and fractionation by selecting a suitably heated vaporizing
Permeable Low Pressure
regulator to accommodate the sample. Dry Purge Gas
Tube
Inlet
Entrainment Removal The removal of entrainment from
liquid or gas samples normally starts with locating a sample FIG. 8.2x
tap and providing a sample probe at the takeoff point. Filtra- Permeable tube sample dryer.
tion is normally used for both gases and liquids, because it
removes both liquid and particulate entrainment from gases for measurements in the parts per million (ppm) range. There-
and particulate matter from liquids. fore, proper selection of materials and conditioning is essen-
For gases requiring further conditioning of heavy load- tial for establishing an equilibrium that will make analysis
ing, cyclone filters can be used if the sample has adequate reliable.
velocity. For liquids, coalescers are frequently used to remove Specifically, water vapor samples reach equilibrium more
both undesirable gases and liquids by gravity. The removal rapidly in stainless steel lines than in copper or plastic tubing.
of free water from a hydrocarbon stream is usually accom- Diffusion is another consideration. Samples system design
plished by passing the liquid through a hydrophilic element, should assure that gases do not permeate the walls of the
causing the water droplets to accumulate on the element. The sample system. This is especially important in high-pressure
hydrocarbon stream is then passed through a hydrophobic systems and ppm analysis. Another problem with diffusion
element that rejects the water, removing it from the bottom is leakage, which can change the sample composition because
with a hydrocarbon bypass stream. gas molecules will flow in both directions of the leak and
Another method of removing moisture from a stream uses can significantly affect ppm analysis. This is best illustrated
a selective permeation device with a drying medium that cre- by the fact that in an oxygen ppm analyzer system, the slight-
ates differential pressures to drive the water through the per- est leak will create a full-scale reading on the instrument even
meable materials, thus removing it from the flowing stream though the leak is from a high-pressure sample to atmo-
(Figure 8.2x). spheric pressure.
Some sample streams may contain corrosive gases or
Selection of Component Materials Adsorption of the sam- water vapor that influence the accuracy of the measurements
ple components of interest on the walls or surface with which or potentially damage the analyzer. Removal of such unde-
the sample comes in contact will affect the analysis, especially sirable matter or components can be accomplished by passing

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1183

the sample through a packed bed of soil chemicals or desic-


Capillary
cant. Further, a liquid treating agent may be applied with Filter Tubing High Pressure
provisions that gas streams be broken up into small bubbles Filter Blowback
to assure proper contact between the liquid and gas phases.
Care should be taken in such systems to avoid alteration of
the sample and to condition the sample to a desired and Vapor
Sample
reproducible form for analysis. Pulled by
Process Vessel
Ejector
Guard
APPLICATIONS
FIG. 8.2z
Gas sampling probes used on combustion processes are usually
Here a brief discussion will follow of the various sample provided with probe-tip filters and blow-back lines for filter cleaning.
probe and sampling system package designs that are used for
gas, liquid, and solids sampling. The discussion will also
Solid Filter with High
cover the more special cases of stack, reactor, condensate, Temperature Capability
trace component, and multiple-stream sampling systems. Line may be Heated
to Prevent
Condensation Analyzer Sample
Gas Sampling Probes Pump

When taking gas samples, the goal is to obtain representative Temperature


samples with minimum time lag, using short, small-volume 80 F or Lower Filter Housing with Glass
sampling lines. Whenever possible, it is preferred to draw Bowl and Coalescing
dry and clean samples in order to minimize the need for Filter Tube, Flow Inside to Outside

