U.S. patent number 3,841,835 [Application Number 05/228,581] was granted by the patent office on 1974-10-15 for means for providing an information signal of sample introduction in apparatus for chemical analysis.
This patent grant is currently assigned to Yanagimoto Seisakusho Co., Ltd.. Invention is credited to Joji Fujimoto, Yasuhiko Inagaki, Kenichi Kishimoto, Hiroshi Miyauchi.
United States Patent |
3,841,835 |
Kishimoto , et al. |
October 15, 1974 |
MEANS FOR PROVIDING AN INFORMATION SIGNAL OF SAMPLE INTRODUCTION IN
APPARATUS FOR CHEMICAL ANALYSIS
Abstract
In apparatus for chemical analysis in which a sample to be
analyzed is injected to a sample introduction section of said
apparatus by means of a syringe having an injection needle which
pierces an elastic plug covering a sample introduction opening
formed in said sample introduction section, the improved means for
providing an information signal of sample introduction comprises a
movable member engageable with said syringe when a sample is
injected by said syringe to said sample introduction section, a
stationary member cooperating with said movable member, an
electrical switch which is closed and opened in response to the
relative movement between said movable member and said stationary
member, and an electrical circuit including said electrical switch
and means for providing an electrical signal for the sample
introduction so that the sample introduction time is automatically
detected and the information signal of sample introduction is
transmitted to a recorder or computer.
Inventors: |
Kishimoto; Kenichi (Osaka,
JA), Miyauchi; Hiroshi (Kyoto, JA),
Inagaki; Yasuhiko (Kyoto, JA), Fujimoto; Joji
(Kyoto, JA) |
Assignee: |
Yanagimoto Seisakusho Co., Ltd.
(Kyoto, JA)
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Family
ID: |
27519306 |
Appl.
No.: |
05/228,581 |
Filed: |
February 23, 1972 |
Related U.S. Patent Documents
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Application
Number |
Filing Date |
Patent Number |
Issue Date |
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161447 |
Jul 12, 1971 |
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Foreign Application Priority Data
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Feb 24, 1971 [JA] |
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46-11624 |
Jul 15, 1970 [JA] |
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45-61881 |
Mar 31, 1971 [JA] |
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46-23853 |
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Current U.S.
Class: |
422/119; 422/547;
73/864.86; 141/329; 422/70; 422/89; 436/55 |
Current CPC
Class: |
G01N
35/1079 (20130101); Y10T 436/12 (20150115) |
Current International
Class: |
G01N
1/00 (20060101); G01n 001/14 (); B65b 001/04 () |
Field of
Search: |
;23/232C,253,254,230,259
;73/425.6,23.1,422GC ;141/329 |
References Cited
[Referenced By]
U.S. Patent Documents
Primary Examiner: Serwin; R. E.
Attorney, Agent or Firm: Morgan, Finnegan, Durham &
Pine
Parent Case Text
CROSS-REFERENCE TO RELATED APPLICATION
This application is a continuation-in-part of co-pending
Application Ser. No. 161,447 filed July 12, 1971, now abandoned,
for APPARATUS FOR CHEMICAL ANALYSIS.
Claims
What we claim is:
1. Apparatus for providing a signal indicating introduction of a
sample to be analyzed into a sample introduction section of a
sample analyzing system by a syringe having an injection needle
which punctures a plug covering the opening of the sample
introduction section, comprising:
a first member positioned adjacent the sample introduction opening
for engagement and movement with the syringe when a sample is
injected into the sample introduction section;
a second member engageable by said first movable member; and
means for producing an output signal in response to engagement of
said second member by said first member.
2. Apparatus as claimed in claim 1 wherein:
said first and second members form a normally open switch which is
closed upon engagement of said first member with said second
member.
3. Apparatus as claimed in claim 2 wherein:
said second member is a metal cap which overlies the plug and
includes an aperture to receive the needle.
4. Apparatus as claimed in claim 3 wherein:
said first member includes an aperture axially aligned with said
aperture of said second member to receive the needle.
5. Apparatus as claimed in claim 4 wherein:
said first member is supported by a flexible shank.
6. Apparatus as claimed in claim 1 wherein:
said second member is a normally open microswitch which is closed
upon engagement by said first member.
7. Apparatus as claimed in claim 6 wherein:
said first and second members are mechanically coupled to a
rotatable member for reorientation for use with another sample
introduction section.
