Method for operating an analytical apparatus

• US 9,023,657 B2
• Filed: 03/15/2010
• Issued: 05/05/2015
• Est. Priority Date: 03/25/2009
• Status: Active Grant

• Current Assignee: Endress + Hauser Conducta Gesellschaft Fur Mess- Und Regeltechnik Mbh + Co. Kg
• Original Assignee: Endress + Hauser Conducta Gesellschaft Fur Mess- Und Regeltechnik Mbh + Co. Kg
• Inventors: Kathe, Ulrich, Bettmann, Oliver
• Primary Examiner(s): HIXSON, CHRISTOPHER
• Application Number:
  US13/258,111
• Publication Number:
  US 20120015447A1
• Time in Patent Office: 1,877 Days
• Field of Search: 436/180
• US Class Current: 436/180
• CPC Class Codes: G01N 2035/00643 detecting malfunctions in conveying systems
• CPC Class Codes: G01N 33/1846 Total carbon analysis
• CPC Class Codes: G01N 35/00594 Quality control, including calibration or testing of components of the analyser
• CPC Class Codes: G01N 35/00613 Quality control
• CPC Class Codes: G01N 35/00623 of instruments
• CPC Class Codes: G01N 35/00693 Calibration
• CPC Class Codes: G01N 35/00712 Automatic status testing, e.g. at start-up or periodic
• CPC Class Codes: Y10T 436/2575 Volumetric liquid transfer

Abstract

A method for operating an analytical apparatus for determining concentration of an analyte, especially an oxidizable substance, in a sample liquid, comprises the steps of: placing the analytical apparatus in maintenance operation; operating a metering system, which includes a pump, especially a peristaltic pump, and a supply line, for metering single volume units of a sample liquid from a source via the supply line into a reactor, wherein there exists in the reactor a temperature, which is greater than the boiling temperature of the sample liquid, so that a volume unit of the sample liquid metered into the reactor transforms at least partially into the gas phase following entry into the reactor, especially due to heat transfer from contact with a surface within the reactor, especially directly after contact with the surface within the reactor, and wherein a carrier gas is flowing through the reactor; registering at least one measuring transducer signal for detection of the transforming of the volume unit of the sample liquid into the gas phase, and deriving, with application of the measuring transducer signal, a signal correlated with an instantaneous operating state of the metering system.

Claims

1. A method for operating an analytical apparatus for determining the concentration of an analyte, especially an oxidizable substance, in a sample liquid, comprises the steps of:

placing the analytical apparatus in a maintenance operation mode;

operating a metering system, which includes a pump, especially a peristaltic pump, and a supply line for metering volume units of a sample liquid from a source via the supply line into a reactor, the temperature inside the reactor being higher than the boiling temperature of the sample liquid, so that said volume units of the sample liquid metered into the reactor transform into the gas phase following entry into the reactor and a carrier gas in flowing through the reactor;

registering at least one measuring transducer signal for detecting the transforming of the volume unit of the sample liquid into the gas phase; and

deriving, with application of the measuring transducer signal a signal correlated with an instantaneous operating state of the metering system, and

said signal correlated with an instantaneous operating state of the metering system is a status signal, or

said signal correlated with an instantaneous operating state of the metering system has a signal value, from which a feeding capacity of the metering system or liquid volume supplied in a certain unit of time can be derived, or

said signal correlated with an instantaneous operating state of the metering system is a signal representing a time span required for transporting sample liquid from the source into the reactor or value derived therefrom, or

said signal correlated with an instantaneous operating state of the metering system is a signal representing a feed rate of the metering system.

2. The method as claimed in claim 1, wherein:

the analytical apparatus over the duration of operation of the metering system is, placed repeatedly in time intervals, from an analytical operation mode to the maintenance operation mode; and

the signal correlated with the instantaneous operating state is ascertained and stored in a memory.

3. The method as claimed in claim 1, further comprising the steps of:

registering a first point in time, at which operation of the metering system is begun for metering volume units of the sample liquid into the reactor;

registering a second point in time, at which the transformation of a volume unit of the sample liquid metered into the reactor is detected based on the measuring transducer signal; and

determining the time difference between the first and second points in time as the signal correlated with the instantaneous operating state of the metering system.

