3900 Series Hydrogenation Apparatus
Contents
1. ANVdWOO LNSWOSISNI SHOWId Z 00 4 HOVO HONI Ydd SET 0 in IL VOCI Ed 2111 4106 818 SHOWTd p AT E 540414 2 8889 Suovia Z 32174 572 99917 J Va LA et 2 A93CA Valve Assembly as show except without gage 21 www parrinst com 3900 Series 7 5 9 lt E c gt I 31 25 OL ION GALS ANNOYD 6 133HS 016 33S 80104 NIV V260Z 304 Z 0 0089 134 N3339 N3349 TVYLNIN 3018 31 1 3NI 1 NMfON8 X2V 18 3070502 TVNOIIVNH3INI 303 S310N anis oNnos9 M xog HOLIMS 30100 NOYA 3 IM ONnOW NO 341 0 089 C3LLY INN 5439 141 080099 3116 8 133HS 0168 335 HOLINS 30084 0150 4 3 803 TIVLYG 5NISIA noxa ZHOS A022 4OLON 09 1 401 VOLIZ v99 S3ovid Niloug dAl 3687 N3389 yovld 9 364 Kar 539 ui 3018 034 8 32. 66 REACTION BOTTLE 500ML N ed B 98CA 66CATC REACTION BOTTLE 500ML PED 29 8CA3 18CA2 FLYWHEEL W SHAFT COLLAR W SET SCREWS 66CA2 REACTION BOTTLE 250ML 66CA2TC REACTION BOTTLE 2500ML PED 30 A58CA CONNECTING ROD ASSY W BUSHINGS 62CA STOPPER 46 NEOPRENE 1 HOLE 31 SR3118 5 16 DIA X 1 1 8 ROLLPIN 42055 32 19CA3 PIN W NUT 61CA4 166CA WASHER 1 ALUMINUM RETAINING RING TRIANGLE PUSH 33 SN2520HX 1 4 20 HEX JAM NUT 34 50CA OIL HOLE COVER 101 2 SPACER FOR 250ML BOTTLE 35 A16CA HYDROGEN TANK 4L T304SS HL0025TB040 POLYPROPYLENE TUBE A16CATC HYDROGEN TANK 4L T304SS PED 5CA3 PIVOT PIN A16CATD HYDROGEN TANK 4L T304 CHINESE SC2520SC04 1 4 20 X 1 4 SHSS 18 8 SS 49CA TANK SUPPORT 65CA BOTTLE GUARD T304 XC0210 TRIM PROTECTIVE BLACK 53CA2 BOTTLE CLAMP BASE 11 TANK CLAMP TD3118SC12 5 16 X 3 4 SH SHLD BOLT STEEL SB3118HX24 9 16 18 X 1 1 2 HHCS 18 8 SS 56CA TIE ROD LONG 34CA3 MOTOR PULLEY W SET SCREW SN3124HX 5 16 24 HEX JAM NUT 18 8 SS 1765EEF 1765 MOTOR 230 50 1 4 1425 RPM MOTOR 115 60 1 6 HP 1725 RPM 42 37CA3 SA3118FT14 VEE BELT NOTCHED 25 5 16 18 X 7 8FHMS 18 8 SS 43 A150CA BELT GUARD 44 SA
3. 787E SEAL W 797E 798E 3X 791E2 MIPPLE 86E3 CONDUIT OUTLET 8 amp 11VB REDUCING BUSHING 207CA3 3 4NPTM 1 2NPTE SUPPORT BRACKET E C3 6 10VB ELBOW 3 AMPTF F 1765EEG 115V 60HZ POWER CORD MOTOR ikje YELLOW BLACK e BLACK WHITE e PURPLE GREEN GREEN YEL FTN I90F PROTECTIVE TT _ BLUE GROUND SYMBOL mec E Po 2X 424E2 RED 24 Parr Instrument Company 3900 Series Hydrogenation Apparatus EXPLOSION PROOF SWITCH ASSEMBLY FOR 1 765 220V Series 3910 384E e TUMBLER SWITC EXPLISIDN PROOF 9 1 782HC STRAIN RELI 1203 CORDSET 97E SEAL FITTING W W797E 798 207CA2 SUPP BRAC fa CD 6 D MOTOR 1675E EL BOW L765EKEK 220V 50HZ POWER CORD MOTOR SWITCH B RED BLAC BLAC BLUE _ WHITE p WHITE 5 BLAC 4 YELLOW GREE E a feen BROWN ioo I J BROWN PROTECTIV 2 GROUND SYMB www parrinst com 25 3900 Series Hydrogenation Apparatus 1384E TUMBLER
4. Earth Ground Functional earth connection This connection shall be bonded to Protective earth at the source of supply in accordance with national and local electrical code requirements A This CAUTION symbol indicates that the surface may be hot www parrinst com 3 3900 Series Hydrogenation Apparatus ENVIRONMENTAL CONDITIONS This apparatus is to be used indoors Operating 10 C to 40 C maximum relative humidity of 80 non condensing Installation Category II over voltage in accordance with IEC 664 Pollution degree 2 in accordance with IEC 664 Altitude Limit 2 000 meters 25 C to 65 C 10 to 85 relative humidity Storage Electromagnetic Compatibility In accordance with 2004 108 EC PROVISIONS FOR LIFTING AND CARRYING Before moving the instrument disconnect all connections from the apparatus Lift the instrument by grabbing underneath each corner INTENDED USAGE If the instrument is used in a manner not specified by Parr Instrument Company the protection provided by the equipment may be impaired THE USER S RESPONSIBILITY The user must realize that it 1s their responsibility to keep their equipment in good condition and to use it only within the prescribed temperature and pressure limits They must be constantly aware of the serious consequences that can result from such things as opening the wrong valve mixing combustible vapors with air or oxidizing gases adding reactants too f
5. Rm NO 271 t Company 3900 Series Hydrogenation Apparatus Operating Instruction Manual 3920 Hydrogenation Apparatus 3900 Series Hydrogenation Apparatus TABLE OF CONTENTS PREFACE 3 Scope 3 Safety Information 3 General Specifications 3 Explanation of Symbols 3 Environmental Conditions 4 Provisions for Lifting and Carrying 4 Intended Usage 4 The User s Responsibility 4 SSEMBLY INSTRUCTIONS 4 OPERATING PROCEDURE 5 STANDARDIZATION 5 Pressure Limits 6 SAFETY BARRICADES 6 GENERAL PRECAUTIONS 6 CATALYSTS 7 HEATER 7 WATER JACKET 7 TEMPERATURE MEASUREMENT AND CONTROL 8 SEMI MICRO OPERATIONS 9 ALTERNATE Parts 9 MAINTENANCE INSTRUCTIONS 9 Fuse Ratings 10 SPECIAL INSTRUCTIONS FOR THE 3921 HyDROGENATOR 11 Motor and Gear Box 11 Bottle Connectors 11 Glass Reaction Bottles 11 Stainless Steel Bottle 12 Bottle Heater 13 Temperature Measurement 13 REFERENCES 13 2 Parr Instrument Company Parts Lists 14 3910 Hydrogenation Apparatus 14 3920 Hydrogenation Apparatus 16 Bottle Clamp Assembly Series 3910 18 Shaker Column Assembly Series 3910 18 Flywheel Assembly Series 3910 19 Connecting Rod Assembly Series 3920 19 AA92CA Single Valve Assembly 20 3A93CA Double Valve Assembly 21 3910 Wiri
6. ONNOHO 134 N3389 N3389 TIVLAG ATENISSV TT EN M m Wa LAN 3018731 I HM anis UNNOYD 3N1 1 NMON8 2V 18 872 39VQNOO9 TVNOIIVNH3INI 303 1 3604 83661 S31ON anis awnoso M xo8 HOLIMS 5 3318392 ISNI 31291 1 0400 NOLON 23219 LHM S Sn S E 3010 3SnJ 20 91 z NOY4 391 ONNOYD YO 38 IM QNnOND 23249 LAN Sd33 HOLIMS H3M0d 41 9 0500 2384 3606 38M ONNOBO 3116 ATH T3NvdlNONJ 26 2 of 108MAS GNNOYD 306 972 T3NVd vO28lZ 3504 83661 M3iBNVO 3504 31291 33Q10H 3504 30291 9 133HS 0266 335 GL MOTT3A TIVLAG DNIYIM HOLIMS 30084 NOISO1dX3 X04 TIVLAG 1 N0113A 2 S30v1Id 7 09 0 amp 1 886 me spe dal 3692 ZH09 A022 HOLOW WHH008V me vane GREER 401 v291Z PR ipe 4917 3 0v1d3038 831114 130500 062 39Nv3O Cavey 3116 3116 T s3ovid du 3LIHM dAl 3682 LL MOT13A 3L HA 81 NO113A wove N N 1HM m 1 0113 LHM 18 7 wa 0 WA p ss s Ta 9 YOLON 04400 YOLON ND 9 2 MOV MOTT3A x O r O r N3389 3504 02366 3504 02366 M3lHNVO 3504 31791 ISNA 31 01 14 Vag 8 1 10 3503 304v US 2 H307T0H 3604 3079 INT A19 0809 YOLON 23 18 HOLIMS 33M0d EO LIN uIMOd Xm gh 0400 38 1 1H lt JO8NAS 4061 NM DENA SONQOHS SOS 1 41
