CN102520084B - Method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water - Google Patents
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Abstract
The invention belongs to the environmental protection and water treatment technical field, and discloses a method for determining trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water. The method comprises the following steps 1) acidifying and pretreating a sample; 2) acidifying, drying and filling a solid phase extraction material; 3) controlling a solid phase extraction process, eluting and purifying an eluate; 4) naturally volatilizing the sample and controlling with constant volume; 5) using a liquid chromatography-mass spectrometry for analyzing dimethyl nitrosamine to obtain the determination result. Compared with the current international test methods, the method of the invention has the characteristics of rapidity, simpleness, little application amount of the poisonous and harmful organic solvent, accurate analysis and the like.
Description
Technical field
The invention belongs to environmental protection and water-treatment technology field, relate to the method for a kind of mensuration trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water (NDMA).
Background technology
N-nitrosodimethylamine (NDMA) is a kind of new Chlorination Disinfection By-products recently extensively detecting in the potable water on the ground such as America & Canada.In water, NDMA is found for 1989 in the waterworks of an employing chloramines disinfection in Ontario, Canada province Ohsweken district, then in the water factory of other several the identical sterilization process of employing, NDMA also detected.The report that at present has NDMA to detect in water factories such as the U.S., Canada, Europe.Investigation is found, adopt the water factory of combined chlorine sterilization, even adopt in the water factory of ion-exchange process and also detected this material [Choi J, Valentine R L.Formation of N-nitrosodimethylamine (NDMA) from reaction of monochloramine:a new disinfection by-product[J] .WaterRes, 2002,36 (4), 817-824.].U.S. EPA is classified as one of 200 kinds of carcinogens [USEPA.Integrated Risk Information Service[R] .USA:United States Environmental Protection Agency, Office of Research and Development, National Center for Environmental Assessment, 1991.], its carcinogenic grade is 2 grades, in exposure concentrations, be only under the condition of 0.7ng/L, theoretical carcinogenic risk coefficient can reach 10
-6.
Conventionally in potable water the concentration of NDMA all in the level of ng/L, conventional sense method is generally carried out water sample by liquid-liquid extraction or Solid-Phase Extraction and is concentrated, and then carry out separation and quantitative [Charrois J W A by chromatograph-mas spectrometer, Arend M W, Froese K L, Hrudey S E.Detecting N-nitrosamines in drinking water at nonogram per litre levels using ammonia positive chemical ionization[J] .Environ Sci Technol, 2004,38 (21): 4835-4841.].2004, EPA (USEPA) has announced the detection method of nitrosamines material in potable water [EPA/600/R-05/054, Determination of Nitrosamines in Drinking Water by Solid Phase Extraction and Capillary Column Gas Chromatographywith Large Volume Injection and Chemical Ionization Tandem Mass Spectrometry (MS/MS) [S] .] Solid-Phase Extraction/capillary gas chromatography/chemical ionization source mass spectrometry.The method adopts Lichrolut EN and Ambersorb 572 as solid phase extraction adsorbents, and NDMA-d6 is internal standard compound, and its analyzing and testing limit (DL) is 0.28ng/L, and report detectability (RDL) is 1.6ng/L.Ontario Ministry of environment (OME) has announced [OME.The Determination of N-nitrosodimethylamine (NDMA) in Water bv Gas Chromatography high Resolution Mass Spectrometry (GC-HRMS) [R] the .Canada:On-tarioMinistry of Environment of NDMA assay method in detection potable water in same year, 2004.], Solid-Phase Extraction adopts Ambersorb 572 as adsorbent, with methylene chloride, carry out elution, by gas chromatography and high resolution mass spectrometry, complete separated and quantitative, its detectability (DL) is 0.4ng/L, report detectability (RDL) is 1.0ng/L.It is reported, there is problem [the Cheng R C.AlternativeMethods for the Analysis of NDMA and Other Nitrosamines in Water and Wastewater such as the recovery is low, measuring accuracy stability is bad, sense cycle is long, operation steps is complicated in these methods, ReportWRF-01-001[R] .Long Beach, California:Water Reuse Foundation, 2006.].
