# US 2014/0150527 A1 · Device for measuring total or fractionated quantity of hydrocarbons in a solid sample

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- Number: US 2014/0150527 A1
- Document ID: US20140150527A1
- Status: Published application
- Kind: A1
- Application number: 14/096,039
- Filed: 2013-12-04
- Published: 2014-06-05
- Earliest claimed: 2012-12-05
- Assignees: Geolog S.r.l.
- Applicants: GEOLOG S.r.l.
- Inventors: Antonio CALLERI
- Web page: https://patentgrep.com/patent/US20140150527A1

## CPC

- G01N 30/68: Flame ionisation detectors
- G01N 30/88: Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N 33/241: {for hydrocarbon content}
- G01N 2030/8854: {involving hydrocarbons}
- 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

A system of analysis operating preferably on a sample of rock derived from oil drilling in a site situation and possibly under difficult environmental conditions, which allows the total quantity of hydrocarbons contained in said sample to be measured, both already present and generable following transformation of organic matter contained in the same sample, in the first case also allowing a quantity of each single hydrocarbon species to be measured. The time range wherein said system succeeds in completing these analyses is sufficiently reduced to allow use of the results for reference and as a decision instrument for drilling, and the configuration of said system guarantees the stability of functioning thereof sufficient for allowing the use thereof also under difficult environmental conditions, on land or at sea, and allows for convenient use thereof also by an operator simply trained in the use of the instrument.

## Claims

### Claim 1

A system at least partially automatic, for the analysis of at least part of a sample at least partially solid and preferably of rocky material derived from oil drilling, wherein said system comprises at least:
a pyrolysis oven suitable for heating said sample in an inert environment;
a gas chromatograph suitable for separating a hydrocarbon mixture released by said sample;
a first flame ionization detector FID and a second flame ionization detector FID suitable for measuring a quantity of one or more hydrocarbon species released by said sample, and which may optionally be at least partially reciprocally integrated or restrained;
a sampler suitable for collecting and/or containing said sample and/or channelling said sample in said system;
a scrubbing means suitable for scrubbing said sample in order to eliminate air, preferably by means of a fluxing of inert gas;
a sorting valve suitable for distributing a flow of hydrocarbons already present as such in the sample towards a first analyser and towards said gas chromatograph, or for directing the flow of those generated by transformation of organic matter contained in said sample only towards said first analyser;
a trap suitable for absorbing a mixture of hydrocarbons already present as such in the sample;
a second heating means, suitable for heating said trap;
a cooling means, suitable for cooling said trap;
one or more communication means suitable for placing in communication the following pairs of components:
said pyrolysis oven with said first analyser;
said pyrolysis oven with said first gas chromatograph;
said gas chromatograph with a second analyser;
a processor suitable for automating the operations of the components of said system;
and wherein:
the sampler provides automatically for channelling the sample towards other components of the system in a known manner;
said pyrolysis oven is provided with at least one known means suitable for supplying inside the same at least one flow of an inert gas;
the trap is internal and/or directly connected to the gas chromatograph and in any case contributes to functioning of said gas chromatograph; and
said trap is made up of at least partially a material able to at least absorb gaseous matter, which preferably is a material made up of graphitised carbons.

### Claim 2 (depends on 1)

A method for using the system of claim 1, wherein said method comprises at least the following sequence of phases, which can be divided in turn into a certain number of steps:
a) said sample passes at least partially, either through gravity or in another known manner, from said sampler to said pyrolysis oven;
b) said sample is at least partially subjected to a first process of heating; this first process of heating preferably consists of maintaining a zone where said sample is situated at a temperature between 523.15 K and 623.15 K, for a time interval that lasts between 2 and 4 minutes;
c) the hydrocarbons already present in said sample are released at least partially from the same sample in an at least partially gaseous state;
d) said hydrocarbons already present are at least partially transported at least by a carrier gas, and divide at least partially into at least two portions, defined here respectively as first portion and second portion;
e) this phase comprises at least the following steps:
said first portion enters at least partially said first analyser, drawn at least by a carrier gas;
the quantity of said first portion is then measured at least partially, in absolute terms and/or in relation to the quantity at least of a part of said sample and/or to any other quantity or value; preferably but not exclusively, on the basis of at least the ratio between first and second portion, the total quantity of at least a part of the total quantity of all the portions is also evaluated, in absolute terms and/or in relation to the quantity at least of a part of said sample and/or to any other quantity or value;
f) this phase, which preferably takes place at least partially simultaneously to phase e), comprises at least the following steps:
said second portion is at least partially separated, by means of said gas chromatograph, into several fractions, also numerous, whereof at least one first fraction comprises at least one hydrocarbon species different from at least one hydrocarbon species comprised in at least one second of said fractions;
said first fraction passes at least partially from said gas chromatograph to said second analyser and then the quantity of said first fraction is measured at least partially, in absolute terms and/or in relation to the quantity of at least a part of said sample and/or to that of at least a part of another of said fractions and/or to any other quantity or value; this step is repeated for all the other fractions which are to be analysed.

