JP3211462B2 - Carbon measuring device - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to an apparatus for measuring carbon content in samples such as solids and liquids, and more particularly to a carbon apparatus for measuring inorganic carbon (hereinafter simply referred to as IC) in contaminated soil, polluted water and sediment. It relates to a measuring device.

[0002]

2. Description of the Related Art In a conventional IC measurement, a sample is placed in an aqueous solution of a non-oxidizing protonic acid, heated and reacted under sufficient stirring, and substantially mixed with a mixed solution of the aqueous solution and the sample. An inert carrier gas containing no carbon dioxide is blown, and the carbon dioxide in the sample generated by the above reaction is extracted into the carrier gas, and the carbon dioxide in the carrier gas is detected by a gas detector. Kaisho 60-1
No. 42256).

[0003]

However, the time required for heating the mixed solution of the non-oxidizing protonic acid aqueous solution and the sample and extracting carbon dioxide becomes long, which is troublesome.
Further, when measuring total organic carbon (TOC), there has been a problem that it is difficult to perform continuous measurement and automation with conventional IC measurement.

An object of the present invention is to provide a carbon measuring apparatus which can reduce the time required for extracting an IC component in a sample and can easily cope with continuous measurement and automation.

[0005]

In order to achieve the above object, the carbon measuring apparatus of the present invention employs a method in which a sample is placed on a boat and the sample is introduced into a heating reaction section by a boat operating mechanism. With an inlet / outlet of a sample boat communicating with the section and an opening / closing mechanism for the sample boat, and an acid dispenser for adding a non-oxidizing protonic acid that does not absorb carbon dioxide to a sample on the boat when the opening / closing mechanism is closed. It is.

Accordingly, by separately installing a reaction section for measuring the total amount of carbon (TC) and arranging the reaction section and the heating reaction section (reaction section for IC measurement) in series, the flow path is simplified.
It is possible to realize a carbon measuring device capable of performing OC (= TC-IC) measurement quickly and with high sensitivity.

[0007] As the non-oxidizing protonic acid, phosphoric acid, acidic phosphate and the like are preferred.

[0008]

In the carbon measuring apparatus constructed as described above, the sample to which the non-oxidizing protonic acid is added is introduced into the reaction section for IC measurement by moving the boat.
Under the action of accelerating the reaction between the component and the acid, stirring, driving away, etc., the carbon dioxide generated by the reaction is rapidly extracted into the gas phase.

[0009]

DESCRIPTION OF THE PREFERRED EMBODIMENTS The carbon measuring apparatus of the present invention will be described below with reference to the drawings.
An apparatus embodiment for measuring TOC by arranging a C measurement reaction section 2 in series is shown.

In the TC measuring reaction section 1, a quartz glass reaction tube (combustion tube) 3 is disposed through a TC furnace (combustion reaction tubular electric furnace) 4. A sample introduction mechanism 6 having an entrance and an opening / closing mechanism is connected. The sample is placed on a ceramic boat 5 and put into the apparatus through an inlet of the sample introduction mechanism 6 and the inlet is closed. Then, the boat 5 is moved in the reaction tube 3 by operating the boat operating rod 7 and the temperature is 900 ° C. It is introduced into the TC furnace 4 which has been heated to a moderate degree.

The rear half of the reaction tube 3 is filled with a well-known oxidation catalyst 8, and organic matter in the sample evaporates or decomposes in the TC furnace 4 (reaction tube 3) to contain oxygen. The organic material reaches the oxidation catalyst layer 8 together with the carrier gas, and all organic substances are oxidized to carbon dioxide gas by the action of the catalyst. This carbon dioxide gas passes through the cooling pipe 9, the drain separator 10, a reaction section 2 for IC measurement to be described later, and the drain separator 10 again together with the carrier gas, for example, a non-dispersive infrared gas analyzer (NDIR) (not shown). T in the sample
C is measured. In addition, 11 and 12 are cooling fans.

The reaction section 2 for IC measurement basically has a TC
The configuration is the same as that of the measurement reaction section 1 except that the sample is
3, the sample is introduced into the apparatus from the entrance of the sample introduction mechanism 14, the entrance is closed, and then the boat operation rod 15 is operated to move the boat 13 through the reaction tube 16 before introducing the boat 13 into the IC furnace 17. The inorganic acid is added from the acid dispenser 18 to the sample on the boat 13. As the acid, phosphoric acid, which is a nonvolatile acid, is preferable.

The temperature of the IC furnace 17 is relatively lower than that of the TC furnace 4 (for example, 250 ° C.).
The reaction between the C component and the acid is promoted, and further, the carbon dioxide converted and generated by the reaction is rapidly extracted into the gas phase by the stirring and the expulsion by heating. The extracted carbon dioxide gas passes through the drain separator 10 together with the carrier gas and, for example, ND
It is guided to an IR (not shown) to measure the IC in the sample. The supply of the carrier gas to the IC measurement reaction section 2 is T
The reaction is performed from the reaction section 1 for C measurement via the cooling pipe 9 and the drain separator 10.

Therefore, in this embodiment, TC measurement and IC
The measurements are not performed simultaneously, but both measurements can be performed consecutively.

[0015]

As described above, according to the present invention, it is only necessary to add a small amount of acid to a sample and introduce it into an IC furnace, so that the time required for heating and carbon dioxide extraction for the sample is greatly reduced. can do. Further, as in the above-described embodiment, it is easy to provide a device configuration for measuring the TOC by arranging the reaction section for TC measurement and the reaction section for IC measurement in series. Simplified, TC measurement and IC measurement can be performed continuously, and the carrier gas flow rate during both measurements is always the same, so that there is no change in the detector sensitivity between both measurements, and stable measurement can be performed. Becomes possible.

[Brief description of the drawings]

FIG. 1 is a schematic view of the device of the present invention.

[Explanation of symbols]

DESCRIPTION OF SYMBOLS 1 ... Reaction part for TC measurement 2 ... Reaction part for IC measurement 3 ... TC reaction tube 4 ... TC furnace 5, 13 ... Sample boat 6,14 ... Sample introduction mechanism 7,15 ... Boat operation rod 8 ... Oxidation catalyst 10 ... Drain Separator 16: IC reaction tube 17: IC furnace

Claims (1)

(57) [Claims] 1. A method in which a sample is placed on a boat and the sample is introduced into a heating reaction section by a boat operating mechanism, comprising a sample boat entrance and an opening / closing mechanism for the sample boat. A carbon measuring device comprising an acid dispenser for adding a non-oxidizing protonic acid that does not absorb carbon dioxide to the sample.