Apparatus for performing a plurality of distillation and reflux operations simultaneously within a compact space

A mini-distillation and reflux system, kit and method in which a heating and glassware arrangement includes a heat source in contact with a heater block having apertures in its top surface for housing boiling tubes upright during a distillation or reflux operation. The boiling tubes contain sample and are for attachment of various configurations of glassware assemblies made up of individual, interchangeably connectable glassware pieces so assembled to perform different types of distillations and refluxes. The glassware pieces are of a scaled down size so that numerous distillations and refluxes can be performed simultaneously at a single heat source within a compact space to consume less laboratory space. The scaled down size of the glassware pieces also allows the boiling tubes and attached glassware assemblies to be housed freestandingly within the heater block apertures thus eliminating the time-consuming set-up of bulky support apparatus formerly necessary to support glassware assemblies above boiling receptacles in conventional distillations and refluxes.

FIELD OF THE INVENTION 
The present invention relates generally to apparatus for performing 
distillations and refluxes and more particularly, to an easily convertible 
miniaturized distillation and reflux system and kit for performing 
laboratory distillations and refluxes. 
BACKGROUND OF THE INVENTION 
Distillation and reflux are common chemical laboratory processes to prepare 
a substance for analysis or a subsequent chemical process. 
The distillation process includes the steps of turning a substance in a 
liquid matrix into a vapor, cooling the vapor to condense it and 
collecting the resulting condensed liquid in order to separate the analyte 
of interest from its original matrix. Distillations are often carried out 
under specific temperatures to allow separation of compounds by their 
boiling point differences. Two common variations on the basic distillation 
process are often used. The first variation includes introducing an inert 
gas such as nitrogen or helium into the distillation apparatus to avoid 
atmospheric contamination or reacting the distilled compounds with 
atmospheric components during distillation. A second variation includes 
generating a gas from a heated liquid and collecting the evolved gas as it 
bubbles through an absorbing solution. 
Reflux is the process of heating a substance in a liquid matrix to boiling 
to generate a vapor, continuously, condensing the vapor and returning the 
condensed vapor to the boiling liquid matrix. Refluxing is often necessary 
for chemical reactions that require elevated temperatures for long periods 
of time to reach completion. Refluxing allows prolonged heating of the 
sample without significant loss of original liquid matrix volume due to 
evaporation. Refluxed chemical reactions may also require the slow 
addition of a reagent during the reflux process to allow completion of 
specific chemical reactions. 
Distillation and reflux processes have applications in both 
industrial-scale chemical production as well as bench-scale laboratory 
uses. With respect to bench-scale laboratory applications, standard 
procedures have developed for performing either the particular type of 
distillation necessary to remove the analyte of interest from the sample 
or the particular type of reflux necessary to chemically process the 
analyte of interest. For analytes such as cyanide, phenolic compounds, 
ammonia, hydrogen fluoride, volatile acids, sulfides and sulfites, to be 
removed from sample by distillation or chemically processed by refluxing, 
according to the standard procedures, a complicated, time-consuming 
distillation or reflux process is required which uses low-throughput, 
large volume, manual distillation or reflux apparatus including expensive, 
fragile, large glassware components that are not interchangeable between 
distillation or reflux methods. 
The current state of the art is illustrated in FIGS. 1-5 which show prior 
art laboratory distillation and reflux apparatus. The prior art apparatus 
of FIGS. 1-5 disclose distillation and reflux glassware which is bulky and 
cumbersome due to the use of large boiling flasks. The large boiling 
flasks require correspondingly large glassware components which are 
expensive, fragile, and which require support apparatus such as rings, 
clamps, ring stands and lattice to support the glassware components above 
the boiling flasks. FIGS. 1-5 further illustrate that conventional large 
boiling flasks typically have one to three inlet necks for placing the 
sample and reagents in the flask and for attaching the other glassware 
pieces required to perform various distillations and refluxes, with the 
particular distillation or reflux method being performed dictating the 
type of multi-necked flask to be used. The different types of multi-necked 
boiling flasks each require specialized glassware components for 
connection only to that particular boiling flask such that glassware 
components are not interchangeable between distillation and reflux 
methods. 