Summary of the invention
The problems such as, sense cycle low for the current conventional sense method recovery is long, operation steps is complicated, the object of this invention is to provide the method for a kind of mensuration trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water (NDMA); The method is simple to operate, measuring accuracy is high, can effectively reduce sense cycle.
Technical scheme of the present invention is as follows:
The invention provides a kind of method of measuring trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water, the method comprises the following steps: 1) water sample acidifying pre-service; 2) acidifying of Solid-Phase Extraction material, dry and filling; 3) control Solid-Phase Extraction process, wash-out and purify eluent; 4) volatilization naturally of sample is controlled with constant volume; 5) application liquid chromatography mass technical Analysis N-nitrosodimethylamine, obtains measurement result.
Described water sample is selected from surface water, underground water or potable water.
Described step 1) in, water sample acidifying pre-service takes a step forward and comprises particle removal step.
In described water sample, particle removal method is: with the membrane filtration of aperture≤0.45 μ m, remove graininess impurity, material selection cellulose acetate film or the poly (ether sulfone) film of filter membrane.
Described step 1) in, acidifying preprocess method is: collect and filter rear water sample to 500mL or 1000mL, then add sulfuric acid or NaOH to regulate pH value to 6～8, then water sample be positioned in brown bottle and adopt lucifuge measure.
Described step 2), in, Solid-Phase Extraction material adopts wooden powder's activated charcoal, its average particle size≤40 μ m.
Described step 2) in, the acidifying of Solid-Phase Extraction material is to adopt the sulfuric acid water acidifying that pH is 2.3.
Described step 2) in, the dry of Solid-Phase Extraction material is by the 105 ℃ of oven dry in baking oven of Solid-Phase Extraction material after acidifying.
Described step 2) in, the packing method of Solid-Phase Extraction material is: weigh the Solid-Phase Extraction material of getting after 1g is dried in the balance, be packed in Solid-Phase Extraction (SPE) void column of the high-molecular polythene of 6mL, sieve plate adopts ultra-high molecular weight polyethylene material, fills out tight and compacting.
Described step 3) method of controlling Solid-Phase Extraction process in is: regulate the vacuum tightness of SPE device, the filtering velocity that makes water sample is 2～5mL/min, by the SPE void column filling; In water sample filter process, should avoid occurring cutout phenomenon.
Described step 3) in, the method for wash-out is: adopt 2ml acetonitrile, and twice-2ml methyl alcohol, twice-2ml acetone, twice wash-out, drains front solvent and in post, soaks 3～4min, guarantees to add the front pillar of solvent thoroughly to drain at every turn.
Described step 3) method that purifies eluent in is: under extraction pillar, add florisil post (Florey tripoli pillar), specification is 0.5g * 3mL, makes solvent when flowing through florisil post, and the impurity that may contain in solvent is removed.
Described step 4) in, the volatilization naturally of sample with constant volume control method is: adopt band scale tapered tube splendid attire eluent, and be placed in 35～40 ℃ of sand-baths, lucifuge evaporates into 1mL naturally, accurate recording final volume.
Described step 5) in, liquid chromatography mass technology adopts ESI source triple level Four bar liquid chromatography mass combined instrument, chromatographic column is C8 and C18 separating column, and mobile phase is adopted as methyl alcohol+2mmol/L ammonium acetate, and flow velocity is 150 μ L/min, sampling volume is 50 μ L, and the bulk analysis time is 10min; Mass spectrographic ion injection electric is 4500kv, and ion source temperature is 350 ℃, and the monitoring ion quantitative result of NDMA is that m/z 75-43 and qualitative results are m/z 75-58, and the monitoring ion of internal standard compound NDMA-d6 is m/z 81-46.
Described step 5) in, Instrument measuring value is for this assay method is by the concentration of N-nitrosodimethylamine in the concentrated water sample obtaining, and actual water sample N-nitrosodimethylamine concentration is that Instrument measuring value is divided by cycles of concentration.
