WO2018218960A1 - Procédé de prétraitement destiné à mesurer un composé organique halogéné total dans de l'eau - Google Patents

Procédé de prétraitement destiné à mesurer un composé organique halogéné total dans de l'eau Download PDF

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WO2018218960A1
WO2018218960A1 PCT/CN2018/000169 CN2018000169W WO2018218960A1 WO 2018218960 A1 WO2018218960 A1 WO 2018218960A1 CN 2018000169 W CN2018000169 W CN 2018000169W WO 2018218960 A1 WO2018218960 A1 WO 2018218960A1
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water sample
water
silver
ions
photolysis
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PCT/CN2018/000169
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Chinese (zh)
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陈白杨
卜毅男
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哈尔滨工业大学深圳研究生院
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    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00—Multistage treatment of water, waste water or sewage
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/30—Treatment of water, waste water, or sewage by irradiation
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/30—Organic compounds
    • C02F2101/36—Organic compounds containing halogen

Definitions

  • the invention relates to a total indicator of halogenated organic matter, in particular to a method for separating and converting total halogenated organic matter in a water sample.
  • the total organic halogenated compound is a general indicator covering chlorinated, brominated, and iodine organic compounds in water. It is an important aggregate in the treatment of drinking water. In terms of industrial wastewater treatment, it is a total indicator for evaluating water quality and measuring the content of halogenated organic matter in water. Disinfection by-products in water are very harmful to human health, and there are many kinds of them. The content and control methods have always been an important issue in the field of drinking water treatment. Despite the great efforts of researchers, only about half of the more than 600 DBPs that have been discovered so far have been studied more clearly. As a total indicator, TOX can simultaneously analyze the content of all halogenated by-products, including unknown halogenated by-products. Therefore, since the establishment of the TOX test method, it has been widely and rapidly applied in various fields of water treatment, such as drinking water treatment, raw water evaluation, landfill leachate treatment, municipal and industrial sewage treatment, and sewage reuse.
  • TOX detection is to convert the organic halogenated compound into an inorganic halogen for measurement.
  • the standard TOX analysis process is mainly carried out in three steps, namely, pretreatment of the organic halogen in the adsorbed and separated water sample by activated carbon, conversion of the organic halogenated compound into inorganic halogen by pyrolysis, and measurement of the inorganic halide by means of IC or the like.
  • TOX analysis is sometimes referred to as adsorbable organic halogen (AOX) and dissolved organic halogen (DOX).
  • AOX adsorbable organic halogen
  • DOX dissolved organic halogen
  • the analysis process of AOX is the same as that of TOX, the dissolved organic halogenated substances in the water sample tested by the AOX method are adsorbed by the activated carbon column, and some suspended substances in the water are adsorbed by the activated carbon column, so the results obtained by AOX analysis include dissolution. Both organic halogens and organic substances in suspended matter.
  • the DOX analysis process involves the water sample being first filtered through a membrane to remove suspended matter from the water sample. Therefore, the results obtained by DOX analysis are only dissolved organic halogens. Because the analysis of DOX, AOX, and DOX is only slightly different in the pre-processing process, and the rest of the analysis process is roughly the same, the overall connotation of these three concepts is the same.
  • a method for measuring total halogenated organic compounds in water is disclosed in Japanese Laid-Open Patent Publication No. JPH 06308111, which uses a reversed phase chromatography column to separate organic halogenated compounds and inorganic halogens in a water sample to be tested; The method is carried out by converting an organic halogenated compound into an inorganic halogen.
  • Standard methods such as EPA1650 use activated carbon adsorption to separate organic halogenated compounds.
  • the special activated carbon column is expensive and the test amount is high, resulting in high test cost.
  • the reversed-phase column method avoids the use of activated carbon, but still needs to use the price. Expensive pyrolysis furnaces convert organic halogenated compounds, so equipment costs remain high.