In use, the prior art distillation or reflux apparatus shown in FIGS. 1-5 
typically require numerous hours for completion of the distillation or 
reflux process due to the lengthy assembly, disassembly and cleaning of 
the glassware. The large boiling flasks of prior art distillation or 
reflux apparatus typically require as much as 500 to 1000 mL of sample and 
such large sample sizes require correspondingly large volumes of costly 
reagent. 
Each large boiling flask also requires a separate heating mantle, thereby 
consuming a lot of precious laboratory bench space. Since the boiling 
flasks often have irregular contact with the heating mantle, variable 
heating and generation of considerable waste heat during use often 
results. The heating mantles often become covered with reagent due to 
reagent spillovers onto the heating mantles causing the heating mantles to 
smoke during use. A support apparatus is required to hold the boiling 
flasks to the heating mantle while a second support apparatus is often 
required to support and distribute condenser water and gas or vacuum hoses 
to the distillation or reflux glassware with both supports requiring much 
lab space and set-up time. 
U.S. Pat. No. 5,022,967 to Stieg discloses microdistillation apparatus 
which includes a plastic digestion tube within a micro-distillation column 
that is meant to be disposable after use. The apparatus uses a hydrophobic 
membrane in place of a conventional glass, cold water condenser and thus 
does not preserve the original distillation mechanism of the conventional 
glass, distillation glassware specified in standard distillation 
procedure. Further, the plastic fabrication of the micro-distillation 
column makes it unsuitable for use with organic solvents. 
Thus, a need exists for laboratory distillation and reflux apparatus in 
which miniaturized glassware receptacles and components are used to 
perform distillations or refluxes of numerous smaller sample volumes, 
i.e., those in the 10 to 50 mL range, simultaneously at a single heat 
source. 
A need also exists for laboratory distillation and reflux apparatus which 
includes glassware components that are interchangeable between 
distillation and reflux methods. 
Still another need exists for laboratory distillation and reflux apparatus 
which includes glassware capable of being free-standing in the heating 
apparatus so as to eliminate the need for bulky support lattices and 
cumbersome heating mantles for each distillation or reflux which consumes 
precious laboratory space. 
It would therefore be advantageous to scale down the glassware and heating 
arrangements of conventional distillation and reflux apparatus into a more 
compactly sized distillation and reflux system which allows numerous 
distillations and refluxes to take place simultaneously at a single heat 
source. The present invention provides an easily convertible 
mini-distillation and reflux system which includes scaled-down glassware 
pieces for connection to a boiling tube to be inserted into apertures of a 
heater block capable of holding glassware upright and freestanding in 
order to distill or reflux numerous samples simultaneously at a single 
heat source. 
One advantage of the mini-distillation and reflux system of the present 
invention is that less laboratory bench space is required for 
distillations since numerous distillations can take place simultaneously 
within a compact space at a single heat source. 
Another advantage of the mini-distillation and reflux system of the present 
invention is that the less bulky, miniaturized glassware is free-standing 
within a heater block to thus eliminate the need for support apparatus. 
Still another advantage of the mini-distillation and reflux system of the 
present invention is that the assembly of both the miniaturized system and 
of the miniaturized glassware pieces is quicker and easier due to its 
smaller size. Thus, time and labor expenses, glassware breakage and 
replacement costs are all decreased. 
Still another advantage of the mini-distillation and reflux system of the 
present invention is the use of a tubing distribution panel for delivery 
of condenser water and inert gases or vacuum to each glassware apparatus. 
The tubing distribution panel allows for quick, easy assembly of 
distillation and reflux equipment by eliminating bulky hose connectors and 
support lattice for hoses and tubing to decrease time and labor expenses. 
