# US 4,391,778 A · Method and apparatus for the analysis of materials by chromatography and mass spectrometry

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- Number: US 4,391,778 A
- Document ID: US4391778A
- Status: Granted
- Kind: A
- Application number: 06/306,942
- Filed: 1981-09-30
- Granted: 1983-07-05
- Earliest claimed: 1981-09-30
- Assignees: The Ohio State University
- Inventors: Brian D. Andresen; Kwokei J. Ng
- Web page: https://patentgrep.com/patent/US4391778A

## CPC

- G01N 30/7206: {interfaced to gas chromatograph (interfaces in general for introducing or extracting samples to be analysed with specially adapted mass spectrometer, see H01J49/04)}
- G01N 30/30: of temperature
- G01N 30/10: using a splitter
- G01N 30/7213: {splitting of the gaseous effluent}
- G01N 2030/3038: {temperature control of column exit, e.g. of restrictors}
- G01N 2030/626: {calibration, baseline}
- 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

To avoid the problem of instrumental drift encountered when using an open-split interface between a temperature-programmed gas-liquid chromatography column and a mass spectrometer, the inert gas supplied to the open-split interface and the interface itself are heated to a temperature above the maximum temperature attained by the chromatography column during the analysis.

## Claims

### Claim 1

An apparatus for the analysis of materials by temperature-programmed gas chromatography and mass spectrometry, said apparatus comprising:
a gas chromatography column having an outlet;
first heating means for progressively increasing the temperature of said column from a lower temperature to an upper temperature;
a mass spectrometer having an inlet;
an open-split interface connecting said outlet of said column to said inlet of said mass spectrometer and;
means of supplying inert gas to said open-interface,
the improvement which comprises second heating means for heating said inert gas and said interface to above said upper temperature, thereby reducing the instrumental drift of the base line signal of the total ionization of said mass spectrometer, said second heating means comprising a heating block having walls defining an interface channel which accomodates said interface and a gas channel which intersects said interface channel and through which gas can be passed into said interface channel, said heating block being provided with thermostatic control means for maintaining the temperature of said block substantially constant during said progressive increase of temperature of said column, and wherein said means for supplying said inert gas to said open-split interface comprises a gas supply line having its one end connected to said open-split interface, said gas supply line having a helical section disposed within said gas channel, said helical section increasing the residence time of said gas within said gas channel and thereby improving the uniformity of temperature of said gas reaching said open-split interface.

### Claim 2 (depends on 1)

Apparatus according to claim 1 wherein said gas channel has a substantially toroidal section which accomodates said helical part of said gas supply line.

### Claim 3 (depends on 1)

Apparatus according to claim 1 wherein a portion of said gas channel is substantially cylindrical in form and said helical section of said gas supply line is disposed within said cylindrical section of said gas channel.