CN105948215A - Water sample preservation method of iodo nitrogen-containing disinfection by-product - Google Patents
Water sample preservation method of iodo nitrogen-containing disinfection by-product Download PDFInfo
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- CN105948215A CN105948215A CN201610493002.8A CN201610493002A CN105948215A CN 105948215 A CN105948215 A CN 105948215A CN 201610493002 A CN201610493002 A CN 201610493002A CN 105948215 A CN105948215 A CN 105948215A
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/02—Devices for withdrawing samples
- G01N1/10—Devices for withdrawing samples in the liquid or fluent state
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- 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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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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
- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/29—Chlorine compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2303/00—Specific treatment goals
- C02F2303/18—Removal of treatment agents after treatment
- C02F2303/185—The treatment agent being halogen or a halogenated compound
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- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Health & Medical Sciences (AREA)
- Water Supply & Treatment (AREA)
- Environmental & Geological Engineering (AREA)
- Organic Chemistry (AREA)
- Physics & Mathematics (AREA)
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- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention discloses a water sample preservation method of an iodo nitrogen-containing disinfection by-product. According to the method, ammonium salt is adopted to serve as a dechlorination agent for a water sample; the pH value of the water sample is adjusted to be 4.5 to 6.5, so that the hydrolysis of the iodo nitrogen-containing disinfection by-product, such as diiodo acetamide (DIacAm), is restrained. The method comprises the following steps: firstly, adding the ammonium salt for the water sample, and controlling the dosage of the ammonium salt to be 2 to 5 times of the molar concentration of free residual chlorine in water; secondly, adding nitrite for the water sample if the water sample preservation time is greater than 1 day, and controlling the dosage of the nitrite to be 1 to 2 times of the molar concentration of total residual chlorine in the water; thirdly, then adjusting the pH value of the water sample to be 4.5 to 6.5 through weak acid, so as to accomplish the preservation of the iodo nitrogen-containing disinfection by-product diiodo acetamide. The method has the advantages that reagents adopted are low in cost and easy to obtain, the preparation method is simple, and subsequent analysis results cannot be affected; the method is efficient and accurate for the preservation of the iodo nitrogen-containing disinfection by-product diiodo acetamide in the water sample.
Description
Technical field
The invention belongs to municipal administration and field of environment engineering technology, relate to the water sample Techniques of preserving of a kind of iodo nitrogenous disinfection byproducts.
Background technology
Drinking water disinfection is made that tremendous contribution to public health security, makes huge numbers of families can obtain the drinking water of safety guarantee.
But disinfectant (chlorine) and the Organic substance in source water or inorganic matter generation chemical reaction, generate disinfection byproduct (DBP).Some of them
By-product the most all has cytotoxicity, genotoxicity and mutability.Toxicology finds in recent years, the poison of nitrogenous disinfection byproducts
Property is typically larger than carbon containing disinfection byproduct (DBP)；And in halo nitrogenous disinfection byproducts, the toxicity of iodo nitrogenous disinfection byproducts is usual
More than bromo and the by-product of chloro.The chronic cell toxicity of two iodo-acetamides (DIAcAm) is to be currently known chronic cell
In the disinfection byproduct (DBP) of toxicity the highest, be the by-product such as chloroform and monoxone of regulation in " drinking water standard "
Hundreds of thousands of times (Plewa and Wagner, Charting a New Path To Resolve the Adverse Health Effects of
DBPs.In Recent Advances in Disinfection By-Products；Xie,et al.；ACS Symposium Series；
American Chemical Society:Washington,DC,2015.).Therefore, for ensureing the safe drinking water of people, to DIAcAm
It is analyzed monitoring to be necessary.Using rational sampling method is the key link of research and application, to chlorination by-product
During thing sampling, need to add dechlorination reagent to terminate chlorination reaction.
Being different from the high stability disinfection byproduct (DBP) such as haloform, two iodo-acetamides (DIAcAm) are unstable, easily in water
Affected by dechlorination reagent and solution acid-basicity.When present stage gathers disinfection byproduct (DBP) water sample in water, how with sodium thiosulfate, Asia
The reducing agents such as sodium sulfate are dechlorination reagent, and add in the way of excess, thus can eliminate chlorine residue thoroughly and remain a part and take off
Chlorine reagent is in water.The dechlorination reagent of this part residual is less on the impact of the high stability disinfection byproduct (DBP) such as haloform, but meeting
Cause the decomposition of DIAcAm, thus cause Instrument measuring analysis result not to be inconsistent with its actual concentrations.Additionally, water sample in alkalescence or
The hydrolysis of DIAcAm is may also lead to during highly acid.Accordingly, it would be desirable to a kind of sampling technique easy, effective ensures that water sample is collected
During the concentration of DIAcAm stable, do not hydrolyze, improve the accuracy of subsequent analysis result.