Still another advantage of the mini-distillation system of the present 
invention is that less sample volume and reagents are required resulting 
in reduction in chemical and waste disposal costs. 
Still another advantage of the mini-distillation and reflux system of the 
present invention is that a single heat source for multiple apparatus 
requires access to fewer electrical outlets and use of a low wattage 
single heat source results in decreased electrical operating costs. 
The mini-distillation and reflux system of the present invention provides a 
distillation and reflux system that incorporates all of the advantages of 
a compactly sized system with interchangeable parts while allowing the 
scaled down interchangeable glassware to function in the same manner as 
the conventional glassware, thus preserving the chemical distillation and 
reflux mechanism of the original, conventional glassware specified in 
standardized distillation or reflux methods. The system further provides a 
major innovation by allowing a single inlet or one-necked boiling tube to 
replace the large volume, multi-necked boiling flasks of conventional 
distillation apparatus while functioning in the same manner as the one-, 
two-, or three-necked boiling flasks of the prior art. 
SUMMARY OF THE INVENTION 
The present invention provides a mini-distillation and reflux system in 
which a scaled down heating and glassware arrangement includes a heat 
source in contact with a heater block and glassware assemblies attached to 
boiling tube are held upright in apertures in the heater block. The 
glassware assemblies are made up of individual, interchangeable glassware 
pieces to form various configurations for performing different types of 
distillations and refluxes. The scaled down glassware pieces are capable 
of functioning in the same manner as conventional distillation glassware 
thereby preserving the chemical distillation and reflux mechanism of the 
original, conventional glassware specified in standardized distillation or 
reflux procedure. A tubing distribution panel may be included as needed 
for attachment of condenser water, vacuum or gas source to the glassware 
assemblies via hose or flexible tubing. A mini-distillation and reflux kit 
includes a heat source, a heater block, at least sixteen interchangeably 
connectable glassware pieces capable of forming at least nine glassware 
assemblies for performing different types of distillations and refluxes, 
and a tubing distribution arrangement. 
A method for performing distillations or refluxes includes using 
miniaturized glassware to form glassware assemblies for attachment to 
boiling tubes for insertion into apertures of a heater block in contact 
with a heat source so that the boiling tubes and glassware assembly 
arrangements are free-standing during a distillation or reflux in order 
for numerous distillations or refluxes to be performed simultaneously at a 
single heat source.

DETAILED DESCRIPTION OF THE INVENTION 
Referring to FIG. 6, in a preferred embodiment of the present invention, a 
mini-distillation and reflux system and kit 10 is shown with insertable 
glassware removed for clarity. A heat source 12 is shown positioned under 
and in contact with a heater block 14. The heat source 12 of the preferred 
embodiment of the invention is shown in FIG. 6 as two conventional hot 
plates such as those sold by Corning Glass Corporation, Model No. PC-300, 
having an electrical rating of 120 VAC, 575 watts, however, any heat 
source capable of supplying equivalent power could be used without 
departing from the spirit or scope of the invention. 
With reference to FIGS. 7, 8 and 9, the heater block 14 of the preferred 
embodiment is shown having an inverted T-shaped cross-section 16 
throughout the length 18 of the heater block 14. The inverted T-shaped 
cross-section of the heater block 14 allows the heater block 14 to have a 
rectangular bottom surface 20 which is larger in area than the rectangular 
top surface 22. A heater block 14 with a bottom surface 20 of larger 
surface area than the top surface 22 is primarily to provide stability for 
the heater block 14 against tipping over and also for providing a larger 
surface area to contact the heat source 12. Thus, the heater block 14 is 
not limited to an inverted T-shaped cross-section. Both a rectangular 
cross-section and a cross-section in the shape of an Erlenmeyer flask, 
i.e., rectangular top and partial triangular bottom cross-section, have 
been contemplated for the heater block 14. 
