阅读说明：本技术 一种高氯含量有机物中氯含量的测定方法 (Method for measuring chlorine content in high-chlorine-content organic matter ) 是由 吴惠勤 黄晓兰 韩必恺 周熙 于 2020-12-11 设计创作，主要内容包括：本发明公开了一种高氯含量有机物中氯含量的测定方法。它包括S1:称取高氯含量有机物样品于容量瓶中,用有机溶剂溶解,并加入助燃剂,定容后吸取定量溶液,分散滴加于滤纸上,有机溶剂挥发后,置于氧瓶中燃烧,氢氧化钾溶液吸收燃烧生成的氯化氢；S2：采用离子色谱对溶液中氯离子含量进行定量。本发明通过有机溶剂溶解高氯含量有机物样品,使有机物分散于滤纸表面。同时,加入助燃剂,帮助高氯有机物燃烧,达到完全燃烧的目的,使有机物中的有机氯全部转化为氯化氢,而被氢氧化钾溶液吸收,从而克服由于成团的有机物燃烧不完全,即样品中有机氯转化不完全,造成测定的氯含量偏低的问题,提高氯含量测定的准确性。(The invention discloses a method for measuring chlorine content in high-chlorine-content organic matters. Weighing an organic matter sample with high chlorine content in a volumetric flask, dissolving the organic matter sample with an organic solvent, adding a combustion improver, absorbing a quantitative solution after constant volume, dispersedly dropping the solution on filter paper, putting the filter paper in an oxygen flask for combustion after the organic solvent is volatilized, and absorbing hydrogen chloride generated by combustion with a potassium hydroxide solution; s2: and (4) quantifying the content of chloride ions in the solution by adopting ion chromatography. According to the invention, the organic matter is dispersed on the surface of the filter paper by dissolving the organic matter sample with high chlorine content by the organic solvent. Meanwhile, the combustion improver is added to help the high-chlorine organic matter to be combusted, so that the purpose of complete combustion is achieved, the organic chlorine in the organic matter is completely converted into hydrogen chloride and absorbed by the potassium hydroxide solution, the problem that the chlorine content is low due to incomplete combustion of the clustered organic matter, namely incomplete conversion of the organic chlorine in the sample is solved, and the accuracy of chlorine content determination is improved.)

1. The method for measuring the chlorine content in the high-chlorine-content organic matter is characterized by comprising the following steps of:

s1: weighing a quantitative high-chlorine content organic matter sample in a volumetric flask, dissolving the high-chlorine content organic matter sample in an organic solvent, adding a combustion improver, absorbing a quantitative solution after constant volume, dispersing and dripping the quantitative solution on filter paper, placing the filter paper in an oxygen flask for combustion after the organic solvent is volatilized, and absorbing hydrogen chloride generated by combustion by a potassium hydroxide solution;

or weighing a quantitative high-chlorine content organic matter sample in a volumetric flask, dissolving the high-chlorine content organic matter sample in an organic solvent, absorbing a quantitative solution after the constant volume, dispersing and dripping the quantitative solution on filter paper, adding a combustion improver on the filter paper after the organic solvent is volatilized, putting the filter paper in an oxygen bottle for combustion, and absorbing hydrogen chloride generated by the combustion by using a potassium hydroxide solution;

s2: and (4) quantifying the content of chloride ions in the solution by adopting ion chromatography.

2. The method according to claim 1, wherein the organic solvent is petroleum ether or tetrahydrofuran.

3. The method according to claim 1, wherein the combustion improver is No. 200 mineral spirit.

4. The assay according to claim 1, 2 or 3, wherein said ion chromatography is performed using AS23 (4X 250mm) column with 4.0mmol/L Na AS mobile phase₂CO₃+1.4mmol/L NaHCO₃Water solution, isocratic elution, the flow rate is 0.8 mL/min; the column temperature is 30 ℃; the sample volume is 10 mu L; DS5 conductivity detector; AERS 500 anion suppressor with suppressor current 23 mA.

The technical field is as follows:

the invention relates to the technical field of analysis and detection, in particular to a method for measuring chlorine content in high-chlorine-content organic matters.

Background art:

the chlorine content of high-chlorine content organic matters is usually an important index for characterizing the high-chlorine content organic matters. Currently, oxygen bottle combustion-ion chromatography is the common method for determining chlorine content. But is not suitable for the determination of samples with high chlorine content because the method has a severely low determination value. Researches find that the high-chlorine substituted organic matter generally has certain flame retardance, and the content of the measured chlorine is low because the clustered organic matter is not completely combusted, namely the organic chlorine in the sample is not completely converted when the sample is directly dripped on the filter paper according to the existing method.

The invention content is as follows:

the present invention has been made in view of the above problems, and an object of the present invention is to provide a method for measuring a chlorine content in a high-chlorine-content organic substance, which can completely burn the high-chlorine organic substance and is suitable for measuring a chlorine content in the high-chlorine-content organic substance.

