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Chapter 5 Optional Fittings

Inside this chapter you will find: HEATER OPTIONS STIRRER MOTORS AND DRIVES STIRRER OPTIONS GAS ENTRAINMENT CATALYST BASKETS CONDENSERS SAFETY RUPTURE DISCS PRESSURE RELIEF VALVES PRESSURE GAGES GAS MEASUREMENT SYSTEMS HIGH PRESSURE BURETTES LIQUID CHARGING SYSTEMS METERING PUMPS LIQUID PIPETTES SOLIDS CHARGING SYSTEMS COOLING COILS LINERS SAMPLE COLLECTION VESSEL BOTTOM DRAIN VALVES VALVES AND FITTINGS SAFETY CHECK VALVES THERMOCOUPLES PRESSURE HOSE EXPLOSION PROOF APPARATUS WINDOWS INSULATED ELECTRICAL GLANDS SPARE PARTS KITS TEMPERATURE LIMITS EXTERNAL VALVES AND FITTINGS Heaters

arr has designed standard reactors designed for tempera- cooling channels are also Pelectrical heaters for all tures to 600 °C and for large included. of the reactors in our product multi-zone heaters. Aluminum block heaters line. Different types of heaters have three distinct features are used for individual reactors Optional and Custom which make them ideal for to best meet the operational Heaters. many applications: needs, heating load, and Parr offers a variety of expected operating tem- heater designs which can be 1. Since the heating elements peratures. The standard heater substituted for the standard are sealed within these type and power rating for each heater normally furnished with housings, explosive vapors reactor model is listed in the each reactor. Most of these cannot reach them and the reactor specification tables. can also be used with Parr heater can be considered The standard designs will typi- non-stirred pressure vessels explosion proof, provided cally be one of the following: as well. The principal features it is equipped with optional and recommended applica- explosion proof wiring and Clamp-On Band Heaters tions for these heaters are a safety cut-out to ensure These are normally used described below. that the heater will not for very small reactors where exceed a specified tempera- maximum watt densities and Flexible Heating Mantles. ture limit allowed for the heat transfer are required due These can be furnished for explosive atmosphere. to the limited surface area many different applications. 2. With heat spread uniformly available on the vessel. These are similar to the rigid throughout the aluminum type described above except block, uniform heating is Rigid Heating Mantles. they are not held in an alu- applied to all surfaces of These are quartz fabric minum housing. They have a the vessel, comparable to mantles housed in aluminum flexible fabric outer case for the rapid response obtained shells. They are used for electrical and thermal insula- with a steam or hot oil moderate sized reactors in tion. This type of mantle is jacket, but without requiring designs where the heater can particularly useful for heating costly steam generators, oil be moved on or off the vessel. vessels with irregular shapes, baths, circulating pumps They are light weight and easy such as those with windows and other accessory equip- to handle, but they are not in the cylinder wall, since they ment. used to support the weight are flexible and can be split 3. Since there is a cooling of the vessel and they are and laced onto a vessel around coil in the aluminum block, generally limited to operating any external protrusion. As this style heater can also temperatures of 350 °C or less. with rigid mantles, they will provide external cooling produce temperatures up to for controlling an exother- Calrod-Type Sheathed 350 °C, but they are limited mic reaction without the Element Heaters. to watt densities of 10 watts internal clutter and clean- These are rugged heaters per square inch. This type of ing problems associated with Calrod-type elements heater can be made to cover with internal cooling coils. held within a metal shell. They any of the vessels offered by Eliminating an internal coil are used for medium to large Parr, and they are sometimes also permits the use of spi- reactors for operating temper- preferred when only moderate ral, paddle or other stirrers atures to 350 °C. In some cases temperatures are required. which cannot be used when the heater shell itself forms a Since they are constructed of an internal coil is installed. part of the reactor support. An cloth, an electrical ground wire advantage of Calrod heaters is cannot be provided. Circulation Jackets. that the heating elements are A jacket can be welded to easily replaceable. Aluminum Block Heaters. the outer wall of most Parr These are available as an pressure vessels to provide a Ceramic Heaters. option for most reactors and means for heating or cooling These are special purpose pressure vessels. For vessels the vessel with a hot or cold heaters with an electric ele- of two gallons or less the liquid or steam. This type ment embedded in a shaped heaters are machined from of heating is ideal for users ceramic body which is held solid blocks of aluminum and who want to duplicate plant within an insulated metal heater wells are machined into operating conditions, using a housing. They are used for the walls of the block. Optional jacketed reactor comparable

www.parrinst.com 102 Parr Instrument Company Optional Fittings 5

to jacketed equipment used in their plant. Since there are no electrical components in a jacket, and since the maximum temperature can be controlled by controlling the temperature of the heating medium, a jack- eted vessel will be accepted as explosion proof and suitable for use in hazardous atmospheres. Rapid and uniform heating can be attained with a jacketed vessel since the heating med­ium is in direct contact with the vessel. By control- ling the temperature of the heating medium, temperature overshoots can be avoided when working with sensitive materials.­ Standard jackets are designed for operating pres- sures up to 100 psig (7 bar) within the jacket. Higher pres- sure jackets can be provided if required.

Cylinder, 2000 mL, with Welded Circulating Jacket.

Model 4666 2-Gallon Non-Stirred Reactor with Welded Jacket, Hinged Split Rings, Pneumatic Lift, and Bottom Drain Valve.

Aluminum Block Heater with Cooling Channel and Heat Shield for 1000 mL Vessel.

1-800-872-7720 Parr Instrument Company 103 Stirrer Motors and Drives

Torque vs. Stirring Speed ring speed must be matched available speed are all depen- he standard, open-type, to provide an effective mixing dent upon the pressure and Tvariable speed motor system. available volume of the driving installed on each Parr reactor As a general rule, the mag- air source. Maximum torques will produce stirring speeds netic coupling installed on each are delivered at relatively from zero to between 600 Parr reactor will have a torque slow speeds and maximum and 800 rpm with a torque rating considerably higher than horsepower is delivered at high adequate to drive the installed the torque obtainable from the speed. impellers in average viscosity motors offered for use with mixtures. Higher horsepower that apparatus. The goal is to Geared, Direct Drive Motors motors and special stirrers can make the motor the weak link A geared, direct drive motor be provided for higher viscosi- so that the magnetic stirrer will can be installed on most fixed ties. Alternate drive pulleys are be protected. Reference torque head floor stand reactors. This available to produce higher rating for applicable magnetic is an attractive arrangement for stirring speeds, but several drive. handling heavy stirring loads. basic rules must be considered Any 1/4 hp or larger, when changing any of these Explosion Proof Motors variable-speed standard or components. Explosion proof motors explosion-proof motor can be The highest torque from designed for Class I, Groups C used. Gear box drives are avail- any motor is obtained at lower and D and Class II, Groups F able with ratios of 3:1, 5:1 and stirring speeds. Increasing and G with variable speed con- 10:1. The 1700 rpm maximum the stirring speed reduces the trol can be furnished for most speed will be reduced in an torque in inverse proportion Parr reactors. amount determined by the to the speed. For operations reduction ratio of the gear involving high viscosity Air Motors box, and the associated torque mixtures, the motor size, the Air-driven motors can be values from the table will be type of impeller and the stir- installed on most reactors. The increased in the same ratio. horsepower rating, torque, and

Stirrer Drive Motors Standard Pulley Optional Pulley Motor HP Explosion Variable Max Speed, Max Torque, Max Speed, Max Torque, Designation Rating Proof Speed RPM* in-lb RPM* in-lb -VS.12 1/8 No Yes 600 12 1700 4 -XP.25 1/4 Yes Yes 600 27 1700 9 -AM.25** 1/4 Yes Yes 1000** 30** — — -VS.25 1/4 No Yes 600 27 1700 9 -VS.50 1/2 No Yes 600 54 1700 18 -XP.50 1/2 Yes Yes 600 54 1700 18 -AM.50** 1/2 Yes Yes 1000** 66** — — -VS.75 3/4 No Yes 600 81 1700 27 -XP.75 3/4 Yes Yes 600 81 1700 27 Values represented are nominal. VS = variable speed, XP = explosion proof, AM = air motor, 1 in-lb = 0.11 Nm, 1 hp = 0.75 Kw *Maximum speed values based on “no load” **HP, RPM, and torque values for air motors are based on a 40psi supply capable of 34cfm for the AM.50 and 10cfm for the AM.25.

www.parrinst.com 104 Parr Instrument Company Optional Fittings 5

Parr Geared Drive Motor mounted on a Series 4553 Stirred Reactor System.

