CN107356539A - A kind of method of nitrogen nutrition salinity in quick detection seawater - Google Patents
A kind of method of nitrogen nutrition salinity in quick detection seawater Download PDFInfo
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Abstract
The present invention relates to a kind of method of nitrogen nutrition salinity in quick detection seawater, comprise the following steps：The collection and pretreatment of seawater sample；Nitrite nitrogen concentration mensuration；Nitrate nitrogen concentration mensuration；Ammonia nitrogen concentration determines.Wherein, developer C1/C2/C3 forms by concentrated hydrochloric acid, sulfanilamide (SN), naphthodiamide salt and water mixed preparing.Concentrated hydrochloric acid, sulfanilamide (SN) and naphthodiamide salt are configured to obtain Single Reagent so that only need developer of addition to complete process color in continuous mode, it is easy to operate, quick；And developer is in colourless, the color and effect stability of developer, it is ensured that the accuracy of result of the test；This Single Reagent avoids naphthodiamide salting liquid in traditional assay method and produces error because color gradually deepens；The present invention determines the concentration of nitrate nitrogen and ammonia nitrogen by minusing, easy to operate, fast；The present invention is simple to operate, quick, time saving and energy saving, error is small, is especially suitable for the field quick detection of nitrogen nutrition salinity in seawater.
Description
Technical field
The present invention relates to quantitative chemical analysis field, specifically a kind of water quality monitoring technology is particularly a kind of quick
The method for detecting nitrogen nutrition salinity in seawater.
Background technology
Nitrogen nutrition salt in seawater --- nitrite nitrogen (NO2 -- N), nitrate nitrogen (NO3 -- N), ammonia nitrogen (NH4 +- N) (with
Lower abbreviation " three nitrogen ") be marine monitoring essential items for inspection.Method for determining in seawater " three nitrogen " concentration is a lot, such as ultraviolet point
Light photometry, the chromatography of ions, chemoluminescence method, Flow Injection Analysis etc., but these methods are present that sensitivity is low, instrument is not portable
Band, it is difficult to the problems such as live the real time measure or complex operation.
China can follow for the measure of " three nitrogen " concentration in seawater《GB 17378.4-2007 marine monitorings specification the 4th
Point：Sea water analysis》Or《The part of GB/T 12763.4-2007 standard of marine survey the 4th：Sewater chemistry key element is investigated》Middle related side
Method, i.e.,：Naphthodiamide (diazonium-azo) AAS of nitrite nitrogen, cadmium (cadmium copper) the post reducing process of nitrate nitrogen or
Zinc Cadmium Reduction, indigo spectrophotometry or hypobromite (sodium) oxidizing process of ammonia nitrogen.Wherein, except the indophenol blue of measure ammonia nitrogen
Outside AAS, the measure of " three nitrogen " concentration is based on diazonium-coupling spectrophotometric principles of nitrite nitrogen in seawater,
I.e. in acid medium, with sulfanilamide (SN) diazo-reaction occurs for nitrite, and reaction product is coupled with hydrochloride naphthodiamide generates again
Red azo dyestuff, colorimetric estimation is carried out under certain wavelength.Nitrate nitrogen obtains nitrous acid by reduction, ammonia nitrogen through peroxidating
Salt nitrogen, then measured by diazonium-coupling AAS of nitrite nitrogen.In this way, " three nitrogen " concentration in measure seawater, nitrous
Hydrochlorate nitrogen concentration can be obtained directly by standard curve, the concentration of nitrate nitrogen and ammonia nitrogen can then be obtained by minusing (first by
The standard curve of nitrate nitrogen or ammonia nitrogen obtains each concentration sum with original nitrite nitrogen in water sample, then subtract in water sample
Original nitrite nitrogen concentration, obtains nitrate nitrogen or ammonia nitrogen concentration).Being determined using the above method in seawater " three nitrogen " to reduce
The error caused by Method And Principle differs, is most widely used.
