Labconco RapidStill I User manual

RapidStill™I
Models
6500000

Copyright © 2017 Labconco Corporation. The information contained in this manual and the
accompanying products are copyrighted and all rights reserved by Labconco Corporation. Labconco
Corporation reserves the right to make periodic design changes without obligation to notify any
person or entity of such change.
Returned or Damaged Goods
Do not return goods without the prior authorization from Labconco. Unauthorized returns will not be
accepted. If your shipment was damaged in transit, you must file a claim directly with the freight
carrier. Labconco Corporation and its dealers are not responsible for shipping damages.
The United States Interstate Commerce Commission rules require that claims be filed with the
delivery carrier within fifteen (15) days of delivery.
Limitation of Liability
The disposal and/or emission of substances used in connection with this equipment may be governed
by various federal, state, or local regulations. All users of this equipment are required to become
familiar with any regulations that apply in the user’s area concerning the dumping of waste materials
in or upon water, land, or air and to comply with such regulations. Labconco Corporation is held
harmless with respect to user’s compliance with such regulations.
Contacting Labconco Corporation
If you have questions that are not addressed in this manual, or if you need technical assistance, contact
Labconco’s Customer Service Department or Labconco’s Product Service Department at 1-800-821-
5525 or 1-816-333-8811, between the hours of 7:30 a.m. and 5:30 p.m., Central Standard Time.
Part #6504000, Rev. P
ECO L123
Warranty
Labconco Corporation provides a warranty to the original buyer for the repair or replacement of parts and
reasonable labor as a result of normal and proper use of the equipment with compatible chemicals. Broken
glassware and maintenance items, such as filters, gaskets, light bulbs, finishes and lubrication are not
warranted. Excluded from warranty are products with improper installation, erratic electrical or utility
supply, unauthorized repair and products used with incompatible chemicals.
The warranty for the RapidStill I will expire one year from date of installation or two years from date of
shipment from Labconco, whichever is sooner. Warranty is non-transferable and only applies to the owner
(organization) of record.
Buyer is exclusively responsible for the set-up, installation, verification, decontamination or calibration of
equipment. This limited warranty covers parts and labor, but not transportation and insurance charges. If the
failure is determined to be covered under this warranty, the dealer or Labconco Corporation will authorize
repair or replacement of all defective parts to restore the unit to operation. Repairs may be completed by 3rd
party service agents approved by Labconco Corporation. Labconco Corporation reserves the rights to limit
this warranty based on a service agent’s travel, working hours, the site’s entry restrictions and unobstructed
access to serviceable components of the product.
Under no circumstances shall Labconco Corporation be liable for indirect, consequential, or special damages
of any kind. This warranty is exclusive and in lieu of all other warranties whether oral, or implied.

T
TA AB BL LE E O OF F C CO ON NT TE EN NT TS S
CHAPTER 1: INTRODUCTION 1
General Description 2
Performance 2
Component Identification 3
CHAPTER 2: INSTALLATION 5
Installation Set-up 5
Assembly 5
Initial Test 8
CHAPTER 3: NORMAL OPERATION 11
Samples Digested Utilizing Micro Digestor 11
Start-Up and Operation 11
Shutdown 13
Calculations 13
CHAPTER 4: ROUTINE MAINTENANCE 14
Glass Still (Replacement) 14
Stopcock 15
CHAPTER 5: REPLACEMENT PARTS 16
CHAPTER 6: WIRING DIAGRAM 17

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In nt tr ro od du uc ct ti io on n
Thank you for displaying confidence in us by selecting a Labconco RapidStill I.
Our design engineers, assemblers and inspectors have utilized their skills and
years of experience to ensure that the Labconco RapidStill I meets our high
standards of quality and performance.
This manual should be read carefully by all the end users in
order to become familiar with the operation of the RapidStill I.
Recommendations are made within the manual to help you
obtain maximum performance and life from your product.
We have included sections on initial set up, operation, and
maintenance to provide you with all the tools necessary to
achieve maximum performance. If you have questions or
concerns, do not hesitate to call us at 1-800-821-5525 for
assistance.
WARNING: The disposal of substances used in connection with
this equipment may be governed by various federal, state or
local regulations. All users of this equipment are urged to
become familiar with any regulations that apply in the user’s
area concerning the dumping of waste materials in or upon
water, land or air and to comply with such regulations.
!