Gear Box Torques 3:1 Gear Box 5:1 Gear Box 10:1 Gear Box Motor HP Max Speed, Max Torque, Max Speed, Max Torque, Max Speed, Max Torque, Rating RPM in-lb RPM in-lb RPM in-lb 1/4 600 27 360 45 180 90 1/2 600 54 360 90 180 180 3/4 600 81 360 135 Not Recommended

Magnetic Drive

Description Maximum Torque, in-lb

General Purpose 16 Footless General Purpose 16 Heavy Duty 60 Footless Heavy Duty 60 Extra Heavy Duty 120 Footless Extra Heavy Duty 120

1-800-872-7720 Parr Instrument Company 105 Stirrer Options

Turbine Type Impellers arr reactors are usually equipped with turbine Ptype impellers which produce an excellent mixing action over the range of stirring speeds at which these reactors typically operate. These impellers are made in four-blade and six-blade styles, with the smaller four-blade impellers used only on Micro and Mini Reactors. These impellers, for reactors with 300 mL volume or greater, may be positioned anywhere on the stirring shaft, with one impeller usually located near the bottom of the vessel to keep solids up in suspension and a second impeller positioned near the base of the vortex to pull reactant gases down into the liquid phase. These impellers gen- erally provide excellent mixing for systems with effective viscosities up to approximately 25,000 centipoise (cP) with a 16 in-lb magnetic drive or Turbine Type Impeller Anchor Stirrer up to 50,000 cP with 60 in-lb magnetic drive.

Anchor Stirrers Anchor stirrers are available in several config- urations for use with moderate to high viscosity materials. This type of stirrer usually works best in vessels with an inside depth to diameter ratio of 1.5 to 1 or less. They are intended to operate at relatively slow speeds and generally require a heavy duty drive system capable of generating and delivering sufficient torque to the agitator. Footless magnetic drives work well with anchor or spiral stirrers. Three basic types are offered: 1. A U-shaped, flat bar anchor. 2. A flat blade, paddle type anchor. 3. A two-arm or three-arm, self centering anchor with PTFE wiper blades.

Spiral Stirrer Paddle Type Anchor All of these designs may not be appropriate or available for each reactor size. Please contact the Parr Technical Service Department for assistance in selecting an anchor stirrer suitable for the intended operating volume and viscosities.

Spiral Stirrers Spiral stirrers can be installed in any 1 liter, 2 liter or 1 gallon reactor to produce a positive downward thrust or upward thrust action when working with viscous polymers or other high viscosity mixtures. They work best in floor stand reactors with adjustable speed and heavy duty drive systems. Either left-hand (downward thrust) or right hand (upward thrust) spirals are available. The downward thrust spiral is gener- ally preferred for heavy suspensions.

Note: Additional internal fittings may be required to Gas Entrainment Impeller Anchor Stirrer with Wiper Blades adapt some stirrer styles to existing reactors in the field.

www.parrinst.com 106 Parr Instrument Company Optional Fittings 5 Gas Entrainment Impellers

arr offers a series of gas Pentrainment impellers for users who want to obtain maximum gas dispersion into a liquid system. This is obtained with a unique impel- ler attached to a hollow stirring shaft through which gases are continuously recirculated from the head space above the liquid through the impeller into the liquid phase. As with all impellers, the speed of the stirrer creates a vacuum at the Gas Entrainment Impeller tip of the impeller. Gas enters openings near the top of the shaft and is pulled through Since these gas entrainment dispersion ports located at the impellers operate best in the tips of the impellers. In the 1000-1200 rpm range, users Parr system with dispersion will want to ensure that their ports located at the very tips stirrer drive system is set up to of the impellers, the higher the deliver these operating speeds; stirring speed — the higher the alternate pulleys and belts are vacuum — and the higher the available to convert existing driving force for this very effec- reactor systems. tive gas dispersion system. These impellers are offered Baffles as a complete package which Because it is the relative includes the impeller, the hol- speed of the tip of the impeller low shaft with coupling, and to the liquid phase that gov- any required foot bearings and erns the mass transfer, baffles, Gas Entrainment Impeller with Hollow Shaft brackets for the intended reac- which impede the rotation of tion. The baffles are a separate the liquid with the impeller, option which must be ordered can greatly enhance the opera- individually. tion of these gas entrainment The gas entrainment stirrers impellers. While some natural may be ordered as an optional baffling is provided by the stirrer when purchasing a internal thermowell, dip tube new reactor system or easily and cooling coils, the remov- installed in an existing system able baffles are recommended in the field. With the wide for use with these gas entrain- variety of reactor head styles ment impellers. These baffles and magnetic stirrers furnished may also be beneficial with on Parr reactors it is best to the more traditional turbine contact us with the numbers type impellers for certain stamped on the head of your applications. vessel so that we will be able to furnish the correct gas entrainment assembly for a particular reactor system.

Removeable Baffle Set

1-800-872-7720 Parr Instrument Company 107 Catalyst Baskets

atalyst baskets can be provided for holding a supported Ccatalyst so that it will not be destroyed or changed by the stir- ring action of the impeller. These can be installed in reactors with volumes ranging from 300 to 2000 mL. Two interchangeable styles are available. Special heads, internal cooling coils, thermowells and dip tubes are required to provide clear space in the vessel for these baskets.

The Static Design In the static design the mesh basket holding the catalyst remains stationary while impellers on the stirring shaft and baffles outside of the basket direct the flow of reactants over the surface of the contained catalyst. A unique gas entrainment impeller pro- vides a uniform flow of both gas and liquid over the fixed catalyst bed held within the annular basket. The Parr design for these baskets includes a rigid bottom support which permits high speed stirring without excessive vibration. Cooling coils, internal tem- perature measurements, and liquid and gas sampling operations can be continued as usual without interference from the installed catalyst basket.

The Dynamic Design In the dynamic design the catalyst is held in an annular shaped, mesh basket which is attached to the stirrer drive in place of the stirring shaft. The rotating basket then serves as an impeller for stirring the reactants. Fixed baffles and coaxial impellers ensure good circulation over the surface of the contained catalyst. The Catalyst Basket Static Design dynamic baskets are available for reactors with volumes of 1000, 1800, and 2000 mL. Dynamic baskets must be installed in reactors equipped with at least 1/4 hp motors to ensure that sufficient stirrer torque and speeds are available for proper operation. Dynamic baskets are interchangeable with static baskets in 1 liter and larger vessels.