  • a method and system for measuring the content of dissolved organic halogen in water is disclosed in Chinese Patent Application Publication No. CN 106093215, which uses an electrodialysis technique to separate a soluble inorganic halogen and a dissolved organic halogen in the water to be measured, by electrodialysis technology.
  • haloacetic acid one of the important disinfection by-products, is currently strictly defined in the national standard for drinking water, it is necessary to explore alternative methods for its detection.
  • Standard methods such as EPA1650 and other equipment for testing TOX and the cost of consumable testing are relatively expensive.
  • the activated carbon column used to separate organic halogenated compounds by means of activated carbon adsorption is expensive and has a large amount of test; on the other hand, heat is used.
  • the pyrolysis furnace used for the conversion of organic halogenated compounds is expensive and costly.
  • the object of the present invention is to find and apply new techniques to avoid the use of activated carbon adsorption and pyrolysis conversion in the process of measuring TOX, thereby reducing the test cost of TOX.
  • the invention provides a pretreatment method for measuring total organic halogenated compounds in water, which specifically comprises the following steps:
  • the photolyzed water sample converts the organic halogenated compound in the water sample into an inorganic halogen ion.
  • the total halogenated organic compound specifically includes an organic chloride, an organic bromide and an organic iodide; after the photolysis of the water sample, the inorganic halogen content in the water sample after photolysis is measured, and the inorganic substance in the water sample before photolysis is subtracted
  • the halogen ion content is equal to the halogen content of the total halogenated organic matter in the water.
  • silver ions may be added by adding an excess amount of silver carbonate powder in water; the excess silver carbonate powder is embodied as being fully reacted, There is still undissolved pale yellow silver carbonate powder in the water sample; excessive silver carbonate powder is added to make the dissolved silver carbonate in the water saturated, and the silver ions in the water react with the inorganic halogen ions to form a precipitate, which is consumed. The silver carbonate powder will continue to dissolve.
  • the silver carbonate in the water will still be saturated; because the saturated solubility of the silver carbonate in water is relatively low, the silver ion concentration in the water after reacting with the inorganic halogen ions It is also relatively low and easy to follow up.
  • the method of adding silver ions may be to add a silver-soluble compound such as silver nitrate or silver sulfate to the water sample; Measure the content of all inorganic halide ions in the water sample, including chloride, bromide and iodide; add silver sulfate or silver nitrate to make the number of moles of silver ions in the water sample 1.2 of the total number of inorganic halides in the water sample. -2 times.
  • a silver-soluble compound such as silver nitrate or silver sulfate
  • the silver ions may be added by using a pretreatment silver column dedicated to ion chromatography; and removing the inorganic particles from the water sample through a silver column.
  • a pretreatment silver column dedicated to ion chromatography and removing the inorganic particles from the water sample through a silver column.
  • the filtration is selected by a disposable needle filter, the filter material is nylon 66, and the pore diameter is 0.22 um.
  • the filtration is selected by vacuum filtration, and the filter material is nylon 66 and the pore diameter is 0.22 um.
  • the remaining silver ion in the deionized sample is selected from the hydrogen column for ion chromatography pretreatment; and the water sample is at a rate of less than 2 ml/min. , through the hydrogen column at a constant speed, to achieve the purpose of removing the remaining silver ions.
  • the remaining silver ions in the water sample are selected by adding sodium sulfide; for the selective addition of silver carbonate to remove inorganic halogen ions in the water sample,
  • the amount of sodium sulfide is the product of the amount of water-like water and 0.1 mmol/L; for the selection of the compound which dissolves silver to remove the inorganic halide ions in the water sample, the amount of the substance added with sodium sulfide is (the mass of the silver compound added - The mass of total inorganic halogen ions in water) / 2+ 0.05 mmol.
  • the photolysis water sample can be specifically selected by a low pressure mercury lamp having a wavelength of 185 nm; the photolysis method can be performed by using an immersion photolysis device or a sample. Placed in a quartz photolysis tube, external low-pressure mercury lamp, directly photolysis;
  • the water sample may be drinking water, rain water, river water, domestic sewage, industrial sewage, landfill leachate, and the like.