7. If the reaction proceeds too rapidly it can usually be checked by stopping the shaker If overheating becomes a dangerous problem the bottle can be cooled by using the A103CA water jacket described below There should be no gas burners or open flames near a hydrogenation apparatus The room must be well ventilated and any gas released from the apparatus should be discharged into an explosion proof hood or ventilating duct Care must be taken to prevent ignition by a static charge from an insulated object For this reason a good ground connection through the power cord or directly to the base of the apparatus must be maintained at all times Loss of gas 1s an annoying factor which can be avoided by careful maintenance and frequent testing It should not be necessary to use extreme force to close any of the valves on this apparatus If a tight seal cannot be secured without a hard turn on the valve handle dismantle the valve and replace the 20VB valve seat and any other worn or damaged parts If the valve leaks through the packing back the needle away from its seat and tighten the 8VB2 packing nut If this does not stop the leak replace the 4VB3 packing rings 3900 Hydrogenation CATALYSTS The most active catalysts for hydrogenation reactions 1n this apparatus are made of platinum and palladium A hydrated platinum oxide often called Adams catalyst is used In many procedures This 1s prepar
8. 084 2612 13NvdlNONJ V26lZ tj T3NVd YVIN VOBIZ TANVd AYJ 2 9812 18 1d O v 079 3504 00366 3514 OZIGE L L I X31XYY 3504 31481 l HIIHYVD 3504 31491 33010H ISNI 30 7 33010H 3504 30 8 9 133HS 0266 335 HOLIMS 40084 NOISOTdX3 404 TIVLIG _ 2 TIVLAG SNIHIA JONVYO 3682 ZHO9 ASTT YOLON DAABBEV ZH09 ASII IOLON THH88EV 61 961 382 801 951 Bake A ee 361 LV O 3614Y 1 1 N N 1 LHM Jm 0 MW ZEN NUD 9 NUD 9 ER 0 01 18 O S 35014 12366 en all AR 18 N3389 MOv18 14 18 19 9 Va sion LN NNOD 11NONOD 3TH 63 6 nnrn LHM 3504 42366 Mo 331 3 35014 31291 Y3G10H 3504 30 HOLIMS H3M0d 3606 18 14 lOBWAS ONNOHD TINVd 242812 1 13 1 GVIGIT 0403 YOLON TILLY 149 0X09 X18 LHM TJOSNAS ONNOYD 406 LHM TANVd VOBIT UIIYYVI 3504 31291 33Q 0H 3504 30291 HOLIMS H3M0d 3606 dive J3NVdlNO NJ EVIGIT 3900 Series Hydrogenation Apparatus 1384 TUMBLER SWITCH EXPLOSION PROOF r A491E2 STRAIN RELIEF 3462 CORDSET
9. For partial or quantitative hydrogenation continue shaking until the pressure drops to a calculated value as deter mined by prior standardization runs 6 Atthe end of the run stop the shaker close the bottle valve and allow the catalyst to settle Any re sidual pressure in the bottle and connecting tube can be discharged by opening the gas release valve 7 Open the bottle clamp and remove the bottle De cant the solution leaving the catalyst the bottle for a second reduction or remove the catalyst on a filter STANDARDIZATION The apparatus can be standardized by making a preliminary run with a known amount of any compound that can be completely and quantitatively reduced The pressure drop per mole of hydrogen consumed in such tests 1s then used as a basis for estimating the progress of a reaction with unfamiliar materials procedure is described in reference 3 for standardizing the apparatus by reducing 11 6 grams 0 I mole of pure maleic acid dissolved in 150 mL of 95 ethanol using 0 1 gram of catalyst The reaction Is carried out as previously described with shaking continued until no more hydrogen is consumed This usually takes twenty to thirty minutes after which the pressure drop in the tank is recorded Since exactly 0 1 mole of hydrogen has been consumed in this run this decrease in tank pressure can be used as a basis for measuring or regulating the amount of hydrogen consumed when treating other compo
10. Parr Instrument Company 16 3900 Series Hydrogenation Apparatus ITEM PART DESCRIPTION ITEM PART DESCRIPTION NO NUMBER 73CA6 NO BASE PLATE NUMBER 427E4 BUSHING INNER 49CA TANK SUPPORT SW31FT 1055HC SPHERICAL BEARING PTFE LINED 5 16 BOLT WASHER 18 8 SS TW31SL 427E3 BUSHING OUTER 5 16 LOCK WASHER STEEL PLATED SN5020HC 1 2 20 HEX CAP NUT 18 8 SS 583118 14 5 16 18 X 7 8 HHCS 18 8 SS 14 2 BOTTLE HOLDER BASE SN3118HX JAM NUT 5 16 18 THD 172CA BOTTLE PAD NEOPRENE XC0210 TRIM PROTECTIVE BLACK 75 BOTTLE HOLDER TOP 11CA TANK CLAMP 79 2 CLAMP SCREW A16CA HYDROGEN TANK 4L T304SS SB2520BT08 1 4 20 X 1 2 BHSCS 18 8 SS SA2520RD28 1 4 20 X 1 3 4 RHMS 18 8 SS A77CA2 FRONT GUARD ASSEMBLY SN2520HX 1 4 20 HEX JAM NUT 18 8 SS A83CA THUMB SCREW 1 4 20 X 1 2L SW25FT 1 4 BOLT WASHER FLAT 18 8 SS 109CA2 SPACER SN2520WG 1 4 20 WING NUT 18 8 SS 89CA2 CRANK PIN W NUT 92 SINGLE VALVE W GAGE 1065HC FLYWHEEL 180HC MOTOR SUPPORT SC3118SC06 5 16 18 X 3 8 SHSS CUP PT 18 8 3A93CA DOUBLE VALVE WIGAGE SB3716SC16 3 8 16 X 1 SHCS 18 8 SS A387E2 GEAR BOX WIBASE 10 1 RATIO SW39FT 625 X 390 X 063 WASHER 18 8 1748 DRIVE KEY MACH 185 SQ X 1 48 A87CA4 CONNECTIN
11. books by Augustine Freifelder and Rylander will be particularly helpful to those users who want additional information regarding hydrogenation techniques catalysts and procedures for treating specific functional groups The following references are therefore highly recommended R L Augustine Catalytic Hydrogenation Marcel Dekker Inc New York 1965 Morris Freifelder Practical Catalytic Hydrogenation Wiley Interscience Div of John Wiley amp Sons Inc New York 1971 Gilman Blatt Organic Synthesis Collective Volume I p 65 John Wiley amp Sons Inc New York 1948 H W Lohse Catalytic Chemistry Chemical Publishing Co Inc New York 1945 Paul N Rylander Catalytic Hydrogenation Over Platinum Metals Academic Press New York 1967 Paul N Rylander Catalytic Hydrogenation in Organic Synthesis Academic Press New York 1979 Paul N Rylander Hydrogenation Methods Academic Press New York 1985 Biennial conferences originally held at the New York Academy of Sciences and now in a variety of locations by ORCS Organic Reaction Catalysis Society In even numbered years starting 1n 1966 have produced excellent collections of papers under the general title Catalytic Hydrogenation and Analogous Pressure Reactions The initial set is published the Annals of The New York Academy of Sciences Vol 145 Art 1 pp 1 206 1967 Currently titled Catalysis of Organic Reactions published by Marcel Dekker In