But in the above-mentioned methods, the process colors of all nitrite be both needed to sulfanilamide (SN) solution (hydrochloric acid solution is matched somebody with somebody) and
Hydrochloride naphthodiamide solution is added in sample in two steps, and development step is cumbersome.Due to hydrochloride naphthodiamide solution concentration used
Higher (1g/L), hydrochloride naphthodiamide solution starts, in golden yellow, to elapse color over time and constantly deepen to burgundy, if will
Itself and sulfanilamide (SN) solution mixed preparing developer, then developer start for yellow, to elapse color over time and constantly deepen to dark brown
Color.The absorbance of reagent blank is increasing over time, not only brings larger error, also causes color developing effect to be difficult to protect
Card.Therefore not by sulfanilamide (SN), hydrochloric acid solution and hydrochloride naphthodiamide solution mixed preparing developer in national standard method, but match somebody with somebody respectively
Sulfanilamide (SN) solution (hydrochloric acid solution is matched somebody with somebody) processed and hydrochloride naphthodiamide solution, need to match somebody with somebody again when hydrochloride naphthodiamide solution colour is too deep
System.
In addition, the nitrate reduction in water sample is nitrite by copper facing cadmium post by Cadmium reduction column, this process is complicated,
It is cumbersome.Cadmium reduction column and hypobromite oxidation method all refer to repeatedly pipette solution, the numerous and diverse tediously long, consumption of operating process be present
When it is laborious the problem of, especially to ocean seawater carry out on-site measurement when, large-scale robot should not be used aboard ship, cumbersome
Operation can not adapt to the site environment on ship.
The content of the invention
According to above-mentioned weak point, it is an object of the invention to：It is dense to provide nitrogen nutrition salt in a kind of quick detection seawater
The method of degree, the method operate very simple, quick.
To achieve the above object, technical program of the present invention lies in：Nitrogen nutrition salinity in a kind of quick detection seawater
Method, comprise the following steps：
Step 1, the collection and pretreatment of seawater sample：The seawater sample in marine site to be measured is gathered, divides three parts, a copy of it warp
Directly as nitrite nitrogen testing sample after membrane filtration, two parts of addition alkaline carbonic acid sodium solutions, mix, stand, wadding in addition
Retrogradation is formed sediment, and is removed and is precipitated through membrane filtration, is added hydrochloric acid solution and is adjusted pH to neutrality, respectively as nitrate nitrogen and ammonia nitrogen
Testing sample；
Step 2, nitrite nitrogen concentration mensuration：9mL nitrous is added in the colorimetric bottle B1 for adding 1mL developers C1 in advance
Hydrochlorate nitrogen testing sample, mix, stand, colorimetric bottle B1 is put into colorimetric bottle groove, make to join to add 10mL water in colorimetric bottle
Than the absorbance A of measure nitrite nitrogen testing sample under (540 ± 3) nm wavelengthw1；Above-mentioned nitrous acid is replaced with 9mL water
Salt nitrogen testing sample, analysis margin absorbance A is determined by nitrite nitrogen same stepsb1；By Aw1Subtract Ab1Obtained value is led to
Peroxynitrite nitrogen standard working curve or corresponding linear regression equation obtain the concentration of the nitrite nitrogen in testing sample；
Step 3, nitrate nitrogen concentration mensuration：1mL reducing agent R1 and 1mL alkaline solutions A1 colorimetric bottle B2 is being added in advance
Middle addition 7mL nitrate nitrogen testing samples, take out after (40 ± 2) DEG C constant temperature (60 ± 5) min is put into insulating box after mixing, stand
It is placed in frozen water and cools down, then add 1mL developer C2, mixes, stands, colorimetric bottle B2 is put into colorimetric bottle groove, with
10mL water is added in colorimetric bottle and makees reference, the absorbance A of nitrate nitrogen testing sample is determined under (540 ± 3) nm wavelengthw2,