In the preferred embodiment, the rectangular top surface 22 of the heater 
block 14 contains eight large circular apertures 24 and four small 
circular apertures 24. FIG. 7 illustrates that the large apertures 24: are 
approximately one-inch in diameter, are evenly spaced across the 
approximately fifteen-inch length of the heater block 14 and are 
centerline along a lengthwise centerline of the heater block 14. The small 
apertures 26 are approximately one-fourth of an inch in diameter, are 
spaced in the length direction of the heater block 14 to be halfway 
inbetween the second and third large apertures 24 from either end of the 
heater block 14, and are spaced in the width equidistant from the 
lengthwise centerline so that the small aperture's circumference is 
tangent to a line tangent to the large aperture's circumference. The 
number and positioning of the large and small apertures, as described in 
accordance with the preferred embodiment, does not limit the invention and 
any number of large and small apertures may be positioned in any manner 
that facilitates the performance of distillation and reflux processes. 
FIGS. 6, 8, and 9 illustrate that the large and small apertures 24, 26 have 
a U-shaped cross-section throughout the depth of the heater block 14. In 
other words, the length of the U-shaped cross-section of large and small 
apertures 24, 26 is less than the distance between the rectangular top 
surface 22 of the heater block 14 and the rectangular bottom surface 20 of 
the heater block 14 so that the apertures do not pierce the heater block 
in order for the large apertures 24 to be capable of holding boiling tubes 
and the small apertures 26 to be capable of holding thermometers. The 
shape of the large and small apertures is not limited and apertures of any 
shape capable of holding boiling tubes and thermometers may be used. 
The heater block 14 has an inverted T-shaped right side surface 28 and an 
inverted T-shaped left side surface 30 such that each surface 28, 30 has a 
handle 32 attached to the upper leg of the inverted T-shaped surface. The 
heater block 14 has a rectangular front upper surface 34, a rectangular 
front lower surface 36, a rectangular back upper surface 38, a rectangular 
back lower surface 40, and back and front rectangular shelves 42, 44. Two 
T-shaped aluminum supports 46 are attached to the back lower surface 40 of 
the heater block 14 by bolts 48 through the crossbars 50 of the T-shaped 
supports 46 to hold the crossbars 50 against the back lower surface 40 of 
the heater block 14. The legs 52 of the T-shaped supports 46 have 
cylindrical apertures 54 through the T-shaped supports' thickness for 
holding a support rod 56 upright as shown in FIG. 6 in order to support a 
tubing distribution panel 58. 
The heater block 14 is preferably made of aluminum, however, any material 
having heat-conductive properties in order to conduct heat from the hot 
plates in contact with the heater block to the boiling tubes to be placed 
in the apertures of the heater block, could be used. 
Referring again to FIG. 6, a tubing distribution panel 58 is shown 
supported above the heater block 14 on two support rods 56 inserted 
through the cylindrical apertures 54 of the legs 52 of the T-shaped 
supports 46 attached to the back lower surface 40 of the heater block 14. 
In the preferred embodiment of the invention, the tubing distribution 
panel 58 includes two condenser water hose support apertures 60, 62 
located on opposing lower left- and right-hand corners of the panel 58 
through which condenser water inlet and outlet hoses 64, 66 are threaded. 
Condenser water inlet hose 64 is threaded through aperture 60 on the left 
side of panel 58 and leads from a condenser water source 68 for connection 
to the first glassware assembly. Condenser water outlet hose 66 is 
threaded through aperture 62 for connection to a last glassware assembly 
and leads to a drain or collector 70. The condenser water inlet and outlet 
hoses 64, 66 are constructed and arranged so as to be connected in series 
for flowing condenser water through the glassware apparatus inserted in 
the heater block 14 as needed to perform various types of distillations 
and refluxes. The tubing distribution panel 58 further includes a main 
channel 71 leading from a gas or vacuum source 72 to eight valves 74, each 
valve 74 for connection, as needed, to one of the glassware apparatus 
inserted in the heater block 14 via vacuum or gas hoses 76. 