12. hydrogenator by wrapping a glass fabric heating mantle 451 around the bottle No special fittings are needed for attaching this heater Simply wrap the mantle tightly around the bottle and run the connecting cord through the slot in the top housing Use the plastic clip furnished with the heater to anchor the cord to the top edge of the bottle clamp then run the cord out laterally on the axis of the shaker arranging it to avoid excessive flexing when the shaker 1s operating The 72CA4 heavy wall bottle should not be used with the heating mantle because the heat will destroy the protective polyvinyl coating on the bottle TEMPERATURE MEASUREMENT Temperatures in the reaction bottle can be measured by installing a stainless sheathed thermocouple using the same fittings described for the 3911 hydrogenator on page 9 but with a longer sheath on the thermocouple to match the larger bottles The various assemblies are identified in the Parts List on page 29 3900 Series Hydrogenation Apparatus REFERENCES No attempt 15 made here to list the hundreds of references to the Parr hydrogenator which have appeared in chemical literature since Dr Roger Adams published his first paper describing an apparatus of this kind in 1923 More than five hundred literature references are cited in Augustine s book on Catalytic Hydrogenation which 1s listed below Additional references can be obtained from other books in this list Among these the
13. unexpectedly fail Working pressures should never exceed 60 psig when using either 250 or 500 mL bottles in the 3911 apparatus and never more than 40 psi for one liter bottle and 30 psi for two liter bottle 1n the 3921 apparatus 6 Parr Instrument Company SAFETY BARRICADES Parr shaker type hydrogenators are usually operated in an open laboratory without additional barricades or protective screens but the operator must realize that additional protection may be necessary if there 1s any possibility that a reaction might run out of control or if unexpected bottle breakage would produce a hazardous spill of toxic or flammable materials Potentially explosive reactions are best handled with the apparatus located behind a suitable barricade or in a pressure test cell If a barricade 1s used 1t should be built of concrete brick or steel in whatever thickness or form 18 considered necessary to protect the operator from flying fragments if the reaction bottle should explode Glass shields either plain or reinforced with wire mesh are not recommended The requirements for barricades differ so widely that each should be designed and built in order to protect against the potential hazards inherent in each installation This subject 1s well covered 1n the references listed on page 15 GENERAL PRECAUTIONS Pressure reactions with hydrogen are not unduly hazardous if the user maintains his hydrogenator in good condition and operates it with t
14. 19V1d3933 93111 J 3116 1330020 0403 80 01 TILL 413 0400 0384 92 NE 1504 8366 YIIYYVI 3503 31481 3503 30 7 HOLIMS 8304 1606 TO8WAS N0039 3 11931084 406 T3NVd 243812 L 133HS 016 335 HOLIMS 30084 NOISOTdX3 303 TIVI3Q DNIYIM 3910 WIRING SCHEMATIC dv 52 3514 8362 XIIA ISNI ILLY X30704 350 30 7 TINVdINOM4 96 2 532 14 2 AL 3687 1 09 1811 40108 1119941 Sin 310 143238 311113 ania 3116 36 v18 4 HOTTIA wie 0 S T3A NYO 3504 173651 n YAU ISNA 30 1 310808 Md SI 33010H 35 4 20 9 2 wig 5 HOLIMS 43004 NNO 1100902 u 1606 7398 du k JONAS 080059 JA119310 d 3061 und T3NVd 243812 s TANYdINOY4 692612 q 01 34 OL 8 39VL 0A 000 4 804 03814 SI LI 3305 OL YOLON 23H 310N S30v1d 2 11 130 7 06 026 1 4330941 s 401 916 dAL 21009 310v1d3233 33111 J 331002 3116 14221 5 dNv 07 3513 02366 82182 2504 21 71 3010 3503 30 7 HOLIMS 8308 3606 2189 08402 38 TOSNAS GNNOYD 3A112310
15. 2520RD10 1 4 20 X 5 8 RHMS 18 8 SS 1765EEG MOTOR 115 60 1 6 1725 RPM 45 SW25NL 1 4 LOCK WASHER INT TOOTH 410S 1765EEK MOTOR 230 50 EP 1 6 1425 RPM 46 SW16NL 8 LOCK WASHER INT TOOTH 410SS X2353 SB3118HX10 AIR MOTOR PACKAGE 3910 5 16 18 X 5 8 HHCS 18 8 SS 47 SA1632RD08 8 32 X 1 2 RHMS 18 8 SS 48 AA92CA SINGLE VALVE ASSY WIGAGE X2291EB SWITCH BOX PKG 115V 3910 3920 49 A118CA GAS HOSE ASSY NYLON 6FT 51 3A93CA DOUBLE VALVE WIGAGE 909E SWITCH POWER 16AMP 1471E CARRIER FUSE 1 4 X 1 1 4 52 64PR FOOT RUBBER W 1 4 20 THRD 911E FILTER INTERFERENCE 10AMP 53 57 328E7 504HCAA HOLE PLUG 1 2 REDUCING BUSHING 1 8 1 4 www parrinst com 15 3900 Series 7 5 52 9 lt E c gt I 3920 HYDROGENATION APPARATUS 2 PL AMOO OOO O OO 4 PL 26 u lt a A I AB 27 DY 3 6 8 80 09 67522696 8 6
16. 3 Controller provides Instructions for tuning the Controller and using the alarm features PTE nr x ET 2 The 4833 Temperature Controller has dual displays one for the process temperature and the other for the set point The operating range of the Controller covers the span from 0 to 100 C with the high limit extending somewhat beyond the temperature limit for the 3911 and 3921 Hydrogenators These hydrogenators should not be operated at temperatures above 80 C The 4833 Controller 1s sensitive to temperature changes of less than 0 5 C but temperature variations in the reaction bottle may be larger than this due to lag in the heating system and turbulence in the bottle In most cases temperatures In a 500 mL bottle will not vary by more than one degree above or below the set point Variations 1n larger bottles may run as much as two degrees but this 15 still within permissible limits for most reactions Bottle temperatures will tend to overshoot at low temperatures in the 30 to 40 range There will be less overshoot at higher settings Overshoot can be avoided by setting the controller several degrees low during the initial period then raising the temperature in one or two steps after cycling has been established slightly below the working level Fail safe protection against a thermocouple break is provided in the controller This can be tested by disconnecting the thermocouple from the
17. 9CA2 SPACER B9CA2 CRANKPIN CONNECTS TO BRACKET ON REARGUARD A76CA2 ASSEMBLY 1065HC www parrinst com 3900 Series Hydrogenation Apparatus 8 2 COLLAR ACA 5 16 18 X 3 8 SHSS A388E SERIES MOTOR SHAFT W KEY 19 ddVL NOTAAL HLIM QH IVHS Hd OL SQVHSHL ddlId TIV HNOO ONIS ONTMOVd 888 9 LAN I8A6 ACOG AAWA VOCO 90 GAOSTV HLON WIddIN GAPCT LAN W ITHEN ONDIOVd LVS qp ONTIOVd AATWA HATVA 5 N N CHAT 8 00 ANVANOD x O INENNALSNI p YYVd N AA92CA SINGLE VALVE ASSEMBLY HOW VOCI 7 5 52 lt c gt I 3900 Series Instrument Company Parr 20 0 e m 3 E lt c 2 rd gt I 1266 7 sxovia 2 3A93CA VALVE ASSEMBLY
