# US 11,309,173 B2 · Liquid sample introduction method and liquid sample introduction device

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- Number: US 11,309,173 B2
- Document ID: US11309173B2
- Status: Granted
- Kind: B2
- Application number: 16/613,160
- Filed: 2017-08-10
- Published: 2021-10-07
- Granted: 2022-04-19
- Earliest claimed: 2017-08-10
- Assignees: Shimadzu Corporation
- Applicants: Shimadzu Corporation
- Inventors: Daisuke Okumura; Shingo Fujioka; Kazuma Maeda
- Web page: https://patentgrep.com/patent/US11309173B2

## CPC

- H01J 49/045: {with means for using a nebulising gas, i.e. pneumatically assisted}
- G01N 1/00: Sampling; Preparing specimens for investigation
- G01N 27/62: by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
- G01N 27/623: combined with mass spectrometry
- G01N 35/1095: {for supplying the samples to flow-through analysers (for a specific analyser see relevant groups, e.g. under G01N15/00, G01N21/00, G01N27/00, G01N30/00, H01J49/00)}
- G01N 2001/002: {Devices for supplying or distributing samples to an analysing apparatus}
- H01J: ELECTRIC DISCHARGE TUBES OR DISCHARGE LAMPS (spark-gaps H01T; electric arc lamps H05B31/00; particle accelerators H05H)
- G01N: INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES (measuring or testing apparatus or processes other than immunoassay, involving enzymes or microorganisms C12M, C12Q)

## Abstract

The other end of an individual sample supply channel one end of which is connected to a gas buffer container the inside of which is empty is connected to one sub-port of a valve that selects one of standard samples to be supplied to an ESI probe. During analysis, the standard sample stored in one of liquid sample containers is selected by switching a connection state of the valve. The standard sample supplied by being pushed by a gas sent to the liquid sample containers through liquid supply gas branch channels is sent to the ESI probe through a sample supply main channel. At the time of finishing analysis, when the valve is switched such that the sub-port and a main port are communicatively connected, a nitrogen gas is sent to the sample supply main channel, and the remaining liquid is discharged.

## Claims

### Claim 1

A liquid sample introduction method using a liquid sample introduction device configured to send a liquid sample and a nebulizing gas to an ionization probe of an ion source in an ion analysis device and to nebulize the liquid sample from a tip of the ionization probe with the help of the nebulizing gas, the liquid sample introduction device including a plurality of liquid sample containers each of which is a closed container and a liquid sample is stored, a liquid supply gas path connected at one end to a middle of a channel for supplying the nebulizing gas to the ionization probe and branched into a plurality of sub-paths each end of which is connected to each of the plurality of liquid sample containers above liquid levels of the liquid sample, a channel switching unit configured to selectively connect one outlet port and one of a plurality of inlet ports, a common sample supply channel one end of which is connected to the ionization probe and another end is connected to the outlet port of the channel switching unit, and a plurality of individual sample supply channels one ends of which are connected to the plurality of liquid sample containers below the liquid levels of the liquid samples and other ends are connected to the plurality of inlet ports of the channel switching unit, the method comprising:
a process of setting one of the plurality of liquid sample containers to be in an empty state, and switching connection of the channel switching unit such that the outlet port and the inlet port connected to the liquid sample container which is in the empty state are connected to each other through one of the plurality of individual sample supply channels at a time of finishing analysis in the ion analysis device.

### Claim 2

A liquid sample introduction device configured to send a liquid sample and a nebulizing gas to an ionization probe of an ion source in an ion analysis device and to nebulize the liquid sample from a tip of the ionization probe with the help of the nebulizing gas, the device comprising:
a) a liquid sample container which is a closed container in which a liquid sample is stored;
b) a gas buffer container which is in a closed state;
c) a gas supply auxiliary path connected at one end to a middle of a path for supplying the nebulizing gas to the ionization probe and branched into sub-paths one of which is connected to the liquid sample container above a liquid level and another to the gas buffer container;
d) a channel switching unit configured to selectively connect one outlet port and one of a plurality of inlet ports to each other;
e) a common sample supply channel one end of which is connected to the ionization probe and another end is connected to the outlet port of the channel switching unit;
f) an individual sample supply channel one end of which is connected to the liquid sample container so as to be positioned below the liquid level of the liquid sample and another end is connected to one of the plurality of inlet ports of the channel switching unit;
g) a replacement gas path one end of which is connected to the gas buffer container and another end is connected to one of the plurality of inlet ports of the channel switching unit; and
h) a control unit configured to switch connection of the channel switching unit such that the outlet port and the inlet port connected to the replacement gas path are connected to each other at a time of finishing analysis in the ion analysis device.