8. Apparatus as claimed in claim 2 wherein:
said output signal producing means includes a flip-flop
electrically coupled to said switch; and
a recorder electrically coupled to said flip-flop.
9. Apparatus as claimed in claim 2 wherein:
said output signal producing means includes a relay electrically
coupled to said switch; and
a recorder electrically coupled to said relay.
10. Apparatus as claimed in claim 1 including:
detection means responsive to said output signal producing means
for detecting sample information;
data processing means;
means for inhibiting the operation of said data processing means;
and
means for selectively connecting said data processing means to said
detection means and said inhibiting means.
11. Apparatus as claimed in claim 10 including:
a manually operable switch for maintaining an electrical connection
between said output signal producing means and said data processing
means upon disengagement of said first member with said second
member.
12. Apparatus as claimed in claim 1 including:
detection means responsive to said output signal producing means
for detecting sample information;
computer means electrically connected to said detection means.
Description
BACKGROUND OF THE INVENTION
This invention relates to improved means for producing an
information signal of sample introduction in apparatus for chemical
analysis in which a sample to be analyzed is injected to a sample
introduction section of said apparatus by means of an injector or
syringe having an injection needle which pierces an elastic cap or
plug covering a sample introduction opening formed in said sample
introduction section.
In various sample analyzing systems, e.g. in vapor phase or liquid
phase chromatographs, what is directly obtained as a result of
analysis is a chromatogram having at least one peak, usually a
plurality of peaks. The time needed from the time when a sample is
introduced into the analyzing system until a chromatogram peak is
emerged is called the "retention time." This retention time is an
important value for the qualitative analysis of the sample.
Accordingly, the sample introduction time must be exactly recorded
in a recorder of such apparatus for chemical analysis. In the case
of processing the analytic data with a computer, in order to
accurately measure the retention time it is required that the start
of introduction of a sample into the analyzing column of the
chromatograph be in exact synchronism with the start of
memorization or calculation operation in a computer.
In vapor phase chromatographs a vaporizable sample liquid to be
analyzed is usually introduced into a sample introduction section
at the end of analyzing column by injecting it into the sample
introduction section with use of a usual syringe or microsyringe
having an injection needle which pierces a sealing cap or plug,
made of elastic material such as heat-resistant silicon rubber,
which covers a sample introduction opening formed in the sample
introduction section of the column.
The primary object of the invention is to provide new and improved
means for producing an information signal of sample introduction in
apparatus for chemical analysis so that the time of sample
introduction is automatically detected the detected signal is
transmitted to a recorder or computer connected to said apparatus
for chemical analysis.
Another object of the invention is to provide an improved vapor
phase chromatograph in which the retention time of each of the
sample constituent can be accurately determined by a recorder or
computer connected to the vapor phase chromatograph.
A further object of the invention is to provide improved means for
producing an information signal of sample introduction in a vapor
phase chromatograph in which the time of injection of a vaporizable
sample liquid to an analyzing column by a syringe is automatically
detected and an electrical signal for informing the time of sample
introduction is produced and transmitted to a recorder or
computer.
SUMMARY OF THE INVENTION
In apparatus for chemical analysis to which the invention is
applied, a sample to be analyzed is injected to a sample
introduction section by means of a syringe having an injection
needle which pierces an elastic cap or plug sealingly covering a
sample introduction opening formed in said sample introduction
section. Improved means for producing an information signal of the
sample introduction according to the invention comprises a movable
member engageable with said syringe when a sample is injected by
said syringe to said sample introduction section, a stationary
member cooperating with said movable member, an electrical switch
which is closed and opened in response to the relative movement
between said movable member and said stationary member, and an
electric circuit including said electrical switch and means for
producing an electrical signal for the sample introduction
information. The electrical switch may comprise an electrical
contact on said movable member and a cooperating electrical contact
on said stationary member, said electrical contacts becoming in
contact with each other when said movable member is moved toward
said stationary member during the sample injecting operation.
In another preferred embodiment the electrical switch is a
microswitch which is operable by movement of said movable
member.
Said movable member may be normally supported in a position spaced
from said elastic cap or plug and has a central opening in
alignment with said elastic cap so that said injection needle may
pass through said central opening and said syringe may engage with
the portion of said movable member defining said central
opening.
The electrical signal for sample introduction information produced
is transmitted to a recorder having a chromatograph or a computer
for processing analytical data from a detector of said apparatus
for chemical analysis.