Summary of the invention
It is an object of the invention to provide the Methods To Preserve Water Samples of a kind of iodo nitrogenous disinfection byproducts, it is ensured that during water sample is collected
The concentration of iodo nitrogenous disinfection byproducts is stable, improves the accuracy of subsequent analysis result.
For reaching above-mentioned purpose, the solution of the present invention is:
The Methods To Preserve Water Samples of a kind of iodo nitrogenous disinfection byproducts, uses ammonium salt as the antichlor of water sample；By the pH of water sample
Regulate between 4.5～6.5 with suppress iodo nitrogenous disinfection byproducts hydrolysis.
Preferably, comprising the steps: that (1) adds ammonium salt in water sample, consumption controls free residual chlorine molar concentration in water
2～5 times；(2) if the water sample holding time was more than 1 day, then adding nitrite in water sample, consumption controls in water total remaining
1～2 times of chlorine molar concentration；(3) use weak acid by between the pH regulator of water sample to 4.5～6.5 immediately, i.e. complete iodo nitrogenous
The preservation of the water sample of disinfection byproduct (DBP).
Preferably, described ammonium salt is ammonium chloride or ammonium sulfate.
Preferably, described weak acid is organic monoacid or salt of weak acid.
Preferably, in water in total residual chlorine amount foundation China " the drinking water sanitary standard method of inspection " (GBT5750-2006)
The method of regulation records.
Described iodo nitrogenous disinfection byproducts is two iodoacetamides.
Owing to using technique scheme, choose the ammonium salts such as ammonium chloride (ammonium sulfate etc. can also) as antichlor, after chlorination,
Water can leave chlorine residue to prevent pathogenic microorganism etc. from breaking out in pipe network.Need during sampling to remove chlorine residue, thus ensure water sample
Chlorination reaction is the most further there is during transport and storage.Sodium sulfite, sodium thiosulfate or Vitamin C would generally be added
Free residual chlorine contained in water removed by the antichlors such as acid.If but these antichlors add excess meeting by two iodo-acetamides
(DIAcAm) the de-iodine of reduction so that it is content changes, thus causes subsequent measurements result distortion.Adopting of novelty of the present invention
With ammonium chloride or ammonium sulfate as antichlor (in fact ammonium chloride and chlorine react generation chloramines, still have certain oxidisability, but
Impact on DIAcAm is less), this antichlor reproducibility is more weak, can eliminate free walker chlorine residue in water, and will not reduce
DIAcAm。
Can directly seal after generally gathering water sample, be sent to laboratory by iced (about≤4 DEG C) subsequently and be analyzed detection.Warp
Cross early stage systematic study to find, if water sample pH>6.5 or pH<when 4.5, in transportation, two iodo-acetamides (DIAcAm)
Hydrolysis can be occurred to generate two iodo acetic acid, so can make the analysis result generation deviation of DIAcAm；The research of the present invention finds,
When using acetic acid (acetic acid), the weak acid such as formic acid, by between pH regulator to 4.5～6.5, can suppress the hydrolysis of DIAcAm, thus
Ensure the accuracy of DIAcAm analysis result in water.
Accompanying drawing explanation
Fig. 1 be embodiment of the present invention initial concentration be 10 μ g/L two iodoacetamides (DIAcAm) reaction 24h after concentration (no
Comparison with in the case of pH value).
Fig. 2 is embodiment of the present invention schematic diagram.
Detailed description of the invention
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further illustrated.
