CN105467041A - Improved measuring method for total organic bromide in water - Google Patents
Improved measuring method for total organic bromide in water Download PDFInfo
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- CN105467041A CN105467041A CN201610060023.0A CN201610060023A CN105467041A CN 105467041 A CN105467041 A CN 105467041A CN 201610060023 A CN201610060023 A CN 201610060023A CN 105467041 A CN105467041 A CN 105467041A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/14—Preparation by elimination of some components
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Abstract
The invention discloses an improved measuring method for total organic bromide in water. The improved measuring method comprises the following steps that firstly, an activated carbon column is filled with activated carbon, an ozone water solution passes through the activated carbon column, then the activated carbon column is treated through a bromine containing solution, and elution is carried out through an eluant; finally, burning and pyrolysis are carried out, generated gas is absorbed through absorption liquid, the concentration of bromide ions is measured, and the recovery rate of a sample is calculated. The activated carbon column is used for adsorbing and enriching the bromine containing solution, and the recovery rate is increased. The content of organic bromide in the water can be accurately measured, detection accuracy is improved, the operation steps are simplified, the time spent on measurement is shortened, and the highest recovery rate of the sample can reach 98% or above. According to the method, total organic bromide in drinking water, underground water, surface water and industrial waste water can be accurately measured.
Description
Technical field
The invention belongs to water quality monitoring technical field, relate to the assay method of total organic bromine in a kind of water of improvement.
Background technology
The natural causes such as the stripping of seawater intrusion, land subsidence, soil and the dissolving of mineral, bromide ion in the underground water of coastland and surface water can be caused to increase, due to the bromide ion containing higher concentration in seawater, seawater intrusion is the main cause that the bromide ion in surface water and groundwater is formed; Secondly, multiple brominated medicament and industrial discharge waste water is used also to make the content of bromide ion in source water increase.In former water, bromide ion concentration drastically influence the formation of Chlorination Disinfection By-products, and 28 kinds in 196 kinds of Chlorination Disinfection By-products is at Br
-formed when existing, cytotoxicity and the genetoxic of bromo DBPs are higher than chloro homolog.The bromo DBPs kind that prior art can measure is not comprehensive, and total organic bromine index is just as the indication parameter of bromo DBPs toxicity, and it measures accuracy and just seems particularly important.
The assay method of organic bromine in prior art, more complicated in operating process, the background bromide ion of activated charcoal is higher, can affect the accuracy of measurement of organic bromine, and the reduction of part organic bromine activated charcoal can make the measurement result of organic bromine on the low side, simultaneously NaNO
3during as eluent, NO in water
3 -ion can affect the mensuration of bromide ion.But, up to the present yet there are no the patent or article that organic bromine in water are measured by the chromatography of ions improved, CN103575685A discloses a kind of method measuring bromide ion, its method used is dual-wavelength spectrophotometry, CN103649730A discloses a kind of assay method and determinator of bromate ion, use fluorescence intensity measurements, article " method of testing of simple and easy trace active organic bromine " be spectrophotometer method.
Summary of the invention
Complicated to the assay method of organic bromine total in water for prior art, the defect that result precision is not high, the object of the present invention is to provide the assay method of total organic bromine in a kind of water of improvement, determine organic bromine and bromate transformation rule, for purification in potable water provides application technology, the method is simple, measures accurately.
To achieve these goals, the technical solution used in the present invention is as follows:
An assay method for total organic bromine in the water of improvement, comprises the following steps:
First, activated charcoal is filled in activated charcoal pillar, with ozone water solution by activated charcoal pillar, and then with the above-mentioned activated charcoal pillar of brominated solution-treated, with elution, finally, burning cracking is carried out, the gas absorbing liquid generated absorbs, and measures the concentration of bromide ion and the recovery of calculation sample.
Described activated charcoal is Powdered Activated Carbon, and order number is 100-1000.
The concentration of described ozone water solution is 0.1-5mg/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
The described concentration containing bromine solutions is 0.1-200 μ g/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
Described is by after water sample effective chlorine solution prechlorination containing bromine solutions, adds bromine-containing compound through the solution filtered, adjust ph obtains; Or, in ultrapure water, add the solution that bromine-containing compound obtains through adjust ph.
The concentration of described effective chlorine solution is 0.1-5mg/L, and consumption is 10 ~ 200mL, and the time of prechlorination is 1 ~ 3h.
Described bromine-containing compound is parabromobenzoic acid.
Described filtration adopts aperture to be that the filter membrane of 0.35 ~ 0.55 μm filters.
Described adjust ph adopts red fuming nitric acid (RFNA), the concentrated sulphuric acid or concentrated hydrochloric acid to regulate, and pH value is 2 ~ 4.