Catalyst Basket Static Design with Uniflow Stirrer

Catalyst Basket Dynamic Design

www.parrinst.com 108 Parr Instrument Company Optional Fittings 5 Condensers

arr offers two styles of con- valve at the top of the con- Pdensers for attachment to denser. If condensate collection the head of a stirred reactor or is not required, the receiver can pressure vessel. These can be be removed and the condenser made in various sizes to match can be mounted directly above the size of the reactor. the reactor for direct reflux into the vessel. Straight Reflux Condenser The reflux condenser Modifications consists of a length of tubing Many users opt to install a connected directly to the head ball valve at the head of the reac- of a vessel and equipped tor below the condenser to use with a water cooling jacket. as a shut-off to the condenser. Condensed vapors are returned Alternate collection vessel vol- directly to the vessel and umes are available upon request. any non-condensable gases The installation of a con- can be released through a denser on any of the Parr needle valve at the top of the reactors requires a larger port in condenser. A spiral wound the head of the vessel, the size of inner packing in the condenser which will vary with the volume ensures maximum effective- of the reactor system. Due to ness in a rather short length. the limited space on the 4560 mini reactors we would change Reflux/Take-Off Condensers either the gage opening or one The reflux/take-off con- of the cooling coil ports to 1/4" denser consists of a water NPT for use with a condenser. jacketed tube, the same as This modification would then described above, assembled either combine the gage and with a receiving vessel condenser functions or eliminate attached to the lower end of the internal cooling loop to the condenser. Any vapor, such accommodate the condenser. as water from a polymerization Reactors with volumes of 1 liter reaction, can be condensed and and greater would be modified collected in the receiver, from with a 3/8" NPT opening or which it can be withdrawn larger depending on the reactor through a bottom valve. Any volume. The standard head non-condensable gases can fittings would be rearranged to Straight Reflux Reflux Take-Off Condenser Condenser be released through a needle accommodate this port.

Condensers Inner Tube Standard Reactor Style Note Part No. Diameter, in. Receiver, mL 4560 / 4590 Reflux/Take-off Mod. Gage Opening 1/4" NPT 1/4 150 A2011HC 4560 / 4590 Reflux Mod. Gage Opening 1/4" NPT 1/4 A2012HC 4560 Reflux/Take-off Mod. Cool Coil Opening 1/4" NPT 1/4 150 A2013HC 4560 Reflux Mod. Cool Coil Opening 1/4" NPT 1/4 A2014HC 4520 / 4530 / 4550 Reflux/Take-off 3/8" NPT 3/8 300 A2001HC 4520 / 4530 / 4550 Reflux 3/8" NPT 3/8 A2002HC 4530 Reflux/Take-Off 3/8" NPT 3/8 300 A2003HC 4530 Reflux 3/8" NPT 3/8 A2004HC 4540 / 4570 / 4580 Reflux/Take-off 3/8" NPT 3/8 300 A2016HC 4540 / 4570 / 4580 Reflux 3/8" NPT 3/8 A2017HC 4555 / 4556 Reflux/Take-off 1/2" NPT 3/4 1000 A2018HC 4555 / 4556 Reflux 1/2" NPT 3/4 A2019HC

1-800-872-7720 Parr Instrument Company 109 Safety Rupture Discs

We have selected alloy 600 as the standard material for these rupture discs. It provides 1/4" NPT (M) excellent corrosion resistance while retaining over 90% of its room temperature rating at temperatures up to 450 °C. For added corrosion resistance we can furnish these discs with gold facing or replace them with discs made of Alloy C276. Discs can be produced to match any oper- Orifice Ring ating pressure and temperature above the stated Rupture Disc minimums. Parr reactors and pressure vessels from 25 mL to 2000 mL use the 526HC alloy 600 disc Nose Cone or 581HC alloy 600 with gold facing. The 1 gallon and larger use the 708HC series discs. The 4580 A888HC2 Rupture reactor systems use the 1415HC series discs. Disc Assembly arr Pressure Vessels are protected by For a complete listing of part numbers, burst Pcustom built rupture discs furnished by ranges and materials see Manual 231M. Fike® Corporation, a specialist in this exotic art. In general, the 1000 psi disc in the Examination of these discs will indicate that 526HC/581HC series discs and the 800 psi in each of these discs is domed. This dome was the 708HC are the lowest available ranges in produced at the factory by taking the individual the alloy 600 material. Alternate disc materials disc to 70% of its burst pressure. are available but they do not offer the same The ASME as well as other pressure vessel corrosion resistant properties and temperature codes dictate that pressure vessels must be capabilities. equipped with a rupture disc designed to burst For applications where users prefer a lower no higher than the design pressure of the ves- range pressure gage, we would add a spring sel. For pressure loads that do not cycle rapidly loaded relief valve set to protect the gage and a such as our vessels, Fike suggests limiting the 1000 psi rupture disc as the fail safe protection. actual operating pressure to no more than 90% Users are invited to contact the Parr Technical of its burst pressure. This combination will limit Support Staff with requirements for special operating pressures to no more than 90% of the rupture discs. design pressure of the vessel.

Rupture Discs for 1/4" Orifice Rupture Discs for 1/2" Orifice

Burst Rating, psig Inconel Disc Gold-Faced Inconel Disc Burst Rating, psig Inconel Disc

1000 526HCPD 581HCPD 1000 708HCP10CT 2000 526HCPF 581HCPF 1500 708HCP16CT 3000 526HCPG 581HCPG 2000 708HCP20CT 4000 526HCP40CT 581HCP40CT 3000 708HCP30CT 5000 526HCPH 581HCPH 3000 1415HCP30CT 8000 526HCPJ 581HCPJ 4500 1415HCP45CT 10000 526HCP100CT

www.parrinst.com 110 Parr Instrument Company Optional Fittings 5 Pressure Relief Valves Gages

pring-loaded relief valves should be viewed Sas supplements and not substitutes for a safety rupture disc which is the primary means protecting the vessel and the operator in case of accidental over-pressure. Spring loaded relief valves can be added to a reactor or vessel to: • Relieve pressures near the maximum operating pressure. • Reseal 593HCPF Gage once excess pressure has been 3-1/2" Dia. relieved. • Protect low pressure components at pres- sures below available rupture disc ranges.

The relief valves listed below can be installed on any Parr vessel. These relief valves are stainless steel and have FKM O-rings. Other 2633HCP10AD 3-1/2" Back Mount Gage valves and O-ring materials are available on special order. pounds per square inch (psi) and bars. Gages in Pascal units are available on special 56HCPF Gage order. Compound gages which 4-1/2" Dia. show vacuum to 30 inches of Mercury and positive pressures to 300 psi (20 bar) are also ages for Parr pressure available. Gvessels can be furnished When ordering a special with either 3-1/2" or 4-1/2" dials gage, specify the gage diam- in any of the ranges shown in eter, the desired range and A175VB the table below. All have stain- scale units. Relief Valve less steel Bourdon tubes and The gage on a pressure 1/4" NPT male connections. vessel should be 150 percent Alloy 400 gages are of the maximum operating available on special order. pressure. This allows the gage Accuracy is .5 percent of full to operate in the most accurate Pressure Relief Valves scale for the 4-1/2" size and 1 pressure range and prevents percent for the 3-1/2" gages. the gage from being stressed Relief Pressure Discharge Part No. All are calibrated in both repeatedly to its full range, Range, psi Connection which will effect the calibration. A140VB2PA 50-150 1/4" NPT (M) A140VB2PB 150-350 1/4" NPT (M) Gages

A140VB2PC 350-600 1/4" NPT (M) Pressure, Range, 4-1/2" Dia. 3-1/2" Dia. 3-1/2" Dia. Back A175VB 750-1500 1/4" NPT (F) psi bar Gage No. Gage No. Mount Gage No. A175VB2 1500-2250 1/4" NPT (F) 0-100 0-14 56HCPA 593HCP1AD 2633HCP1AD A175VB3 2250-3000 1/4" NPT (F) 0-200 0-28 56HCPB 593HCP2AD 2633HCP2AD A175VB4 3000-4000 1/4" NPT (F) 0-600 0-40 56HCPC 593HCP6AD 2633HCP6AD A175VB5 4000-5000 1/4" NPT (F) 0-1000 0-70 56HCPD 593HCPD 2633HCP10AD Note: When ordering any of the above relief valves, 0-2000 0-137 56HCPF 593HCPF 2633HCP20AD the user may specify a desired set pressure. 0-3000 0-210 56HCG 593HCPG 2633HCP30AD 0-4000 0-280 NA 593HCP40AD — 0-5000 0-350 56HCPH 593HC50AD — 0-7500 0-517 56HCP75AD NA — 0-10000 0-700 56HCPK NA — 30" Hg Vac/300 psi 56HCP3YB 593HCP3YB 2633HCP3YB

