Rapid Distillation Apparatus MODEL 65000 INSTRUCTION MANUAL Product designs are subject to change without notice © 1988, 2013 Labconco Corporation 6504000 REV. N / ECO H435 Printed in U.S.A.
TABLE OF CONTENTS Introduction General Description Performance Component Identification 1 1 2 Installation Installation Factors Assembly Start-Up and Initial Check-Out Normal Operation 4 4 5 7 Samples Digested Utilizing Micro-Digestor Start-Up and Operation Shutdown 7 7 Samples Digested Utilizing Rapid Digestor Start-Up and Operation Principle Apparatus Reagents Determination 9 9 9 9 10 Calculations 11 Routine Maintenance Schedule Console Glass Still Stopcock 12 12 13 Replacement Parts 14 Wiri
INTRODUCTION General Description The Labconco Rapid Distillation Apparatus is designed expressly for rapid, semi-automatic steam distillation from sulfuric acid digest prepared from nitrogen-bearing materials such as feeds, grains, soils, plant tissue, water effluent, organic waste food products, etc. Sample digestions are accomplished utilizing either Labconco’s Micro Distillation Apparatus or Rapid Digestor units. The distillation apparatus can be used for micro or macro levels of nitrogen determination.
INTRODUCTION Component Identification (1) Console. A one piece assembly molded out of linear polyethylene to provide both chemical resistance and light weight capabilities for the distillation apparatus. (2) Still. One piece still fabricated from borosilicate glass and featuring chemically inert PTFE stopcocks. Because the still does not incorporate rubber or plastic tubing connections, the possibilities of leakage have been greatly reduced. (3) Variable Heat Control.
INTRODUCTION Component Identification 5 2 3 1 Figure 2 3
INSTALLATION Your Rapid Distillation Apparatus has been shipped to you in one carton. In unpacking, remove the packing material carefully, checking all material for two separately packed parts. The carton will contain a heater element assembly and clmaps wrapped in protective paper, and the one-piece glass still packed between foam pads inside of a cardboard carton. Inspect this material thoroughly prior to installation and report any damage that may have occurred in transit.
INSTALLATION (5) Obtain several lengths of Tygon tubing (5/16" bore x 1/16" wall). Tubing IS NOT furnished with the unit and may be obtained from local laboratory supply dealers. Tubing will be used for connecting water lines (refer to steps 6, 11 and 12). (6) Measure distance from tube connector on steam reservoir through the tubing access port in console (upper left corner) to a water outlet. Cut tubing and connect to tube connector on still and water source.
INSTALLATION (2) Fill steam reservoir flask 2/3 full with ammonia free distilled water. Adjust flow control valve to give approximately 7 ml/minute flow. Proper adjustment of valve will replace the water lost from the distillation. If the flow control valve is to be used for low level nitrogen determinations, it may be necessary to install a deionization cartridge (available from your laboratory supply dealer) between the flow control valve and water source.
NORMAL OPERATION Samples Digested Utilizing Micro-Digestor – Start-up and Operation The Labconco Rapid Distillation Apparatus is designed to conform with standard Micro Kjeldahl distillation techniques. The preparation of digested samples, chemical treatment of the sample prior to distillation and titration techniques following the distillation are adequately described in A.O.A.C. Methods of Analysis and other technical references, and should be referred to in ALL cases.
NORMAL OPERATION chamber until all of the solution is added. Leave column of caustic in the funnel stem to act as a liquid seal. NOTE: If reaction is uncontrollable, REDUCE all future acid digest sample volumes and re-calculate required alkali solution strengths so that inner chamber contents will have a normality of 4 to 8. A small amount of caustic should be left in the addition funnel to act as a liquid seal during each distillation.
NORMAL OPERATION Samples Digested Utilizing Rapid Digestor – Start-up and Operation Same as information under Samples Digested Utilizing Micro-Digester. Principle (1) After sample digestion, utilizing the Labconco Rapid Digestor-4, Rapid Digestor-25, or equivalent digestion apparatus, a portion of the sample is transferred to the Rapid Distillation Apparatus. Ammonia is steam distilled into standard acid and back titrated with standard alkali.
NORMAL OPERATION Determination (1) Samples are digested utilizing the Labconco Rapid Digestor 5 place of the 25 place units equipped with 250 ml volumetric digestion tubes (refer to digestion methods available upon request from Labconco). After digestion, remove rack of tubes from digestor and allow to cool for 8 – 10 minutes (cooling time depends upon air flow around tubes).
CALCULATIONS 11
ROUTINE MAINTENANCE Console The console is constructed of plastic and resists staining. To preserve its general appearance, acid and alkali “spills” should be removed as soon as possible by washing and sponging with a damp cloth. Glass Still (Replacement) (1) Disconnect line cord from 115 volt AC outlet disconnect heater plug connections. (2) Remove heater assembly and stopper. (3) Disconnect ALL tubing connections on glass still. (4) Remove clamp screws (4). (5) Remove clamps (2).
ROUTINE MAINTENANCE Stopcock The Labconco Rapid Distillation Apparatus is equipped with (2) PTFE stopcocks. The PTFE stopcocks do not require lubricants. The plug and glass barrel may be cleaned with Acetone to wash away any solid particles that might accumulate during long service. If solid particle s become lodged between the plug and glass barrel, or project from the glass surfaces, they can score the PTFE plug around its bore and result in a “leaky” plug.
REPLACEMENT PARTS 3 12 13 10 14 9 11 1 8 18 4 Figure 5 14
REPLACEMENT PARTS ITEM 1 2 *3 4 *5 *6 *7 8 9 PART NUMBER 65001 13525 13237 18765 19175 13432 13410 65008 65042 10 11 12823 65021 12 13 14 *15 *16 *17 18 65056 65058 19030-08 13174 19093-26 65045 13270 DESCRICPTION Glass micro still assembly with PTFE stopcocks PTFE plug replacements for PTFE stopcock Heat controller Knob, for heat controller Fastener, nylon round head, canoe type Fuse holder Fuse only – 115 Volt AC AGC-3 Receiver flask platform assembly Heater assembly, complete with stopper and male
WIRING DIAGRAM Figure 6 16
REFERENCES Many excellent reference texts and booklets are currently available. The following is a brief listing: Official Methods of Analysis of the Association of Official Analytical Chemists, Thirteenth Edition, Washington, District of Columbia, 1980. Hambleton, L.G. and Noel, R.J., Journal of the Association of Analytical Chemists, 58:143-145, 1975.
WARRANTY We are committed to providing our customers with quality equipment and service after the sale. Part of this objective involves keeping you informed of changes and new product additions.
SHIPPING CLAIMS If shipment is received in visibly damaged condition, be certain to make a notation on the delivering carrier’s receipt and have his agent confirm the damage on your receipt. Otherwise, the damage claim may be refused. If concealed damage or pilferage is discovered, notify the carrier immediately and retain the entire shipment intact for inspection. Interstate Commerce Commission rules require that the claim be filed with the carrier within 15 days after delivery. NOTE: Do not return goods.
CONTACTING LABCONCO If you have any questions that are not addressed in this manual, or if you need technical assistance, please contact Labconco’s Customer Service Department at either (800) 821-5525 of (816) 333-8811, between the hours of 8:00 a.m. and 5:00 p.m., Central Standard Time. Labconco’s mailing address is: Labconco Corporation 8811 Prospect Avenue Kansas City, Missouri 64132-2696 Fax # 816-363-0130 Visit Labconco through the Internet at: http://www.labconco.com or email: labconco@labconco.