The present invention compared with the existing technology, has the following advantages and beneficial effect:
1, by assay method of the present invention, can effectively improve the extraction efficiency of underwater trace NDMA, greatly reduce the matrix interference in liquid matter analytic process simultaneously, guarantee accuracy and the accuracy of test;
2, the inventive method is compared with existing method of testing in the world, and it is quick, easy that this method has, and poisonous and harmful organic solvent use amount seldom, is analyzed the features such as accurate.
3, the present invention has improved accuracy and analysis precision that NDMA detects greatly, and detectability can reach 2ng/L, has effectively overcome the difficult problems such as conventional sense method NDMA detects limit for height, and the liquid-liquid extraction recovery is low, and toxic solvent use amount is few simultaneously.
4, the whole mensuration process of method of the present invention easy operating, cost are lower, can be widely used in earth's surface and groundwater monitoring, large, the monitoring and the analysis that neutralize small-sized water factory.
5, detection method step of the present invention is less, simple to operate, and sense cycle is shorter; Because mobile phase adopts methyl alcohol and 2mmol/L ammonium acetate and gradient is set, N-nitrosodimethylamine is can be in LC-MS-MS detection method effectively separated and go out peak, select that to NDMA, to have compared with wooden powder's activated charcoal of high absorption capacity be solid phase extraction adsorbents simultaneously, thereby can obtain the higher NDMA recovery, measuring accuracy good stability.
Accompanying drawing explanation
Fig. 1 is the operational flowchart of the embodiment of the present invention.
Fig. 2 be in the embodiment of the present invention the different pH of water sample to measurement result figure.
Fig. 3 be in the embodiment of the present invention different types of elution to measurement result figure.
Fig. 4 applies this method to measure NDMA concentration change figure in water-purifying process in the embodiment of the present invention.
Embodiment
Below in conjunction with accompanying drawing illustrated embodiment, the present invention is further illustrated.
Embodiment 1
Water sample is Mill-Q water (ultrapure water).At 12 groups of volumes, be in 500mLMill-Q water (ultrapure water) and add NDMA standard items, making NDMA concentration is 1 μ g/L, due to this water sample no suspended substance and granule foreign, thereby without filtration.
Acidifying preprocess method: using NaOH or sulfuric acid to regulate the pH value of 12 groups of water samples to be measured water sample is 1,2,3,4,5,6,7,8,9,10,11,12, is positioned in brown bottle by water sample and adopts lucifuge measure to preserve.
The acidifying of Solid-Phase Extraction material, dry and filling; Using wooden powder's activated charcoal of using as Solid-Phase Extraction, its average particle size≤40 μ m, is used the sulfuric acid water acidifying that pH is 2.3, wooden powder's activated charcoal 105 ℃ of oven dry in baking oven after acidifying; Weigh wooden powder's activated charcoal of getting after 1g is dried in the balance and be packed in Solid-Phase Extraction (SPE) void column of the high-molecular polythene of 6mL, sieve plate adopts ultra-high molecular weight polyethylene material, fills out tight and compacting, will extract pillar access extraction equipment.
Control Solid-Phase Extraction process, wash-out and purify eluent; Adopt commercially available SPE device, regulate the vacuum tightness of SPE device, make the filtering velocity of water sample in 2mL/min, by the SPE post filling; In water sample filter process, should avoid occurring cutout phenomenon, the general no more than 24h of adsorption time.When being about to find time, takes off water sample extraction pillar.
The method that purifies eluent is: under extraction pillar, access florisil post (Florey tripoli pillar, 0.5g, 3mL specification), access washing device.Elution step is 2ml acetonitrile (twice)-2ml methyl alcohol (twice)-2ml acetone (twice) wash-out, drains front solvent and in post, soaks 4min, guarantees to add the front pillar of solvent thoroughly to drain at every turn.In elution process, solvent streams, through florisil post, is removed the impurity that may contain in solvent in florisil post.
Naturally the volatilization of sample with constant volume control method is: adopt the tapered tube splendid attire eluent with scale, and be placed in 40 ℃ of sand-baths, lucifuge evaporates into 1mL naturally, accurate recording final volume.