1-800-872-7720 Parr Instrument Company 111 Gas Measurement Systems

arr offers a variety of 2. The supply tank can be The main consideration in Paccessories for its line fitted with a constant selecting mass flow meters of pressure reaction vessels pressure regulator. The is to specify a pressure and to enable the investigator regulator must be selected a measurement range appro- to accurately determine the to match the planned oper- priate to the reaction. Some amount of gas consumed in a ating pressure. This regula- additional considerations are: reaction conducted at elevated tor will deliver gas to the • Mass flow meters tend pressures and temperatures. reaction vessel at constant to have an accuracy of 1% There are essentially two pressure overcoming the of the full-scale flow rate. methods used to measure the limitation described in (1) Since the meter must be amount of gas delivered to a above. sized to record the maxi- reaction vessel. These are: 3. Initial and final pressures mum expected flow rate, 1. The measurement of the in the supply tank can the accuracy is poor when pressure drop in an auxil- be measured with analog the reaction is nearly com- iary supply vessel of known gages, or continuous pres- pleted and the flow rate is volume. sure readings can be made lower. Some systems over- 2. The measurement and and recorded using pres- come this by placing two integration of the flow sure transducers. While the meters in parallel and shift- rates using an electronic transducers add cost, they ing over to the lower flow mass flow meter. also add increased resolu- rate meter once the initial tion and the opportunity to surge is over. Each of these methods has follow the rate of the pres- • Meters are calibrated for its advantages and limitations sure drop and hence the a specific gas. If the user as discussed below. rate of reaction. will work with only one gas, 4. Enhanced precision can e.g. hydrogen, this is not a Intermediate Supply Tanks be achieved by measuring significant restriction. Certainly the simplest the temperature in the sup- • Electronic flow meters method to measure the ply tank and applying cor- are relatively fragile and amount of gas consumed in a rections as appropriate. must be protected with reaction is to feed the gas from filters to ensure reliable a vessel of known volume Parr has put together service. and to measure the pressure a series of high pressure drop in this vessel during the burettes in complete packages Mass Flow Controllers course of the reaction. The for direct connection to our Mass Flow Controllers add consideration in this method reactors. The basic ones are an automated control valve is to select a supply vessel listed on the following page. to the mass flow meter to with a volume matched to the These burettes can also be provide gas flows that are amount of gas that will be con- equipped with digital pressure proportional to an electronic sumed in the reaction. It needs transducers, internal thermo- set point. Although normally to be large enough to contain couples and data acquisition used to provide a constant enough gas to complete the and reduction support. Please flow rate to reactors operated reaction and small enough that contact our customer support in a continuous-flow mode, the pressure drop will be sig- group for information on these a unique application in batch nificant and measurable. This possibilities. reactions is to allow the set basic technique can be applied point to be dictated by the in a number of ways: Mass Flow Meters error signal from the reactor Contact Parr Technical pressure transducer. As gas is 1. The supply tank can be Service for help with mass consumed, the pressure drop connected directly to the flow meters or controllers. signal can be configured to reaction vessel. This is the Because these meters must increase inlet flow. This signal simplest and least expen- be individually specified and can be sent to multiple control- sive. The principal limitation calibrated to the specified gas lers, enabling the make-up of this approach is that the as well as the desired flow rate gas to be a mixture with an reaction pressure will fall and operating pressure, no operator-specified ratio. This as gas is consumed and the attempt has been made here technique is often used in reaction will not be conduct- to identify the possible selec- the study of co-polymers and ed at a constant pressure. tions and specifications. ter-polymers.

www.parrinst.com 112 Parr Instrument Company Optional Fittings 5

High Pressure Gas Burettes Parr high pressure burettes Reservoirs with larger arr offers a series of high can be furnished in various volumes are available as Ppressure burettes intended sizes as shown in the adjoining are regulators with different to introduce gas (commonly table, each with a regulator to delivery ranges. Modifications hydrogen) to a reactor at a deliver gas to the reactor over can be made to these basic constant pressure. The burettes the designated pressure range. systems to add an internal consist of a high pressure The moles of gas shown in the thermocouple to the reservoir reservoir equipped with an table represent the amount of and/or a pressure transducer inlet valve, a pressure gage hydrogen that will be held in for digital readout and/or and a relief valve. A constant the burette at the maximum recording. pressure regulator with a check pressure. The deliverable vol- valve, a connecting hose and ume will be a function of the a support stand are included difference in pressure between with each pipette. the pipette and the reactor. The amount of gas con- The size of the burette selected sumed in a reaction can be should be large enough to determined by knowing the provide sufficient gas to com- volume of the high pressure plete the reaction while still reservoir and observing the maintaining sufficient pressure pressure drop in the reservoir in the burette to force gas into during a reaction. the reactor.

High Pressure Gas Burettes

Burette Delivery Pressure Range

Maximum Total H2 Volume, mL 0-1800 psi 0-1200 psi 0-700 psi Pressure, psi Volume, Moles 150 1800 0.8 A2280HC A2280HC2 A2280HC3 300 1800 1.5 A2281HC A2281HC2 A2281HC3 500 1800 2.6 A2282HC A2282HC2 A2282HC3 1000 1800 5.1 A2283HC A2283HC2 A2283HC3 2250 1800 11.5 A2284HC A2284HC2 A2284HC3 A2283HC High Pressure Gas Burette 500 5000 7.1 A2285HC A2285HC2 A2285HC3

Liquid Charging Systems

Liquid Metering Pumps described under these catalog reactor. Special pumps can iquid metering pumps are numbers include an inlet filter, be furnished to meet require- L commonly used to intro- a reverse-flow check valve ments outside the range of duce liquids into a reactor or and the outlet tubing to the these pumps. vessel at elevated pressures on a continuous basis. A wide variety of pumps are available Liquid Metering Pumps to meet various pressure, flow, Remote Flow Rate, Pressure, Wetted and control requirements. The Part No. Control mL/min Max. psi Material pumps listed here cover some 0-10 VDC of the more common pressure A2286HC 0.01-10 2500 PEEK No and flow requirements associ- A2287HC 0.01-10 5000 Stainless No ated with Parr reactors and pressure vessels. The pumps A2288HC 0.04-40 1500 Stainless No A2289HC 0.01-10 5000 Stainless Yes A2290HC 0.04-40 1500 Stainless Yes A2291HC 1.0-80 5000 Stainless No