The method for measuring the chlorine content in the high-chlorine-content organic matter comprises the following steps of:

s1: weighing a quantitative high-chlorine content organic matter sample in a volumetric flask, dissolving the high-chlorine content organic matter sample in an organic solvent, adding a combustion improver, absorbing a quantitative solution after constant volume, dispersing and dripping the quantitative solution on filter paper, placing the filter paper in an oxygen flask for combustion after the organic solvent is volatilized, and absorbing hydrogen chloride generated by combustion by a potassium hydroxide solution;

or weighing a quantitative high-chlorine content organic matter sample in a volumetric flask, dissolving the high-chlorine content organic matter sample in an organic solvent, absorbing a quantitative solution after the constant volume, dispersing and dripping the quantitative solution on filter paper, adding a combustion improver on the filter paper after the organic solvent is volatilized, putting the filter paper in an oxygen bottle for combustion, and absorbing hydrogen chloride generated by the combustion by using a potassium hydroxide solution;

s2: and (4) quantifying the content of chloride ions in the solution by adopting ion chromatography.

Preferably, the organic solvent is an organic solvent capable of dissolving the sample, such as petroleum ether or tetrahydrofuran.

Preferably, the combustion improver is an organic solvent with combustion-supporting effect such as No. 200 solvent oil.

Preferably, the ion chromatography is performed by using AS23 (4X 250mm) chromatographic column and 4.0mmol/L Na AS mobile phase₂CO₃+1.4mmol/L NaHCO₃Water solution, isocratic elution, the flow rate is 0.8 mL/min; the column temperature is 30 ℃; the sample volume is 10 mu L; DS5 conductivity detector; AERS 500 anion suppressor with suppressor current 23 mA.

Compared with the prior art, the invention has the advantages that:

according to the invention, the organic matter is dispersed on the surface of the filter paper by dissolving the organic matter sample with high chlorine content by the organic solvent. Meanwhile, the combustion improver is added to help the high-chlorine organic matter to be combusted, so that the purpose of complete combustion is achieved, the organic chlorine in the organic matter is completely converted into hydrogen chloride and absorbed by the potassium hydroxide solution, the problem that the chlorine content is low due to incomplete combustion of the clustered organic matter, namely incomplete conversion of the organic chlorine in the sample is solved, and the accuracy of chlorine content determination is improved.

The specific implementation mode is as follows:

the following examples are further illustrative of the present invention and are not intended to be limiting thereof.

Example 1 measurement of chlorine content in commercially available 52-type chlorinated paraffin

(1) Instruments and reagents

Ion chromatography: dionex ICS-600 (Agilent, USA), Sadoris TP-114 electronic balance (Sartorious, USA). Potassium hydroxide (Aladdin reagent) and water is secondary distilled water.

(2) Chlorinated paraffin oxygen bottle combustion

Original method (GB 1679-: 20mg (to the nearest 0.01mg) of chlorinated paraffin was weighed into an ashless filter paper, folded and placed into a platinum wire on the stopper of a combustion bottle, 15mL of potassium hydroxide (30mmol/L) was added to the combustion bottle, and a medium flow rate of oxygen was blown onto the liquid surface for about 60 seconds. Igniting the tail end of the filter paper, quickly plugging the plug, inclining the combustion bottle to enable the liquid to form a liquid seal around the plug, fully shaking to enable the liquid to be completely absorbed after the liquid is completely combusted, and standing for 15 min. And transferring the solution in the combustion bottle to a 50mL volumetric flask, washing the plug, the platinum wire and the water in the combustion bottle for several times by using deionized water, combining the washing solution to the 50mL volumetric flask, and fixing the volume by using the deionized water.

The experimental method comprises the following steps: weighing 2g of chlorinated paraffin in a 5mL volumetric flask, dissolving with petroleum ether, adding 1mL of No. 200 solvent oil, and metering the volume of the petroleum ether to 5 mL. Transferring 50 μ L of the test solution, dropwise adding into ashless filter paper, volatilizing petroleum ether, folding, placing into platinum wire on the stopper of a combustion bottle, adding 15mL potassium hydroxide (30mmol/L) into the combustion bottle, and blowing oxygen gas at medium flow rate on the liquid surface for about 60 s. Igniting the tail end of the filter paper, quickly plugging the plug, inclining the combustion bottle to enable the liquid to form a liquid seal around the plug, fully shaking to enable the liquid to be completely absorbed after the liquid is completely combusted, and standing for 15 min. And transferring the solution in the combustion bottle to a 50mL volumetric flask, washing the plug, the platinum wire and the water in the combustion bottle for several times by using deionized water, combining the washing solution to the 50mL volumetric flask, and fixing the volume by using the deionized water.