Above-mentioned nitrate nitrogen testing sample is replaced with 7mL water, analysis margin absorbance A is determined by nitrate nitrogen same stepsb2；By
Aw2Subtract Ab2Obtained value obtains including nitrite by the standard working curve or corresponding linear regression equation of nitrate nitrogen
The nitrate nitrogen concentration of nitrogen, the nitrate nitrogen concentration comprising nitrite nitrogen is subtracted to the nitrite nitrogen that is measured in step 2
Concentration, obtain the nitrate nitrogen concentration in testing sample；
Step 4, ammonia nitrogen concentration determines：1mL oxidants R2 and 1mL alkaline solution A2 and the colorimetric bottle mixed are being added in advance
7mL ammonia nitrogen testing samples are added in B3, mixes, stand (15 ± 5) min, add 1mL developer C3, then mixes, stand, will
Colorimetric bottle B3 is put into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, ammonia is determined under (540 ± 3) nm wavelength
The absorbance A of nitrogen testing samplew3, above-mentioned ammonia nitrogen testing sample is replaced without ammonia seawater with 7mL, by ammonia nitrogen same steps measure point
Analyse Blank absorbance values Ab3；By Aw3Subtract Ab3The standard working curve or corresponding linear regression equation that obtained value passes through ammonia nitrogen
The ammonia nitrogen concentration for including nitrite nitrogen is obtained, the ammonia nitrogen concentration for including nitrite nitrogen is subtracted what is measured in step 2
The concentration of nitrite nitrogen, obtain ammonia nitrogen concentration in testing sample.
Preferably：Developer C1 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, dense salt
Acid, sulfanilamide (SN), the concentration of hydrochloride naphthodiamide are respectively (2.0 ± 1.2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
Preferably：Reducing agent R1 is formed by hydrazine sulfate, copper sulphate, zinc sulfate and water mixed preparing, wherein, hydrazine sulfate,
Copper sulphate, sulfuric acid zinc concentration are respectively (0.36 ± 0.04) g/L, (0.22 ± 0.04) g/L, (0.22 ± 0.08) g/L.
Preferably：Developer C2 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, dense salt
Acid, sulfanilamide (SN), the concentration of hydrochloride naphthodiamide are respectively (8 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
Preferably：Oxidant R2 is formed by potassium bromate, KBr, concentrated hydrochloric acid and water mixed preparing, wherein, potassium bromate,
KBr, the concentration of concentrated hydrochloric acid are respectively (0.25 ± 0.07) g/L, (0.36 ± 0.07) g/L, (1.8 ± 0.2) % (V/V).
Preferably：Developer C3 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, dense salt
Acid, sulfanilamide (SN), the concentration of hydrochloride naphthodiamide are respectively (20 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
Preferably：Artificial seawater, salinity are 28 ‰ -35 ‰.
Preferably：Preparation method without ammonia seawater is：Collection and seawater similar in aqueous ingredient to be measured, use membrane filtration
Afterwards, it is 10 to add sodium carbonate regulation pH, adds boiling and boils to original volume, and it is 7 to add hydrochloric acid solution regulation pH value, then without ammonia sea
In water plus chloroform, mixing are closed to be stored in polyethylene bottle.
Preferably：Alkaline solution A1 is sodium hydroxide solution, wherein, the concentration of sodium hydroxide is (14.4 ± 1.8) g/
L。
Preferably：Alkaline solution A2 is sodium hydroxide solution, wherein, the concentration of sodium hydroxide is (67.5 ± 7.5) g/
L。
The beneficial effects of the present invention are：In the present invention, early stage is attempted concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water
Single Reagent is hybridly prepared into, optimized, hydrochloride naphthodiamide concentration needed for developer is relatively low (＜ 0.1g/L), at this
Mixed preparing developer under part, not only color developing effect is more preferable than conventional method, and obtained Single Reagent is colourless solution,
Under conditions of closed, lucifuge, freezer storage, the color and effect of this Single Reagent can be stablized more than one month.Therefore, originally
Invention realizes the preparation of Single Reagent.