1-800-872-7720 Parr Instrument Company 113 Solids Charging Systems

Liquid Charging Pipettes One of the modifications Larger diameter valves are o introduce liquids into most frequently requested is available for 1 gallon and Treactors or vessels at a port or other means to feed larger vessels. These ball elevated pressures, liquids, solids, or slurries into valves will withstand the full the most economical the vessel without removing pressure developed in a reac- way is to use the head. This can be done in tor at moderate temperatures, A143VB Ball Valve a pressure various ways. but their pressure rating falls pipette as a off rapidly at temperatures secondary Ball Valve Solids Charging above 100 °C. vessel. These Ports are often used ball valve with a 3/8" for liquid addition Adiameter opening can Solids Charging Ports to a batch process. be installed on any one liter Orifice Nominal Liquid is forced into the or larger vessel and used Part No. Diameter, Size reactor from the pipette in conjunction with a high in. by applying gas pres- pressure pipette for injecting A143VB 1/4" NPT (F) 0.250 Solids Charging Auger sure to the pipette slurries under pressure. These A132VB 3/8" NPT (F) 0.375 greater than the pres- are opened or closed with a sure within the vessel. quarter turn of the handle. 396VBAD 1/2" NPT (F) 0.406 If the passages in the connecting line are large enough, slurries Capped Openings Tubing can be connected or catalyst suspen- capped opening in the to the fitting, but this type sions can also be Ahead of a reactor can of connector is normally A2113HC charged into the reac- serve as a convenient solids used only where solids or Liquid tor in this manner. charging port, offering the slurries will be added at Charging The pipettes listed largest possible diameter atmospheric pressure. Pipette below offer a choice of and a significantly shorter volumes and are rated passage than a ball valve. A Capped Openings for pressures to 1800 psi. male connector with a cap They include a nitrogen is usually used to close the Available A550HC Catalyst Reactor filling connection for opening. These will have a Fitting Sizes Addition Device attachment to a nitrogen reliable metal to metal seal Mini 1/4" NPT (F) tank. More elaborate and the ability to withstand the 1 & 2 Liter 3/8" NPT (F) pipette systems can be full temperature and pressure assembled to special order to for which the vessel is rated. Gallon & up 1/2" NPT (F) include additional fittings, such as a pressure gage for the pipette, a pressure relief valve or a large opening ball valve. Catalyst Addition Devices pressure within the reac- Special pipettes can also be arr has developed a unique tor, the cap is forced open furnished for higher pressures Pdevice for adding small and the catalyst or other to 5000 psi. amounts of solids (or liquids) contents of the holder will from a sealed container held be released into the reac- within a reactor. It is of particu- tor. This device works best Liquid Charging Pipettes lar interest to users performing in the taller, 450 mL and kinetic studies of catalytic 600 mL Mini Reactors, Pipette Pressure reactions. This device consists and in the 1 liter and Part No. Volume, Rating, A550HC Open mL psi of a small cylindrical chamber larger Parr Reactors. with a cap that is sealed to A2113HC3 50 1800 the body with an O-ring. It A2113HC4 150 1800 attaches to the underside of Liquid A2113HC 300 1800 the vessel head with a 1/8" Complete Mounting NPT connection. To discharge Assembly No. Thread A2113HC2 1000 1800 the contents of the holder, gas Reactor Size, cc pressure is applied through a Mini 6 A550HC3 1/8" NPT valve installed on the top of One Liter 8 A550HC 1/8" NPT the head. When the applied pressure is greater than the Larger 20 A550HC2 1/8" NPT

www.parrinst.com 114 Parr Instrument Company Optional Fittings 5 Cooling Coils Liners

nternal cooling coils are These coils provide reasonable emovable, open top, Iavailable for all but the surface area, minimum inter­ Rcylindrical liners made smallest Parr reactors. These ference with stirring patterns, either of borosilicate glass coils provide an extremely a reasonable amount of baf- or PTFE can be furnished effective means of removing fling, and ease of cleaning and to fit most Parr reactor and heat from the vessel to control maintenance. most of the general purpose an exothermic reaction or for Spiral Coils - Spiral coils vessels. These liners slide cooling the reactor at the end consist of multiple loops into the cylinder and require of a test. Since heat is trans- wound just inside the inside no additional fittings, but ferred through the relatively diameter of the vessel. They they may not coordinate with thin wall of the coil instead of are normally available only some alternate accessories the thick wall of the vessel, for the 4" and 6" ID vessels and stirrers. Although they cooling rates are generally although other sizes have been will not keep corrosive vapors much faster than heating rates; built on special order. They from reaching the surfaces of Serpentine Cooling particularly at temperatures do maximize the cooling area the cylinder and head, they Coil 1000 mL above 80 °C. Water is normally available, but sometimes at make it much easier to add used as the cooling medium the expense of uniform stirring and remove liquid reactants, although compressed air and ease of cleaning. and they give some protection can be used for modest The individual reactor to the cylinder when working cooling loads. Cooling coils specifications will dictate the with corrosive solutions. It are offered in three standard style of coil or coils available must be noted, however, that configurations: for each reactor. On some adding a PTFE liner will slow Single Loop - Single loop reactors the coils are included the heat transfer rate into and coils consist of a vertical run of as standard while on some out of the vessel, and it may tubing formed into a “hairpin” reactors they are optional. be necessary to adjust the shape. These are normally Cooling coils are available temperature control method to installed on small reactors in the same choice of materials prevent overheating. where there is minimum space as the reactor bodies them- available. selves. All cooling coils are Serpentine Coils - removable. Plugs are available Liners Serpentine coils consist of six to close the openings in the Glass PTFE to eight vertical runs of tubing head and in most cases these Fits Cylinder Liner Liner uniformly spaced around the openings can be converted to ID, in. Size, mL Part No. Part No. circumference of the vessel. alternate inlets/outlets if cool- Spiral Cooling Coil 1000 mL ing is not required. 1.3 50 1431HC 1431HCHA 1.3 100 1431HC2 1431HC2HA 1.5 75 2920HC 2920HC2HA 2-1/2 250 762HC10 NA 2-1/2 500 762HC2 NA 2-1/2 300 762HC 762HC4HA 2-1/2 450 762HC2 762HC5HA 2-1/2 600 762HC3 762HC6HA 2 100 762HC7 762HC7HA 2-1/2 160 762HC8 762HC8HA 3-1/4 600 2312HC 2312HC3 3-1/4 1200 2312HC2 2312HC4 3-3/4 1000 1441HC 1441HCHA 3-3/4 1800 1442HC 1442HCHA 4 1000 398HC 398HCHA 4 2000 399HC 399HAHA 6 1 Gallon 894HC 894HC4HA 6 2 Gallon 894HC2 894HC5HA Glass Liners 2000 and 1000 mL Sizes PTFE Liners 2000 and 1000 mL Sizes Temperature Limit: 565 ˚C Temperature Limit: 225–250 ˚C

1-800-872-7720 Parr Instrument Company 115 Sample Collection Vessels

sample collection vessel can be added to Standard material of construction is T316 Amost reactor systems. Designed to efficiently Stainless Steel but it can be provided in any of and safely allow for the withdrawal of liquid or the other alloys if required. A high pressure sam- vapor samples at elevated temperatures and ple collection vessel without a cooling sleeve for pressures, this quick close, O-ring seal vessel has pressures to 5000 psi is available upon request. a volume of 10 mL and is designed for operating pressures to 3000 psi (200 bar). The typical arrangement for this sample ves- Sample Collection Vessels sel includes a cooling sleeve, isolation and vent Part No. Description valves. A drain valve may also be added to Sample Collection vessel, 10 mL, with cooling the vessel. 4351 sleeve, isolation & vent valves for connection to The isolation valve is mounted at the head of 1/8”NPT valves this vessel and is used to seal the vessel once the Sample Collection vessel, 10 mL, with cooling sample is transferred. The vent valve is installed 4352 sleeve, isolation & vent valves for connection to in a tee and is used to release any residual pres- 1/4”NPT valves sure in the line between the sample valve and the Sample Collection vessel, 10 mL, with cooling sample vessel. Samples can be removed either 4353 sleeve, isolation & vent valves for connection to by opening the collection vessel and pouring it 3/8”NPT valves out or by use of the drain valve. -D Optional Drain Valve Bottom Drain Valves