Described eluent is NaCl solution or NaNO
3solution, concentration is 4 ~ 8mg/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
Described burning cracking carries out in cracking instrument, and the temperature of burning is 900-1000 DEG C.
Described absorbing liquid to be concentration be 20 ~ 40% superoxol, consumption is 10 ~ 200mL.
The concentration of described bromide ion adopts ion chromatograph to measure, and leacheate is the NaHCO of 20 ~ 40mmol/L
3with the Na of 45 ~ 55mmol/L
2cO
3.
The computing formula of the described recovery is: the recovery=measured value/standard value × 100%.
Owing to have employed technique scheme, the present invention has the following advantages and beneficial effect:
The present invention adopts activated charcoal pillar, and to containing, bromine solutions adsorbs, enrichment, improves the recovery.
The present invention compared for NaCl and NaNO
3to the elute effect of inorganic bromine, and select suitable NaCl concentration, reach best elute effect, decrease the error that inorganic bromide ion is measured follow-up organic bromine, improve measuring accuracy.
The present invention simulates the Conduce Disciplinarian of organic bromine in chlorination after Ozone-Active Carbon Process, determines organic bromine and bromate transformation rule, and for purification in potable water provides application technology, the method is simple, measures accurately.
The present invention can measure the content of organic bromine in water exactly, improves accuracy in detection, simplifies operation steps.
The present invention can improve organic bromine accuracy of measurement, and reduce and measure the time used, sample recovery rate can reach more than 98%, and the present invention can accurately measure organic bromine total in potable water, underground water, surface water and industrial waste water.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet of the assay method of total organic bromine in the water improved in the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further detailed explanation.
Embodiment 1
(1) as shown in Figure 1, Fig. 1 is the schematic flow sheet of the assay method of total organic bromine in the water improved in the embodiment of the present invention.Select that size is 100-200 order, 200-300 order, 500-600 order and 800-900 object Powdered Activated Carbon 50mg be filled in activated charcoal pillar, configuration concentration is the Ozone Water 10mL of 2mg/L, adjust flux be 4mL/min by activated charcoal pillar, until all pass through.Utilize Ozone Water process Powdered Activated Carbon, reduce organic bromine reduction on the activated carbon;
(2) get a certain amount of parabromobenzoic acid, with ultrapure water be configured to concentration be 100ug/L containing bromine solutions, and utilize red fuming nitric acid (RFNA) that its pH is adjusted to 3.
(3) to get the concentration configured in 30ml step (2) be 100ug/L, pH be 3 containing bromine solutions, adjust flux be 4mL/min by activated charcoal pillar, until all pass through.This step allows organic bromine adsorb on activated charcoal pillar, selects the suitable water yield by activated charcoal pillar according to organic bromine concentration in water, not only can ensure adsorption effect but also can reduce the absorption time used;
(4) configuration concentration be 6mg/L containing Cl
-naCl solution, get 30ml and regulate flow velocity to be 3mL/min, the activated charcoal pillar 10min of elution step (3), makes the complete wash-out of inorganic bromide ion, and only remaining organic bromine in activated charcoal pillar gets rid of the interference that when measuring organic bromine, inorganic bromide ion brings.This step utilizes certain density eluent by activity eluted charcoal pillar, by the inorganic bromine wash-out on activated charcoal.
(5) with the activated charcoal pillar that step (4) obtains by AQF-100 cracking instrument, it is cracking of burning under the condition of 900-1000 DEG C in temperature, organic bromine is burnt and is cracked into bromize hydrogen gas, and the bromize hydrogen gas of cracking generation is absorbed with the hydrogen peroxide absorbing liquid that concentration is 30%, after cracking, the concentration determination of bromide ion adopts ICS-1000 ion chromatograph, with the NaHCO of 30mmol/L during measurement
3with 48mmol/LNa
2cO
3as negative ion leacheate; The working sample recovery, the recovery=measured value/standard value × 100%, the result recorded is as shown in table 1.
Table 1
| TOBr standard value (μ g/L) | Activated charcoal order number (order) | TOBr measured value (μ g/L) | The recovery (%) |
| 100 | 100-200 | 98.11 | 98.1 |
| 100 | 200-300 | 98.21 | 98.2 |
| 100 | 500-600 | 97.36 | 97.4 |
| 100 | 800-900 | 96.67 | 96.7 |
As can be seen from the data of table 1, the method can well measure the concentration of organic bromine in water, and the recovery is all higher, and Powdered Activated Carbon recovery between 200-300 order is higher.