Application liquid chromatography mass technical Analysis NDMA, obtains measurement result; Liquid chromatography mass technology adopts ESI source triple level Four bar liquid chromatography mass combined instrument, and chromatographic column is C18 separating column, and mobile phase is adopted as methyl alcohol+2mmol/L ammonium acetate, and flow velocity is 150 μ L/min, and sampling volume is 50 μ L, and the bulk analysis time is 10min; Mass spectrographic ion injection electric is 4500kv, and ion source temperature is 350 ℃, and the monitoring ion quantitative result of NDMA is that m/z 75-43 and qualitative results are m/z 75-58, and the monitoring ion of internal standard compound NDMA-d6 is m/z 81-46.
Instrument measuring value is for this assay method is by the concentration of NDMA in the concentrated water sample obtaining, and actual water sample NDMA concentration is that Instrument measuring value is divided by cycles of concentration.By actual water sample NDMA concentration, divided by 1ug/L, as shown in Figure 2, wherein every kind of pH value is done three groups of parallel laboratory tests to obtain under different water sample pH value conditions recovery variation tendency.
Fig. 2 be in embodiment the different pH of water sample to measurement result figure.As shown in Figure 2, under condition of neutral pH, the NDMA recovery is higher, is positioned at 70%～90%, and relative standard deviation is positioned at 1.70%～2.60%, has higher stability.Under peracid and excessively alkali condition, the recovery declines to some extent, and especially pH is that 2 o'clock recovery are down to 40% left and right, and under extreme pH condition, the recovery is unstable, and relative standard deviation is up to 6.40%, and therefore, while detecting sample, the control of pH value is most important.
Embodiment 2
Water sample is Mill-Q water (ultrapure water).At 5 groups of volumes, be in 500mLMill-Q water (ultrapure water) and add NDMA standard items, making NDMA concentration is 1 μ g/L, and water sample pH value is 7, so this water sample is without filtering and regulate pH.
Acidifying preprocess method: water sampling 500mL, is positioned in brown bottle by water sample and adopts lucifuge measure to preserve.
The acidifying of Solid-Phase Extraction material, dry and filling; Using wooden powder's activated charcoal of using as Solid-Phase Extraction, its average particle size≤40 μ m, is used the sulfuric acid water acidifying that pH is 2.3, wooden powder's activated charcoal 105 ℃ of oven dry in baking oven after acidifying.Weigh wooden powder's activated charcoal of getting after 1g is dried in the balance and be packed in Solid-Phase Extraction (SPE) void column of the high-molecular polythene of 6mL, sieve plate adopts ultra-high molecular weight polyethylene material, fills out tight and compacting, will extract pillar access extraction equipment.
Control Solid-Phase Extraction process, wash-out and purify eluent; Adopt commercially available SPE device, regulate the vacuum tightness of SPE device, make the filtering velocity of water sample in 2mL/min, by the SPE post filling; In water sample filter process, should avoid occurring cutout phenomenon, the general no more than 24h of adsorption time.When being about to find time, takes off water sample extraction pillar.
The method that purifies eluent is: under extraction pillar, access florisil post (Florey tripoli pillar, 0.5g, 3mL specification), access washing device.Five groups of water samples adopt respectively five kinds of types of elution in table 1, investigate respectively eluant, eluent kind, eluting order, the impact of eluant, eluent volume on the recovery.Drain front solvent and in post, soak 4min, guarantee to add the front pillar of solvent thoroughly to drain at every turn.In elution process, solvent streams, through florisil post, is removed the impurity that may contain in solvent in florisil post.
Table 1
Naturally the volatilization of sample with constant volume control method is: adopt the tapered tube splendid attire eluent with scale, and be placed in 40 ℃ of sand-baths, lucifuge evaporates into 1mL naturally, accurate recording final volume.
Application liquid chromatography mass technical Analysis NDMA, obtains measurement result; Liquid chromatography mass technology adopts ESI source triple level Four bar liquid chromatography mass combined instrument, and chromatographic column is C8 separating column, and mobile phase is adopted as methyl alcohol+2mmol/L ammonium acetate, and flow velocity is 150 μ L/min, and sampling volume is 50 μ L, and the bulk analysis time is 10min; Mass spectrographic ion injection electric is 4500kv, and ion source temperature is 350 ℃, and the monitoring ion quantitative result of NDMA is that m/z 75-43 and qualitative results are m/z 75-58, and the monitoring ion of internal standard compound NDMA-d6 is m/z 81-46.