In the preferred embodiment of the invention, sixteen glassware pieces as 
shown in FIGS. 10-25 are capable of forming nine glassware assemblies as 
shown in FIGS. 26-34, although the number of glassware pieces and 
assemblies does not limit the invention since it is contemplated that as 
many glassware pieces and assemblies as needed to perform varying 
distillations and refluxes may be incorporated. 
The glassware pieces are of a scaled down size in order to be 
interchangeably connectable to each other for ultimate connection of the 
assembled glassware pieces to a boiling tube 78 as shown in FIG. 10. The 
boiling tube 78 has one inlet or neck and is capable of holding up to a 
50-mL volume of sample. The boiling tubes may be inserted into the large 
apertures 24 through the top surface 22 of the heater block 14 after 
attachment of a glassware assembly in order to perform various types of 
distillations and refluxes. 
FIG. 11 illustrates a reagent tube inlet adapter 80 which is a glassware 
piece specially designed to be attached to a boiling tube 78 as shown in 
FIG. 10 in order to allow the boiling tube to function as a two-necked 
flask. The adapter 80 allows for air flow and addition of reagents through 
the funnel-shaped inlet 82 attached to a long z-shaped inlet tube 84 which 
extends to the bottom of the boiling tube 78 when the adapter 80 is 
inserted into the boiling tube 78. 
FIGS. 12 and 13 illustrate a cold finger condenser jacket 86 and cold 
finger condenser 88, respectively. The condenser 88 includes a cold finger 
90 through which condenser water flows. The condenser 88 is surrounded by 
the jacket 86 so that when the condenser 88 condenses vapor, the 
condensate drips back into the boiling tube 78, while gases enclosed by 
the jacket 86 are allowed to proceed to the next attached glassware piece. 
FIGS. 14, 15 and 23 illustrate a first bubbler 92, bubbler vessel 94 and 
second bubbler 96, respectively, which can be connected in series to first 
bubbler 92. Air and generated gases enter the bubbler 92 and proceed to 
flow through a short glass tube 98 which terminates as a glass frit 100 or 
impinged tube bottom. The frit 100 allows gases to be discharged as fine 
bubbles into a solution contained in the bubbler vessel 94. The bubbler 92 
includes a vacuum inlet stem 102 to which a vacuum source or second 
bubbler 96 may be attached. 
FIGS. 16 and 24 illustrate a sloped T-joint 104 and sloped T-joint with gas 
bubbler 106, respectively. Both sloped T-joint 104 and sloped T-joint with 
gas bubbler 106 are for connection to a boiling tube 78. The sloped 
T-joint 104 is attached to a condenser so that the downward slope of the 
T-joint arm 108 allows vapor to condense on the sloped T-joint 104 and 
flow down into the condenser rather than back to the boiling tube 78. The 
sloped T-joint with gas bubbler 106 functions in the same way as the 
sloped T-joint 104: except that an inert gas is introduced into the 
T-joint with gas bubbler 106 and exits the bottom of the bubbler stem 110 
which extends to the bottom of the boiling tube 78. The bubbling action 
agitates the heated sample. Thus, the sloped T-joint with gas bubbler 106 
when attached to the boiling tube 78 allows the boiling tube 78 to have 
two inlets and to act in a manner similar to a two-necked flask of the 
prior art. 
FIGS. 17 and 18 illustrate a stopper 112 and gas inlet 114, respectively. 
Both the stopper 112 and gas inlet 114 seal the top of a sloped T-joint 
104, however, the stopper 112 does so to allow vapor to travel down the 
sloped arm 108 of the T-joint 104 rather than escape, whereas the gas 
inlet 114 allows introduction of an inert gas at the top of the T-joint 
104. 
