JPH0587723A - Method for measuring amount of carbon - Google Patents

Abstract

PURPOSE:To obtain a device for measuring an amount of carbon which improves a reaction efficiency between an organic body within a sample liquid and ozone which is an oxidizer and can measure an accurate amount of carbon. CONSTITUTION:Ozone gas which is generated by an ozone gas generation device 6 is introduced into a deaerator 4, thus enabling a sample liquid to be subjected to bubbling by the ozone gas. Therefore, an inorganic carbon such as carbon dioxide and ion bicarbonate which are dissolved into the sample liquid is deaerated and further ozone gas is dissolved into the sample liquid in saturation state. Then, ozone which is dissolved into the sample liquid by the deaerator 4 converts an organic body within the sample liquid to carbon dioxide efficiently within a reaction vessel 6.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a carbon content measuring device capable of detecting a minute amount of carbon compounds contained in water with high accuracy.

[0002]

2. Description of the Related Art As a carbon content measuring device of this type, as shown in Japanese Patent Application No. 1-186555, a sample solution containing an inorganic carbon and an organic material is subjected to a bubbling treatment under acidic conditions. It is conventionally known that a pretreatment method of first quantifying an organic substance after removing inorganic carbon in a sample liquid is adopted. Specifically, in this carbon content measuring apparatus, after adding a strong acid such as sulfuric acid to a sample solution containing organic or inorganic carbon, helium, nitrogen, etc. were added to the sample solution in the deaerator. An inert gas is sent to bubble the sample solution, and first, inorganic carbon such as carbon dioxide and hydrogen carbonate ions dissolved in the sample solution is expelled to the outside. Next, by feeding the sample solution into a reactor, adding ozone as an oxidant to the sample solution from which inorganic carbon has been removed in the sample solution, and then heating the sample solution under high pressure. The organisms remaining in the sample solution are oxidized and converted into carbon dioxide, which is quantified by a detector,
From this quantitative result, the amount of organic carbon in the sample solution is calculated.

[0003]

By the way, in the carbon content measuring device configured as described above, in the reactor,
Since ozone as an oxidant is added in a gaseous state to the sample liquid from which the inorganic carbon has been removed, that is, ozone and the sample liquid are caused to react by gas-liquid contact, the reaction efficiency is improved. Poorly, this may cause the organism to pass through the reactor without being oxidized, resulting in a problem that the carbon content of the organism cannot be accurately measured.

The present invention has been made in view of the above circumstances, and it is possible to enhance the reaction efficiency between the organism in the sample liquid and ozone as the oxidant, and to make it possible to accurately measure the amount of carbon. The purpose is to provide a quantity measuring device.

[0005]

In order to achieve the above object, in the present invention, a deaerator for removing inorganic carbon in a sample liquid, and a deaerator provided on the downstream side of the deaerator, And a reactor for oxidizing the organisms in the sample liquid to generate carbon dioxide, and measuring the carbon content of the organic carbon concentration in the sample liquid measured from the carbon dioxide produced in the reactor. In the apparatus, an oxidant gas supply device to which an oxidant gas for bubbling the sample solution is supplied is connected to the deaerator.

[0006]

According to the present invention, the oxidant gas such as ozone gas is supplied from the oxidant gas supply device to the sample solution in the deaerator, so that the sample solution is bubbled. As a result, the inorganic carbon in the sample solution is degassed and removed, and the oxidant gas is dissolved in the sample solution. Then, after this, the sample solution in which the oxidant gas is dissolved is supplied to the reactor, and in this reactor, the organism in the sample solution is converted into carbon dioxide by the oxidant gas dissolved in the sample solution. Will be converted. That is, in the reactor, the ozone gas, which is an oxidant gas, does not come into gas-liquid contact with the sample solution as in the conventional case, but the organism in the sample solution and the oxidant gas dissolved in the sample solution And can be reacted directly in the same solution.

[0007]

DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be described below with reference to FIG. In FIG. 1, reference numeral 1 is a sample liquid supply pump, and a sample liquid supply pipe 2 for supplying a fixed amount of sample liquid containing an organic substance is provided on the suction side of the sample liquid supply pump 1. A pipe 3 is provided on the discharge side of the sample liquid supply pump 1, and a deaerator 4 is provided downstream of the pipe 3. The deaerator 4 has an air supply pipe 5 for feeding ozone gas, which is an oxidant, connected to a lower portion thereof, and the ozone gas supplied through the air supply pipe 5 becomes a bubble inside the deaerator 4. By bubbling the sample solution, carbon dioxide, inorganic carbon such as hydrogen carbonate ions dissolved in the sample solution is degassed, and the ozone gas is saturated in the sample solution by bubbling the ozone gas. It is supposed to be dissolved in the state. Then, the ozone dissolved in the sample solution in the deaerator 4 converts the organic matter in the sample solution into carbon dioxide in the reactor 12 described later.

Incidentally, what is indicated by reference numeral 6 in FIG.
An ozone gas generator for sending ozone gas to the deaerator 4 through the air supply pipe 5, and a reference numeral 8 indicates
Exhaust pipes 8, 8 ... For discharging ozone gas not dissolved in the sample solution by bubbling in the deaerator 4 and discharging inorganic carbon expelled from the sample solution by the bubbling. In addition, the ozone gas generator 6
Is a device that produces ozone from oxygen (oxygen-enriched gas) obtained by separating air into nitrogen and oxygen, or a device that produces ozone from oxygen supplied from a separate oxygen supply source (gas cylinder, etc.). It is built in.