Embodiment 2
Identical with the method for embodiment 1, when other conditions are constant, select 200-300 order Powdered Activated Carbon, the concentration containing bromine solutions be 20,50,100,200ug/L, the result recorded is as shown in table 2.
Table 2
| TOBr standard value (μ g/L) | TOBr measured value (μ g/L) | The recovery (%) |
| 20 | 19.32 | 96.6 |
| 50 | 48.89 | 97.8 |
| 100 | 98.21 | 98.2 |
| 200 | 197.65 | 98.8 |
As can be seen from the data of table 2, the recovery that the method records is all higher, and when other conditions are all identical, the recovery increases along with the increase of organic bromine concentration.
Embodiment 3
Identical with the method for embodiment 1, when other conditions are constant, select 200-300 object Powdered Activated Carbon, select respectively the concentration of Ozone Water be 0.1mg/L, 2mg/L, 3.5mg/L, 5mg/L by activated charcoal pillar, the result recorded is as shown in table 3.
Table 3
| TOBr standard value (μ g/L) | Consistency of ozone water (mg/L) | TOBr measured value (μ g/L) | The recovery (%) |
| 100 | 0.1 | 94.37 | 94.4 |
| 100 | 2 | 98.21 | 98.2 |
| 100 | 3.5 | 96.93 | 96.9 |
| 100 | 5 | 96.12 | 96.1 |
As can be seen from the data of table 3, time consistency of ozone water is 2mg/L, the recovery of organic bromine is higher.
Embodiment 4
Identical with the method for embodiment 1, when other conditions are constant, select 200-300 object Powdered Activated Carbon, the concentration containing bromide ion in bromine solutions is 200 μ g/L, and the NaNO of 5mg/L selected respectively by eluent
3the NaCl solution of solution and 6mg/L carries out wash-out to the inorganic bromide ion in Powdered Activated Carbon, and the result recorded is as shown in table 4.
Table 4
| TOBr standard value (μ g/L) | Elute soln and concentration (mg/L) | TOBr measured value (μ g/L) | The recovery (%) |
| 200 | The NaCl solution of 6mg/L | 197.65 | 98.8 |
| 200 | The NaNO of 5mg/L 3Solution | 193.14 | 96.6 |
As can be seen from the data of table 4, select the elute effect of the NaCl solution of 6mg/L to inorganic bromide ion better.
Embodiment 5
The mensuration of total organic bromine after prechlorination in East Taihu Lake water:
(1) selection of activated charcoal: select 200 ~ 300 object Powdered Activated Carbons, loads in activated charcoal pillar by 50mg;
(2) pre-service of Powdered Activated Carbon: adopt concentration to be the Ozone Water 10mL of 2mg/L, with the flow velocity of 4mL/min by activated charcoal pillar;
(3) sample pretreatment: adopt concentration to be 1 respectively, 2,3,4mg/L effective chlorine solution, water sample East Taihu Lake water after prechlorination 2h, add parabromobenzoic acid to be configured to contain the solution that bromine concentration is 50 μ g/L, utilize 0.45 μm of filter membrane to be filtered by water sample, and adopt nitric acid that its pH is adjusted to 3;
(4) adsorption and enrichment of organic bromine: by the water sample of East Taihu Lake water pretreated for 20mL step (3), with the flow velocity of 4mL/min by activated charcoal pillar;
(5) wash-out of inorganic bromine: adopt concentration be 6mg/L containing Cl
-naCl solution, with the activated charcoal pillar 10min of the flow velocity elution step (4) of 3mL/min, the inorganic bromide ion in abundant elution samples, remaining organic bromine, in activated charcoal pillar, is that next step measures organic bromine exclusive PCR.
(6) mensuration of inorganic bromide ion: activated charcoal pillar step (5) obtained with AQF-100 cracking instrument, it is cracking of burning under the condition of 900-1000 DEG C in temperature, organic bromine is burnt and is cracked into bromize hydrogen gas, and the bromize hydrogen gas of cracking generation is absorbed with the hydrogen peroxide absorbing liquid that concentration is 30%, after cracking, the concentration determination of bromide ion adopts ICS-1000 ion chromatograph, the NaHCO of period 30mmol/L
3with the Na of 48mmol/L
2cO
3as negative ion leacheate, the working sample recovery, the recovery=measured value/standard value × 100%, the result recorded is as shown in table 5.
Table 5
| TOBr adds scalar (μ g/L) | Effective chlorine density (mg/L) | TOBr mark-on measures definite value (μ g/L) | Recovery of standard addition (%) |
| 50 | 1 | 48.8 | 97.6 |
| 50 | 2 | 49.1 | 98.2 |
| 50 | 3 | 48.2 | 96.4 |
| 50 | 4 | 49.1 | 98.2 |
As can be seen from the data of table 5, the method all reaches more than 96% for the recovery of the organic bromine in the former water water sample of different effective chlorine solution prechlorination after 2 hours, illustrates that the method is high to the measuring accuracy of organic bromine in former water water sample.