The problem existed for existing water sample Techniques of preserving, it is an object of the invention to provide a kind of improvement two iodo-acetamides
(DIAcAm) method that such a high toxicity iodo nitrogenous disinfection byproducts water sample preserves.As in figure 2 it is shown, the method bag
Include following steps: (1) is added the ammonium salts such as a certain amount of ammonium chloride or ammonium sulfate in water body and (controlled free residual chlorine in water to rub
2～5 times of that concentration)；(2) as water sample (more than 1 day) need to be preserved for a long time, a certain amount of nitrous acid must be added again in water sample
Salt (controls 1～2 times of total residual chlorine molar concentration in water)；(3) weak acid (organic monoacid such as acetic acid, formic acid or weak is used immediately
Hydrochlorate) by between the pH regulator of water body to 4.5～6.5, i.e. complete the preservation of DIAcAm water sample.Specific as follows:
The present invention uses ammonium salt such as ammonium chloride or ammonium sulfate etc. as antichlor (this paragraph is as a example by ammonium chloride), added ammonium chloride
Dosage (molar concentration) need to control 2～5 times of chlorine residue molar concentration in water, i.e. [ammonium chloride dosage]=2～5 × [water
In free property residual chlorine amount], in water, free property residual chlorine amount can be according to China " the drinking water sanitary standard method of inspection "
(GBT5750-2006) in, the method for regulation records that (free residual chlorine measures and is set to the logical property known assay method, does not protects in the present invention
Protect scope).It is true that ammonium chloride and chlorine (i.e. HOCl etc.) react generation monochloro amine (NH2Cl), NH2Although Cl still has
Certain oxidisability, but less to DIAcAm stability influence (in one day) at short notice, and the ammonium chloride of excess or
Ammonium sulfate can suppress the formation of free residual chlorine (HOCl etc.), as shown in formula 1 and 2, thus avoids the free property such as HOCl
The chlorine residue oxygenolysis to DIAcAm.
NH4Cl+HOCl f NH2Cl+HCl+H2O (1)
(NH4)2SO4+2HOCl f 2NH2Cl+H2SO4+2H2O (2)
If desired for the preservation water sample of longer time, time i.e. more than one, it is contemplated that monochloro amine (NH2Cl) still have certain weak
Oxidisability, needs to add the nitrites such as a certain amount of sodium nitrite again, can remove NH further2The oxidisability of Cl.Now
Water sample not only comprises free residual chlorine (HOCl etc.) but also comprises combined residual chlorine (NH2Cl etc.), by being added sodium nitrite
Dosage (molar concentration) be also required to control 1～2 times of total residual chlorine molar concentration in water sample, i.e. [sodium nitrite dosage]=
1～2 × [total residual chlorine amount in water], in water, total residual chlorine amount also can be according to China " the drinking water sanitary standard method of inspection "
(GBT5750-2006) in, the method for regulation records that (total residual chlorine measures and is set to the logical property known assay method, does not protects model in the present invention
Enclose).After adding the process of ammonium salt and nitrite, need to add the weak acid such as acetic acid or acetate immediately or salt of weak acid regulates
In water sample pH to 4.5～6.5, to prevent DIAcAm to be hydrolyzed into iodo acetic acid (formula 3).As in figure 2 it is shown, after dechlorination
In tap water, configuration concentration is the DIAcAm of 10 μ g/L, and research finds, under different pH condition, keep in Dark Place water sample 24
After hour, DIAcAm concentration corresponding during pH to 4.5～6.5 is closest to 10 μ g/L, i.e. DIAcAm during pH=4.5～6.5
Stability is preferable.
Embodiment one: the present embodiment is two iodo-acetamides (DIAcAm) hydrolysis and a kind of DIAcAm of chlorination in suppression water
Methods To Preserve Water Samples, it is achieved by the steps of: assume that by measuring the free residual chlorine content found in water sample be 0.05
Mmol/L, then just can add the ammonium chloride (i.e. 0.1mmol/L) of free residual chlorine molar concentration in 2 times of water, if
The water sample plan holding time is less than one day, can add a small amount of acetic acid (i.e. acetic acid) immediately and control near 4.5 by water sample pH,
Then keep in Dark Place.If the water sample plan holding time was more than one day, aforementioned add superchlorination ammonium after, need to measure again
The content of total residual chlorine, it is assumed that for 0.15mmol/L, then just can add the sodium nitrite of total residual chlorine molar concentration in 1 times of water
(i.e. 0.15mmol/L), and control, 4.5, to keep in Dark Place subsequently by water sample pH with a small amount of acetic acid (i.e. acetic acid).
The chemical drugs acetic acid, sodium nitrite and the ammonium chloride that are used of the present embodiment are cheap, will not produce secondary pollution,
Without complicated subsequent treatment, subsequent measurement also will not be produced impact.
