Sampler-injector for liquid chromatography

Claim 1

AN AUTOMATIC SAMPLER-INJECTOR FOR USE WITH A LIQUID CHROMATOGRAPHIC COLUMN COMPRISED OF, IN COMBINATION: I. A SAMPLE CONTAINER COMPRISED OD: A. A CYLINDER HAVING A CLOSED END AND AN OPEN END, AND B. A STOPPER ADAPTED TO SLIDE SNUGLY INTO THE OPEN END OF SAID CYLINDER, AFTER LIQUID TO BE SAMPLED HAS BEEN PLACED THEREIN, SAID STOPPER BEING ADAPTED TO BE PIERCED BY A NEEDLE, AND II. MEANS FOR REMOVNG A SAMPLE FROM SAID SAPLE CONTAINER, MEASURING SAID SAMPLE, AND INJECTINGSAID SAMPLE INTO SAID LIQUID CHROMATOGRAPHIC COLUMN COMPRISED OF: A. A SHARPLY POINTED HOLLOW NEEDLE SPATIALY DISPOSED RTICALLY ABOVE SAID SAMPLE CONTAINER, SAID NEEDLE HAVING AN ANNULAR COLLAR AFFIXED THEREAROUND AT A SUFFICIENT DISTANCE FROM THE POINT THEREOF TO PERMIT SAID POINT OF SAID NEEDLE TO PENETRATE SAID STOPPER, B. MEANS FOR POSITIONING SAID SAMPLE CONTANER ENEATH SAID NEEDLE SO THAT SAID SAMPLE CONTAINER AND SAID NEEDLE ARE IN THE SAME VERTICAL PLANE, C. MEANS FOR CONTACTING SAID STOPPER IN SAID SAMPLE CONTANER WITH SAID NEEDLE, PIERCINGSAID STOPPER WITH SAID POINT OF SAID NEEDLE, CONTACTING SAID STOPPER WITH SAID COLLAR AND MOVING SAID STOPPER TOWARD THE CLOSED END OF SAID CYLINDER, SAID MOVEMENT ENDING WHEN THE POINT OF SAID NEDDLE NEARS THE CLOSED END OF SAID CYLINDER AND THEN REVERSING SAID MOVEMENT UNTIL SAID CYLINDER AND SAID NEEDLE-COLLAR ASSEMBLY RE RETURNED TO THEIR STARTING POSITION, D. A CONDUIT CONNECTING SAID NEEDLE WITH THE FIRST PORT OF A SIX PORT VALVING MEANS, C. A DISCHARGE CONDUIT CONNECTED TO A SECOND PORT OF SAID VALVING MEANS, F. A SAMPLING LOOP CONNECTED TO A THIRD AND FOURTH PORT OF SAID VALVING MEANS, G. MEANS FOR FLUSHING A SAMPLE FROM SAID SAMPLING LOOP INTO SAID LIQUID CHROMATOGRAPHIC COLUMN CONNECTED TO A FIFTH PORT OF SAID VALVING MEANS, H. A CONDUIT TO SAID LIQUID CHROMATOGRAPHIC COLUMN CONNECTED TO THE SIXTH PORT OF SAID VALVING MEANS, I. MEANS FOR ALIGINING THE FIRST PORT WITH THE FOURTH PORT, THE SECOND PORT WITH THE THIRD PORT, AND THE FIFTH PORT WITH THE SIXTH PORT OF SAID VALVING MEANS AS SAID NEEDLE CONTACTS SAID STOPPER, AND MEANS FOR ALIGNING THE FIRST PORT WITH THE SECOND PORT, THE THIRD PORT WITH THE SIXTH PORT, AND THE FOURTH PORT WITH THE FIFTH PORT OF SAID VALVING MEANS AS SAID CYLINDER AND SAID NEEDLE-COLLAR ASSEMBLY ARE RETURNED TO THEIR STARTING POSITIONS, J. MEANS FOR FLUSHING SAID SAMPLE FROM SAID SAMPLING LOOP INTO SAID CHROMATOGRAPHIC COLUMN, AND K. MEANS FOR ADVANCING THE NEXT SAMPLER CONTAINER TO A POSITION DIRECTLY BENEATH SAID NEEDLE.