Concentrated hydrochloric acid, sulfanilamide (SN) and hydrochloride naphthodiamide are prepared to obtain Single Reagent so that only need to add in continuous mode
Add a developer to complete process color, hydrochloride naphthodiamide is added compared to sulfanilamide (SN) solution is first added in conventional method
Solution completes process color in two steps, and this method is easy to operate, quick；And Single Reagent is in colourless, the color of developer and
Effect stability, it is ensured that the accuracy of result of the test, while hydrochloride naphthodiamide solution is avoided in traditional assay method because of face
Color gradually deepens and produces error；The present invention determines the concentration of nitrate nitrogen and ammonia nitrogen by minusing, easy to operate, fast；
The present invention is simple to operate, quick, time saving and energy saving, error is small, is especially suitable for the field quick detection of nitrogen nutrition salinity in seawater.
Brief description of the drawings
Fig. 1 is the length scanning figure of Nitrite Nitrogen color development system of the present invention；
Fig. 2 is the standard working curve of Nitrite Nitrogen of the present invention；
Fig. 3 is nitrate nitrogen standard working curve in the present invention；
Fig. 4 is ammonia nitrogen standard working curve in the present invention；
Fig. 5 is the stability test figure for being used to survey the developer C1 of nitrite nitrogen in the present invention；
Fig. 6 is the stability test figure for being used to survey the developer C2 of nitrate nitrogen in the present invention；
Fig. 7 is the stability test figure for being used to survey the developer C3 of ammonia nitrogen in the present invention；
Fig. 8 is the stability test figure for the oxidant R2 for being used for ammonia nitrogen experiment in the present invention.
Embodiment
With reference to specific embodiment, the present invention will be further described.
The present invention relates to a kind of method of nitrogen nutrition salinity in quick detection seawater, comprise the following steps：
Step 1, the collection and pretreatment of seawater sample：The seawater sample in marine site to be measured is gathered, divides three parts, a copy of it warp
Directly as nitrite nitrogen testing sample after membrane filtration, two parts of addition alkaline carbonic acid sodium solutions, mix, stand, wadding in addition
Retrogradation is formed sediment, and is removed and is precipitated through membrane filtration, is added hydrochloric acid solution and is adjusted pH to neutrality, respectively as nitrate nitrogen and ammonia nitrogen
Testing sample；
Wherein, gained testing sample is stored in polyethylene bottle, should be entered on the analysis work rule of testing sample in 3h
OK, carried out as next day need to be delayed to, then should be stored in 4 DEG C of refrigerations in refrigerator as early as possible, to next day analysis, need to such as postpone more than 1 day
Carry out, then need to -20 DEG C of preservations to analyze its snap frozen after thawing immediately；
By alkaline carbonic acid sodium solution by Ca2+、Mg2+Separated with precipitated form from seawater sample, sea can be eliminated
Ca in water sample2+、Mg2+To interference caused by nitrate nitrogen and ammonia nitrogen determination, (nitrate reduction, ammoxidation process are both needed in alkali
Carried out under the conditions of property, Ca in seawater sample2+、Mg2+It can be reacted with alkali and produce floccule or precipitation, nitrate nitrogen and ammonia nitrogen are surveyed
Fixed output quota life interference), then sample pH value is adjusted to neutrality with hydrochloric acid so that testing sample pH is the same as standard series and sample blank basic one
Cause, avoid, because the addition of alkaline carbonic acid sodium causes testing sample pH to change, making measurement result produce error.Wherein, nitrate
The amount of seawater sample can determine according to situation used in nitrogen and the preparation of ammonia nitrogen testing sample, but need to ensure alkaline carbonic acid sodium solution and hydrochloric acid
The addition sum of solution in contrast when, can be neglected.