Chapter 1: Introduction
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General Description
The Labconco RapidStill I 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
Digestion Apparatus or Rapid Digestor units.
Performance
Your Labconco RapidStill I has been designed to accept digested samples up to
4 ml (maximum) equivalent of concentrated acid, and is capable of giving
reproducible results in ranges as low as 10 micrograms (gamma) #1% nitrogen.
The RapidStill I may also be utilized for other steam distillations that DO NOT
exceed the volume limitations of the units mixing chamber (approximately 50 to
55 ml).
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Chapter 1: Introduction
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Component Identification
(1) Power Switch Switches power to the Heater. When ideal Heat Control
setting is achieved, use this switch to turn Heater ON and OFF.
(2) Heat Control The electric immersion heater provides fast, efficient heat.
Steam generation starts very rapidly from a cold start. Control input to the
heater and steam output by adjusting this knob.
(3) Fill Valve The Fill Valve is opened only when filling Boiling Flask. Use
distilled water from the Water Bottle to keep water level in the steam
reservoir approximately 2/3 full during distillation.
(4) Aspirator Stopcock The unit has a built-in glass aspirator to purge spent
samples after determination. The water used for cooling of this condenser
is also used for aspirating. A twist of the Aspirator Stopcock draws the
sample and rinse water down the drain.
(5) Sample Addition Funnel Use this funnel to transfer digested sample to
the Mixing Chamber.
(6) Sample Addition Stopcock The upper PTFE stopcock that allows for
the addition of samples or pH controlling solutions.
(7) Mixing Chamber The inner bulb in the lower portion of the still where
the sample is mixed with appropriate solutions during the distillation.
(8) Cooling Water Connections Note the two barbed fittings extending
through the back of the housing. Connect the “IN” fitting to a cold water
source and the “OUT” fitting to a drain.
(9) Condenser Cold water flows through the outer wall of the tall column to
condense steam.
(10) Boiling Flask The round flask reservoir which contains distilled water to
be heated during the distillation.
(11) Flask Shelf Shelf is adjustable in height. Positioning the flask is
important to maintain relationship between the condenser outlet and liquid
level in the Receiving Flask.
(12) Heater Heater is energized when there is sufficient water in the Boiling
Flask. Heater may be unplugged from the housing if required.
(13) Water Bottle Use distilled water only in the still. Water Bottle is
squeezed to introduce water to the Boing Flask via the Fill Valve.

Chapter 1: Introduction
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In ns st ta al ll la at ti io on n
Your RapidStill I has been shipped to you in one carton. When unpacking, remove
the packing material carefully, checking all material for two separately packed
parts. The carton will contain:
Base Housing
Glass Still
Heater
Stainless Steel Flask Shelf
“U” Clamp (large) (1)
“U” Clamp (small) (2)
Clamp Nuts (6)
Fill Valve and Tube
Pinch Clamps (2)
Power Cord
NOTE: Plastic tubing and valve for connection of the condenser to water and drain
source is NOT included.
Inspect this material thoroughly prior to installation and report any damage that
may have occurred in transit.
Installation Set Up
Assembly
(1) Lay the Base Housing on its back and position the Glass Still assembly on
the console, as shown. Do not connect to electrical power source until set
up is complete.

Chapter 2: Installation
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(2) Starting with the large U-clamp, place both the large and small U-clamps
around the glassware and through the brackets. Gently tighten the clamp
nuts so that the glassware is firmly held to the Base Housing.
(3) Carefully attach the condensing water tubing to the glass barb fittings. Do
not add clamps or any lubricant (other than water) to these connections.
Turn Base Housing upright.
(4) Locate the RapidStill I where there is convenient 115 volt outlet and
accessibility to cold tap water and drain.

Chapter 2: Installation
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(5) Obtain several lengths of flexible plastic or silicone tubing (3/8" ID x 1/16"
wall). Tubing IS NOT furnished with the unit and may be obtained from
laboratory supply dealers. Connect tubing from the rear of the housing to a
drain or sink for effluent. Connect tubing for the inlet from the rear of the
housing to a cold water source (<25oC) with fine flow control through a
valve or faucet. Two pinch clamps have been provided. Check for leaks.
(6) Keep power OFF. Insert the heater element into the Boiling Flask and press
the stopper into the Flask opening firmly. Heater should not be in contact
with any of the glass. NOTE: This must be sealed for distillation. Plug the
Heater into the Base Housing connector.