18. CTIONS Periodic cleaning may be performed on the exterior surfaces of the instrument with a lightly dampened cloth containing mild soap solution All power should be disconnected when cleaning the instrument There are no user serviceable parts inside the product other than what 16 specifically called out and discussed this manual Advanced troubleshooting instructions beyond the scope of this manual can be obtained by calling Parr Instrument Company in order to determine which part s may be replaced or serviced The connecting rod has oil impregnated bronze bearings which do not require heavy lubrication Place a drop or two of light oil on each bearing about once a month Lubricate the flywheel shaft by placing a few drops of light oil In the oil cup at regular intervals A light application of a lithium grease such as Lubriplate on the shaker pivots 1s also advisable The spacing of these pivots should be adjusted so that the bottle clamp swings freely without excessive friction To inspect and replace the valves unscrew the 8VB2 packing nut and remove the needle and knob The internal parts can then be removed with a small wire hook These will come out in the following sequence 6VB packing cover two 4VB3 packing rings 21VB lantern ring and 20VB valve seat If the plastic valve seat will not slide out of its socket use a 1 1 2 wood screw as a removal tool Replace these parts in the same order insert the valve needle and t
19. Fiberglass Covered 40 A123CA2 72CA 2000 Borosilicate Glass 30 A123CA 72CA3 2000 Borosilicate Glass Fiberglass Covered 30 A123CA 72CA4 2500 Hand Blown Heavy Wall Borosilicate Glass A123CA A129CA3 1700 Stainless Steel Bottle Assembly A155CA Tube with 133CA2 Spacer Spool A226CA Cylinder only Stainless Steel 1700 mL A129CA3 72 71 66 Stainless 2 0 L 1 0 L 500mL 250 mL Bottle Bottle Bottle Bottle Bottle HEATING MANTLES Mantle No Watts Volts Use with Bottle No A450EEB 100 66 66 2 450 100 230 66 66 2 451 200 115 7 72CA A129CA3 or A226CA 451 200 71 72 A129CA3 or 226 29 3900 Series Hydrogenation Apparatus Motor ASSEMBLY A86HC NEEDLE VALVE A85HC A415VB REGULATOR W GAGE 491HC LUBRICATOR HEX NIPPLE MUFFLER REF 494HC 414 ELBOW ELBOW 221CA2 BASE PLATE SB2520HX12 HHCS SW25FT WASHER SN2520HX NUT TYP 4 PLACES 78HW COUPL ING 758HC2 CLAMP TYP 2 PLACES 1 8 NPT REF 60HWBB HOSE BARB TYP 2 PLACES JR0025T8125 HOSE 8FT 491 2 HEX LONG NIPPLE 209CA AIR MOIOR SWITCH Box ASSEMBLY 219 _ FRONT PANEL SEE NOTE POWER SA1140RD06 SWITCH W TN1140HL 2 PLACES 1470 FUSEHOLDER 1471E FUSE CARRIER 911E 139E__ FUSE FILTER RECEPTACLE SEE NOTE 115V SINGLE FUSE NOTE 230V DUAL F
20. G ROD ASSEMBLY LG 49 A388EEL X2291 SWITCH BOX PACKAGE MOTOR 110 220V 60 HZ 1 4 HP 49A X2290EA 909E SWITCH POWER 16 AMP MOTOR GROUP 115 60 X2290EF 49B MOTOR GROUP 230 50 1470E FUSEHOLDER INTERNATIONAL 1 4 X2290EG MOTOR GROUP 115 60EP 490 1471E CARRIER FUSE 3AG 1 4 X 1 1 4 159X40EGX MOTOR GROUP 115 60 EPX 49D 911E FILTER INTERFERENCE 10AMP X2290EK MOTOR GROUP 230 50 EP 50 328 7 HOLE PLUG 1 2 159X40EKX MOTOR GROUP 230 50 EPX 31 12 REACTION BOTTLE 2000ML 159X40EY MOTOR GROUP AIR 71CA REACTION BOTTLE 1000ML 220CA FLYWHEEL GUARD 71CATC REACTION BOTTLE 1000ML PED 583118 10 5 16 18 X 5 8 HHCS 18 8 SS 72CATC REACTION BOTTLE 2000ML PED 583118 36 5 16 18 X 2 1 4 HHCS 18 8 SS 62 STOPPER 6 NEOPRENE 1 HOLE 92 5 ROCKER COLUMN TC2520SC04 166CA RETAINING RING TRIANGLE PUSH 1 4 20 X 1 4 SHSS ALLOY STEEL TW75FT 82CA2 WASHER 9 32 3 4 BOLT WASHER STEEL PLATED HL0025TB040 POLYPROPYLENE TUBE TB7516HX16 3 4 16 X 1 HHCS STEEL GRD5 PLATED A76CA2 REAR GUARD ASSEMBLY 60 TB5020HX36 1 2 20 X 2 1 4 HHCS STEEL A118CA A102CA GAS HOSE ASSY NYLON 6FT MALE CONN 1 4T 1 8 BRASS www parrinst com 17 3900 Series Hydrogenation Apparatus BOTTLE CLAMP ASSEMBLY SERIE
21. GROUND TO MOTOR JUNCTION BOX AND 1 2 FOOT PIECE OF XA1801AB BLACK WIRE FROM CORD 21 16GA UNSHIELDED WIRE USING Vi 424E2 BUTT SPLICES CONNECT THE WHITE WIRE TO THE YELLOW WIRE AND THE BLACK WIRE TO THE 1 BLUE WIRE CONNECT TO BLACK AND WHITE WIRES TO THE SWITCH AS SHOWN ABOVE 2 INSTALL 190F BY GROUND SCREW IN 1384E BOX GROUND STUD ASSEMBLY DETAIL NOT TO SCALE SWITCH BOX W GROUND STUD www parrinst com 27 3900 Series Hydrogenation Apparatus THERMOCOUPLE ASSEMBLIES Assembly Equipped with Fits Bottle No Thermocouple No No Size A159CAPA A295E 66CA2 2 310 159 2 295 66 200 159 A295E2 71 1000 159 4 295 2 72 2000 72 4 3000 A295EPA 250 500 mt A159CASPA A295E2 129CA3 1700 295 2 1000 1780 Ara 4 A161CA NI A159CA2 T Thermocouple Assembly 250 500 mL 1000 1750 2000 mL A162CA 250 162 2 500 mL 162 1000 mL 162 4 2000 mL 162 5 11750 mL 28 Parr Instrument Company 3900 Series Hydrogenation Apparatus REACTION BOTTLES FOR PARR HYDROGENATORS Apparatus Bottle No Size Bottle Type Maximum Requires No mL Working Connector Pressure No psig 66CA2 250 Borosilicate Glass 60 A122CA2 66 500 Borosilicate Glass 60 A122CA 66CA3 500 Borosilicate Glass Fiberglass Covered 60 A122CA 71 1000 Borosilicate Glass 40 A123CA2 71CA2 1000 Borosilicate Glass
22. IAL INSTRUCTIONS FOR THE 3921 HYDROGENATOR 3 EE All instructions given in the preceding sections of this Manual apply equally to both the 3911 and 3921 Hydrogenators Both models use the same hydrogen tank and valves but the 3921 apparatus has a larger and heavier bottle clamp and shaker mechanism to accommodate larger reaction bottles AND GEAR Box Before starting the motor replace the uppermost pipe plug on the gearbox with the blue plastic vent plug which is furnished The hole in the vent plug must point up See Boston gear instruction sheets for lubricating instructions BOTTLE CONNECTORS Attach the valves to the gas tank and connect the polypropylene tube to the reaction bottle by sliding the tube through the 82CA2 washer and 166CA retaining ring then push the tube through the bottle stopper leaving a projection of about one inch below the stopper To complete the assembly set the bottle on top of the rubber pad in the holder slide the tube through the slot in the clamping screw and tighten the screw firmly Always attach the steel guard screen to the front of the bottle holder before pressurizing the bottle An 80CA2 spacer must be placed between the clamping screw and the stopper to compensate for the difference in bottle heights when using a 1000 mL bottle Customer installed location of Blue Plastic Vent Plug Assemble the inlet tube with the 80CA2 spacer and 166CA retaining ring above the stopper an