ottom drain valves can be added to most smaller vessels. High pressure and larger diam- BParr reactors. These valves are particularly eter valves are available where required. useful for those working with polymers or other These valves will withstand the full operat- material that must be discharged from the ing pressures and temperatures of the vessels reactor while they are still hot and before they in which they are installed. They are available can solidify. These valves are also quite useful in nearly all of the current Parr materials of for the 1 gallon and larger vessels which are construction. Air actuated valves are available too large to conveniently lift from the heater for larger reactors. Users can also specify that a for product recovery. Bottom valves are rarely reactor ordered with a bottom valve shall have a installed on the micro and mini reactors with tapered bottom so that it will drain easily through their small volumes and light vessel weights. the valve opening. The standard bottom drain valve has a Not all Parr reactors will accept a bottom rising stem, that is flush with the inside cylinder drain valve. Since the valve extends approxi- bottom so that there is no dead space between mately 8 inches below the bottom of the vessel, the bottom of the vessel and the shut off point the entire vessel must be raised by this amount of the valve. In the fully open position the stem to accommodate the valve. This makes some A465VB Bottom is retracted completely to open a clear passage models too tall for convenient bench top opera- Drain Valve for draining the vessel. tion. The specification tables for each model will When the valve is reclosed, any material in identify those reactors in which a bottom drain this passage will be pushed back into the reac- can be readily installed, and those which will tor by the not accept a bottom drain, or those which will rising stem. require custom modification of the heater and Bottom Drain Valves Valves with support stand to accommodate a bottom valve. 3/8" diameter Opening Outlet Max. Max. Part No. Press., Temp, Seal clear passage Needle Valves and Ball Valves Dia., in. Connection psi °C are recom- eedle valves and ball valves can also be A485VB 0.25 1/4" NPT (F) 3000 225 PTFE mended for Ninstalled as bottom outlet valves. Needle A485VB2 0.25 1/4" NPT (F) 3000 350 Silver vessels with valves are generally used on the smaller reactors. A465VB 0.38 3/8" NPT (F) 2000 350 Grafoil volumes While ball valves can be used for large discharge A465VB2* 0.38 3/8" NPT (F) 2000 350 Grafoil from 1000 passages, they are generally limited in their A465VB3 0.38 3/8" NPT (F) 2000 350 Silver mL to 2 operating temperature/pressure capabilities and gallons. A they leave a fairly large dead space between the A177VB 0.31 3/8" NPT (F) 5000 500 Grafoil 1/4" valve is bottom of the vessel and the seat of the valve. A296VB 0.69 1" NPT (F) 1900 265 PTFE available for * Set up for a Band Heater. 600 mL and

www.parrinst.com 116 Parr Instrument Company Optional Fittings 5 Valves and Fittings

arr stocks and can install • Regulating Valves with NPT • Tube Connectors Pa wide variety of valves or tube connection. • Pipe Connectors and fittings for use with reac- • Ball Valves with NPT or • Plugs tors and pressure vessels. tube connection. • Union Coupling Adapters These include: • High Pressure Valves • Needle Valves with NPT or • Severe Service Valves Please contact our customer tube connection. • Remote Operating Valves service department for details.

Manual Control Valves for T303 Stainless Steel Valves-No Gage Compressed Gas Tanks ank valves with couplings Fits CGA Tank Outlet No. Typical Usage Tto fit standard compressed Valve No. gas cylinders are available in A120VBPN 510 Propane, butane, ethylene oxide stainless steel for corrosive A120VBPP 660 Chlorine, sulfur dioxide, nitric oxide gases and in nickel plated brass for non-corrosive gases. The brass valves have a 2-1/2" Nickel-Plated Brass Valves with Cylinder Pressure Gage diameter pressure gage which Fits CGA Tank shows the tank pressure. Both Outlet No. Typical Usage styles have a 1/4" NPT female Valve No. outlet which will accept any A120VBPQ 320 Carbon dioxide, methyl bromide pressure hose or gas tube A120VBPR 350 Hydrogen, carbon monoxide, ethylene assembly. These valves do not regulate the delivery pressure A120VBPS 540 Oxygen of the gas. Pressure regulators A120VBPT 580 Nitrogen, argon, helium are available on special order. A120VBPU 590 Air Note: Can be furnished with DIN/BSP connections on special order

Safety Check Valves henever gases or liquids back pressure will force liquid Ware introduced into a ves- back into the gas tank or into sel under pressure, the supply the gas supply system. pressure must be greater than Parr stocks the poppet the pressure in the vessel to check valves listed above for prevent reverse flow back into incorporation into the user’s 363VB Check Valve the supply system. Protection supply lines. These valves against reverse flow can be have a 10 psi normal cracking obtained by installing a check pressure and are rated for valve in the supply line. With 3000 psi maximum working a check valve in the line, the pressures. Check valves with valve will snap shut if the other specifications can be supply pressure is too low, or furnished on special order. 364VB Check Valve if the pressure in the vessel should rise above the supply pressure. This protection Poppet Check Valves is particularly important on stirred reactors where gas Part No. Material Connections enters through a dip tube. 363VBAD Stainless 1/4" NPT (F) With liquids in the vessel, any 364VBAD Stainless 1/4" Tube

1-800-872-7720 Parr Instrument Company 117 Thermocouples

arr offers a variety of ther- inserted into a protective well. The A470E2 extension wire is Pmocouples for use in our Thermowells are used on used to connect the thermocouple reactors and pressure vessels. larger vessels to protect the to the control or readout device. The “standard” thermocouple thermocouple from physical The standard length is six feet, but is a Type J (iron-constantan) damage and on all vessels of a longer lengths are available. which is well suited to the corrosion resistant alloy other operating temperature range than stainless steel. Type J Thermocouples with 1/8" Diameter of these vessels. Other Dual element thermo- materials as well as platinum couples with two separate Part Number Stem Length, in. Sheath Material resistance (RTD) elements are thermo­couples in a single A472E 7.5 T316 Stainless Steel available as special orders. sheath and spring loaded A472E2 9.5 T316 Stainless Steel These thermocouples are thermocouples designed to be sealed in 1/8" diameter stain- installed through the heater to A472E3 11.5 T316 Stainless Steel less steel sheaths and have a the outside wall of the vessel A472E6 15.5 T316 Stainless Steel standard plug connection at are also available. A475E5 21.5 T316 Stainless Steel the end of the probe. Thermocouples should be These thermocouple assem- approximately four inches A472E4 5.5 T316 Stainless Steel blies can either be sealed longer than the depth of the A472E8 2.5 T316 Stainless Steel directly into the head of the vessel so that a smooth bend vessel using a male connector can be made at the top to clear Most of the above listed thermocouples are also available as with an 1/8" NPT thread or other head fittings. Type K (Chromel-Alumel).

