JPS60133364A - Detection of sulfur in liquid or solid sample - Google Patents

Abstract

PURPOSE:To detect S components in a sample handily by a method wherein a liquid or solid sample is sampled into a test tube having an air introduction port for combustion on the side thereof, an injection cylinder mounted at the end of the test tube and a sample is heated to sample a gas containing SO2 gas generated into the injection cylinder. CONSTITUTION:A liquid or solid sample 1a is sampled into a test tube 1 having an air introduction port 1b for combustion on the side thereof and the tip of an outer cylinder 3a of an injection cylinder 3 is connected to the test tube 1 with a vacuum rubber tube 2. The sample 1a is heated with a heater 4 and after an inner cylider 3b is pulled out, a gas containing SO2 generated is sucked into the cylinder 3. Then, the injection cylinder 3 of completed suction is connected to a glass tube 5 housing an SO2 detecting agent 5b with cotton plugs 5 and 5a applied at both ends thereof and the vacuum rubber tube 2 and then, the gas in the cylinder 3 is extruded to observe the presence of decoloring of the detecting agent 5b. This enables a handy and quick detection of S components in the liquid or solid sample.

Description

DETAILED DESCRIPTION OF THE INVENTION The present invention relates to an improved method for detecting sulfur in liquid or solid samples.

In analytical chemistry, it is important to detect sulfur contained in gases, liquids, or solids using a quick and simple method and to understand its concentration, especially in flue gas emitted from various combustion equipment. Measuring the sulfur concentration in water is essential when considering equipment performance evaluation and environmental measures. JIS K as a method for detecting sulfur in gas
[0103] Various methods are specified in "Method for analyzing total sulfur oxides and sulfur dioxide in exhaust gas," among which a detection tube method is described as a simple method. A method of detecting sulfur using a detection tube will be explained with reference to FIGS. 1 to 5. Here, FIG. 1 is a diagram showing a configuration example of a sample gas sampling device, FIG. 2 and FIG. 6 are diagrams showing a detection tube and a dehumidification tube, respectively, and FIG. 4 is a diagram showing a vacuum type It is a side view of a gas extractor,
FIG. 5 is a diagram showing an example of sulfur dioxide concentration determined by the detector tube method.

Each symbol in Figures 1 to 4 has the following meaning.

A...Sample gas sampling tube B...Silicon rubber C...
Detection tube D...Dehumidification tube E...Thermometer F...Heater G...Vacuum gas sampling tube H...Diamond cutter ■ ・1 detection tube installation hole J...Piston hole) One on the handle - Piston stopper L...Gas outlet M...
Suction speed adjustment plate a...Detecting agent b, b/... Cotton C, Q'
...melt sealing part d...dehumidifier e, e'...glass wool f, f'...melting part Next, the equipment used in the detection tube method and its operation method will be explained.

(1) Detector tube: The detector tube (Figure 2) has an inner diameter of 2.5 mm.
.

Fill a glass tube with a total length of about 130 m + n with a certain amount of detection agent a, so that the length of 1 meter of filling is 60 to 80 squares, and fix both ends with cotton wires b and b'. Q' is melt-sealed. Detecting agent A is prepared by adhering 100 m of a bulk potassium solution (θ2 w, "v%) to 100 g of 250-300 μm silica gel particles, drying it, and reacting with sulfur dioxide to turn orange.

(11) Dehumidification tube: The dehumidification tube (Figure 3) removes moisture from exhaust gas, and is used in conjunction with the detection tube.

The dehumidifying tube is made by filling a glass tube with an inner diameter of about 5 mm and a total length of about 100 mm with dehumidifying agent d, making the length of the filling layer about 30 mm, fixing both ends with glass wool e and θ', and fixing both ends of the glass tube. f.

fl is melt-sealed. Dehumidifier is 250-300μ
40 tnl of sulfuric acid was attached to ±100 g of bamboo. Currently, a type of detection tube is commercially available in which a dehumidifier is integrally sealed at the tip of the detection tube in order to remove a small amount of moisture.

(liD Sample gas sampler; A vacuum type gas sampler is used to collect sample gas. The vacuum type gas sampler (Figure 4) is
It is a metal pump with an internal volume of 100 m, and in order to keep the suction speed of the sample gas constant, the suction speed adjustment plate M (made of stainless steel, thickness 0.26 aun) has a diameter of 925mm, a center hole diameter of o,
1mm) and pull the piston handle all at once to automatically inhale the sample gas.

4V) Sulfur dioxide concentration table In the sulfur dioxide concentration table (Figure 5), the interval between the 0-0 line and the L-L line corresponds to the length of the detection agent layer, and a straight line representing the sulfur dioxide concentration is placed in the middle. , and the sulfur dioxide concentration is scaled at both ends.

(1) Turn on the power to the heater (F in Figure 81) of the sample gas sampling device, and suck the exhaust gas with a suction pump (not shown) (at this time, keep the part B sealed).

(11) When the reading on thermometer E reaches 120℃ or above, cut off both ends of the detection tube C and the dehumidifying pipe, and connect them with rubber tubes.
Insert it into the measurement location, attach the other end to the vacuum gas sampler G, and while sucking the exhaust gas with the suction bonder, pull the piston/handle of the vacuum gas sampler all at once to fix it, and leave it for 3 minutes. .

011) Remove the detection tube C, align both ends of the detection agent layer with the 0-0 line (gas inlet side) and the L-L line on the sulfur dioxide concentration topsoil, and immediately measure the sulfur dioxide concentration at the boundary of the colored layer. Read it.

