# US 6,653,143 B2 · Process and device of elemental analysis

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- Number: US 6,653,143 B2
- Document ID: US6653143B2
- Status: Granted
- Kind: B2
- Application number: 09/050,912
- Filed: 1998-03-31
- Published: 2001-08-30
- Granted: 2003-11-25
- Earliest claimed: 1998-03-31
- Assignees: Thermoquest Italia S.p.A.
- Inventors: Luigi Ragaglia; Giacinto Zilioli; Franca Andreolini; Liliana Noemi Krotz
- Web page: https://patentgrep.com/patent/US6653143B2

## CPC

- G01N 31/12: using combustion (G01N25/20 takes precedence)
- Y10T 436/11: Automated chemical analysis
- Y10T 436/117497: with a continuously flowing sample or carrier stream
- Y10T 436/17: Nitrogen containing
- Y10T 436/176152: Total nitrogen determined
- Y10T 436/176921: As part of an elemental analysis
- Y10T 436/23: Carbon containing
- Y10T 436/25875: Gaseous sample or with change of physical state
- 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)
- Y10T: TECHNICAL SUBJECTS COVERED BY FORMER US CLASSIFICATION

## Abstract

Elemental analysis of a sample is carried out in an oxygen atmosphere in a combustion reactor and the volume of oxygen required for analysis is determined by means of the algorithm Qo=Δ(Qc) [1] where Qo is the volume of oxygen required and Qc is the weight of the sample to be analyzed and Δ=Qo1/Qc1 where Qo1 is the volume of oxygen necessary for the combustion of a predetermined quantity Qc1 of the sample to be analyzed, the volume of oxygen Qo is then fed in pulsed mode to the combustion reactor, by means of a flow detector.

## Claims

### Claim 1

A process for providing automatically only a required amount of oxygen for elemental analysis by complete flash combustion of samples in an oxygen atmosphere in a combustion reactor normally fed with a flow of inert carrier gas wherein oxygen consumption is minimized, comprising:
experimentally determining a Δ constant for each type of sample to be analysed according to the following formula:
Δ=Q01/QC1
where:
Qc1 is a predetermined quantity of a sample of the same type of the sample to be analyzed, Q01 is the volume of oxygen required for the combustion of predetermined quantity Qc1 of a sample of the same type as the sample to be analyzed, and
Δ is a constant for the type of sample to be analyzed and storing the constant Δ for each sample as data in an electronic database inputting the type and quantity of a sample into a processor connected to the electronic data base to compute a value Qo for the volume of the the oxygen required for the analysis of that sample, by using the following formula stored in the electronic database:
Qo=Δ(Qc)
where:
Qo is the volume of oxygen required for combustion,
Qc is the weight of the sample to be analysed,
Δis the constant for the sample type to be analysed,
switching off the flow of inert carrier gas to the combustion reactor;
supplying the required amount of oxygen by connecting the combustion reactor to a source of oxygen by means of a mass flow regulator and using the same oxygen flow rate used for the determination of OO1;
restoring the flow of inert carrier gas to the combustion reactor at the end of the oxygen introduction step;
thereby feeding in pulsed mode the required volume of oxygen QO to said combustion reactor automatically from a source of oxygen through a valve operated by a calculating device via a flow detector.

### Claim 2 (depends on 1)

A process according to claim 1, wherein QO1 is calculated by: measuring the time TC necessary for the combustion of the pre-determined quantity of sample QC1, measuring the flow-rate P of the oxygen fed to the combustion reactor, and multiplying TC by P.

### Claim 3 (depends on 2)

A process according to claim 2, wherein said flow of oxygen is constant during the combustion step of the sample.

### Claim 4 (depends on 1)

A process according to claim 1, wherein a flow of an inert carrier gas is fed to the analysis device before and after the pulsed oxygen, and a flow of said carrier is fed to a reference branch of the combustion chamber.

### Claim 5

A device for providing automatically only a required amount of oxygen for a flash elemental analysis of a sample wherein oxygen consumption is minimized, comprising:
a combustion reactor,
a supply of a flow of an inert carrier gas to the device,
an oxygen feeding system comprising:
a source of oxygen,
a feed line from the source of oxygen to the combustion reactor,
a pulse-feeder for pulse-feeding oxygen to the reactor,
a mass flow regulator on said feed line of oxygen, and
valve means for disconnecting the combustion reactor from the flow of inert carrier gas, and
a calculating device connected to the oxygen feeding system for determining automatically a Δ constant for each type of sample to be analyzed according to the following equation:
Δ is Qo1/QC1
where:
QC1 is a known quantity of sample; and
QO1 is the only volume of oxygen necessary for complete combustion of a known quantity QC1 of the sample to be analyzed and for computing automatically the volume of oxygen required and to be fed for analysis of the sample by using the same oxygen flow rate used for the determination of Qo1 and using the following equation:
QO=Δ(QC) (1)
QO is the volume of oxygen required,
Qc is the weight of the sample to be analyzed,
where:
Δ is the constant for the sample type to be analysed.

### Claim 6 (depends on 5)

A device according to claim 5, further comprising an electronic device for:
containing a plurality of constants Δ for a corresponding plurality of types of samples;
containing formula Qo=Δ (Qc) and being capable of receiving data related to a type and quantity of sample to be analyzed for calculating said volume of oxygen Qo required for a predetermined quantity of a sample of the same type.

### Claim 7 (depends on 6)

A device according to claim 6 wherein said flow detector is connected with a proportional valve and with said electronic device.

### Claim 8 (depends on 6)

A device according to claim 6, further comprising a feed for feeding said inert carrier gas to said combustion reactor and to a reference line dedicated to the carrier gas alone.