23. Nd 3061 TINYd YVIY 2812 O 3SN4 0Z36 Malwa 35041149 31010 3504 30 7 be M TJNVdlNOHJ 9 2612 A TIVISC DNISIM 7HO9 AGSII IOLON VAYGGLT n VOLIT 1482 401 2917 312 143938 331114 3116 O 16114 0 9 3504 97266 HIIHYVD ISNI 1 7 430704 3504 30 9 0402 YOLON C3LLY HOLIMS u3ll0d 4149 0803 0382 3606 J08MAS GNNOYD 3 11931084 106 LHM TINYd YVIY VIBIZ T3NVd1NOH4 242612 Instrument Company Parr 22 V 0 m 7 5 E lt c 5 o O gt I 3920 WIRING ScHEMATIC 23 4 133HS 0266 335 4 4 HOLIMS JOOMd NOISOTdX3 404 TIVLSd 5NIMIA V PNE 8 ZHOG A022 40LON MH3H888V me a S39V d v 901 v991 310V1d3233 33111 4 A z 1 3682 3116 MSN 1350502 A0 Z leg gt N3389 384 i K IHM 0 t Y Xv18 38 1 WA 24096 335 HOLOW 9398 V N04 Z 31905 OL LON av 9
24. S 3910 251 04 POLY TUB SA 332RD04 16 32 RHMS SWI3FT 59 6 WASHER KNURLED N 2 PLAC u 54 E CLAMP UJ 4 4 gt e 5 BOTTLE GUARD BCA EACTION BOTTLE 70 OD A58CA CONNECTING ROD 53CA2 BOTTLE CLAMP BASE SN3124HX 5 16 HEX NUI SHAKER CoLUMN ASSEMBLY SERIES 3910 SC2520SC04 5CA3 1 4 20 SHSS PIN TYP 4 PLACES TYP 2 PLACES So 9590000 095 0000 o 98009900 8895 2200 809800 00 969 297 00080799 SN2520HX 89897 1 4 20 JAM NUT 559 BCA3 LYWHEEI SHAFT SC2520SC04 3910 1 4 20 SHSS SHEET 18 Parr Instrument Company FLYWHEEL ASSEMBLY SERIES 3910 SC2520SC04 SSS TYP 2 PLACES JOCA OIC HOLE COVER SA3118F114 5 16 18 FHMS s pb INSERT FRONT MACHINE SCREW BEFORE INSTALLING FLYWHEEL SC3118SC06 SB3716SC16 3 8 16 X 1 SHCS SW39FT WASHER A87CA4 SN3118HX CONNECTING ROD 5 16 18 HEX LOCK NUT 10
25. SWITCH EXPLOSION PROOF CORDSET 1787E SEAL FITTING W 797E amp 798E A388EEG 115V 60HZ MOTOR 791E2 POWER CORD SWITCH NIPPLE YELLOW TYP 3 PLACES BLACK BLACK WHITE 786 3 WHITE P1 BLACK CONDUIT OUTLET 208CA GREEN GREEN SUPPORT BRACKET P2 BLACK RED 190F PROTECTIVE GROUND SYMBOL ORANGE A388EEG 220V 60H7 MOTOR TO 1964E REDUCER POWER CORD SWITCH COUPL ING ON MOTOR YELLOW BLACK BLACK WHITE P1 BLACK GREEN GREEN N RED 190F PROTECTIVE ORANGE GROUND SYMBOL P2 BLACK 201E 16017 201 STRAIN TE om 115VAC A388EEG A491E2 DIC 230VAC 88 1782HC 230V CORDSET GROUND TO MOTOR JUNCTION BOX NOTE 1 INSTALL 190F PROTECTIVE GROUND SYMBOL FROM CORD 21 16GA UNSHIELDED WIRE BY GROUND SCREW IN 1384E BOX oo SWITCH BOX W GROUND STUD GROUND STUD ASSEMBLY DETAIL NOT TO SCALE 26 Parr Instrument Company 3900 Series Hydrogenation Apparatus 1384 TUMBLER SWITCH EXPLOSION PROOF S S 1787E SEAL FITTING W 797E amp 798E 791E2 NIPPLE TYP 4 PLACES 786 5 CONDUIT OUTLET A388EEK 220V 50HZ TO MOTOR POWER CORD SWITCH a BLACK 4 YELLOW m lan 1 BLUE u fe 5 BLACK SUPPORT reser J BROWN 190F seer 2 2 WHITE GROUND SYMBOL SEE NOTE 2 3 ORANGE 8 8 RED 4 YELLOW 201E 16017 201E NOTES GRN YEL 1 CUT 1 2 FOOT PIECE OF 1801 WHITE WIRE
26. USE Parr Instrument Company 30 Revision 06 24 09 211 53rd Street Moline Illinois 61265 USA Phone 1 309 762 7716 or 1 800 872 7720 Fax 1 309 762 9453 E mail parr parrinst com http www parrinst com
27. ast or failing to observe and prevent sudden increases in temperature or pressure Qualified personnel should make frequent checks to be sure that all safety rules are being observed In the absence of a supervised safety program the user must take time to become completely familiar with their equipment and to consider any hazards inherent in the reactions they intend to perform 4 Parr Instrument Company 2 ASSEMBLY INSTRUCTIONS Unpack all parts carefully and check against the packing list furnished with the shipment Rinse or blow air through the hydrogen tank to remove any dust or foreign material Likewise blow out the gas hose and valves to be sure that they are dust free and clean Set the apparatus on a sturdy bench or table where there 1s convenient access to an electrical outlet with the appropriate supply voltage and current ratings 1n accordance with national and local electrical code requirements The supply voltage must not exceed the marked nominal voltage shown on the instrument by more than 10 The supply voltage receptacle must have an earth ground connection Attach the valves to the hydrogen tank and tighten the couplings firmly with a wrench This tank 1s filled through the AA92CA valve which 15 attached to the right end The gage on this valve shows the tank pressure when the valve 1s closed The gage on the 3A93CA valve at the left end of the tank shows the pressure in the reaction bottle and connecting
28. c New York www parrinst com 13 3900 Series Hydrogenation Apparatus PARTS LISTS 3910 HYDROGENATION APPARATUS 38 43 35 0 6 8 8 N N 17 2 PL 2 PL 2 PL N 7 amp zi Wa 4 PL 52 14 Parr Instrument Company ITEM PART NO 1 NUMBER 221CA DESCRIPTION BASE PLATE 221CA2 221CA3 BASE PLATE AIR BASE PLATE EXP ITEM PART NO 25D NUMBER 139E8 3900 Series Hydrogenation Apparatus DESCRIPTION FUSE 3AG SLO BLO 250V 2 5 AMP 25E 139E26 FUSE SLO BLO 6 AMP 250V 2CA2 SHAKER COLUMN 583118 14 5 16 18 X 7 8 HHCS 8 18 SS 139 21 FUSE SLO BLO 250V 5 0 AMP 54CA BOTTLE CLAMP TOP 139E20 FUSE 3AG SLO BLO 250V 4 0 AMP 453E CLIP 3 8 DIA TENSION CLEAR SA1332RD04 6 32 X 1 4 RHMS SLOTTED X2291EE SWITCH BOX PKG 230V 3910 3920 SW13FT 6 BOLT WASHER 18 8 SS SW31FT 5 16 BOLT WASHER 18 8 SS 59CA KNURLED NUT TIE ROD FLYWHEEL BASE O Q ROD A55CA TIE ROD SHORT ASSEMBLY 4CA
29. ch material Refer servicing to qualified personnel EXPLANATION OF SYMBOLS 3900 Series Hydrogenation Apparatus GENERAL SPECIFICATIONS Electrical Ratings 3911 amp 3921 Rated 115 Vac 60 Hz 8 0 Amps or 115 Vac 60 Hz 3 6 Amps or 115 Vac 60 Hz 3 3 Amps or 230 Vac 50 Hz 2 1 Amps or 230 Vac 50 Hz 8 0 Amps The electrical ratings are identified on the data plate of the instrument Before connecting any Parr Hydrogenation Apparatus to an electrical outlet the user must be certain that the electrical outlet has an earth ground connection and that the line load and other characteristics of the installation do not exceed the following limits Voltage Fluctuations in the line voltage should not exceed 10 of the rated nominal voltage shown on the data plate Frequency Hydrogenation apparatus can be operated from a 50 or 60 Hertz power supply without affecting the apparatus The frequency ratings are identified on the data plate of the instrument Current The total current drawn should not exceed the rating shown on the data plate by more than 10 percent Off Position This CAUTION symbol may be present on the Product Instrumentation and literature If present on the product the user must consult the appropriate part of the accompanying product literature for more information Protective Earth PE terminal Provided for connection of the protective earth green or green yellow supply system conductor