(3) Ion chromatography for measuring chloride ion content

A chromatographic column: AS23 (4X 250 mm); mobile phase: 4.0mmol/L Na₂CO₃+1.4mmol/L NaHCO₃Water solution, isocratic elution, the flow rate is 0.8 mL/min; the column temperature is 30 ℃; the sample volume is 10 mu L; DS5 conductivity detector; AERS 500 anion suppressor with suppressor current 23 mA.

The chlorinated paraffin is subjected to two parallels by adopting the conditions, the test numbers are respectively 1 and 2, the chlorine content is respectively measured by adopting the original method and the experimental method, and the analysis of the result is shown in table 1. As can be seen from Table 1, the original method measurement value of chlorine content in the commercially available 52-type chlorinated paraffin is 48.4%, the experimental method measurement value is 52.8%, and the actual chlorine content in the 52-type chlorinated paraffin is closer to the actual chlorine content, thereby proving the accuracy of the method of the invention.

Table 1 chlorine content in chlorinated paraffin sample (%)

	Original method	The experimental method
			1	47.3	52.5
2	49.4	53.1
			Mean value of	48.4	52.8
Relative deviation of	4.34	1.14

EXAMPLE 2 determination of chlorine content in polyvinyl chloride plastics

(1) Instruments and reagents

Ion chromatography: dionex ICS-600 (Agilent, USA), Sadoris TP-114 electronic balance (Sartorious, USA). Potassium hydroxide (Aladdin reagent) and water is secondary distilled water.

(2) Polyvinyl chloride plastic oxygen bottle combustion

The polyvinyl chloride plastic is crushed for later use.

Original method (GB 1679-: 20mg (to the nearest 0.01mg) of polyvinyl chloride plastic was weighed into an ashless filter paper, folded and placed into a platinum wire on a stopper of a combustion bottle, 15mL of potassium hydroxide (30mmol/L) was added to the combustion bottle, and oxygen gas was blown on the liquid surface for about 60 seconds at a medium flow rate. Igniting the tail end of the filter paper, quickly plugging the plug, inclining the combustion bottle to enable the liquid to form a liquid seal around the plug, fully shaking to enable the liquid to be completely absorbed after the liquid is completely combusted, and standing for 15 min. And transferring the solution in the combustion bottle to a 50mL volumetric flask, washing the plug, the platinum wire and the water in the combustion bottle for several times by using deionized water, combining the washing solution to the 50mL volumetric flask, and fixing the volume by using the deionized water.

The experimental method comprises the following steps: weighing 0.5g of polyvinyl chloride plastic sample, dissolving tetrahydrofuran, transferring to a 10mL volumetric flask, and fixing the volume. 40 μ L of the solution was pipetted onto filter paper. After the tetrahydrofuran was volatilized, 50. mu.L of No. 200 mineral spirit was added, the mixture was folded and placed in a platinum wire on a stopper of a combustion flask, 15mL of potassium hydroxide (30mmol/L) was added to the combustion flask, and oxygen gas was blown on the surface of the liquid for about 60 seconds at a medium flow rate. Igniting the tail end of the filter paper, quickly plugging the plug, inclining the combustion bottle to enable the liquid to form a liquid seal around the plug, fully shaking to enable the liquid to be completely absorbed after the liquid is completely combusted, and standing for 15 min. And transferring the solution in the combustion bottle to a 50mL volumetric flask, washing the plug, the platinum wire and the water in the combustion bottle for several times by using deionized water, combining the washing solution to the 50mL volumetric flask, and fixing the volume by using the deionized water.

(3) Ion chromatography for measuring chloride ion content

A chromatographic column: AS23 (4X 250 mm); mobile phase: 4.0mmol/L Na₂CO₃+1.4mmol/L NaHCO₃Water solution, isocratic elution, the flow rate is 0.8 mL/min; the column temperature is 30 ℃; the sample volume is 10 mu L; DS5 conductivity detector; AERS 500 anion suppressor with suppressor current 23 mA.

The polyvinyl chloride plastics are subjected to two parallels under the conditions, the test numbers are respectively 1 and 2, the chlorine content is measured by adopting the original method and the experimental method respectively, and the analysis of the results is shown in table 2. As can be seen from Table 2, the original method measurement value of the chlorine content in the polyvinyl chloride plastic is 39.8%, the experimental method measurement value is 43.6%, and the method is closer to the real chlorine content of the polyvinyl chloride plastic, thereby proving the accuracy of the method of the invention.

TABLE 2 chlorine content (%)

	Original method	The experimental method
			1	40.1	44.1
2	39.5	43.1
			Mean value of	39.8	43.6
Relative deviation of	1.51	2.29

The above is only a preferred embodiment of the present invention, and it should be noted that the above preferred embodiment should not be considered as limiting the present invention, and the protection scope of the present invention should be subject to the scope defined by the claims. It will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the spirit and scope of the invention, and these modifications and adaptations should be considered within the scope of the invention.