FIGS. 19 and 20 illustrate a mini-Graham condenser 116 and condenser stem 
118. The mini-Graham condenser 116 functions to condense vapors in a 
coiled glass tube 120 encased in a jacket 122 of cold water. The condensed 
distillate exits through the bottom of the condenser 116 to the condenser 
stem 118 which is submerged in a solution contained in a collection vessel 
(not shown). 
FIG. 21 illustrates a Y-shaped adapter 124 having a main tubular section 
and a tubular exit port 126 which connects to a boiling tube 78 to allow 
the one-necked boiling tube 78 to function as a multi-necked flask. The 
adapter 124 includes a long z-shaped gas inlet stem 84 having a crimped 
stem on an upper end where a source of inert gas may be applied. The 
bottom of the z-shaped inlet stem 84 is not crimped and extends almost to 
the bottom of the boiling tube 78 where the flow of bubbles exiting the 
inlet stem 84 serves to agitate and purge the boiling tube contents with 
inert gas. The port 126 is sloped upward to form a Y with the adapter 124 
and to assist condensed vapors forming on the walls of the adapter 124 to 
drip back down into the boiling tube 78. 
FIG. 22 illustrates a side arm addition funnel 130. Inert gas flow may be 
introduced at the top of the funnel 130. Liquid reagents are held in the 
funnel 130 by a stopcock 132 which when opened allows the reagent to flow 
downward. The side arm addition funnel 130 allows inert gas flow to bypass 
the stopcock 132 thus permitting gas flow to continue through the side arm 
128 even when the stopcock 132 is closed. 
FIG. 25 illustrates a joint reducer 134 which connects a boiling tube 78 to 
another glassware piece such as a mini-Graham condenser 116 or a side arm 
addition funnel 130. 
FIGS. 26-29 show four embodiments of a first glassware assembly 136 for 
performing a basic distillation and made up of a mini-Graham condenser 
1.16 attached to a sloped T-joint 104 which in turn is attached to the 
boiling tube 78. A first embodiment of the first glassware assembly 136 as 
shown in FIG. 26 also includes a stopper 112. The first embodiment is used 
to distill liquid samples under atmospheric conditions where the vapors 
generated in the heated boiling tube 78 are condensed in a mini-Graham 
condenser 116 and the condensed liquid distillate is collected in an open 
collection vessel (not shown). 
A second embodiment of the first glassware assembly 136 is shown in FIG. 27 
which in addition to the components of the first embodiment in FIG. 26 
includes a condenser stem 118. The second embodiment is used to distill 
liquid samples under atmospheric conditions in a manner similar to the 
first embodiment except that the second embodiment is used to collect 
distillates that require immediate chemical stabilization or preservation. 
The generated sample vapors are condensed in a mini-Graham condenser 116. 
The condensed liquid distillate drips down an extender tube 138 and is 
collected in a preservative solution contained in a collection vessel (not 
shown). The extender tube 138 is submerged in the preservative solution. 
A third embodiment of the first glassware assembly 136 is shown in FIG. 28 
which is similar to the second embodiment shown in FIG. 27 but replaces 
the stopper 112 with a gas inlet 114. The third embodiment is used to 
distill liquid samples in a manner similar to the first embodiment except 
that the third embodiment is used to collect distillates that require 
distillation under an inert gas atmosphere and also require immediate 
chemical stabilization or preservation. An inert gas is introduced into 
the top of the T-joint 104 via gas inlet 114. The generated sample vapors 
are condensed in a mini-Graham condenser 116. The condensed liquid 
distillate drips down an extender tube 138 and is collected in a 
preservative solution contained in a collection vessel (not shown). The 
extender tube 138 is submerged in the preservative solution. 