A pipe 9 is connected to the outlet of the deaerator 4, and a pressurizing pump 10, a reactor 12 and a fixed throttle 13 are sequentially provided in the middle of the pipe 9. The pressurizing pump 10 is for supplying a mixed liquid composed of the sample liquid and the reaction liquid at a constant pressure and a flow rate into a reactor described later, and the reactor 12 is a drum heater 12
A pipe 9 is spirally wound along a groove (not shown) formed around A, and a thermocouple (not shown) for detecting the temperature inside the pipe is attached to the pipe wall of the pipe 9. In addition, the temperature inside the pipe 9 is controlled to be always constant.

Then, in this reactor 12, ozone gas, which is an oxidant in the sample liquid, is reacted with an organic substance in the sample liquid to generate carbon dioxide from the organic substance. .. The fixed throttle 13 is for increasing the reaction pressure inside the reactor 12 (about 20 atm or more), and vaporizes the sample liquid even if the temperature of the reactor 12 exceeds the boiling point of water. Is something that will not happen. An extractor 20 for extracting carbon dioxide from the sample liquid in which the reaction is completed in the reactor 12 is provided at the end of the pipe 9 and on the downstream side of the fixed throttle 13.

The extractor 20 is provided vertically, and an extraction tower (not shown) for separating the mixed liquid supplied through the nozzle 14 at the end of the pipe 9 into carbon dioxide and drain water (residual). ) And a cooling tower (not shown) for cooling the extraction tower from the surroundings, and a fluid supplied from the pipe 9 (reactor 1
2 is connected to a pipe 23 for feeding an inert gas such as helium or nitrogen for stirring (in which the carbon dioxide generated from the organism is contained in the extractor 20). Further, a pipe 26 provided with a carbon dioxide concentration analyzer 25 for measuring the concentration of carbon dioxide in the gas to be measured is connected to the upper part of the extraction tower of the extractor 20.

Then, based on the result analyzed by the carbon dioxide concentration analyzer 25, the sample liquid supply pipe 2
The ratio of the organic matter contained in the sample liquid supplied from the company is appropriately calculated. It should be noted that the one provided in the middle of the pipe 23 to which the inert gas is supplied is a mass flow controller 23A, and this mass flow controller 23A allows a constant flow rate of the inert gas to be sent to the extractor 20. There is.
Also, provided in the lower part of the extraction tower of the extractor 20 is a pipe 27 for discharging the drain after the carbon dioxide is separated in the extraction tower.

According to the carbon amount measuring device constructed as described above, the ozone gas is bubbled inside the deaerator 4 to bubble the sample solution, and first, the ozone gas is dissolved in the sample solution. By degassing inorganic carbon such as carbon dioxide and hydrogen carbonate ion, and then bubbling the ozone gas, the ozone gas is dissolved in the sample solution in a saturated state. Then, after this, the sample liquid in which ozone gas is dissolved is supplied to the reactor 12, and the reactor 1
In 2, the organic substance in the sample liquid is converted into carbon dioxide by ozone gas which is an oxidant. That is, in the reactor 12, the ozone gas which is an oxidant does not come into gas-liquid contact with the sample solution as in the conventional case, but the organic substance in the sample solution and the ozone gas dissolved in the sample solution are separated from each other. The reaction can be performed directly in the same solution, whereby the reaction efficiency between the ozone gas and the organic substance can be increased, and accurate carbon content can be measured.

Although ozone is used as the oxidant gas in this embodiment, it is not limited to this and hydrogen peroxide in a gaseous state may be used as the oxidant gas. Also,
In order to efficiently remove carbon dioxide, inorganic carbon such as hydrogen carbonate ions, etc. dissolved in the sample solution in the deaerator 4, sulfuric acid which is a strong acid is added to the pipe 3 on the upstream side of the deaerator 4. Means for adding to the sample solution may be provided. Further, in the extractor 20, nitrogen gas for extracting carbon dioxide was supplied from a gas cylinder, but the present invention is not limited to this, and when ozone is generated from oxygen separated from air in the ozone gas generator 6. Similarly, nitrogen separated from air may be used as the extraction gas of the extractor 20.

[0014]

As described in detail above, according to the present invention, the ozone gas, which is the oxidant gas, does not come into gas-liquid contact with the sample liquid in the reactor as in the conventional case, but the sample liquid The organic substance in the inside and the oxidizing gas dissolved in the sample solution can be directly reacted in the same solution, whereby the reaction efficiency between the oxidizing gas and the organic substance can be increased, The effect that an accurate amount of carbon can be measured is obtained.

[Brief description of drawings]

FIG. 1 is a piping diagram of a carbon content measuring device.

[Explanation of symbols]

 4 Deaerator 6 Ozone gas generator (oxidant gas supply device) 12 Reactor

Claims (1)

[Claims] 1. A deaerator for removing inorganic carbon in the sample solution, and a degasser provided downstream of the deaerator to oxidize an organism in the sample solution to generate carbon dioxide. In order to bubble the sample liquid in the degasser, the carbon content measuring device having a reactor for measuring the organic substance concentration in the sample liquid from the carbon dioxide produced in the reactor. The oxidant gas supply device to which the oxidant gas of 1 is connected is connected to the carbon content measuring device.