JPS58132662A - Measuring device for halogen - Google Patents

Abstract

PURPOSE:To enable the automatic analysis of organic and inorganic halides by providing a flask for decomposing a halide with alkali, a flask for titrating alkali halide thus produced, and a device for detecting and quantifying halogen in the flask for titration, etc. CONSTITUTION:A sample is supplied from an automatic sample gathering and injecting device 5 to a flask 1 for decomposing a halide through a supply pipe 21, while a halide- decomposing agent (glycol solution of NaOH or the like) is injected into the flask from a constant-quantity injection device 6 via the pipe 21, and heat decomposition is applied thereto by a heater 14. After the decomposition, the content of the flask is dripped, via a cooling conduit 2, into the inner tank 31 of a flask 3 for titration having the inner and outer tanks 31 and 32, while water used for cleansing the flask 1 and an AgNO3 water solution are dripped into said tank 31 from a device 8 for supplying cleansing water in a constant quantity and a device 7 for supplying AgNO3 in a constant quantity, respectively. While the content of the tank 31 being agitated by an agitator 13, halogen is detected and quantified by a device 4 for potentiometric or coulometric titration, and the result is processed by a data processing device 11. These devices are automated by an attachment 12. This constitution enables continuous analysis in a short time, the incorporation of an analyzing device into a manufacturing process, and the quick control thereof.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention decomposes a sample containing a halogen compound with an alkali to form an alkali halide, and then determines the amount of halogen (tlI).
The present invention relates to a halogen measuring device.

The halogen measuring device currently in common use introduces a sample containing a halogen compound into a combustion tube filled with a catalyst and combusts it with oxygen, air, or a warm mixture of these and an inert gas, producing a known halogen gas. A method of detecting and quantifying with a colorimetric analysis needle or a coulometric titration device is used. However, since the generally used halogen measurement AT is a method aimed at measuring organic halogen compounds, inorganic halogen compounds such as sodium bromide are not completely measured, and other inorganic halogen compounds It is necessary to use a method suitable for quantification, and the decomposition of the sample requires conditions of high temperature of 700 to 1100° C. in an oxygen stream, which has operational safety drawbacks.

In general, automatic analysis needles that measure the atomization of substances in a specimen continuously or four times are widely used in the industrial world, and this is because the atomization of halogen compounds in the manufacturing process is
*The same applies to automatic halogen measuring devices for measuring halogen compounds, but conventional halogen measuring devices send samples containing halogen compounds to an analytical testing laboratory, where they are injected into the halogen measuring device and analyzed. Generally, this information is sent back to the process, and this method requires a considerable amount of time, making continuous management of the process difficult.

The present invention solves the above-mentioned drawbacks of the conventional halogen measuring device and provides a halogen measuring device convenient for measuring the halogen content in a sample during automatic fishing. That is, the present invention provides θ) a flask for halogen compound decomposition (this is an injection tube for injecting a sample, an injection tube for injecting a halogen compound decomposition agent, a sample heating device, and a cooling substance that evaporates during decomposition of a halogen compound) ■ A cooling conduit to guide the molecule to the titration flask while cooling it ■ A titration flask (this is a stirrer to stir the decomposed liquid, and to keep the temperature inside the flask at a constant temperature) (2) A device for detecting and quantifying the amount of halogen in the titration flask (2) A device for detecting and quantifying the amount of halogen in the titration flask. This is a halogen measuring device that will later measure the amount of halogen.