A fourth embodiment of the first glassware assembly 136 is shown in FIG. 29 
as similar to the second embodiment shown in FIG. 27 including the stopper 
112 and the condenser stem 118 but in addition replaces T-joint 104 with 
T-joint with gas bubbler 106, with the bubbler stem 110 extending down 
into the boiling tube 78. The fourth embodiment is used to distill liquid 
samples in a manner similar to that of the first embodiment except that 
the fourth embodiment is used to distill samples that require agitation or 
mixing of the boiling tube contents during the distillation. An inert gas 
is introduced into the T-joint with gas bubbler 106 at the top of the 
bubbler stem 110 and exits the bottom of the bubbler stem 110 which 
extends to the bottom of the boiling tube 78. The bubbling action agitates 
the heated sample and replaces the magnetic stirring often used for 
conventional distillations. The generated sample vapors are condensed in a 
mini-Graham condenser 116 and the condensed liquid distillate is collected 
in an open collection vessel (not shown). If the distillate requires 
immediate chemical stabilization or preservation, the fourth embodiment 
can also use the condenser stem 118. If the condenser stem 118 is used, 
the condensed liquid distillate drips down an extender tube 138 and is 
collected in a preservative solution contained in a collection vessel (not 
shown). The extender tube 138 is submerged in the preservative solution. 
A second glassware assembly 140 having two embodiments as shown in FIGS. 30 
and 31 is used for gas evolution distillation. FIG. 30 shows a first 
embodiment having a reagent inlet tube adapter 80 connecting a boiling 
tube 78 to a cold finger condenser jacket 86 and also serves as the inlet 
for air flow and adding reagents since the inlet's funnel shape 82 
accommodates pouring of reagents. The cold finger condenser 88 is 
surrounded by a jacket 86. The exit port 142 of the cold finger condenser 
jacket 86 is attached to a bubbler 92. The bubbler 92 is contained in a 
bubbler vessel 94 and has a vacuum inlet stem 102 which may be attached in 
series to a second bubbler 96. 
The first embodiment is used to distill a liquid matrix sample and collect 
gases that are generated during the distillation process. The distillation 
is carried out under a flow of air created by a vacuum applied to the 
vacuum inlet stem 102 of the bubbler 92 of the second glassware assembly 
140. The liquid sample and distillation reagents are heated in the boiling 
tube 78 where both gases and vapors are generated. The gases and vapors 
are carried by a flow of air through a cold finger condenser jacket 86 
where vapors are condensed by the cold finger condenser 88 and drip down 
into the boiling tube 78. The gases are not condensed and flow forward 
through a bubbler 92 and bubbler vessel 94 containing a solution to 
chemically trap and retain the gas species. A second bubbler 96 can be 
attached in series with the first bubbler 92 to allow greater chemical 
trapping capacity of gases and different trapping solutions can be placed 
in each bubbler vessel 94 to selectively trap or remove different gases. 
A second embodiment of the second glassware assembly 140 is shown in FIG. 
31. An inlet adapter 124 connects a boiling tube 78 to a side arm addition 
funnel 130 and to a first bubbler 92. The bubbler 92 is contained in a 
bubbler vessel 94 and has a vacuum inlet stem 102 which may be attached in 
series to a second bubbler 96. The inlet adapter 124 includes a long gas 
inlet stem 84 and the side arm addition funnel 130 includes a gas inlet 
114. 
The second embodiment is used to generate and collect gases under inert gas 
flow without the use of a cold finger condenser 88 and jacket 86. The use 
of a side arm addition funnel 130 allows the addition of reagents from the 
funnel 130 to the sealed apparatus while maintaining inert gas flow 
throughout the second glassware assembly 140. The liquid sample is placed 
in the boiling tube 78 and the liquid reagent is placed in the side arm 
addition funnel 130. The second glassware assembly 140 is sealed and inert 
gas flow is introduced at the top of the side arm addition funnel 130 via 
a gas inlet 114 and at the top of the gas inlet stem 84 of inlet adapter 
124. The reagent is released from the side arm addition funnel 130 into 
the heated boiling tube contents. The inert gas, and gases and vapors 
generated from the sample, flow forward through the inlet adapter 124 to a 
bubbler 92 and bubbler vessel 94 containing a solution to chemically trap 
and retain the gas species. A second bubbler 96 can be attached in series 
to first bubbler 92 to allow greater chemical trapping capacity of gases 
or different trapping solutions can be placed in each bubbler vessel 94 to 
selectively trap or remove different gases. 