Pressure Hose hot surfaces on the vessel or heater. One of these hoses is hree different pressure hose included with each complete Tassembles are available for Parr Series 4500, 5100, and high pressure gas connections 5500 Stirred Pressure Reaction A506HC A490HC to both stirred and non-stirred Apparatus. Hose Assembly vessels. The standard hose The A490HC Hose Assembly Pressure Hose is a 6 foot length with a male is a braided, stainless steel is “bendable”, but it is not as “A” socket connector on one hose with a PTFE lining, rated flexible as the other hoses. It side and a 1/8" NPT (M) nipple for 2500 psi. It is reasonably is recommended for corrosive with a 1/4" NPT (M) bushing on flexible and recommended for gases, high temperature trans- the other end. The “A” socket use with corrosive gases and fers and other high pressure side of the hose attaches to liquids, and for applications­ applications. Special versions couplings installed on the inlet requiring additional abra- of this assembly can be made A495HC valve of all stirred reactors as sion resistance, but it is not of other corrosion resistant Pressure Hose well as to a side port of the intended for high temperature­ materials. Larger tubing can be gage block assembly for the liquids or gases. used, but it is rigid rather than non-stirred vessels. The choice The A506HC Assembly is a flexible. of either 1/8" NPT or 1/4" NPT 6-foot length of 1/8" OD stain- Special hoses with different on the opposite end of the less steel tubing, rated for 7500 lengths or end fittings can be hose allows for attachment to psi. This small diameter tubing assembled for special orders. most gas tank valves, pressure regulators or other gas supply sources. Pressure Hose The A495HC Hose Assembly A495HC Pressure hose assembly, 6-ft, reinforced Nylon is made of nylon. It is rated for 2500 psi and is very flex- A495HC5 Pressure hose assembly, 6-ft, reinforced Nylon, with non-return valve ible and easy to use with dry, A495HC7 Pressure hose assembly, 10-ft, reinforced Nylon non-corrosive gases (nitrogen, A490HC Pressure hose assembly, 6-ft, PTFE-lined, braided stainless steel hydrogen and oxygen). Care must be taken to ensure that A490HC5 Pressure hose assembly, 6-ft, PTFE-lined, braided stainless steel, with non-return valve the nylon hose does not come A506HC Gas tube assembly, 6-ft, 1/8" OD, T316SS in direct contact with any Alternate lengths available upon request.

www.parrinst.com 118 Parr Instrument Company Optional Fittings 5 Explosion Proof Apparatus

ll Parr reactors are nor- A mally equipped with open Class I locations are further type, variable speed motors, subdivided into four Groups, electric heaters and controllers A, B, C and D which identify intended for use in non-hazar­ specific explosive gases and dous environments. These vapors. Explosive dusts and standard units can be used fibers in Class II are subdivided in most laboratories without into Groups E, F and G. Most undue hazard, but there will be hazardous applications for Parr situations where the installed apparatus will occur in atmo- equipment must be considered spheres identified by Class I, explosion proof. Parr offers Group A for acetylene, Group various optional stirrer drives B for hydrogen and Groups C and heating systems to meet and D for most other combus- these strict requirements. tible gases and vapors. Class II, Group F covers coal dust. USA and International Most other combustible dusts, Codes such as flour and grain, are in Designing electrical Group G. Minimum ignition equipment to be operated temperatures and energy lev- in a hazardous location is a els are established for specific complex subject, governed by materials in each group. extensive national electrical The European Community codes and supplemented by uses a significantly different local regulations which require convention identified as ATEX that all electrical equipment or Atmospheres Explosives. In installed in a governed loca- this, the user must identify the tion must be approved for use level of protection required for with the specific gas, vapor their installation. Parr will work or dust that will be present in with our customers operating that location. USA electrical under ATEX to provide equip- codes classify hazardous loca- ment meeting current ATEX tions according to the nature requirements. and concentration of specific hazardous or flammable mate- Explosion Proof Motors Model 4524 Reactor, 2000 mL, Fixed Head Style with rials. These are divided into Because of sparking from Aluminum Block Heater three classes: brush contacts, electric motors Class I - Flammable liquids, clearly represent the principal gases or vapors. explosion hazard introduced Class II - Combustible by a stirred reactor. Electric ignition sources. This requires or electrically conductive motors approved for Class I- a special, air purged motor dusts. Division 2, Groups C and D, which can be provided when Class III - Easily ignitable and Class II, Groups F and required. fibers or flying particles. G atmospheres are readily An alternate method of available in most sizes and dealing with the explosion There are two divisions voltages. These sealed motors hazard is to use an air driven within each of these classes. are suitable for most hazard- motor. These are powered Division 1 - Where the ous applications, and they are by compressed air and offer flammable material exists in sometimes used with hydro- a convenient and satisfactory the atmosphere under nor- gen, but they are not approved drive system for use in flam- mal operating conditions. for Class B atmospheres. To mable atmospheres, including Division 2 - Where the haz- meet Class B requirements, hydrogen. They are available ardous material is confined a motor must be purged by in sizes suitable for all Parr within a closed system from building up a positive pres- reactors. which it may be released sure of air within the motor only under abnormal condi- to prevent explosive gases or tions, such as a leak vapors from reaching electrical in the system.

1-800-872-7720 Parr Instrument Company 119 Explosion Proof Apparatus, Continued

or housings. The user must provide all local wiring and connections to a power sup- ply, and must ensure that the installation meets all require- ments of the local electrical code. Certain sensors, such as thermocouples, pressure trans- ducers and tachometer pickups carry such low electric loads that they are a potential igni- tion source only in the event of a most unusual failure. In many installations these low hazard components are not seen as a problem. They can, however, be protected with isolation barriers which will make them intrinsically safe even in an unusual failure. These energy limiting elec­ tronic barriers can be provided where required.

Explosion Proof Controllers The most commonly used method for dealing with the ignition hazard introduced by Air Motor a temperature or process controller is simply to locate the controller outside of Explosion Proof Heaters Electric heaters purged with the hazardous atmosphere. The easiest way to provide clean air can also be consid- Another choice is to install the an explosion proof heater is to ered explosion proof, but it controller in a cabinet which use a steam or hot oil jacket is doubtful that seals can be can be purged with clean air and ensure that the highest maintained in a purged heater within the hazardous location. temperature that can be to provide true protection over reached in the jacketed cylin- a long period of time. Special Systems der is well below the minimum Please see page 102 for Parr can furnish systems ignition temperature for the additional information on approved for use in hazardous specific hazardous atmosphere heater selection. locations up through Class I, in which it will be installed. An Division 1, Group B in which aluminum block heater can be Explosion Proof Wiring specific hazardous gases will considered explosion proof In an explosion proof be present. Each of these if it has explosion proof wiring, system, all electric wiring with formally approved systems and if it is operated with an significant voltage or current must be designed and built auxiliary controller that will carrying capability must be on a custom basis, with all hold the surface temperature routed in approved sealed current carrying wiring and below a safe maximum. conduit or in specially sealed fittings installed in accordance flexible cables. All termina- with the requirements tions and switches must be discussed above. contained in approved boxes

www.parrinst.com 120 Parr Instrument Company Optional Fittings 5 Windows

indows can be installed Win Parr stirred reactors and pressure vessels for visual observations, light transmis- sion and other purposes. They usually are installed in pairs so that light can be introduced through one window while the other is used for viewing. Our standard material for these windows is quartz. Sapphire is also available for small diameter windows. Alternative window materials are avail- able for specific transmission requirements. They can be mounted in several different ways.

Screw-in Circular Windows The simplest window is a screw-in type with a 1/2" 100 mL Vessel Based On 2430HC3 diameter viewing area. The Cylinder, with Two Quartz Windows element in these windows is sealed in a fitting which screws into the vessel using a standard 1/2" NPT male pipe Integral Windows thread. Obviously, the vessel Parr has developed designs wall must be thick enough to for installing windows in the Pressure vessel with multiple 1-inch diameter provide full engagement for wall of the vessel so that the windows installed. this thread. PTFE and inside face of the window is O-ring seals restrict the maxi- very close to the inside wall of mum operating temperature to the vessel. This eliminates the 225 or 275 °C, depending upon large dead space associated and for observing the liquid the O-ring material. Pressure with screw-in windows. These level in the vessel. Multiple ratings range from 2000 to windows are offered in the two windows can be stacked on 5000 psi, depending upon the styles described below. The larger vessels. window material and its thick- maximum size of the window Windows in both the round ness. Although these windows will depend on the size of the and oblong styles can be are rather small for straight cylinder in which it will be furnished in larger sizes upon optical viewing, they work well installed. request. The windows we have for small video systems and Circular Windows with a noted above as standard are for laser and other analytical 0.5" or 1.0" diameter viewing maintained in our inventory for beams. A limitation of this area are the standard. Circular readily available replacements. design is that there is a dead windows are available in a All reactors and pressure space approximately 1-1/4" variety of materials including vessels equipped with win- long between the inner face of sapphire for very high pres- dows require custom designed the window and the inside wall sures. This type of window heaters and supports. Flexible of the vessel. is generally used for visual, heating mantles and attached photographic or optical sensor circulating jackets are the most observations. commonly used heaters for Oblong Windows with a window vessels. viewing area 3.50" long and Windows are sealed into .62" wide are the standard size these vessels with O-rings. For and can be installed on vessels this reason, vessels equipped of 100 mL and larger. These with windows are restricted to windows are commonly used operating temperatures of 225 for visual observations in both or 275 °C depending upon the the vapor and liquid phases O-ring material selected.