4. The method as claimed in claim 3, wherein:

the placing of the analytical apparatus into the maintenance operation mode includes a step of removing sample liquid from the supply line, especially by having the pump feed sample liquid from the supply line back into the source until gas escapes from the supply line into the source.

5. The method as claimed in claim 3, wherein:

as a second point that point is registered, for the first time after the first point in time, a transformation of a volume unit metered into the reactor into the gas phase is detected.

6. The method as claimed in claim 1, wherein:

the measuring transducer signal is a pressure signal of a pressure measuring transducer.

7. The method as claimed in claim 6, wherein:

for detection of the transformation of a volume unit metered into the reactor, a sequence of pressure signals is registered, which are correlated with pressure reigning in the reactor.

8. The method as claimed in claim 7, wherein:

a current pressure signal of the sequence is compared with a base value of the pressure in order to ascertain a pressure change, and said pressure change is compared with a predetermined threshold value, and based on a result of the comparison, it is registered, whether the pressure change corresponds to a pressure pulse effected by transformation into the gas phase of a volume unit metered into the reactor.

9. The method as claimed in claim 8, wherein:

the base value of the pressure is formed by average formation, especially by sliding average formation using at least two pressure signals preceding the current pressure signal in the series of pressure signals.

10. The method as claimed in claim 8, wherein:

it is registered to that the pressure change corresponds to a pressure pulse effected by transformation into the gas phase of a volume unit, especially a drop, metered into the reactor is registered when the pressure change exceeds the predetermined threshold value.

11. The method as claimed in claim 1, wherein:

over the duration of operation of the metering system, a trend of the stored signals, especially the time differences, correlated with the operating state of the metering system is determined and evaluated.

12. The method as claimed in claim 11, wherein:

a point in time for maintenance measures, especially for cleaning or for replacement of the supply line, is derived from the trend.

13. The method as claimed in claim 3, wherein:

an adjusting of the analytical apparatus is performed based on the signal, especially the time difference, correlated with the operating state of the metering system.

14. The method as claimed in claim 13, wherein:

the trend of the time differences ascertained in the course of the duration of operation of the analytical apparatus or the metering system is taken into consideration in adjusting the analytical apparatus.

15. The method as claimed in claim 2, wherein:

the signal, especially the time difference, correlated with the operating state of the metering system is used for controlling the metering system.

16. A method for operating an analytical apparatus for determining the concentration of an analyte, especially an oxidizable substance, in a sample liquid, comprises the steps of:

placing the analytical apparatus in a maintenance operation mode;

operating a metering system, which includes a pump, especially a peristaltic pump, and

a supply line, for metering volume unit of a sample liquid from a source via the supply line into a reactor, the temperature inside the reactor being higher than the boiling temperature of the sample liquid, so that said volume units of the sample liquid metered into the reactor transforms into the gas phase following entry into the reactor and a carrier gas is flowing through the reactor;

registering at least one measuring transducer signal for detecting the transforming of the volume units of the sample liquid into the gas phase; and

deriving, with application of the measuring transducer signal, a signal representing an instantaneous operating state of the metering system.

17. The method according to claim 16, said signal representing an instantaneous operating state of the metering system is a status signal, or

said signal representing an instantaneous operating state of the metering system has a signal value, from which a feeding capacity of the metering system or liquid volume supplied in a certain unit of time can be derived, or

said signal representing a time span required to transporting sample liquid from the source into the reactor or a value derived therefrom, or

said signal representing an instantaneous operating state of the metering system is a signal representing a feed rate of the metering system.

18. The method according to claim 16, said signal representing an instantaneous operating state of the metering system being a time interval required for feeding a volume unit of the sample liquid, especially a droplet of said sample liquid, from the source into the reactor.

19. The method according to claim 18, comprising the steps:

moving liquid present in the supply line back into the source;

feeding a volume unit of sample liquid from the source into the reactor;

registering a first pressure pulse, which marks the transformation to the gas phase of a first drop of the sample liquid metered into the reactor;

determining the time difference between the point in time of beginning of feeding said volume unit of sample liquid from the source into the reactor and the point in time at which said first pressure pulse is registered as the signal representative of the instantaneous operating state of the metering system.