  • the invention provides a pretreatment method for detecting total halogenated organic compounds in water, and removes inorganic halogen ions in the water sample by adding silver ions, and converts the organic halogenated compounds into inorganic halogen ions by photolysis to achieve separation and conversion of the pretreatment.
  • the purpose of pretreatment of organic matter; the water sample after pretreatment can directly determine the total content of halogenated organic compounds in water by measuring the content of inorganic halogen ions; on the basis of the accuracy to meet the test requirements, the activated carbon and pyrolysis furnace are avoided in principle. Use, reducing the cost of testing.
  • FIG. 1a is a flowchart of a preprocessing method provided by Embodiment 1.
  • FIG. 1b is a diagram showing the effect of a pretreatment method for removing halogen ions provided in Example 1.
  • FIG. 1c is a schematic view showing the structure of a pretreatment method optical solution box provided in Embodiment 1
  • Figure 1d is a graph showing the recovery rate of individual photolysis organic matter in a pretreatment method provided in Example 1.
  • Figure 1e is a diagram showing the effect of a pretreatment method provided by Example 1 on different substances.
  • Embodiment 2a is a flow chart of a preprocessing method provided in Embodiment 2
  • Figure 2b is a diagram showing the effect of a pretreatment method for different substances provided in Example 2.
  • FIG. 3a is a flowchart of a preprocessing method provided in Embodiment 3.
  • Figure 3b is a diagram showing the effect of a pretreatment method for different substances provided in Example 3.
  • Figure 4b is a diagram showing the effect of a pretreatment method provided by Example 4 on different substances.
  • Figure 4c is a diagram showing the effect of a pretreatment method provided by Example 4 on actual water samples.
  • the method for pretreating total halogenated organic compounds in water comprises first removing inorganic halide ions in the water sample, adding silver ions to the water sample, and reacting the silver ions with the inorganic halogen ions to form a precipitate, and after being fully reacted, filtering The precipitation is removed to achieve the purpose of removing inorganic halide ions from the water sample.
  • the silver ions for example, by pre-treatment of the silver column by ion chromatography, and the water sample can be passed through the silver column at a constant speed; or the silver sample which is easy to dissolve can be added to the water sample.
  • Inorganic compounds such as silver nitrate, silver sulfate, etc.; in order to ensure the appropriate amount of silver-containing inorganic compounds, to achieve the purpose of removing inorganic halide ions, and not introducing too much silver ions to affect subsequent measurements, etc.
  • the concentration of the inorganic halogen ion in the water sample needs to be measured first, and after calculation, the amount of the silver-containing inorganic compound in the water sample is selectively selected; for example, the volume of a certain water sample is 1 L, and the measurement is performed.
  • the concentration of chloride ion in the water sample is 35.5 mg/L.
  • the total inorganic halide ion content in the water sample is 1 mmol, and 1 mmol of silver ion can be used together with the inorganic halide ion in the water sample.
  • a slight excess of silver ions was added to the water sample to ensure complete reaction, then 1.2-2 mmol of silver ions were added to the water sample.
  • the method of adding the silver ions to the water sample may select a slightly soluble silver-containing compound, for example, adding an excessive amount of silver carbonate powder; the excess silver carbonate powder is embodied in the water sample after sufficient reaction.
  • the undissolved pale yellow silver carbonate powder is present to keep the silver ion saturated state in the water sample; the excess silver carbonate powder is added to make the dissolved silver carbonate in the water saturated, and the silver ions in the water continuously react with the inorganic halogen ions to form Precipitation and consumption, the excess silver carbonate powder will continue to dissolve.