The present invention will be explained with reference to the drawings. In FIG. 1, l is a flask for decomposing halogen compounds, and is made of an AI-sized quartz tube or hard glass tube, or a corrosion-resistant metal. Further, 1 is 1g2 FIG. 4 To explain in detail, 21 is an injection tube for injecting a sample, and 22 is an injection tube for injecting a halogen compound decomposer. As the decomposing agent, strongly alkaline alcohols or glycols such as caustic soda and caustic potash are preferable, such as methanol, diethylene glycol, triethylene glycol, etc. The selection of these substances depends on the form of the halogen compound contained in the sample, It is selected appropriately depending on the boiling point, etc. 23 heats the injected sample and decomposer for one session,
This is the part that decomposes the halogen compound in the sample to generate an alkali halide, and the heating ff1 degree is 100 to 30 degrees.
It is necessary to maintain a constant temperature selected between 0°C. This change in temperature and heating time causes a large error in the amount of halogen detected and quantified in the sample. 24 is 23
A cooling tube 25 for cooling the substances that evaporate during the decomposition of the halogen compound in the sample, and which circulates wood, is installed inside. The upper part of the flask is opened to the atmosphere in order to maintain the entire flask under normal pressure. 264 minutes A cleaning tube for cleaning the inside of the scale flask, 2
After being thermally decomposed for a certain period of time in step 3, an appropriate amount of washing water is flowed through 26, and the decomposition liquid is washed into the titration flask 3 through the drain pipe 27 and the cooling conduit 2 shown in FIG. The titration flask 3 is a hard glass flask of a size suitable for overnight use, and is used to detect and quantify the alkali halide in the decomposed liquid. To explain this in more detail in Figure 3, the titration flask 3 has an inner tank 31 and an outer tank 3.
The decomposition liquid and cleaning liquid introduced into the internal tank 31 detect and quantify the amount of halogen therein, and then flow an appropriate amount of water from the cleaning pipe 33 to clean the internal tank 31.
Washing water overflowing from the tank 32 flows into an external tank 32, and is discharged through a drain pipe 34, and the washing water accumulated in the tank 31 is discharged through a drain pipe 35. Internal tank 31
It is better to soak the halogen 1lIII standard electrode installed in water in terms of maintenance, so the drain pipe 35
Appropriate amount of cleaning liquid is dispensed by 36 connected to 3.
f14jlI so that it remains within 1. If the next sample is to be measured, the cleaning solution in 31 is drained before the decomposition solution enters 31. The tip of a pipe 37 branching off from the drain pipe 35 is open to the atmosphere, which has the effect of smoothly draining the cleaning liquid in the pipe 31. Returning to FIG. 1 again, 4 is a device for detecting and quantifying the amount of halogen in the titration flask 3, and a commercially available potentiometric titration device or electrot*meter can be used. 5 is an automatic sample collection/injection device connected to 21 in Figure 2, 6 is a device for injecting a certain amount of decomposing agent and connected to 22 in Figure 2, and 7 is for detecting and quantifying the amount of halogen. This is a device for injecting a fixed amount of a nitric acid aqueous solution of an appropriate concentration into the internal tank 31 of the titration flask 3. 8 is a device for making water for washing flow at a certain rate;
10 is a cock used to supply water to the device 8 from the outside. 11 is a data processing device, and 12 is an accessory device for automating the halogen measuring device, both of which may be commercially available items. Reference numeral 13 is a stirrer for stirring the solution in the internal tank 31 of the one-time use flask 3, and 14 is a heating section for heating the decomposition flask 1.

According to Zeroyamei, the sample, decomposition solution, etc. are automatically injected into the decomposition flask and thermally decomposed, the inside of the decomposition flask is automatically cleaned, and the solution is transferred to the titration flask and decomposed. The amount of halogen in the liquid is automatically measured, and after the measurement, the solution in the titration flask is automatically cleaned in preparation for the next measurement. In this way, it is possible to eliminate the shortcomings of conventional measuring devices in terms of operation and safety, and to measure both organic and non-horizontal halogen compounds. It is used as an automatic analyzer for quantitative titration.

Example 1) Analysis conditions Decomposition flask temperature f 200-250℃ Decomposition agent Aqueous solution of sodium hydroxide and triethylene glycol
35- Decomposition time 30 minutes Sample amount 1.5- Measurement of alkali halide Nitric acid faIII standard method using potentiometric measuring device 2) Analysis method and quantitative results Determine the correction coefficient of the nitrate** aqueous solution in advance using the sodium chloride standard solution. , No. 10 Samples with unknown amounts were quantified using a conventional method using a potentiometer. The quantitative results were in good agreement with the known amounts as shown in Table 1.

We also measured representative substances for organic halogen compounds and amorphous halogenated compounds. The results were in good agreement with the known amounts as shown in Table 2.

[Brief explanation of drawings]

FIG. 1 is a schematic overall view of the halogen measuring apparatus of the present invention, FIG. 2 is a detailed view of a flask for decomposing a halogen compound, and FIG. 5 is a detailed view of a titration flask. Patent applicant Mitsubishi Gas Chemical Co., Ltd. Representative Kazuyoshi Nagano Figure 7 1! ＞2 Diagram tail 3 Procedural amendment (voluntary) Raskohei>if ----------Ninth name;'EA
Arrived. I also used the old -bs + 1 conversion.〉Revision and attached scope of patent claims■ Flask for decomposing halogen compounds (The stiffness is an injection tube for injecting a sample, a halogen compound decomposition agent) (It includes an injection tube for injecting the halogen compound, a sample heating device, and a cooling tube for cooling the substances that evaporate during the decomposition of the halogen compound.) ■ A cooling conduit for guiding the decomposition liquid to the titration flask while cooling it. ■ A titration flask (equipped with a stirrer to stir the decomposition liquid) and a device for detecting and quantifying the amount of halogen in the 111i titration flask.The halogen compound is decomposed with an alkali to produce an alkali halide. A halogen column measuring device that measures the amount of halogen after

Claims (1)

[Claims] ■ Flask for decomposing halogen compounds (this is an injection tube for injecting a sample, an injection tube for injecting a /10-gen compound decomposition agent, a sample heating device, a substance that evaporates during the decomposition of a halogen compound) ) ■ Cooling conduit α to guide the decomposition liquid to the titration flask while cooling it> * titration flask (This is a stirrer for stirring the decomposition liquid, and the flask internal temperature (equipped with a heating device to maintain the temperature at a constant temperature, an injection tube for injecting samples and reagents), and a device for detecting and quantifying the amount of halogen in the titration flask. Halogen measuring device that measures the amount of halogen after converting it into an alkali halide