Instrument measuring value is for this assay method is by the concentration of NDMA in the concentrated water sample obtaining, and actual water sample NDMA concentration is that Instrument measuring value is divided by cycles of concentration.
Fig. 3 be in embodiment different types of elution to measurement result figure.As shown in Figure 3, there is no acetone in type of elution B, the recovery is minimum, so the effective wash-out NDMA of acetone.The type of elution A recovery is the highest, and therefore, when investigation other factors affects the recovery, type of elution can be defined as A, and concrete operations mode is: 2mL acetonitrile (twice)-2mL methyl alcohol (twice)-2mL acetone (twice).Before elution, 2mL solvent soaks 3-4 minute in post.Before adding 2mL solvent, should make pillar drain at every turn.
Embodiment 3
Fig. 1 is the operational flowchart of the embodiment of the present invention.Water sample is surface water.Set-up procedure before extraction: the cellulose acetate film that first each water sample of water purification process is less than or equal to 0.45 μ m by aperture filters, elimination suspension, granule foreign, each water sample of water purification process is faintly acid.Acidifying preprocess method: get and filter rear water sample 500mL, be positioned in brown bottle and adopt lucifuge measure, using NaOH to regulate the pH value of water sample to be measured is 7, and keeps in Dark Place.
The acidifying of Solid-Phase Extraction material, dry and filling; Using wooden powder's activated charcoal of using as Solid-Phase Extraction, its average particle size≤40 μ m, is used the sulfuric acid water acidifying that pH is 2.3, wooden powder's activated charcoal 105 ℃ of oven dry in baking oven after acidifying.Weigh wooden powder's activated charcoal of getting after 1g is dried in the balance and be packed in Solid-Phase Extraction (SPE) void column of the high-molecular polythene of 6mL, sieve plate adopts ultra-high molecular weight polyethylene material, fills out tight and compacting, will extract pillar access extraction equipment.
Control Solid-Phase Extraction process, wash-out and purify eluent; Adopt commercially available SPE device, regulate the vacuum tightness of SPE device, make the filtering velocity of water sample in 2mL/min, by the SPE post filling; In water sample filter process, should avoid occurring cutout phenomenon, the general no more than 24h of adsorption time.When being about to find time, takes off water sample extraction pillar.
The method that purifies eluent is: under extraction pillar, access florisil post (Florey tripoli pillar, 0.5g, 3mL specification), access washing device.Elution step is 2ml acetonitrile (twice)-2ml methyl alcohol (twice)-2ml acetone (twice) wash-out, drains front solvent and in post, soaks 3～4min, guarantees to add the front pillar of solvent thoroughly to drain at every turn.In elution process, solvent streams, through florisil post, is removed the impurity that may contain in solvent in florisil post.
Naturally the volatilization of sample with constant volume control method is: adopt the tapered tube splendid attire eluent with scale, and be placed in 40 ℃ of sand-baths, lucifuge evaporates into 1mL naturally, accurate recording final volume.
Application liquid chromatography mass technical Analysis NDMA, obtains measurement result; Liquid chromatography mass technology adopts ESI source triple level Four bar liquid chromatography mass combined instrument, and chromatographic column is C18 separating column, and mobile phase is adopted as methyl alcohol+2mmol/L ammonium acetate, and flow velocity is 150 μ L/min, and sampling volume is 50 μ L, and the bulk analysis time is 10min; Mass spectrographic ion injection electric is 4500kv, and ion source temperature is 350 ℃, and the monitoring ion quantitative result of NDMA is that m/z 75-43 and qualitative results are m/z 75-58, and the monitoring ion of internal standard compound NDMA-d6 is m/z 81-46.
Instrument measuring value is for this assay method is by the concentration of NDMA in the concentrated water sample obtaining, by the numerical value of measuring divided by cycles of concentration, thereby draw the concentration of NDMA in former water sample.
Fig. 4 applies this method to measure NDMA concentration change figure in water-purifying process in embodiment.The former water of Raw=in figure, BP=Biological Pretreatment, Sed=precipitation, Fil=filters, ozone after PO=, BAC=biological activated carbon, Fin=water outlet.