  • the silver carbonate in the water will still be saturated; because the saturated solubility of silver carbonate in water is relatively low, according to the MINEQL software, Considering the solubility of silver carbonate and the concentration of carbonate ions in water, the concentration of saturated silver ions is about 0.18 mmol/L in the presence of excess silver carbonate solids at 25 ° C in water; therefore, after the reaction of silver ions with inorganic halide ions, Silver ions are still saturated in water, but the concentration of silver ions is relatively low and easy to carry out.
  • the formed precipitate needs to be filtered.
  • What kind of filtering equipment or device can be used according to the actual situation, but the pore size of the filter membrane is suitable, and the membrane material is not Adsorption of halogenated organic compounds in water.
  • a filter needle with a pore size of 0.22 um and a nylon 66 material can be used? Filter.
  • silver ions are used to precipitate and filter the original inorganic halide ions in the water sample, and it is necessary to remove the silver ions remaining in the water sample.
  • the silver ions remaining in the water sample are removed to ensure that the inorganic halogen ions generated during the photolysis of the halogenated organic compound in the water sample are not removed from the residual silver ions in a subsequent step.
  • the pretreatment hydrogen column or the sodium column of the ion chromatography may be selected, and the remaining silver ions in the water sample may be adsorbed and removed by cation exchange with the water sample through the hydrogen column or the sodium column.
  • Removing the silver ions remaining in the water sample may also be carried out by adding a substance which can produce a lower solubility than silver halide to the silver sample.
  • a substance which can produce a lower solubility than silver halide for example, in the silver halide, the minimum equilibrium constant of the Ksp precipitation of the solubility product is silver iodide.
  • the precipitate equilibrium constant of 8.3 ⁇ 10 -17, and the silver sulfide precipitate equilibrium constant is 6.3 ⁇ 10 -50, much less than the equilibrium constant of the precipitation of silver iodide; when the water sample precipitate silver sulfide, water samples even then
  • the addition of halogen ions also does not form a silver halide precipitate; therefore, sulfides can be selected to remove the remaining silver ions in the water sample.
  • the silver ion is removed by reacting the sulfide ion with the silver ion to form a precipitate.
  • a water sample has a volume of 1 L, and an excess of silver carbonate is added to the water sample.
  • the concentration of silver ions in the water sample should be the concentration of the saturated solution of silver carbonate, that is, about 0.18 mmol/L. In order to remove the remaining silver ions, the solution is added to the water sample.
  • the water sample is filtered, that is, the purpose of removing the remaining silver ions in the water sample is completed; and the sulfur remaining in the water sample is theoretically formed after the precipitation of silver sulfide
  • the ion is about 0.01 mmol and does not affect subsequent measurements.
  • Example 1 Pretreatment method for detecting total halogenated organic compounds in water I
  • the operation steps are as shown in Fig. 1a.
  • the inorganic halogen in the water sample is removed.
  • the method is to add excess silver carbonate powder to the water; after sufficient reaction, filter; remove the remaining silver ions in the water sample.
  • the water sample is pretreated by ion chromatography to treat the hydrogen column; the photolyzed water sample is used to convert the organic halogenated compound into an inorganic halogen; the inorganic halogen content in the water sample after photolysis is measured, and the inorganic halogen ion content in the water sample before photolysis is subtracted. That is equal to the content of halogen contained in the total halogenated organic matter in water.
  • the specific calculation formula is:
  • Total organic chlorinated compound content chloride ion content in water sample after photolysis - residual chloride ion content in water sample before photolysis
  • Total organic brominated compound content bromide ion content in water sample after photolysis - residual bromide ion content in water sample before photolysis
  • Total organic iodide content iodide ion content in water sample after photolysis - residual iodide ion content in water sample before photolysis
  • test water samples are configured, and the water samples are configured with ultrapure water, and the total amount of each water sample is 1 L, and one of the water samples contains a halogenated organic substance, trichlorophenol 1 mg/L, and tribromophenol.