30. controller which should turn off the heater SEMI MICRO OPERATIONS Small samples can be treated 1n a 3911 hydrogenator by replacing the standard 500 mL bottle with a smaller 250 mL bottle 66CA2 This requires a 101 CA2 spacer to compensate for the difference in bottle heights To install the 250 mL bottle remove the stopper and the 61CA4 washer from the gas inlet tube and slide the 101CA2 spacer onto the tube then clamp the bottle and spacer In the holder in the usual manner Since small samples may require only small amounts of hydrogen it may be advantageous to replace the standard four liter hydrogen tank with an alternate one liter tank A16CA2 for semi micro operations The same tank valves are used on both sizes and are easily transferred to the small tank Augustine reference 1 on page 15 describes an interesting holder for handling small samples in a 3911 hydrogenator which he prepares by sealing a 50 mL or smaller heavy walled flask 1nside a larger bottle 3900 Hydrogenation ALTERNATE PARTS If bottle pressure measurements are not required the gage can be removed from the 3A93CA valve assembly and replaced with a 94CA plug Teflon tubing can be furnished in place of the standard 119CA polypropylene tube for use with chemicals which might attack polypropylene The same fittings are used to attach either Teflon or polypropylene tubing to the 3A93CA valve MAINTENANCE INSTRU
31. d clamp the bottle In the shaker In the usual manner The 82CA2 washer is not required when using a spacer GLASS REACTION BOTTLES The 1000 and 2000 mL reaction bottles 71CA and 72CA supplied with this apparatus have been individually pressure tested to 80 psig and 60 psig respectively In spite of these tests the Parr Instrument Company cannot guarantee that these bottles will not break at lower pressures The user must therefore be constantly aware of the hazards involved in handling large volumes of liquids in glass bottles under pressure and he must take whatever precautions he considers necessary to protect himself from injury in case a bottle should unexpectedly fail It 1s recommended that working pressures in these 1000 and 2000 mL bottles should never exceed 40 psi and 30 psi respectively Pressures should be held below this maximum whenever possible Alternate 1000 and 2000 mL reaction bottles with a fiberglass covering 71CA2 and 72CA3 can be furnished for the 3921 hydrogenator These coated bottles are no stronger than the plain bottles but the fiberglass envelope will usually retain any broken glass and prevent the loss of valuable reactants in case of accidental breakage The maximum working pressures mentioned above applies to both plain and coated www parrinst com 11 3900 Series Hydrogenation Apparatus bottles alike Both styles use the same connecting tube and fittings If higher pressures up to 60 ps
32. ed by drying and heating chloroplatinic acid in air to form a brown oxide which can then be reduced to the more active black form by shaking with hydrogen either before or after mixing with the sample Instructions for preparing this and other catalysts are given in the references on page 10 Raney nickel 1s used In certain procedures but other less active nickel catalysts require pressures outside the range of this apparatus Platinum oxide and other catalytic chemicals can be obtained from most laboratory supply houses BorrLE HEATER Bottle temperatures up to 80 C can be developed in the 3911 hydrogenator by wrapping a glass fabric heating mantle A450E around the 500 mL bottle The mantle then takes the place of the perforated metal guard screen No special fittings are needed for attaching this heater Simply wrap the mantle tightly around the bottle and run the connecting cord through the slot 1n the bottle clamp Use the plastic cable clip 453E furnished with the heater to anchor the heater cord to the top of the bottle clamp then run the cord out from the shaker pivot arranging it for minimum flexing when the shaker Is Operating WATER JACKET The 500 mL reaction bottle can be cooled while it 1s clamped in the shaker mechanism by installing an A103CA water Jacket This jacket fits Into the bottle clamp in place of the 65CA perforated steel guard A soft rubber ring seals the neck of the bottle into the jacket The only c
33. f the distance from the neck of the bottle This distance can be changed by loosening the cap nut at the top of the connector and sliding the probe up or down in the tee fitting Loop the thermocouple wire downward and fasten 1 above the tee fitting using one of the cable ties furnished with the bottle connector then run the wire along the polypropylene tube fastening it firmly to the tube at several points to prevent excessive flexing and breakage Bring the bottle heater cord upward and fasten it under the clip at the top of the shaker then run the cord parallel to the shaker pivots and plug it into the heater 8 Parr Instrument Company socket on the controller To activate the heater plug the thermocouple and the heating mantle into sockets on the rear panel of the controller and connect the controller to an electric supply that corresponds to the voltage of the heater Turn the DISPLAY A159CA2 and HEATER switches ON Thermocouple and set the controller to the Assembly desired operating temperature using the UP and DOWN arrow keys on the front of the controller module The indicator light in the heater switch will illuminate when the switch 15 ON and current Is being supplied to the heater The set point can be changed at any time regardless of whether the heater 15 on or off Copies of Parr Bulletin 311M Supplemental Instructions for the 4833 Controller and the CAL 9500 User s Manual furnished with the 483