Chapter 2: Installation
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(7) NOTE: Make certain the Power Switch is in the OFF position. Connect the
Power Cord to the back of the Base Housing. Power Cord may be plugged
into outlet at this time.
Initial Test
The start-up process should begin as follows:
(1) Make sure the Power Switch is in the OFF position.
CAUTION: Never energize the Heater unless heater element
is properly immersed in water.
(2) Fill Boiling Flask 2/3 full with ammonia-free distilled water or deionized
water through the Fill Valve. It is important to maintain a sufficient level in
the Boiling Flask at all times. The Fill Valve should be closed.
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Chapter 2: Installation
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(3) Check Sample Addition Stopcock; it must be closed.
(4) Close Aspirator Stopcock.
(5) Turn on tap water source and fill the Condenser. The rate of water through
the Condenser will be adjusted later based on the temperature of the
distillate.
(6) Place a small graduated cylinder on Flask Shelf at output of condenser and
measure distillation rate.
Sample
Addition
Stopcock
Aspirator
Stopcock
Water Level

Chapter 2: Installation
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(7) Turn Heat Control dial to “9.” Press Power Switch to ON.
(8) The water in the Boiling Flask will begin boiling in about 5 to 6 minutes.
The Heat Control setting should be turned down until a distilling rate of
5 ml/min. is obtained at the output. Replace water lost in the Boiling Flask
during distillation.
(9) Measure the temperature of distillate and adjust cooling water input at tap
water source to maintain distillate temperature of 25°C or lower.
(10) For low level nitrogen determinations, allow steam distillation to continue
until distillate is nitrogen free. Removal of nitrogen entrained in the
Boiling Flask water may require 30 minutes at initial start-up, or if the
apparatus has been out of use for sufficient time to allow nitrogen
containing fumes to be reabsorbed in the Boiling Flask. Add
approximately 15 ml of ammonia-free distilled water to the Mixing
Chamber through the Sample Addition Funnel. Close Sample Addition
Stopcock after test liquid drains through. Open the Aspirator Stopcock and
siphon off all liquid in the Mixing Chamber to check out aspirator
operation. Water flow to Condenser can be adjusted to increase or decrease
“siphon” rate. When Mixing Chamber is cleared of the test liquid, close
the Aspirator Stopcock.
(11) The RapidStill I is now ready for samples. Refer to the following
appropriate method for the determination of nitrogen content from
predigested samples.

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No or rm ma al l O Op pe er ra at ti io on n
Samples Digested Utilizing Micro
Digestor
Start-up and Operation
The Labconco RapidStill I 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
described in the A.O.A.C. Methods of Analysis and other technical references, and
should be referred to in ALL cases.
(1) Turn on cooling water to the Condenser.
(2) Turn the Power Switch ON to energize Heater. Check Boiling Flask level
and adjust to 2/3 full if required. Set the Heat Control at “9” on the dial.
Allow steam reservoir water to come to a roll.
(3) Reduce the Heater Control setting to a desired 4 to 5 ml/min distilling rate,
(refer to Installation Set Up, Initial Test).
(4) Open the Aspirator Stopcock and aspirate the Mixing Chamber. Close the
stopcock when complete.
(5) Place the Receiving Flask containing the distillate receiving solution on
Flask Shelf at outlet of the Condenser.
(6) Check the Sample Addition Stopcock to ensure it is closed. Place entire 4
ml maximum acid digestion sample in Sample Addition Funnel.
(7) Open the Sample Addition Stopcock slowly to transfer digested sample to
the Mixing Chamber. Close the stopcock.

