Closed heat-decomposing appliance, pretreatment method of sample using it, analytical method and device therefor

Abstract

Disclosed are a closed heat-decomposing appliance comprising a heating section with one side closed and other side having common ground portion, screw portion or O-ring-mounted portion and a closed introducing section that allows to connect to this heating section and common ground portion, screw portion or O-ring via O-ring-mounted portion and has cock or valve as a mechanism for closing and introducing the absorbing liquid to absorb the testing components from outside after heat-decomposition, or has packing or septum to introduce the absorbing liquid with needle pipe as well, and a pretreatment method of sample using this appliance. The purpose is to provide a closed heat-decomposing appliance for the pretreatment on accurate quantitative determination or detection of the testing components in sample, which requires no combustion assistant, which is not obstructed by ash present in sample absorbing the testing components, which requires no complicated and dangerous procedures, which can be used repeatedly, and which allows to inject the absorbing liquid after heat-decomposition, and a pretreatment method using it.

What is claimed is:  
     
         1 . A closed heat-decomposing appliance being an appliance for horizontally or slantly inserting heating section into a heating device to heat, decomposing the inner organics in the presence of oxygen gas, taking out from the heating device and cooling, then introducing the absorbing liquid to absorb the testing components, comprising a heating section with one side closed and other side having common ground portion, screw portion or O-ring-mounted portion and a closed introducing section that allows to connect to this heating section by common ground portion, screw portion or O-ring via O-ring-mounted portion and has cock or valve as a mechanism for closing and introducing the absorbing liquid to absorb the testing components from outside after heat-decomposition, or has packing or septum to introduce the absorbing liquid with needle pipe as well.  
     
     
         2 . A pretreatment method comprising the steps of setting up the sample which may sometimes contain organics in the closed heat-decomposing appliance of  claim 1 , filling up oxygen and closing, then heating to decompose the organics, followed by cooling, and thereafter introducing the absorbing liquid into said closed heat-decomposing appliance to absorb the testing components in said sample.  
     
     
         3 . The pretreatment method of sample of  claim 2 , wherein the testing components) is(are) one kind or two or more kinds selected from a group consisting of halogen and sulfur.  
     
     
         4 . The pretreatment method of sample of  claim 2  or  claim 3 , wherein the amount of oxygen gas to be filled up is not less than 2.5 times the amount of oxygen gas required for complete combustion of sample.  
     
     
         5 . A device for heat-decomposing the sample which may sometimes contain organics using the closed heat-decomposing appliance of  claim 1 , comprising an appliance-installing section to install said closed heat-decomposing appliance, a heating means to heat-decompose the sample in said closed heat-decomposing appliance and a moving means to reversibly move said closed heat-decomposing appliance installed at said appliance-installing section to said heating means.  
     
     
         6 . A pretreatment method of sample, comprising the steps of setting up the sample which may sometimes contain organics together with oxygen in the closed heat-decomposing appliance of  claim 1  and closing, and then heating said closed heat-decomposing appliance with device of  claim 5  to decompose the organics which may be sometimes contained in said sample.  
     
     
         7 . A device for heat-decomposing the sample and dissolving the testing components produced, comprising, adding further to the device for heat-decomposing sample of  claim 5 , a cooling means to cool the closed heat-decomposing appliance after heat-decomposition of sample in said closed heat-decomposing appliance, an injecting means to inject the absorbing liquid into said cooled closed heat-decomposing appliance, a mixing means to stir and/or shake for making the absorbed liquid in said closed heat-decomposing appliance uniform, and a moving means to reversibly move said closed heat-decomposing appliance from appliance-installing section to any of said heating means, cooling means, injecting means and mixing means.  
     
     
         8 . A pretreatment method of sample, comprising the steps of setting up the sample which may sometimes contain organics together with oxygen in the closed heat-decomposing appliance of  claim 1  and closing, then heating said closed heat-decomposing appliance to decompose the organics which may be sometimes contained in said sample, thereby producing the testing components, cooling said closed heat-decomposing appliance, injecting the absorbing liquid into said heat-decomposing appliance to dissolve the testing components, and further stirring and/or shaking said closed heat-decomposing appliance to make said absorbed liquid in the closed heat-decomposing appliance uniform, with the device of  claim 7 .  
     
     
         9 . A device for analyzing the testing components, comprising, adding further to the device for heat-decomposing the sample and dissolving the testing components produced of  claim 7 , an analytical means to analyze the testing components in absorbing liquid and a moving means to sample part of the absorbing liquid inside the closed heat-decomposing appliance and to move to said analytical means.  
     
     
         10 . An analytical method, comprising the steps of setting up the sample which may sometimes contain organics together with oxygen in the closed heat-decomposing appliance of  claim 1  and closing, then heating said closed heat-decomposing appliance to decompose the organics, followed by cooling, injecting the absorbing liquid to dissolve the testing components, stirring and/or shaking said closed heat-decomposing appliance to make the absorbed liquid in the closed heat-decomposing appliance uniform, and then analyzing the testing components in absorbed liquid with the device of  claim 9 .  
     
     
         11 . A device in the device of  claim 7  or  claim 9 , comprising 
 a needle pipe,  
 a motor buret,  
 a switchable valve with actuator,  
 a moving means of needle pipe to pierce through packing or septum of the closed heat-decomposing appliance and to move to washing boat, and  
 a washing port to wash the contaminated needle pipe, as an injecting means of absorbing liquid into the closed heat-decomposing appliance.  
 
     
     
         12 . A device in the device of  claim 7  or  claim 9 , comprising a means to reciprocate the closed heat-decomposing appliance in the axial direction of closed heat-decomposing appliance, while rotating it centering to the axis of closed heat-decomposing appliance, leaving horizontal, as a mixing means.  
     
     
         13 . A device in the device of  claim 7  or  claim 9 , comprising a cross type motor robot with mechanical hand or a mechanical hand and cross type motor robot with axis for rotating it, as a moving means.