BRIEF DESCRIPTION OF THE DRAWINGS
FIG. 1 is a schematic sectional view showing means for providing an
information signal of sample introduction in a vapor phase
chromatograph embodying the present invention;
FIG. 2 is an electrical circuit diagram including means for
producing an information signal of sample introduction in
connection with the apparatus illustrated in FIG. 1;
FIG. 3 is a perspective view of another embodiment of the invention
in which a microswitch is used;
FIG. 4 is a top plan view of the device as shown in FIG. 3;
FIG. 5 is a cross sectional view taken along the lines 5--5 of FIG.
4; and
FIG. 6 is a block diagram of apparatus for chemical analysis ane
data processing system including means for producing an information
signal of sample introduction according to the invention.
DESCRIPTION OF THE PREFERRED EMBODIMENTS
Referring now to the drawings, the sample introduction section of a
vapor phase chromatograph having improved means for producing an
information signal of sample introduction embodying the present
invention is illustrated in FIG. 1. The sample introduction section
11 is connected to one end of a vapor phase chromatographic column
12 by a connector 13 provided with a carrier gas inlet opening 14
and a sample introduction opening 15. The sample introduction
opening 15 is sealingly covered by an elastic plug 16 which is made
of heat-resistant silicon rubber. The sample introduction section
11 is supported at its portion defining said sample introduction
opening 15 by a panel 17. The reference numeral 18 indicates an
opening formed in the panel 17 for supporting that portion defining
the sample introduction opening 15 of the section 11. The elastic
plug 16 is mounted on a metal holder 19 which is then placed on the
panel 17. The metal holder 19 is formed with a small central
opening 20 for insertion of the needle of a syringe therethrough.
The metal holder 19 functions as a stationary electrical contact of
an electrical switch which is normally opened. A movable electrical
contact 21 cooperating with the stationary contact 19 is normally
spaced from the stationary contact 19 and is supported by a
flexible shank 22, one end of which is fixed at 23 on the panel 17.
The shank 22 may be formed as an integral portion with the contact
21. The movable contact 21 has a small central opening 24 in
alignment with the central opening 20 of the stationary contact 19
so that the injection needle of a syringe can pass through the
central opening 24.
A sample liquid is injected into the sample introduction section 11
of the apparatus by means of a syringe or microsyringe 25 and,
after being vaporized, is conveyed by a carrier gas introduced from
the carrier gas inlet 14 to the column 12. In the sample injecting
operation, the needle of the syringe passes through the openings 20
and 24 of the electrical contacts 19 and 21 and then pierces the
elastic plug 16. In this operation the front end of the cylinder of
the syringe 25 engages with the movable electrical contact 21 to
push it toward the stationary contact 19 so that these two electric
contacts may become in contact with each other. The reference
numeral 30 generally indicates an electrical on-off switch
consisting of the stationary contact 19 and the movable contact 21.
The switch 30 is inserted in an electrical circuit including means
for producing an electrical signal for the sample introduction
information. The leading wires are led out either directly from the
electrical contacts 19 and 21 or indirectly from the panel and the
flexible shank 22 if both the panel and the flexible shank are made
of electrically conductive material. In the latter case the panel
17 may be grounded while the fixed end of the flexible shank 22 may
be connected to an electrically conductive terminal core 31 which
is then connected to a leading wire. The reference numeral 23
indicates an insulating terminal support for holding the terminal
core 31 and the flexible shank 22.
In the above mentioned way, the on-off switch 30 consisting of the
movable and stationary contact members is electrically closed
whenever a sample is injected, thereby actuating a circuit which
then provides a signal indicating "injection" or "introduction" to
the recording section of the apparatus. FIG. 2 shows an example of
the signal circuit. The signal circuit generally indicated by the
reference numeral 40 includes the electrical switch 30 consisting
of the movable contact 21 and the stationary contact 19, a power
source 41, a resistor 42, and means 43 for producing an electrical
signal which is connected in parallel to the resistor 42. Means 43
for producing an electrical signal may be a relay or flip-flop
which is used to provide a writing signal to a recorder 44. The
stationary contact 19 may be grounded at 17 which may be the
electrically conductive panel 17 illustrated in FIG. 1.
With the above arrangement according to the invention, while the
injection needle of the sample injecting syringe is piercing
through the silicon rubber plug 16 to inject a sample into the
sample introduction section, that is, the syringe is pressing the
movable contact 21 to the stationary contact 19, the switch
consisting of the movable and stationary contacts 21 and 19 are
kept in closed position, at the state of which the relay or the
flip-flop 43 is energized to produce an electrical signal which is
then transmitted to a recorder 44.