Embodiment two: the present embodiment is two iodo-acetamides (DIAcAm) hydrolysis and a kind of DIAcAm of chlorination in suppression water
Methods To Preserve Water Samples, it is achieved by the steps of: based on measuring free property contents of residual chlorine (molar concentration) in water sample, throw
Add the ammonium chloride of free residual chlorine molar concentration in 5 times of water, if the water sample plan holding time less than one day, adds a small amount of
Water sample pH is controlled, 6.5, to keep in Dark Place subsequently by acetic acid (i.e. acetic acid).If the water sample plan holding time was more than one day, need
To measure the content of total residual chlorine again, add the sodium nitrite of total residual chlorine molar concentration in 2 times of water, and with acetic acid (i.e. acetic acid)
Control water sample pH, 6.5, to keep in Dark Place subsequently.
Embodiment three: the present embodiment is two iodo-acetamides (DIAcAm) hydrolysis and a kind of DIAcAm of chlorination in suppression water
Methods To Preserve Water Samples, it is achieved by the steps of: based on measuring free property contents of residual chlorine molar concentration in water sample), add
The ammonium chloride of free residual chlorine molar concentration in 3.5 times of water, if the water sample plan holding time is less than one day, adds a small amount of vinegar
Water sample pH is controlled, 5.5, to keep in Dark Place subsequently by acid (i.e. acetic acid).If the water sample plan holding time was more than one day, need
Measure the content of total residual chlorine again, add the sodium nitrite of free residual chlorine molar concentration in 1.5 times of water, and by acetic acid (i.e. second
Acid) control, 5.5, to keep in Dark Place subsequently by water sample pH.
Embodiment four: the present embodiment selects ammonium sulfate to substitute ammonium chloride as antichlor unlike embodiment one, other steps
And parameter is identical with detailed description of the invention one.
Embodiment five: the present embodiment selects formic acid to regulate water sample pH value unlike embodiment one and substitutes acetic acid, other steps
And parameter is identical with embodiment one.
Embodiment six: the present embodiment selects potassium nitrite to substitute sodium nitrite unlike embodiment one, other steps and ginseng
Number is identical with detailed description of the invention one.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and apply the present invention.It is familiar with
These embodiments obviously easily can be made various amendment by the personnel of art technology, and should General Principle described herein
Use in other embodiments without through performing creative labour.Therefore, the invention is not restricted to the embodiments described, this area skill
Art personnel should be at the protection model of the present invention according to the announcement of the present invention, the improvement made without departing from scope and amendment
Within enclosing.
Claims (6)
1. the Methods To Preserve Water Samples of an iodo nitrogenous disinfection byproducts, it is characterised in that: use ammonium salt as the antichlor of water sample；
By between the pH regulator of water sample to 4.5～6.5 with suppress iodo nitrogenous disinfection byproducts hydrolysis.
The Methods To Preserve Water Samples of iodo nitrogenous disinfection byproducts the most according to claim 1, it is characterised in that include walking as follows
Rapid: (1) adds ammonium salt in water sample, consumption controls 2～5 times of free residual chlorine molar concentration in water；(2) if water sample preserves
Time is more than 1 day, then adds nitrite in water sample, and consumption controls 1～2 times of total residual chlorine molar concentration in water；(3) with
I.e. use weak acid by between the pH regulator of water sample to 4.5～6.5, i.e. complete the preservation of the water sample of iodo nitrogenous disinfection byproducts.
The Methods To Preserve Water Samples of iodo nitrogenous disinfection byproducts the most according to claim 1, it is characterised in that: described ammonium salt
For ammonium chloride or ammonium sulfate.
The Methods To Preserve Water Samples of iodo nitrogenous disinfection byproducts the most according to claim 1, it is characterised in that: described weak acid
For organic monoacid or salt of weak acid.
The Methods To Preserve Water Samples of iodo nitrogenous disinfection byproducts the most according to claim 2, it is characterised in that: total remaining in water
Chlorine dose records according to the method for regulation in China " the drinking water sanitary standard method of inspection " (GBT5750-2006).
6. according to the Methods To Preserve Water Samples of described iodo nitrogenous disinfection byproducts arbitrary in claim 1 to 5, it is characterised in that:
Described iodo nitrogenous disinfection byproducts is two iodoacetamides.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109292896A (en) * | 2018-09-30 | 2019-02-01 | 同济大学 | A kind of method of humic acid in control drinking water |
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