filters, dryers, knockout traps, or steam tracing. Valve Normally Closed

The sample tap should be located on the side of the Condensate Reservoir
Stack Gas Temperature
(Optional)
pipeline to minimize liquid or dirt entrainment, and the sam- to 900 F
Valve Normally Open
ple should be taken from the center of the pipe. If it is
necessary to periodically remove the probe for cleaning or
to perform a sampling traverse, it is desirable that the probe FIG. 8.2aa
be inserted through a packing gland and block valve, as Stack gas sampling.
shown in Figure 8.2y.
Stack Gas Sampling
The volume of the sampling system should be kept to a
minimum, while the velocities through the sample lines should When sampling hot, wet stack gas, a filter capable of with-
be high to protect against the settling of entrained liquids or standing the gas temperature should be installed in the stack
particulates that can cause plugging. Sample line tubing can at the tip of the sample line to prevent solids from entering
be small as 1/8 in. (3 mm) in diameter, and sample flow the gas sample line. After the sample is cooled, a coalescing
velocities should be between 5 and 10 ft/sec (1.5 to 3 m/sec). filter is used to remove suspended liquids before the sample
When the sample is taken from a combustion zone or other goes to the analyzer (Figure 8.2aa).
dirty processes, a filter is usually provided at the tip of the The sample flow direction is from inside to outside. Filter
sample probe, and a high-pressure filter blow-back line is housings with Pyrex glass bowls are often used in this appli-
provided for periodic filter cleaning (Figure 8.2z). cation to permit visual check of the liquid level in the filter
housing. Since there is often a considerable amount of liquid
Small Bead Around End of Probe to Prevent present in the sample, steps must be taken to drain the housing
Pulling the Probe Completely Through the to ensure that liquid does not build up and carry downstream
Packing Gland to the analyzer.
The liquid coalescing filter should be located as close to
the analyzer as possible to minimize the chance of condensa-
Probe tion between the filter and the analyzer. Additional precautions
that can be taken to avoid downstream condensation are to
cool the sample below ambient temperature upstream of the
Packing Gland coalescing filter and to heat the line gently between the filter
Gate Valve and the analyzer.

FIG. 8.2y Automatic Stack Sampling In these sampling packages, a


Gas sampling probe should be inserted from the side of the pipe to microprocessor directs the automatic sampling method,
2
near the center of the pipe. which can be selected to follow U.S. Environmental Protection

2003 by Bla Liptk


1184 Analytical Instrumentation

Agency (EPA) Methods 1 to 6, 8, 17, and 23 or international Spring Cap Nut


methods specified by VDI, BS, or ISO. The microprocessor Outer Spring Cap
stores all measurements, reviews and diagnoses all inputs, Outer Spring
controls the required parameters, calculates isokinetic condi-
Diaphragm
tions, and either reports the results in a printed form or
transfers them to a floppy disc. Control Side
Besides the controller, such a package usually consists Inner Spring Sample Side
of a probe, a filter (hot) box, a cold box, a flexible sample Stem Seal
line, glassware, a node box, and a monorail system. The probe
is usually 3, 5, 7, or 10 ft (0.9, 1.5, 2.1, or 3 m) and made of
stainless steel with a glass liner. Most probes are jacket heated Sample Outlet
and are provided with both a liner thermocouple and a stack
temperature thermocouple. Valve Stem
The measured variables include the temperatures of the
Adjustable
stack, probe liner, filter box, condenser outlet, and the dry Fitting
gas meter. The pressures are detected by an absolute and a
differential pressure transducer and are used to measure the
pressure of the stack gas, the barometric pressure, and the
velocity pressure of the stack gas. The normal capacity of
the vacuum pump that draws the sample is 0.75 CFM (21
Sample Tube
l/min), and the dry gas meter has an operating range of 0.1
to 1.5 CFM (2.8 to 42 l/min).
The node box provides the interface between the filter
box and the cold box by measuring the temperatures in both. Sample Inlet
It measures and stores the temperature, pressure, and velocity Valve
in the stack. The monorail eliminates the need for bulky
supports. FIG. 8.2cc
Adjustable automatic load sampler.