Step 2, nitrite nitrogen concentration mensuration：9mL nitrous is added in the colorimetric bottle B1 for adding 1mL developers C1 in advance
Hydrochlorate nitrogen testing sample, mix, stand, colorimetric bottle B1 is put into colorimetric bottle groove, make to join to add 10mL water in colorimetric bottle
Than the absorbance A of measure nitrite nitrogen testing sample under (540 ± 3) nm wavelengthw1；Above-mentioned nitrous acid is replaced with 9mL water
Salt nitrogen testing sample, analysis margin absorbance A is determined by nitrite nitrogen same stepsb1；By Aw1Subtract Ab1Obtained value is led to
Peroxynitrite nitrogen standard working curve (preparing standard series using artificial seawater) or corresponding linear regression equation obtain to be measured
The concentration of nitrite nitrogen in sample.
Step 3, nitrate nitrogen concentration mensuration：1mL reducing agent R1 and 1mL alkaline solutions A1 colorimetric bottle B2 is being added in advance
Middle addition 7mL nitrate nitrogen testing samples, take out after (40 ± 2) DEG C constant temperature (60 ± 5) min is put into insulating box after mixing, stand
It is placed in frozen water and cools down, then add 1mL developer C2, mixes, stands, colorimetric bottle B2 is put into colorimetric bottle groove, with
10mL water is added in colorimetric bottle and makees reference, the absorbance A of nitrate nitrogen testing sample is determined under (540 ± 3) nm wavelengthw2,
Above-mentioned nitrate nitrogen testing sample is replaced with 7mL water, analysis margin absorbance A is determined by nitrate nitrogen same stepsb2；By
Aw2Subtract Ab2Obtained value passes through the standard working curve (preparing standard series using artificial seawater) of nitrate nitrogen or corresponding line
Property regression equation obtains including the nitrate nitrogen concentration of nitrite nitrogen, and the nitrate nitrogen concentration comprising nitrite nitrogen is subtracted
The concentration of the nitrite nitrogen measured in step 2, obtain the nitrate nitrogen concentration in testing sample.
Step 4, ammonia nitrogen concentration determines：1mL oxidants R2 and 1mL alkaline solution A2 and the colorimetric bottle mixed are being added in advance
7mL ammonia nitrogen testing samples are added in B3, mixes, stand (15 ± 5) min, add 1mL developer C3, then mixes, stand, will
Colorimetric bottle B3 is put into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, ammonia is determined under (540 ± 3) nm wavelength
The absorbance A of nitrogen testing samplew3, above-mentioned ammonia nitrogen testing sample is replaced without ammonia seawater with 7mL, by ammonia nitrogen same steps measure point
Analyse Blank absorbance values Ab3；By Aw3Subtract Ab3Obtained value (prepares mark by the standard working curve of ammonia nitrogen using artificial seawater
Quasi- series) or corresponding linear regression equation obtain the ammonia nitrogen concentration for including nitrite nitrogen, nitrite nitrogen will be included
Ammonia nitrogen concentration subtracts the concentration of the nitrite nitrogen measured in step 2, obtains ammonia nitrogen concentration in testing sample.
Use without ammonia seawater in ammonia nitrogen concentration continuous mode is most important, because the shadow of ammonia nitrogen determination ammonia in by water
Sound is larger, using without ammonia determination of seawater sample blank, ammonia therein can be avoided to produce error to experimental result.
Wherein, developer C1 is to be formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, dense salt
Acid, sulfanilamide (SN), the concentration of hydrochloride naphthodiamide are respectively (2.0 ± 1.2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
Wherein, the preferable concentration of concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide is respectively 2% (V/V), 4g/L, 0.05g/L.
Reducing agent R1 is formed by hydrazine sulfate, copper sulphate, zinc sulfate and water mixed preparing, wherein, hydrazine sulfate, copper sulphate, sulphur
Sour zinc concentration is respectively (0.36 ± 0.04) g/L, (0.22 ± 0.04) g/L, (0.22 ± 0.08) g/L.Wherein, hydrazine sulfate,
The preferable concentration of copper sulphate, zinc sulfate is respectively 0.36g/L, 0.22g/L, 0.22g/L.