  • water sample contains inorganic halogen chloride ion 10mg/L, bromide ion 10mg/L, iodide ion 10mg/L; another water sample contains monochloroacetonitrile 1mg/L, monobromide Acetonitrile 1 mg / L, monoiodoacetonitrile 1 mg / L, chloride ion 10 mg / L, bromide 10 mg / L, iodide ion 10 mg / L.
  • the source of silver ions is silver carbonate. To ensure the excess of silver carbonate added to the water sample, 0.5 g of silver carbonate powder is added.
  • the selected filter membrane is a Jinteng needle-type disposable filter membrane with a pore size of 0.22 um and a diameter of 1.5 cm.
  • the filter material is nylon 66.
  • the ion chromatography pretreatment hydrogen column selected is a 1 cc hydrogen column of Dai'an Company.
  • the photolysis solution uses a low-pressure mercury lamp with a wavelength of 185 nm.
  • the photolysis tank structure is shown in Figure 1c.
  • Figure 1d To verify the photolysis efficiency, the photolysis recovery rate of several substances of organic matter 1 mg/L was pre-tested. The specific results are shown in Figure 1d. All the steps involved in the measurement are measured three times, and the average is taken as the result record.
  • the effect of removing inorganic halide ions is shown in Fig. 1b.
  • the effect of the pretreatment method of this embodiment on different substances is shown in Fig. 1e.
  • the operation steps are shown in Figure 2a. Specifically, the inorganic halogen in the water sample is first removed. The method is to add silver nitrate to the water. The specific method is to measure the total inorganic halide ion content in the water sample.
  • the remaining silver ions in the water sample are selected by pre-treatment of the water sample by ion chromatography; photolysis of the water sample, conversion of the organic halogenated compound to inorganic halogen; The inorganic halogen content in the water sample after the solution is subtracted from the inorganic halide ion content in the water sample before photolysis, which is equal to the halogen content in the total halogenated organic matter in the water.
  • the test water sample is configured, and the water sample is configured with ultrapure water, the total amount is 1 L, and the water sample contains halogenated organic matter trichlorophenol 1 mg/L, tribromophenol 1 mg/L, and triiodophenol 1 mg/L. Containing inorganic halogen chloride ion 10mg / L, bromide ion 10mg / L, iodide ion 10mg / L.
  • the source of silver ions is silver nitrate.
  • the selected filter membrane is a Jinteng needle-type disposable filter membrane with a pore size of 0.22 um and a diameter of 1.5 cm.
  • the filter material is nylon 66.
  • the photolysis solution uses a low-pressure mercury lamp with a wavelength of 185 nm, and the structure of the photolysis box is shown in the figure. All the steps involved in the measurement are measured three times, and the average value is taken as the result record. The effect of the pretreatment method of this embodiment on different substances is shown in Fig. 2b.
  • the operation steps are shown in Figure 3a.
  • the method is to pre-treat the water sample by ion chromatography. Because the silver column is attached with silver ions, when the water sample passes through the silver column, it can be reduced.
  • the content of halogen ions in the water sample filtering; removing the remaining silver ions in the water sample by selecting the water sample by ion chromatography to pretreat the hydrogen column; photolyzing the water sample to convert the organic halogenated compound into an inorganic halogen; measuring light
  • the content of inorganic halogen in the water sample is subtracted from the content of inorganic halogen ions in the water sample before photolysis, which is equal to the content of halogen in the total halogenated organic matter in water.
  • Total organic chlorinated compound content chloride ion content in water sample after photolysis - residual chloride ion content in water sample before photolysis
  • Total organic brominated compound content bromide ion content in water sample after photolysis - residual bromide ion content in water sample before photolysis
  • Total organic iodide content iodide ion content in water sample after photolysis - residual iodide ion content in water sample before photolysis
  • the test water sample is configured, the water sample is configured with ultrapure water, the total amount is 1 L, and the water sample contains halogenated organic matter trichlorophenol 1 mg/L, tribromophenol 1 mg/L, and triiodophenol 1 mg/L;
  • the water sample contains 10 mg/L of inorganic halogen chloride ion, 10 mg/L of bromide ion and 10 mg/L of iodide ion.