Automatic Liquid Samplers


sampler illustrated in Figure 8.2cc can take samples at pres-
Automatic liquid samplers collect intermittent samples from
sure up to 1500 psig (105 bars).
pressurized pipelines and deposit them in sample containers.
The sample can be collected on a time-proportional or on a
Sampling of High-Pressure Condensate In high-pressure
flow-proportional basis. Figure 8.2bb illustrates a sampler that
boiler systems, measurements of condensate conductivity,
withdraws a predetermined volume of sample every time the
specific ion concentration, and feed-water additive concen-
actuator piston is stroked. In the time-proportional mode, this
sampling frequency is constant, while in the flow-proportional trations are often required. In a continuous sampling system,
mode, this unit would vary the sampling frequency as a func- the high-pressure steam or condensate is cooled below 100F
tion of flow. (38C) and then reduced to near atmosphere pressure for
In some automatic liquid samplers, the sampling fre- metering to the analyzers. Filtration is required upstream of
quency is adjusted by pneumatic pulse relays or by electronic the pressure-reducing valves to prevent pitting to the valve
controls (Figure 8.2cc). Pulse duration is usually adjustable seats by suspended particles and to eliminate variations in
from 0.25 sec to 1 min, while pulse frequency can be adjusted flow rate to the analyzers.
from a few seconds to up to an hour. The intermittent in-line A stainless steel filter housing with the appropriate pres-
sure rating and 25-micron filter tube is recommended. Since
the analyzer system is often located some distance from the
sampling point, slipstream filtration is usually required.
Figure 8.2dd shows a sampling system in operation at a steam
generation facility.

Chemical Reactor Samplers When samples are taken from


chemical reactors by opening manholes, the operators can be
exposed to dangerous fumes while the product can be
FIG. 8.2bb degraded or cause explosions. To eliminate these problems,
Intermittent collection of samples. (Courtesy of Bristol Equipment reactor sampling systems have been designed that allow the
Co.) safe taking of samples.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1185

Condensate
Pressure Stainless Steel Filter
Regulators Housing, 800 psig (56 barg)
Rating, With 25 Micron
Samples to Filter Tube
Conductivity Cells
Slipstream

FIG. 8.2dd
High-pressure stream sampling.

Diaphragm Pump of Teflon-Frequently


Used for its Ideal Flow Rate, Corrosion
Resistance and Minimal Damage to Crystals
pH Probe Sample Return

Sample Out Liquid/Gas Addition


Ball Valve of Glass and Teflon-Also Serves
As Sight Glass for Liquid Monitoring

Sampler

FIG. 8.2ee
4
Continuous or intermittent sampling of chemical reactor.

The design illustrated in Figure 8.2ee requires only one installed below the process liquid (or sludge) level and traps
nozzle (3 in. or 75 mm) and utilizes a Teflon-coated sampler some air at the top of the chamber as it fills with the process
assembly that can be used up to 150 psig (10.5 bars) and fluid. When a sample is required, compressed air is intro-
350F (177C). For continuous sampling applications, such duced, which closes the Duckbill inlet and discharges the
as for closed-loop pH control, a Teflon diaphragm pump is sample from the bottom of the chamber. When a new sample
used to continuously return the analyzed sample. is to be drawn into the sample chamber, the compressed air
is vented and a new fill cycle is initiated.
Duckbill Samplers This sampler should be considered An automatic controller is provided on which the user
when liquid or sludge samples are to be collected at remote can adjust the frequency at which samples are to be taken
locations, from below the level in tanks, sewers, channels, into a composite sample collection bottle.
5
sumps, lakes, or rivers. As shown in Figure 8.2ff, this device
has no moving mechanical components, only a rubber (EPT,
Solids Sampling
Buna-N, or Viton) bucket-shaped Duckbill , which is inside
a housing made of polyvinyl chloride (PVC), aluminum, or When solids in bins or silos need to be sampled, one of the
stainless steel. This rubber insert closes around fibers or various solids feeders (described in Section 2.23) can be con-
particulate matter without jamming. It is operated by com- sidered. When solids are to be sampled while flowing by
pressed air. gravity or while pneumatically conveyed under the pressure,
The sample enters by gravity through the bottom con- the choice of sampling devices becomes more limited. The
nected Duckbill inside the sampling chamber, which is screw-type solids sampler can be used on these applications

2003 by Bla Liptk


1186 Analytical Instrumentation

Process
Stream

Motor

Sample

FIG. 8.2gg
Archimedian screw solid sampler.

Analyzer

Sample Return
Actuator #1

Actuator #2

FIG. 8.2hh
The tray-type solids sampler.