A third glassware assembly 144 having three embodiments as shown in FIGS. 
32-34 is used for refluxing and digestion processes. FIG. 32 shows a first 
embodiment having a joint reducer 134 connecting a boiling tube 78 to 
mini-Graham condenser 116. The first embodiment operates as a basic reflux 
apparatus by having liquid contents placed in the boiling tube 78 heated 
to boiling such that the generated vapors rise to the condenser 116. The 
vapors are condensed in the condenser 116 and the liquid condensate drips 
from the condenser 116 and returns to the boiling tube 78. 
FIG. 33 shows a second embodiment similar to the first embodiment of FIG. 
32, but incorporating a side arm addition funnel 130 attached to the top 
of mini-Graham condenser 116. The second embodiment refluxes sample in a 
manner similar to the first embodiment of the third glassware assembly 144 
but allows addition of a reagent solution held in the funnel 130 during 
the reflux process. Reagent solution is placed in the funnel 130 and 
liquid sample is placed in boiling tube 78. The glassware assembly is then 
attached to the boiling tube 78 and the boiling tube contents are heated 
to boiling. The generated vapors rise to the condenser 116 connected to 
the top of the boiling tube 78. The vapors are condensed in the condenser 
116 such that the liquid condensate drips from the condenser 116 and 
returns to the boiling tube 78. A side arm addition funnel 130 connected 
to the top of the condenser 11.6 allows a liquid reagent to be dispensed 
through the condenser 116 and into the refluxing contents of the boiling 
tube 78. The stopcock 132 of the sidearm addition funnel 130 can be 
adjusted to allow a slow addition of reagent over time. 
FIG. 34 shows a third embodiment in which a joint reducer 134 connects a 
boiling tube 78 to a side arm addition funnel 130. The third embodiment 
allows heated chemical digestion of samples that do not require refluxing. 
Digestion reagent is placed in the side arm addition funnel 130. Sample is 
placed in boiling tube 78 and the sidearm addition funnel 130 is connected 
to the top of the boiling tube 78. Sample is heated and digestion reagent 
is dispensed into the boiling tube 78 at a desired rate. 
In operation, the mini-distillation and reflux systems works as follows. 
Sample is prepared and placed in a boiling tube 78. The correct glassware 
assembly for the appropriate type of distillation or reflux to be 
performed is chosen and connected to the boiling tube 78. For those 
glassware assemblies having hanging glassware pieces, most notably the 
bubblers, which could tend to become disconnected from the glassware 
assemblies due to the weight of the collected liquids, plastic clips such 
as Keck clips, patent pending, or spring clamps may be used to more 
securely attach the glassware pieces to the assemblies. 
The boiling tube 78 with the attached glassware assembly is then placed in 
one of the large apertures 24 of the heater block 14 and thus becomes 
free-standing during the performance of the distillation or reflux. 
Depending upon the particular type of distillation or reflux to be 
performed, the vacuum or gas hoses 76 and/or the condenser water hoses 64, 
66 may be connected to the glassware assemblies 136, 140, 144. The inert 
gas or vacuum and/or the condenser water is then applied to the assembly 
as dictated by distillation or reflux method. 
The heat source 12 is turned on to the appropriate temperature for the 
particular type of distillation or reflux to be carried out. The heat 
source 12 is in contact with the heater block 14 and warms the heater 
block 14 through conduction. The heater block 14 in turn warms the boiler 
tube 78 and its contents. 
The forms of the invention shown and described in this disclosure represent 
illustrative preferred embodiments thereof. It is understood that the 
invention is defined in the claimed subject matter which follows and that 
various modifications in light of reading the description are incorporated 
therein.