The detection tube method in ``Analytical power and method for total sulfur oxides and sulfur dioxide in exhaust gas'' is intended for gases such as exhaust gas, and cannot be applied to samples such as liquids and solids. It is possible.

Therefore, the present invention provides a method for easily detecting sulfur contained in a liquid or solid, and combines the conventional detection tube method for measuring sulfur contained in a gas with a combustion decomposition vessel for a sample. By combining these methods, it is possible to detect sulfur contained in liquids or substances.

That is, the present invention collects a liquid or solid sample in a thin test tube having a combustion air inlet on the side, attaches a syringe to the end of the test tube, and then collects the sample from the test tube. The sample is heated to burn and decompose the sample, gasifying the sulfur content in the sample into sulfur dioxide, and sucking the inner cylinder of the syringe to collect gas containing sulfur dioxide into the syringe. Next, remove the test tube from the syringe, attach a sulfur dioxide detection tube filled with a sulfur dioxide detection tube to the tip of the syringe E7, and detect the sulfur dioxide by pushing down the inner tube of the syringe. The following relates to a method for detecting sulfur in a liquid or solid sample, which is characterized by introducing a gas containing sulfur dioxide in the syringe into a tube and qualitatively determining the concentration of sulfur dioxide from a discolored detection agent layer. Next, the method of the present invention will be explained based on FIGS. 6 and 7.

Figure 6 is a diagram showing the procedure for burning a liquid or solid sample in a combustion decomposition vessel and collecting the combustion decomposition gas into a syringe, and Figure 7 shows sulfur detection using a detection tube from the gas collected from the syringe. It is a diagram showing the situation. , 1 The combustion decomposition vessel 1 for combustion decomposition of the analysis sample 1a is:
It is connected to the tip of a syringe barrel 3 via a vacuum rubber tube 2. A combustion air inlet 1b is provided in the lower side wall of the combustion decomposition vessel 1.

The syringe barrel 3 consists of an outer barrel 3a and an inner barrel 3b, and contains the analysis sample 1.
It is used to suck in air and collect the generated combustion exhaust gas during combustion decomposition of a, and also to forcefully feed the combustion exhaust gas to the detection tube 5, as shown in FIG. Reference numeral 4 denotes a heating means, which can be a medicinal lamp, an alcohol lamp, a Bunsen burner, or the like, and is a heating source for heating the bottom of the combustion decomposition vessel 1 and gasifying the sulfur contained in the analysis sample 1a. The tip of the syringe 6 that has collected the combustion exhaust gas is connected to the detection tube 5 through the vacuum rubber tube 2, as shown in FIG.
connected to.

The detection tube 5 is filled with a detection agent 5b that reacts with sulfur dioxide to exhibit a unique coloration, and cotton plugs 5a are stuffed at both ends to retain the detection agent 5b.

The detection operation is performed according to the following procedure.

(1) Weigh a certain amount of the analysis sample 1a into the combustible analyzer 1.

(2) Connect the tip of the syringe 3 and the combustion decomposition container 1 to the vacuum rubber tube 2
Connect via.

(3) While gradually heating the bottom of the combustion decomposition vessel 1 with the heating means 4, pull up the inner cylinder 3b of the syringe barrel 6.

(4) Continue this operation until the analysis sample 1a is completely burned and decomposed.

(5) Remove the syringe barrel 6 from the combustion decomposition vessel 1.

(6) Connect the tip of the syringe barrel 3 to the detection tube 5 via the vacuum rubber tube 2.
Connect to.

(7) Detection agent 5b in which the inner cylinder 3b of the syringe barrel 6 is pushed into the outer cylinder 6a and the combustion exhaust gas in the inner cylinder 3b is filled into the detection tube 5.
Pass through the layers.

(8) The amount of sulfur is determined from the length of the colored layer of the detection agent 101).

Thus, according to the method of the present invention, sulfur in a liquid or solid can be detected simply and quickly. −

[Brief explanation of the drawing]

1 to 5 are diagrams for explaining a conventional sulfur detection method using a detection tube. Among these, Fig. 1 shows an example of the configuration of the sample gas sampling device, Figs. 2 and 3 show a detection tube and a dehumidification tube, respectively, and Fig. 4 is a side view of the vacuum type gas sampling device. Figure 5 shows an example of sulfur dioxide concentration determined by the detector tube method. 6 and 7 are schematic diagrams illustrating the method of the present invention. Among these, FIG. 6 shows how sulfur is collected by a combustion decomposition vessel, and FIG. 7 shows how sulfur is detected by a detection tube. Sub-Agent 1) Meifu Agent Ryo Hagiwara - Figure 1 Figure 2

Claims (1)

[Claims] A liquid or solid sample is collected in a thin test tube with a combustion air inlet on the side, a syringe is attached to the end of the test tube, and the sample collection part of the test tube is heated and collected. The sample is burned and decomposed to gasify the sulfur content in the collected sample to sulfur dioxide, and the inner cylinder of the syringe is sucked to collect gas containing sulfur dioxide into the syringe. Remove the test tube from the syringe, attach a sulfur dioxide detection tube filled with sulfur dioxide detection agent to the tip of the syringe, and press down the inner barrel of the syringe to detect the amount of sulfur dioxide in the syringe. A method for detecting sulfur in a liquid or solid sample, characterized by introducing a gas containing sulfur dioxide and qualitatively determining the concentration of sulfur dioxide from a discolored detection agent layer.