Sampling Difficult Processes

An analyzer system enhances process control by providing


specific measurement of physical or compositional data of a
FIG. 8.2ff
process or ambient condition. With the advent of computer
Duckbill sampler. (Courtesy of Markland Specialty Engineering technology, the need for such analysis has increased substan-
Ltd., www.sludgecontrols.com) tially to provide on-line data that the computers use to opti-
mize process control. Some of these advances have also
improved the handling of such difficult tasks as sampling for
(Figure 8.2ff), but it is limited in the amount of pressure or trace component analysis or sampling multiple streams.
vacuum it can seal against, and it does not provide an inter-
mixed, representative sample. Screw samplers also introduce Trace Analysis Sampling Trace analysis sampling systems
large transportation lags and cannot easily return the sample necessitate more stringent requirements than normal analyzer
into the process. sample systems because of contamination, adsorption, and
An improved sampler design is described in Figure 8.2gg. desorption (Figure 8.2hh). Care should be taken in the selec-
This sampler can be sealed against small pressures or vacu- tion of construction materials and proper applications of
ums. It is operated by two actuators. During the sample col- design criteria to avoid alteration of the sample. The follow-
lection phase, both actuators are extended into the process ing is a list of recommended practices for such systems:
line. When a representative sample has been collected, it is
withdrawn and simultaneously intermixed by pulling back 1. Stainless steel seamless tubing is the preferred mate-
actuator 1. As the analyzer is right above the withdrawn rial because it provides inertness, smooth surfaces, and
sample, the composition can be measured as soon as the low porosity.
sample has been taken. After analysis, actuator 1 is once again 2. All components should be thoroughly cleaned of oil,
extended to return the old sample into the process. When it gas, or other contaminating materials.
is time to take a new sample, actuator 2 is also extended and 3. Dense fluorocarbons or other soft inert materials may
another sample is collected. be used as diaphragms as required.

2003 by Bla Liptk


8.2 Analyzer Sampling: Process Samples 1187

4. Tubing sizes are critical, especially where low flows are analyzer. However, because this system is more complex than
used, because they limit the amount of increase in the single-stream sample conditioning, the following consider-
adsorptiondesorption phenomenon. A rule of thumb ations should be reviewed to determine if multistreaming is
is to use the smallest possible tubing to achieve maxi- feasible:
mum flow to accommodate the sample loop design.
5. Packless shutoff valves with a diaphragm or bellows 1. The potential problem of cross-contamination among
seals should be used; however, due to their high cost, multiple streams
serious consideration must be given to this area, and 2. The importance of each analysis and frequency of
conventional valves are suitable for most applications. analysis
6. Filtration of the sample in ppm analysis can create 3. The loss of information from more than one analysis
significant problems unless the filter is totally inert. in case of analyzer failure
Therefore, stainless steel filters using a high flow rate 4. The cost of an additional analyzer vs. the cost of
or dense fluorocarbon inert materials are recommended multistreaming
for such applications. 5. Maintenance requirements
7. Conditioning of the lines and system to accommodate
the ambient temperature requirements for preventing After reviewing the above, one can decide if multistream-
condensation of components of interest in the sample ing is feasible and whether it should be manual or automatic.
must be considered; if necessary, heat tracing of the Whether manual or automatic, multistreaming requires good-
lines must be furnished. quality valves for stream switching.
8. When it is necessary to provide an aid for transporting A typical multistream sampling system is shown in
the sample from its sample point to the sample system Figure 8.2ii. A common and important requirement in all
through the analyzer, as is frequently done in ambient such systems is that a continuous bypass be provided for each
monitoring systems, a sample pump, ejector, or aspirator sampling point to avoid dead-end sample lines. The sample
is necessary. In such cases, the pump must be a dia- system should be laid out in such a manner that contamina-
phragm. If practical, an ejector to pressurize the sample tion between streams is avoided. This is best accomplished
or an aspirator to aspirate it through the measuring device by arranging the solenoid valve in a double-block double-
can be used. Both are more desirable than a sample pump. bleed configuration, which is rather expensive.
More often, a three-way solenoid valve is used for each
Multistream Switching Multistream switching is usually stream, with the venting port always at low pressures to create
used when it is practical to analyze several streams using one a relief in case of a leak. To prevent contamination, dead

Instrument
PI Air
Field Analyzer House
Supply
F
TI

Liquid PI Steam
PI
Sample
200 PSIG
F
70F Drain
(1378 kPa, 21C) TC
Steam FI
Drain To
Heated Enclosure Steam Atmosphere Return to Header FI A
Mounted at Traced Vent
Sample Tap
FI
Saturated PI ATM
Vapor Bleed
Sample F
4 PSIG Calibration
120F Sample
(27.6 kpa,
49C) Drain Steam Heated Enclosure
Bubbler for
Leak Detection

FIG. 8.2ii
Two-stream sampling system for trace analysis with a double-block, double-bleed configuration.