### Claim 3 (depends on 1)

A method for using the system of claim 1, wherein said method comprises at least the following sequence of phases, which can be divided in turn into a certain number of steps:
a) said sample passes at least partially, either through gravity or in another known manner, from said sampler to said pyrolysis oven;
b) said sample is at least partially subjected to a first process of heating; this first process of heating preferably consists of maintaining the zone where said sample is situated at a temperature between 523.15 K and 623.15 K, for a time interval that lasts between 2 and 4 minutes;
c) the hydrocarbons already present in said sample are released at least partially from the same sample in an at least partially gaseous state;
d) said hydrocarbons already present are at least partially transported at least by a carrier gas, and divide at least partially into at least two portions, defined here respectively as first portion and second portion;
e) this phase comprises at least the following steps:
said first portion enters at least partially said first analyser (18), drawn at least by a carrier gas;
a quantity of said first portion is then measured at least partially, in absolute terms and/or in relation to a quantity of at least a part of said sample and/or to any other quantity or value; preferably but not exclusively, on the basis of at least the ratio between first and second portion, the total quantity of at least a part of the total quantity of all the portions is also evaluated, in absolute terms and/or in relation to the quantity of at least a part of said sample and/or to any other quantity or value;
f) this phase, which preferably takes place at least partially simultaneously to phase e), comprises at least the following steps:
said second portion is at least partially separated, by means of said gas chromatograph, into several fractions, also numerous, whereof at least one first fraction comprises at least one hydrocarbon species different from at least one hydrocarbon species comprised in at least one second of said fractions;
said first fraction passes at least partially from said gas chromatograph to said second analyser, and then the quantity of said first fraction is measured at least partially, in absolute terms and/or in relation to the quantity of at least a part of said sample and/or to that of at least a part of another of said fractions and/or to any other quantity or value; this step is repeated for all other fractions which are to be analysed.
g) said sample is at least partially subjected to a second process of heating; this second process of heating preferably means that the temperature of the zone where said sample is situated has a trend characterised by a rising section or ramp, with an increase equal to a value between 20 K and 30 K per minute and up to a temperature situated between 873.15 K and 973.15 K, followed by a constant section at this temperature for a time interval lasting between 1 and 4 minutes;
j) hydrocarbons generated by transformation of at least part of the organic matter contained in said sample are released at least partially from the same sample in an at least partially gaseous state;
k) this phase comprises at least the following steps:
said generated hydrocarbons, transported at least partially by at least one carrier gas, enter at least partially said first analyser;
the quantity of these generated hydrocarbons is then measured at least partially, in absolute terms and/or in relation to a quantity of at least a part of said sample and/or to any other quantity or value.

### Claim 4 (depends on 2, 3)

The method according to claims 2 or 3, wherein:
said method comprises all the phases described, which can be at least partially simultaneous and/or at least partially in the sequence presented and/or repeated cyclically at least twice, or also numerous times;
or said method comprises at least two of these phases, which can be in turn at least partially simultaneous and/or at least partially in the sequence presented and/or repeated cyclically at least twice, or also numerous times.

### Claim 5 (depends on 4)

The method of claim 4, wherein said gas chromatograph comprises at least:
a communication means suitable for receiving the mixture of hydrocarbons already present in the sample and that arrives from said pyrolysis oven;
a first valve and a second valve, which can optionally be at least partially reciprocally integrated or restrained;
a pre-column and a final column of chromatographic separation, which can optionally be at least partially reciprocally integrated or restrained or also constitute a single separation column, and which are at least partially in communication with said second valve;
and wherein said gas chromatograph is moreover configured, by means of at least one known means, in such a way as to at least be capable of being used according to a procedure which comprises the following sequence of phases, preferably controlled by said processor or by at least one other:
a mixture of gaseous hydrocarbon species, which preferably corresponds to said second portion wherein the hydrocarbon molecules are divided, and which were already present in the sample, being drawn by a carrier gas, passes, via said first valve, enters said trap, and is absorbed by the latter;
the trap is heated in such a way as to release or desorb said mixture;
a flow of a carrier gas passes through said first valve, enters said trap, draws said mixture along the same trap and makes said mixture pass through said first valve;
said mixture is drawn by a flow of carrier gas until it enters the pre-column and flows along the same, in such a way as to start to separate into various hydrocarbon species;
said trap is optionally, at the same time, cooled by means of said cooling means;
said mixture, drawn by a carrier gas, passes through said second valve, travels along the final column, so that the separation and/or the moving away among the various hydrocarbon species of said mixture is increased.