Above-mentioned is can understand and apply the invention for ease of those skilled in the art to the description of embodiment.Person skilled in the art obviously easily can make various amendment to these embodiments, and General Principle described herein is applied in other embodiments and need not through performing creative labour.Therefore, the invention is not restricted to embodiment here, those skilled in the art, according to announcement of the present invention, do not depart from improvement that scope makes and amendment all should within protection scope of the present invention.
Claims (10)
1. an assay method for total organic bromine in the water improved, is characterized in that: comprise the following steps:
First, activated charcoal is filled in activated charcoal pillar, with ozone water solution by activated charcoal pillar, and then with the above-mentioned activated charcoal pillar of brominated solution-treated, with elution, finally, burning cracking is carried out, the gas absorbing liquid generated absorbs, and measures the concentration of bromide ion and the recovery of calculation sample.
2. the assay method of total organic bromine in the water of improvement according to claim 1, it is characterized in that: described activated charcoal is Powdered Activated Carbon, order number is 100-1000.
3. in the water of improvement according to claim 1, the assay method of total organic bromine, is characterized in that: the concentration of described ozone water solution is 0.1-5mg/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
4. the assay method of total organic bromine in the water of improvement according to claim 1, is characterized in that: the described concentration containing bromine solutions is 0.1-200 μ g/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
5. the assay method of total organic bromine in the water of improvement according to claim 1, is characterized in that: described is by after water sample effective chlorine solution prechlorination containing bromine solutions, adds bromine-containing compound through the solution filtered, adjust ph obtains; Or, in ultrapure water, add the solution that bromine-containing compound obtains through adjust ph.
6. the assay method of total organic bromine in the water of improvement according to claim 5, it is characterized in that: the concentration of described effective chlorine solution is 0.1-5mg/L, and consumption is 10 ~ 200mL, the time of prechlorination is 1 ~ 3h;
Preferably, described bromine-containing compound is parabromobenzoic acid;
Preferably, described filtration adopts aperture to be that the filter membrane of 0.35 ~ 0.55 μm filters;
Preferably, described adjust ph adopts red fuming nitric acid (RFNA), the concentrated sulphuric acid or concentrated hydrochloric acid to regulate, and pH value is 2 ~ 4.
7. in the water of improvement according to claim 1, the assay method of total organic bromine, is characterized in that: described eluent is NaCl solution or NaNO
3solution, concentration is 4 ~ 8mg/L, and flow velocity is 3 ~ 5mL/min, and the amount passed through is 10 ~ 200mL.
8. the assay method of total organic bromine in the water of improvement according to claim 1, it is characterized in that: described burning cracking carries out in cracking instrument, the temperature of burning is 900-1000 DEG C.
9. the assay method of total organic bromine in the water of improvement according to claim 1, is characterized in that: described absorbing liquid to be concentration be 20 ~ 40% superoxol, consumption is 10 ~ 200mL.
10. the assay method of total organic bromine in the water of improvement according to claim 1, is characterized in that: the concentration of described bromide ion adopts ion chromatograph to measure, and leacheate is the NaHCO of 20 ~ 40mmol/L
3with the Na of 45 ~ 55mmol/L
2cO
3;
Preferably, the computing formula of the described recovery is: the recovery=measured value/standard value × 100%.
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Cited By (3)
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| WO2017202029A1 (en) * | 2016-05-26 | 2017-11-30 | 哈尔滨工业大学深圳研究生院 | Method and system for measuring content of dissolved organic halogens in water |
| CN110044762A (en) * | 2019-04-26 | 2019-07-23 | 华中科技大学 | A method of catalysis reduction-debromination measures total organic bromine content |
| CN111204899A (en) * | 2020-01-17 | 2020-05-29 | 同济大学 | Method for establishing multistage barrier treatment for controlling bromate generation in ozone oxidation process |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2017202029A1 (en) * | 2016-05-26 | 2017-11-30 | 哈尔滨工业大学深圳研究生院 | Method and system for measuring content of dissolved organic halogens in water |
| CN110044762A (en) * | 2019-04-26 | 2019-07-23 | 华中科技大学 | A method of catalysis reduction-debromination measures total organic bromine content |
| CN111204899A (en) * | 2020-01-17 | 2020-05-29 | 同济大学 | Method for establishing multistage barrier treatment for controlling bromate generation in ozone oxidation process |
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