2003 by Bla Liptk


1188 Analytical Instrumentation

To Vent or Common Sample Return Point

PI

Stream 1 FI Flow
Indicator
with
FI
Adjusting
PI Valve

Stream 2 FI FI Analyzer

Pressure Bleed
Relief
Gauge Orifice
Valve
PI Shut-Off
Valves Calibration Gas
Stream 3 FI
Pressure
Regulator Flow
3-Way
Indicator
Solenoid
with
Adjusting
Valve

FIG. 8.2jj
Typical multistream automatic sampling system.

volume of the sample system should be considered, as well Converse, J. G., Calibration & Maintenance Are Part of a Reliable Sample
as equalization of the pressures upstream of the three-way Preparation Systems Design, ISA Conference, Houston, October 1992.
Cornish, D. C. et al., Sampling Systems for Process Analyzers, London:
valves. The problem is more severe in ppm sampling systems Butterworths, 1981.
because of the adsorptiondesorption effects, and careful Dubois, R. et al., The New Sampling Initiative, 47th Annual ISA Analysis
consideration should be given to the design criteria described Division Symposium, April 2002.
above. Dubois, R., van Vuuren, P., and Tatera, J., New Sampling Sensor Initiative,
An Enabling Technology, 47th Annual ISA Analysis Division Sympo-
sium, Denver, April 1418, 2002.
References Erk, G. F., Engineering Analyzer Systems, InTech, August 1979.
Foundos, A. P., Reliable Sample Conditioning Improves Process Analysis,
InTech, January 1990.
1. Baker, G., Erk, G., Hudelson, J., Manka, D., Siebert, K., and Wachel,
Fussell, E., Molding the Future of Process Analytical Sampling, InTech,
L., Automated Stream Analysis for Process Control, Vol. 2, Orlando, FL:
August 2001, 32.
Academic Press, 1984, pp. 97101, 105106.
Houser, E. A., Principles of Sample Handling and Sampling Systems Design
2. American Petroleum Institute, API RP 550, Part II, Process Stream
for Process Analysis, Pittsburgh, PA: Instrument Society of America, 1977.
Analyzers.
Lodge, J. P., Methods of Air Sampling and Analysis, Chelsea, MI: Lewis
3. Nichols, J. H. and Brink, J. A., Jr., Use of Fiber Mist Eliminators in
Publishers, 1988.
Chlorine Plants, Electrochemical Technology, JulyAugust 1964.
McMahon, T. K., The New Sampling/Sensor Initiative, Control, August 2001.
4. System Samples Materials without Opening Manway, Chemical Pro-
Meyers, R. A., Encyclopedia of Analytical Chemistry: Instrumentation
cessing, mid-November 1986.
Applications, New York: John Wiley & Sons, 2000.
5. www.sludgecontrols.com.
Sherman, R. E., Process Analyzer Sample-Conditioning System Technology,
New York: John Wiley & Sons, 2002.
Strauss, R., Filtering Samples to On-Line Analyzers: Advanced Control and
Bibliography Instrumentation, Houston, TX: Gulf Publishing Co., 1987.
Sugar, J. W. and Brubaker, J. H., Sampling for Waste Water Analyzers,
American Petroleum Institute, Manual on Installation of Refinery Instru- InTech, June 1973.
ments and Control Systems: Part IIProcess Stream Analyzers, latest Van den Berg, F. W. J. et al., Selection of Optimal Process Analyzers for
edition. Plant-Wide Monitoring, Analytical Chemistry, 74(13), 2002.
Anderson, R., Sample Pretreatment and Separation, 1987. Webster, J. G., The Measurement and Instrumentation and Sensors Hand-
Clevett, K. J., Handbook of Process Stream Analyzers, Chichester, U.K.: book, Boca Raton, FL: CRC Press, 1999.
Ellis Horwood, Ltd., latest edition. Woodget, A. and Cooper, D., Sample and Standards, 1987.

2003 by Bla Liptk