Chapter 3: Normal Operation
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(8) Rinse Sample Addition Funnel with 3 to 4 ml ammonia-free distilled water,
leaving some water in the bottom as a liquid seal.
(9) Raise the Flask Shelf; positioning it so that the condensate outlet is slightly
below the receiving liquid surface level.
(10) Add strong alkali solution (calculated to produce excess base in mixing
chamber when completely added) to Sample Addition Funnel. Carefully
open the Sample Addition Stopcock and allow alkali to slowly flow into
the Mixing Chamber. Stop flow if “neutralizing action” becomes too
vigorous or causes receiving solution to syphon backward. Continue
intermittent addition of alkali to Mixing 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 subsequent 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 Sample Addition Funnel to act as a liquid seal
during each distillation. If foaming is a problem during distillation, add 1
or 2 drops of anti-foam reagent.
(11) Allow distillation to proceed. The average time of distilling is 5-10
minutes.
(12) Lower the Flask Shelf and allow distillation to continue approximately one
minute.
(13) Place the Receiving Flask aside. It is now ready for titration.
(14) Place an additional flask on Flask Shelf. Open the Aspirator Stopcock to
“drain out” the mixing chamber. Open Sample Addition Stopcock to allow
any remaining liquid to pass into the Mixing Chamber. Close the Sample
Addition Stopcock. Drain fluids by opening the Aspirator Stopcock.
Follow with several good rinses of ammonia-free distilled water. Add rinse
water through the Sample Addition Funnel; closing the Sample Addition
Stopcock and aspirating the rinse solution to the drain.
NOTE: Close the Aspirator Stopcock before addition of each rinse.
The RapidStill I is ready to process the next sample.
NOTE: If long delays are encountered between sample runs, rinse the
Mixing Chamber with distilled or deionized water prior to new sample
distillation.

Chapter 3: Normal Operation
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Shutdown
(1) Turn OFF Heater with the Power Switch.
(2) Remove the Receiving Flask.
(3) Rinse the Mixing Chamber thoroughly, leaving it about ½ full (10 to
12 ml –refer to Step 14 of Start-up and Operation).
(4) Turn off cooling water source to the Condenser.
Calculations
Standard acid to add to receiving flask (ml) =
(% nitrogen expected in sample) x (sample aliquot taken x g sample weight) + 2
(normality of standard acid) x 1.4007 x 250
%Nitrogen = (ml std acid x normality –(ml std base x normality) x 1.4007
effective weight
%Protein = (ml std acid x normality –(ml std base x normality) x 1.4007 x factor
effective sample weight
where:
effective sample weight = weight of sample in grams x sample aliquot
250
Factor = wheat 5.70
milk 6.38
rice 5.95
all other 6.25
NOTE: Labconco recommends the use of this method with the Labconco
RapidStill I. However, alternative methods may be readily adapted to the
apparatus.

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Ro ou ut ti in ne e M Ma ai in nt te en na an nc ce e
Glass Still (Replacement)
(1) Disconnect the Power Cord from the outlet before performing any service
work.
(2) Remove Heater assembly by unplugging it and remove stopper from flask.
(3) Disconnect ALL tubing connections on glass still.
(4) Lay the Base Housing down on its back.
(5) Remove U-clamp nuts and bolts (3).
(6) Lift still assembly from Base Housing and lay carefully aside.
(7) Remount new glass still assembly and reconnect all parts and tubing, by
reversing above steps.

Chapter 4: Routine Maintenance
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Stopcock
The Labconco RapidStill I is equipped with two 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 particles 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.
When alkalis or other liquids corrosive to glass are used in PTFE-glass stopcock
valve assemblies, rinse all valve components thoroughly with water after each use.
Roughness of the glass barrel due to liquid concentrate formed on evaporation may
score the plug. Additional information is provided with this unit and may be
referred to for service.

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Re ep pl la ac ce em me en nt t P Pa ar rt ts s
ITEM
PART
NUMBER
DESCRICPTION
1
6500100
Glass Still Assembly with PTFE stopcocks
2
1352500
PTFE plug replacements for PTFE stopcock
3
6507700
Heat Controller
4
1876500
Knob, for Heat Controller
5
1327000
Power Switch
6
1331300
Power Cord, 115V
7
1327200
Circuit Breaker, 3 amp
8
6506900
Shelf for Receiving Flask
9
6504201
Heater assembly, complete with stopper and male plug;
115 VAC, 280 Watts
10
6507200
Large U-Clamp bolt (1 required)
11
6507100
Small U-Clamp bolt (2 required)
12
6507500
Nuts, for U-Clamps (6 required)
13
1624400
Tubing for U-Clamps (1/4” ID)
14
1355400
Fill Valve
15
1317400
Transformer (230 V to 115 V, 50/60 Hz, 300 Watt)
16
6507600
Water Bottle
17
1625000
Tubing for water outlet (3/8" ID) (6" required)
18
6523100
Tubing for water inlet (12mm ID) (9" required)

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Wi ir ri in ng g D Di ia ag gr ra am m