FIGS. 3 to 5 illustrate another embodiment of the invention. FIG. 3
is a perspective view showing the sample injecting section of a
vapor phase chromatograph and a microswitch disposed adjacent
thereto. The reference numeral 51 indicates the top plate or panel
of a casing in which a chromatographic column (not shown) is
supported. The panel 51 is bored with an opening 52 for insertion
of a sample injection syringe (shown with reference numeral 69 in
FIG. 5). The sample introduction section 53 for the column is
disposed slightly below and coaxially with said opening 52. The
reference numeral 54 indicates a microswitch holder which is formed
in a shape of a rectangular, horizontally extending box. The holder
54 is supported on a pillar 55 vertically extending from the top
surface of the panel 51 and deposited on a collar 56 which is
secured on the pillar 55 by a set screw 57. The distance between
the holder 54 and the panel 51 can be changed by adjusting the
position at which the collar 56 is secured on the pillar 55. The
holder 54 is provided with an adjust screw 58 which engages the
pillar 55 so that the holder 54 may be secured on the pillar 55 at
a desired horizontally orientated position. In FIGS. 3 to 5, the
front head 65 of the holder 54 is oriented toward the center of the
opening 52 of the panel.
A microswitch 60 is supported within the holder 54 by a bracket
54a. The microswitch 60 is provided with an on-off operating button
61 and a resilient blade 62 for actuating the button 61. The blade
62 may usually be in slight contact with the button 61. The blade
62 is fixed at its one end on the top surface of the housing of the
microswitch 60. The free end 62b of the blade 62 is connected to
the top end of a connecting rod 63 which vertically extends through
a guide hollow 64 formed in the front head 65 of the holder 54. The
connecting rod 63 is vertically slidable in the hollow 64. The
connecting rod 63 extends through the opening 52 of the panel 51
and has a tongue 66 at its bottom end. The tongue 66 extends
horizontally and has an opening 67 for insertion of the injection
needle of the syringe 53 therethrough. The opening 67 of the tongue
66 is positioned in alignment with the axis of the sample
introduction section 53 and the tongue 66 is usually kept spacedly
from the top end of the sample introduction section 53.
As more clearly illustrated in FIG. 5 the sample introduction
section 53 may comprise a tubular body 71, an elastic plug 72 made
of silicone rubber covering the top opening of the tubular body 71,
and a cap 73 covering the elastic plug. The cap 73 is secured to
the tubular body 71 by screw threading so that the elastic plug 72
is clamped between them. The cap 73 also has a central opening 74
through which the needle of the syringe 69 can pass.
When the injection needle held by the injection syringe 69 is
inserted into the sample introduction section 53, with the needle
passing through the opening of the tongue 66 and the opening 74 of
the cap 73 and then piercing the elastic plug 72, the injection of
the sample into the tubular body 71 which is connected to a column
can be achieved simply by operating the injection syringe 53.
During the operation of piercing the needle of the syringe through
the elastic plug 72, the syringe 53 engages the tongue 66 to move
it downward. The movement of the tongue 66 in the downward
direction is transmitted to the blade 62 which then pushes the
button 61 for placing the microswitch 66 in an electrically closed
position. During this operation the tongue 66 may be in contact
with the top surface of the cap 73.
In the above way, the microswitch 60 is electrically closed
whenever a sample is injected, thereby actuating a circuit which
then provides a signal indicating "injection" to the recording
section of the apparatus. The electrical circuit including means
for producing an electrical signal may be constructed in the same
manner as illustrated in FIG. 2 but it should be noted that the
switch 30 in FIG. 2 should be replaced by the microswitch 60
illustrated in FIGS. 3 to 5.
In the embodiment illustrated in FIGS. 3 to 5, since the holder 54
may be rendered rotatable around the axis of the pillar 55 by
loosening the screw 58, the holder 54 may be oriented to another
sample introduction section (not shown) which may be constructed in
the same manner as the sample introduction section 53 illustrated
in FIGS. 3 to 5. It will be understood that any change in
orientation of the holder 54 should be done after pulling up the
connection rod 63 with the tongue 66 above the panel 61.
The electrical signal produced in response to the sample injection
in such a manner as disclosed in the above may also be transmitted
to a computer. The whole system including means embodying the
present invention and a data processing system is illustrated in a
block diagram of FIG. 6. The apparatus illustrated in FIG. 6
includes a a vapor phase or liquid phase chromatograph 81 as the
sample analysing system. The chromatograph 81 includes a
chromatographic column and such means for introducing a sample into
the chromatographic column by a syringe as shown in FIG. 1 or FIGS.