34. hange required when adding a water Jacket 1s to use the special cut down stopper which 1s furnished or cut 1 4 inch from the top of the regular 62CA stopper to shorten the overall height of the combined assembly Always install the soft rubber sealing ring with the large diameter downward and the smaller diameter at the top otherwise it will be very difficult to remove the bottle from the cooling jacket A103CA Woater Jacket www parrinst com 7 3900 Series Hydrogenation Apparatus 3 MEASUREMENT AND CONTROL z vi K T L i Y i AWAA I TEMPERATI we CONTROLI ER 4833 Temperature Controller Reaction temperatures can be measured and controlled with a Parr 4833 Temperature Controller which operates with an 295 Type J iron constantan thermocouple installed in the reaction bottle The thermocouple is sealed in an 1 8 diameter stainless steel sheath and held in an A159CA bottle connector assembly which carries both the probe and the gas passage through a single opening in the bottle stopper A295E thermocouples are made in two lengths to fit different bottle sizes as listed on page 29 To install the A159CA bottle connector remove the existing gas inlet tube and fittings and install the new fittings which are provided Clamp the bottle in the shaker with the thermocouple positioned so that the tip of the probe reaches a point three fourths o
35. he realization that hydrogen 1s highly flammable and that pressures and reaction rates must be carefully controlled at all times 2 All catalysts must be handled cautiously because of their highly reactive nature Do not add dry catalyst to a bottle containing a flammable solution or vapor The vapor might ignite Instead add the catalyst first and cover it immediately with the sample in solution Precautions must also be taken to wash the catalyst from the thermocouple the inlet tube and the stopper when opening the bottle Any catalyst left on these parts may ignite when exposed to the air If breakage or spills occur flush the contaminated area immediately with large volumes of water and keep the area wet until all traces of catalyst have been removed Vacuum filtration through a paper filter can be dangerous 1 air 1s drawn through the filter in the presence of a catalyst To reduce this hazard keep the paper covered with solution while it is under suction or use a filter made of a non flammable material Care must be taken to keep the apparatus free of impurities which might poison the catalyst Although a small amount of air trapped in the bottle will not interfere with most hydrogenations the reaction rate can sometimes be improved by evacuating the bottle before adding hydrogen Or the air can be removed by filling the bottle with hydrogen to 20 or 30 psig and venting it at least three times before starting the shaker
36. ig are required for treating large amounts of reactants users are urged to purchase the special 2500 mL heavy duty bottle 72CA4 which 15 made specifically for this purpose This is a hand blown borosilicate glass bottle with an extra heavy wall which is much stronger than the standard machine made bottles STAINLESS STEEL BOTTLE The breakage hazard which is always present when using glass bottles can be eliminated by substituting a 1700 mL stainless steel reaction bottle which can be used at working pressures up to 60 psig maximum The complete stainless steel bottle assembly with cover spacer spool connecting tube and fittings can be ordered under Cat No A129CA3 To install the stainless bottle slide the 133CA2 spacer spool onto the polypropylene tube with the parts arranged so that the plain end of the spool will rest on the cover leaving the shallow depression 1n the other end of the spool to engage the clamping screw Attach the O ring to the cover close the bottle and slide the assembly into the holder Tighten the clamping screw and attach the guard screen before pressurizing the bottle 12 Parr Instrument Company 2 A155CA TUBE ASSY TO BE INSTALLED BY CUSTOMER 135652 SPACER A138A MALE CONN 226 BOTTLE A129CA3 Stainless Steel Bottle Assembly 2 BOTTLE HEATER The 7 one liter bottle 72 two liter bottle and the A129CA3 stainless bottle assembly may be heated in the 3921
37. ighten the SV B2 packing nut firmly with a wrench Caution Always back the valve needle away from its seat before tightening the packing nut It will be necessary to use a new plastic ferrule 1n the A102CA connector whenever a new polypropylene tube 15 installed A new 102 connector 18 furnished www parrinst com 9 3900 Series Hydrogenation Apparatus with each replacement A154CA polypropylene tube so that a complete set of parts will be available when changing tubes If the body and cap nut in the old connection are in good condition they can be used with the ferrule from the new connector But if there is any question about the old parts discard them and install a new connector The steps required to attach the tube to the connector are as follows Be sure that the end of the tube has been cut squarely then disassemble the connector and slide the cap nut and ferrule onto the tube Insert the tube into the connector body and tighten the cap nut firmly 10 Parr Instrument Company Fuse RATINGS The replacement of protective fuses should be performed by qualified personnel Parr No Type 139E21 Slo blo Ratings 5 Amps 250 Vac 139E20 Slo blo 4 Amps 250 Vac 139 8 Slo blo 2 5 Amps 250 Vac 139E25 Slo blo 10 Amps 250 Vac 139 26 Slo blo 6 Amps 250 Vac Note Check the labels on Switch box for correct fuse rating 2 3900 Series Hydrogenation Apparatus SPEC
38. ng Schematic 22 3920 Wiring Schematic 23 Explosion Proof Switch Assembly for 1765EEG 115V Series 3910 24 Explosion Proof Switch Assembly for 1765EEK 220V Series 3910 25 Explosion Proof Switch Assembly for A388EEG 115V amp 220V Series 3920 26 Explosion Proof Switch Assembly for A388EEK 220V Series 3920 27 Thermocouple Assemblies 28 Reaction Bottles for Parr Hydrogenators 29 Heating Mantles 29 Air Motor Assembly 30 Switch Box Assembly 30 PREFACE ScoPE These Instructions describe the steps to be taken when setting up and operating any Parr 3911 or 3921 Hydrogenator All operating and safety instructions given here apply equally to all units since both operate in the same manner and use the same hydrogen supply system few specific instructions applying only to the larger 3921 apparatus are given on page 13 User s should study all of these instructions carefully before starting to use this apparatus so that they will fully understand the capabilities and limitations of his equipment and so that they will be well aware of the precautions to be observed in its operation SAFETY INFORMATION To avoid electrical shock always Disconnect the electrical power before maintenance or servicing To avoid personal injury Do not use In the presence of flammable or combustible materials fire or explosion may result This device contains components which may ignite su