Claim 15

A method for automatically sampling and injecting consistently uniform volumes of liquids containing components to be separated in a liquid chromatographic column into said column comprising: a. placing a quantity of the liquid to be sampled in a cylinder closed on one end and open on the other; b. inserting a snugly fitting stopper adapted to be pierced by a needle and to Act as a piston into the open end of said cylinder containing said liquid; c. placing the thus prepared cylinder of (b) in one of a plurality of vertical cavities in a feedingpositioning device equipped with means to advance such device one cavity at a time; d. disposing vertically a sharply pointed hollow needle above said cylinder of (c), said needle having an annular collar affixed around the circumference thereof at a sufficient distance from the point thereof to permit said point of said needle to penetrate said stopper; e. connecting a conduit between said needle and the first port of a six-port valving means; f. connecting a conduit from the second port of said valving means to a waste receptacle; g. connecting a closed sampling loop having a volume equal to the volume of the sample desired to be injected into said chromatographic column to the third and fourth ports of said valving means; h. connecting a means for flushing a sample from said sample loop to the fifth port of said valve; i. connecting a conduit from the sixth port of said valving means to the inlet to said chromatographic column; j. aligning said valving means so that (ports 1) and (4), (2) and (3), and (5) and (6) are in communication with each other, respectively; k. contacting said stopper in said sample container with said needle, piercing said stopper with said point of said needle, contacting said stopper with said collar and moving said stopper toward the closed end of said cylinder utilizing said stopper as a piston forcing the liquid into and through said needle and into the first port of said valving means, out the fourth port into said sampling loop and through said sampling loop into the third port and out through the second port of said valve to said waste receptacle, stopping the downward movement of said stopper when the point of said needle nears the bottom of said cylinder; l. aligning the ports of said valving means so that (ports 1) and (2, 3) and (6,) and (4) and (5) communicate with each other, respectively; m. flushing the sample from said sampling loop with solvent flowing into the fifth port, out through the fourth port into said sampling loop and back into the third port and out through the sixth port of said valve into said chromatographic column; and n. returning said cylinder and said needle-collar assembly to their starting positions.

Claim 16

A method for automatically sampling and injecting consistently uniform volumes of liquids containing components to be separated in a liquid chromatographic column into said column comprising: a. placing a quantity of the liquid to be sampled in a cylinder closed on one end and open on the other; b. inserting a snugly fitting stopper adapted to be pierced by a needle and to Act as a piston into the open end of said cylinder containing said liquid; c. placing the thus prepared cylinder of (b) in one of a plurality of vertical cavities in a feedingpositioning device equipped with means to advance such device one cavity at a time; d. disposing vertically a sharply pointed hollow needle above said cylinder of (c), said needle having an annular collar affixed around the circumference thereof at a sufficient distance from the point thereof to permit said point of said needle to penetrate said stopper; e. connecting a conduit between said needle and the first port of a six-port valving means; f. connecting a conduit from the second port of said valving means to a waste receptacle; g. connecting a closed sampling loop having a volume equal to the volume of the sample desired to be injected into said chromatographic column to the third and fourth ports of said valving means; h. connecting a means for flushing a sample from said sample loop to the fifth port of said valve; i. connecting a conduit from the sixth port of said valving means to the inlet to said chromatographic column; j. aligning said valving means so that (ports 1) and (4), (2) and (3), and (5) and (6) are in communication with each other, respectively; k. contacting said stopper in said sample container with said needle, piercing said stopper with said point of said needle, contacting said stopper with said collar and moving said stopper toward the closed end of said cylinder utilizing said stopper as a piston forcing the liquid into and through said needle and into the first port of said valving means, out the fourth port into said sampling loop and through said sampling loop into the third port and out through the second port of said valve to said waste receptacle, stopping the downward movement of said stopper when the point of said needle nears the bottom of said cylinder; l. aligning the ports of said valving means so that (ports 1) and (2, 3) and (6,) and (4) and (5) communicate with each other, respectively; m. flushing the sample from said sampling loop with solvent flowing into the fifth port, out through the fourth port into said sampling loop and back into the third port and out through the sixth port of said valve into said chromatographic column; and n. returning said cylinder and said needle-collar assembly to their starting positions.