3 to 5. The apparatus also includes a detector 82 which produces
electric signals in response to the sample introduced into the
column of the chromatograph 81. The detector 82 may be of any known
type, e.g. in case of a vapor phase chromatograph, it may be a
thermal conductivity cell or a frame ionization detector. The
electric signal output from the detector 82 is amplified or
attenuated by an amplifier or attenuator 83 and then imparted to a
known recorder 44 to obtain a chromatogram. The output terminals 85
are also connected to normally open contacts 86a of a double-pole,
double throw switch 86. The common contacts 86b of the switch 86
are electrically connected to a A-D converter 87, the digital
output of which is then applied to a computer 88 which serves as
data processing means. The normally closed contacts 86c of the
switch 86 are electrically connected to a calculation start
inhibition signal source 89. In this manner the computer 88 is
selectively connected by switching means in the form of a double
pole, double throw switch 86 either to the detector 82 or to the
calculation start inhibition signal source 89 so that the computer
89 may be supplied with the analytical data represented by electric
signals, or, be inhibited from calculation operation,
respectively.
The double-pole, double throw switch 86 is actuated by a relay coil
43. The circuit 40 for energizing the relay coil 43 may be
substantially identical with that illustrated in FIG. 2 and
includes an electric source 41 and a switch 30. The switch 30 is
operatively connected to sample injecting means of the
chromatograph 81. Preferably a second switch 84 which is manually
operable is inserted in parallel with the switch 30. The second
switch 84 is used for holding the circuit 40 in a conductive
condition even if the first switch is opened after once closed.
So far as the switch 30 is not closed the relay coil 43 is never
energized and accordingly, the common contacts 86b of the switch 86
are kept in contact with the normally closed contacts 86c so that
the computer 88 is not supplied with any analytical data from the
detector 82 but inhibited from calculation operation owing to the
fact that the computer 88 is electrically connected through the
common contacts 86b and the normally closed contacts 86c. The
calculation start inhibition signal source 89 may supply a negative
voltage signal or a sufficiently large positive voltage signal to
the computer 88 through the A-D converter 87. In case where a
negative voltage signal is applied to the computer 88, the computer
will be able to discriminate any input signals, if applied to the
computer, not to be calculated by means of code bit representing a
negative sign obtained from an accumulator contained in the
computer. In the case where a sufficiently large positive voltage
signal is applied to the computer, the computer discriminates the
input signals as not to be calculated as well, by virtue of
overflow bits owing to said large signal.
As mentioned before, if a sample is injected to the chromatographic
column, by means of a syringe, the first switch 30 is closed to
energize the relay 43 which in turn operates to switch the common
contacts 86b from the normally closed contacts 86c to the normally
open contacts 86a so that the A-D converter 87 and the computer 88
is released from the inhibition of calculation operation and is
supplied with analytical data which corresponds to the signal
values obtained as a chromatogram at the recorder 44. Thus, the
initiation of the introduction of a sample to the chromatographic
column is exactly synchronized with the initiation of the supply of
the analytical data to the computer which in turn starts the data
processing as it is in an operational state so that the
determination of the retention time of each of the sample
constituents can be expected with a high accuracy.
The manually operable second switch 84 should be closed after the
first switch is closed and before the first switch is opened at the
termination of the sample introduction. Preferably, the second
switch is closed after the lapse of the retention time of any
sample constituent to be analyzed so that calculation operation may
be continued even after the introduction of a sample to the column
is terminated. If the two switches 30 and 84 are opened, the relay
coil 43 is denergized to return the common contacts 86b to the
initial positions at which the A-D converter 87 and the computer 88
are electrically connected to the calculation start inhibition
signal source 89 again.
In the above described embodiment of the invention, the calculation
operation of the computer 88 is started in synchronism with the
initiation of the sample introduction. However, the present
invention is never limited to the synchronism of the initiation of
the sample introduction with the start of calculation operation in
the computer but applicable to the synchronism of the sample
introduction with the start of the general supply of the analytical
data to the computer when the computer is kept at the inhibition
state of the calculation operation. For example, the invention can
be applied to the so-called TSS (Time Sharing System) in which the
supply of the data to the computer is carried out at the different
time from that during which the calculation is carried out.
* * * * *