39. the hose if it is not required but do not unscrew the fittings which anchor the end nipples to the hose itself Before using a new apparatus for the first time assemble it with an empty bottle and test for gas leaks as follows Fill the tank with hydrogen to 40 psig then close the tank filling valve Open the bottle valve and allow the full tank pressure Into the bottle then close the bottle valve The tank and bottle gages should now read the same Record these pressures and continue to observe them over a period of four to six hours The pressures should remain constant throughout this period unless there 1s a significant change in room temperature If a noticeable drop 1s observed In either gage find and correct the leak before starting to use the apparatus Any leaks can usually be detected by brushing the joints with a soap solution OPERATING PROCEDURE Samples to be treated a Parr hydrogenator are placed in a reaction bottle with a catalyst and clamped in a shaking mechanism A gas connection 1s made to the bottle from a multiple valve and all air 1s removed either by evacuation or by flushing with hydrogen Hydrogen is then introduced from a 4 liter reservoir while the bottle 15 shaken vigorously to initiate the reaction Heating or cooling can be applied if necessary After the reaction reaches the desired point the shaker 1s stopped the bottle vented and the product and catalyst are recovered The individual steps in
40. this operating procedure are listed below These can be varied to suit each individual application 1 Place the catalyst solvent and sample in the reac tion bottle adding the catalyst first to avoid possible vapor ignition by the dry catalyst The total volume of solution should not exceed two thirds the capac ity of the bottle 2 Attach the stopper with connecting tube and slide the bottle into the guard screen then set the as sembly in the bottle holder and tighten the knurled clamping nuts 3 If air is removed from the bottle by evacuation at tach a vacuum hose to the nipple on the 3A93CA 3900 Hydrogenation valve close the bottle valve open the gas release valve and evacuate until the solvent starts to boll If a low boiling solvent 16 not used evacuate to negative pressure sufficient to remove most of the A1r can also be removed by alternately filling the bottle with hydrogen to 20 or 30 psig and venting it at least three times After purging the bottle close the gas release valve and leave it closed throughout the run 4 Starting with the hydrogen tank filled to 30 psig open the bottle valve and read the bottle pressure gage after equilibrium has been established 5 Start the shaker and follow the progress of the reac tion by observing the bottle pressure gage If com plete hydrogenation is desired continue shaking until there 15 no further pressure drop
41. tube The front knob on the 3A93CA valve controls the flow of gas from the tank to the bottle The rear knob at the opposite end of the block 18 used when discharging gas from the bottle or when evacuating the bottle through the hose nipple The 25 inch length of polypropylene tubing leading to the reaction bottle must be firmly connected to the outlet fitting on the 3A93CA valve No special clamps or fittings are required to fasten this tube into the bottle stopper Simply slide the end of the tube through the 61CA4 washer and through the 166 retaining ring then push the tube through the one hole Neoprene stopper leaving a projection of about one inch below the bottom of the stopper Slide the safety screen over the bottle place the bottle into the holder and tighten the thumb nuts on the ends of the two tie rods The clamping pressure developed by the thumb nuts will hold the bottle in the shaker mechanism and tt will also anchor the connecting tube in the stopper A 6 ft hose 118 is furnished for connecting the apparatus to the pressure regulator or needle valve on a commercial hydrogen tank Screw one end of the hose into the socket in the AA92CA valve and connect the other end to the pressure regulator or tank valve The 1 8 NPT pipe threads on the ends of the pressure hose should be coated with Teflon tape plastic lead 2 or other thread dope to ensure tight seals The 1 8 to 1 4 bushing can be removed from
42. unds www parrinst com 5 3900 Series Hydrogenation Apparatus Battle Pressure Gage Gas Release Sx Valve AF Exhaust Nipple 3A93CA Bottle Valve Tank Pressure Gage W Tank Filling AA92CA Valve Reaction Bottle 8 I has supply Hose Gas Tank and Valve System Standardization tests are not limited to runs with maleic acid Fumaric acid 1s equally suitable for this purpose or any other pure compound can be used provided that it is completely or quantitatively reduced If the intended usage for the apparatus involves the consumption of only a small amount of hydrogen the apparatus can be standardized with the tank valve closed The gage will then give a more significant reading as gas 1s consumed from the connecting tube and bottle alone while these parts are 1solated from the tank PRESSURE LIMITS The use of glass bottles 1n these reactors introduces certain pressure limitations and a potential hazard which the user must understand Although each bottle is pressure tested before it 1s sold the physical characteristics of glass are such that it 1s impossible to guarantee these bottles against breakage or to predict their service life For this reason each apparatus 1s equipped with a bottle shield to restrain flying glass in case of breakage The user must take whatever additional precautions he considers necessary to protect himself from injury in case a bottle should
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