As can be seen from Figure 4, all do not detect NDMA in micro-polluted raw, in Biological Pretreatment, precipitation, filtering technique, do not generate NDMA, rear ozone treatment can directly generate finite concentration NDMA, and its concentration can reach 13.7ng/L.Follow-up BAC process has certain removal effect to NDMA, the NDMA that can adsorb and degrade in part water, and its clearance can reach 21.3%.In water outlet, NDMA concentration is 11.5ng/L.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (2)
1. a method of measuring trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water, is characterized in that: the method comprises the following steps: 1) water sample acidifying pre-service; 2) acidifying of Solid-Phase Extraction material, dry and filling; 3) control Solid-Phase Extraction process, wash-out and purify eluent; 4) volatilization naturally of sample is controlled with constant volume; 5) application liquid chromatography mass technical Analysis N-nitrosodimethylamine, obtains measurement result;
Described step 1) in, water sample acidifying pre-service takes a step forward and comprises particle removal step;
In described water sample, particle removal method is: with the membrane filtration of aperture≤0.45 μ m, material selection cellulose acetate film or the poly (ether sulfone) film of filter membrane;
Described step 1) in, acidifying preprocess method is: collect and filter rear water sample to 500mL or 1000mL, then add sulfuric acid or NaOH to regulate pH value to 6～8, then water sample be positioned in brown bottle and adopt lucifuge measure;
Described step 2), in, Solid-Phase Extraction material adopts wooden powder's activated charcoal, its average particle size≤40 μ m; Described step 2) in, the acidifying of Solid-Phase Extraction material is to adopt the sulfuric acid water acidifying that pH is 2.3; Described step 2) in, the dry of Solid-Phase Extraction material is by the 105 ℃ of oven dry in baking oven of Solid-Phase Extraction material after acidifying; Described step 2) in, the packing method of Solid-Phase Extraction material is: weigh the Solid-Phase Extraction material of getting after 1g is dried in the balance, be packed in the Solid-Phase Extraction SPE void column of high-molecular polythene of 6mL, sieve plate adopts ultra-high molecular weight polyethylene material, fills out tight and compacting;
Described step 3) method of controlling Solid-Phase Extraction process in is: regulate the vacuum tightness of SPE device, the filtering velocity that makes water sample is 2～5mL/min, by the SPE void column filling; Described step 3) in, the method for wash-out is: adopt 2ml acetonitrile-twice, and 2ml methyl alcohol-twice, 2ml acetone-twice, wash-out, drains front solvent and in post, soaks 3～4min;
Described step 3) method that purifies eluent in is: under extraction pillar, add florisil post, specification is 0.5g * 3mL;
Described step 4) in, the volatilization naturally of sample with constant volume control method is: adopt band scale tapered tube splendid attire eluent, and be placed in 35～40 ℃ of sand-baths, lucifuge evaporates into 1mL naturally, accurate recording final volume;
Described step 5) in, liquid chromatography mass technology adopts ESI source triple level Four bar liquid chromatography mass combined instrument, chromatographic column is C8 or C18 separating column, and mobile phase is adopted as methyl alcohol+2mmol/L ammonium acetate, and flow velocity is 150 μ L/min, sampling volume is 50 μ L, and the bulk analysis time is 10min; Mass spectrographic ion injection electric is 4500kv, and ion source temperature is 350 ℃, and the monitoring ion quantitative result of N-nitrosodimethylamine is that m/z75-43 and qualitative results are m/z75-58, and the monitoring ion of internal standard compound N-nitrosodimethylamine-d6 is m/z81 – 46; Described step 5) in, Instrument measuring value is for this assay method is by the concentration of N-nitrosodimethylamine in the concentrated water sample obtaining, and actual water sample N-nitrosodimethylamine concentration is that Instrument measuring value is divided by cycles of concentration.
2. the method for mensuration trace nitrogen-containing disinfection by-product dimethyl nitrosamine in water according to claim 1, is characterized in that: described water sample is selected from surface water, underground water or potable water.
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