  • the silver column is selected as the Dion pretreatment column with a specification of 1 cc.
  • the selected filter membrane is a Jinteng needle-type disposable filter membrane with a pore size of 0.22 um and a diameter of 1.5 cm.
  • the filter material is nylon 66.
  • the ion chromatography pretreatment hydrogen column selected is a 1 cc hydrogen column of Dai'an Company.
  • the photolysis solution uses a low-pressure mercury lamp with a wavelength of 185 nm, and the structure of the photolysis box is shown in the figure. All the steps involved in the measurement are measured three times, and the average value is taken as the result record. The effect of the pretreatment method of this embodiment on different substances is shown in Fig. 3b.
  • the inorganic halogen in the water sample is removed.
  • the method is to add excess silver carbonate powder to the water; after sufficient reaction, filter; remove the remaining silver ions in the water sample.
  • Sodium sulfide is added to the sample to remove the remaining silver ions by the precipitation of silver ions with silver ions;
  • the photo-decomposition water sample converts the organic halogenated compound into an inorganic halogen; and the inorganic halogen content in the water sample after photolysis is measured, minus
  • the content of inorganic halogen ions in the water sample before photolysis is equal to the content of halogen in the total halogenated organic matter in water.
  • the specific calculation formula is:
  • Total organic chlorinated compound content chloride ion content in water sample after photolysis - residual chloride ion content in water sample before photolysis
  • Total organic brominated compound content bromide ion content in water sample after photolysis - residual bromide ion content in water sample before photolysis
  • Total organic iodide content iodide ion content in water sample after photolysis - residual iodide ion content in water sample before photolysis
  • test water samples were measured using the pretreatment method IV, and the total amount of each water sample was 1 L, and the specific components are shown in Table 1.
  • the silver ion source is silver carbonate. To ensure that the silver carbonate added to the water sample is in an excess state, 0.5 g of silver carbonate powder is optionally added.
  • the selected filter membrane is a Jinteng needle-type disposable filter membrane with a pore size of 0.22 um and a diameter of 1.5 cm.
  • the filter material is nylon 66.
  • the photolysis solution uses a low-pressure mercury lamp with a wavelength of 185 nm, and the structure of the photolysis box is shown in the figure. All the steps involved in the measurement are measured three times, and the average value is recorded as the result. The effect of the pretreatment method of this embodiment on different substances is shown in Figures 4b and 4c.

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Abstract

L'invention concerne un procédé de prétraitement destiné à mesurer des composés organiques halogénés totaux dans de l'eau. Tout d'abord, la plupart des ions halogènes inorganiques sont éliminés d'un échantillon d'eau par l'ajout d'ions argent à l'échantillon d'eau, de sorte que les ions argent réagissent avec les ions halogènes inorganiques pour former un précipité, ce dernier étant ensuite filtré; d'autre part, les ions argent résiduels dans l'échantillon d'eau sont éliminés; et enfin, l'échantillon d'eau est photolysé, convertissant les composés organiques halogénés dans l'échantillon d'eau en ions halogènes inorganiques à l'aide d'une lampe à rayonnement ultraviolet (2). Ensuite, la teneur en ions halogènes inorganiques dans l'échantillon d'eau avant la photolyse est soustraite de la teneur en ions halogènes inorganiques dans l'échantillon d'eau après la photolyse, de façon à obtenir la teneur en halogène contenue dans les composés halogénés organiques dans l'échantillon d'eau dans un état initial. Le procédé de prétraitement évite les processus nécessitant l'utilisation de charbon actif coûteux et d'un four à pyrolyse dans le procédé existant au motif que la précision répond aux exigences de test, et ceci peut réduire de manière considérable le coût de test.
PCT/CN2018/000169 2017-06-01 2018-05-09 Procédé de prétraitement destiné à mesurer un composé organique halogéné total dans de l'eau WO2018218960A1 (fr)

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