1-800-872-7720 Parr Instrument Company 121 Insulated Electrical Glands Temperature Limits

variety of insulated electri- external lead wires can easily here are a number of fac- A cal leads can be installed be attached. Ttors that determine the in any Parr reactor or pressure maximum temperature rating vessel for electrical measure- Power Leads of a pressure vessel. For most ments or to supply power to Power leads can be provided applications it is the an internal heater or other with either single or multiple material. Vessels with O-ring devices. Three different gland flexible wires in sizes from 14 seals are limited to 225 °C designs are available. These to 18 gage. Current ratings unless exotic materials are screw into a vessel and will range from 5 to 20 amperes at used to extend this tempera- have pressure and tempera- up to 600 volts. Either PTFE or ture to 275 °C. Parr’s design ture ratings to match those of ceramic insulation is available. for contained PTFE gaskets the vessel in which they will Ceramic glands can be used extends the operating be used. to the full temperature rating temp­erature range to 350 of any Parr vessel. Pressure °C. Flexible Graphite (FG) Transducer Glands ratings will vary from 1000 to material essentially removes Transducer glands are used 10000 psi, depending upon the the gasket as the limiting for applications requiring a design of the gland, its size and factor. Maximum temperature number of small insulated the type of insulation used. limits for the metals used in wires in a single gland. Wire these vessels are established sizes from 14 to 24 gage are Miscellaneous Sensors by ASME code and other used to carry small currents Parr has installed a number standards. Most metals have and voltages in the millivolt of different sensors in its maximum temperature­ limits range. A unique feature of this various reactors and pres- between 400 and 800 °C. The design is that multiple wires sure vessels, including both allowable strength for these (up to 16) can be individually single point and continuous metals falls off rapidly as they insulated through a single liquid level sensors, pH elec- reach maximum operating gland. trodes and dissolved oxygen temperature. Finally, the electrodes. Each of these difficulties encountered with Electrode Glands installations must be carefully screw threads and other clo- Applications requiring a developed in consultation sure components operating at single electrical conductor with the user, the electrode high temperatures establish a with current carrying capaci- or probe supplier and the practical temperature limit for ties from 20 to 100 amperes Parr Engineering Department. externally heated vessels. We and voltage ratings to 2000 Glass electrodes with O-ring have found 600 °C to be volts can be handled with an seals will carry rather severe a reasonable limit. electrode gland. These glands temperature and pressure have a single conductor (or restrictions. There are also Internally Heated Vessels electrode) in sizes from 0.093 space restrictions which gener- Exposed Heaters. Another to 0.312-inches in diameter, ally dictate that accessories of approach has proven useful in with the ends of the conductor this type can only be installed extending the maximum tem- threaded so that internal and in 1000 mL or larger vessels. perature limit. In this design the heater or furnace is placed inside the pressure vessel. The heater is surrounded by a layer Spare Parts Kits of insulation. This creates a ach stirred reactor is fur- of heavy usage. These kits hot zone in the center of the Enished with a set of spare include replacement gaskets, vessel and prevents the walls parts and fittings including a O-rings, rupture discs, drive from exceeding their allow- 6-foot gas supply hose, head belts, and seals. These kits are able limit. Properly designed, gaskets, rupture discs, and a a convenient package of the temperatures as high as 1200 set of replacement parts for small perishable items required °C can be achieved in the core the stirrer drive. for normal maintenance of the of the vessel while the walls A reserve supply kit of reactor. remain below 250 °C. This spare parts can be ordered When ordering any kit for an system is very energy efficient. from Parr Technical Service existing reactor please specify Internal heaters can be less to provide sufficient parts and the preferred gasket/seal mate- tools to handle most normal rial, the range of the rupture replacements and emergency disc, material of the reactor, repairs during the first year and the length of the drive .

www.parrinst.com 122 Parr Instrument Company Optional Fittings 5 External Valves and Fittings

powerful than external heat- Materials of Construction As an alternative, Parr has ers. Internally heated vessels n the standard configuration, designed an oil filled are equipped with insulated Ithe valves, gage, magnetic isolator gage protector to iso- electrical feed-throughs to drive and other external parts late the gage (and transducer, power the heater and multiple on Parr reactors are furnished if required) on small reactors thermocouples to monitor in stainless steel, even when a and pressure vessels where and control the temperatures different material is specified space is limited. These isola- in the hot zone and the vessel for the cylinder, head and tors can be furnished in any of inner wall. internal wetted parts. The the current Parr materials of The reactions or studies external stainless components construction. carried out in internally heated are typically only exposed to vessels must be limited to the vapor of the reactants and Pressure Transducers those which will not destroy are at much lower temperature Pressure transducers are the exposed internal heaters than the cylinder and internal only available in stainless and insulation. These are fittings. These conditions allow steel and Alloy C-276. Parr normally gas-solid reactions stainless steel external fittings provides a mounting adapter or controlled atmosphere to perform satisfactorily in with a water cooling jacket heat treatment studies. The most cases. If external parts on pressure transducers to heating elements are normally made of a material other than protect them from excessive ceramic. Some users have stainless steel are required for temperatures. These can be developed induction style safety or other reasons, Parr augmented with piston style heaters and insulators and can accommodate this in most isolators similar to gage have extended their investiga- cases. Any request for external protectors when corrosion tions to above 2500 °C. parts made of a specific mate- resistance is required. When Although internal heaters rial must be stated clearly a gage and a pressure trans- can be installed in almost when ordering. ducer are installed, a single any non-stirred Parr pressure isolator can protect both. vessel the 1.8 liter, Model Valves 4683 High Pressure/High Most reactor valves are Magnetic Drives Temperature vessel is an available in Alloy 400 as well Magnetic drives can be excellent starting point. It can as stainless steel at a reason- furnished in all of the current accommodate a cylindrical, able cost premium. Valves Parr materials of construc- insulated heater 1.75" diameter made of Alloy C-276 are also tion except nickel, which is by 8" deep, capable of produc- available, but generally only magnetic. ing and sustaining internal on special designs and at a temperatures to 1200 °C. considerable cost premium. Rupture Discs Protected Heaters. Soft materials such as titanium The standard material of Internally heated vessels and zirconium generally make construction for rupture discs have also been manufactured poor performing valves. is Alloy 600. A gold facing is with cartridge type heating available for the smaller discs elements inserted in specially Gages used on vessels up through 2 designed “thermowells”. Pressure gages are avail- liters in volume. Alloy C-276, These wells protect the heater able in Alloy 400 and stainless Tantalum and other premium from the reactants and expand steel. Other materials of materials are available on the applications that can be construction are not avail- special order. studied. Cartridge type heaters able. The standard method have a maximum temperature for protecting the gage in a of 760 °C. corrosive environment is to install a diaphragm gage pro- tector. These have a flexible diaphragm which isolates the gage from the reactants and a sealed hydraulic connection for pressure transfer to the gage. These assembles are too large to install on all but the largest Parr reactors.

1-800-872-7720 Parr Instrument Company 123 Notes

www.parrinst.com 124 Parr Instrument Company