Developer C2 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, concentrated hydrochloric acid, sulfanilamide (SN),
The concentration of hydrochloride naphthodiamide is respectively (8 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.Wherein, concentrated hydrochloric acid,
The preferable concentration of sulfanilamide (SN), hydrochloride naphthodiamide is respectively 8% (V/V), 4g/L, 0.05g/L.
Oxidant R2 is formed by potassium bromate, KBr, concentrated hydrochloric acid and water mixed preparing, wherein, it is potassium bromate, KBr, dense
The concentration of hydrochloric acid is respectively (0.25 ± 0.07) g/L, (0.36 ± 0.07) g/L, (1.8 ± 0.2) % (V/V).Wherein, bromic acid
The preferable concentration of potassium, KBr, concentrated hydrochloric acid is respectively 0.25g/L, 0.36g/L, 1.8% (V/V).
Developer C3 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, wherein, concentrated hydrochloric acid, sulfanilamide (SN),
The concentration of hydrochloride naphthodiamide is respectively (20 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.Wherein, concentrated hydrochloric acid,
The preferable concentration of sulfanilamide (SN), hydrochloride naphthodiamide is respectively 20% (V/V), 4g/L, 0.05g/L.
For developer C1/C2/C3, concentrated hydrochloric acid content is relevant with the acid-base value of system before chromogenic reaction.Because of colour developing
Reaction need to be carried out in acid condition, and nitrate reduction and ammoxidation stage are both needed to carry out in the basic conditions, and therein
Alkali can not react completely, thus the hydrochloric acid in developer C2 and C3 some be used to neutralize above remaining alkali, wherein dense salt
Acid content is higher.Developer C1 is used for nitrous nitrification, and system is neutral, therefore the salt in developer C1 before chromogenic reaction
Acid need to only provide the acid condition needed for chromogenic reaction, and wherein concentrated hydrochloric acid content is relatively low.
Artificial seawater and without ammonia seawater.Wherein, artificial seawater is prepared with sodium chloride and water, and salinity is 28 ‰ -35 ‰.Without ammonia
The preparation method of seawater is：Collection and seawater similar in aqueous ingredient to be measured, after membrane filtration, adding sodium carbonate regulation pH is
10, add boiling and boil to original volume, it is 7 to add hydrochloric acid solution regulation pH value, then adds chloroform in without ammonia seawater, is mixed,
It is closed to be stored in polyethylene bottle.The effect for adding chloroform is to suppress microbial action in water, prevents microbial metabolism from entering
The conversion of row nitrogen, result is set to produce deviation.
Alkaline solution A1 is sodium hydroxide solution, wherein, the concentration of sodium hydroxide is (14.4 ± 1.8) g/L.
Alkaline solution A2 is sodium hydroxide solution, wherein, the concentration of sodium hydroxide is (67.5 ± 7.5) g/L.
In operating process, oxidant, reducing agent and alkaline solution are required to be respectively configured.Because such as ammonia nitrogen
Oxidant R2 is formed by potassium bromate, KBr and hydrochloric acid solution mixed preparing, and three reacts generation bromine water, and bromine water property is stable,
Bromine water and alkaline solution A2 reaction generation sodium hypobromites, ammoxidation can be in the basic conditions nitrite by sodium hypobromite, but
Sodium hypobromite solution property is unstable, and mixed preparing can influence oxidation effectiveness in advance；Reducing agent for example in nitrate nitrogen measure again
R1 is made up of three kinds of sulfate liquors (hydrazine sulfate, copper sulphate, zinc sulfate), although its property is stable, if with alkaline solution A1
Mixing, reduction effect may be influenceed, therefore selection is prepared respectively, is mixed when current.
Embodiment 1
1st, water sample is tested：Seawater sample in the marine site of Qingdao.
2nd, nitrite nitrogen color development system maximum absorption wavelength determines, as a result as shown in figure 1, the wavelength of final choice is
(540 ± 3) nm, every time test select unified wavelength.
3rd, reagent preparation
3.1st, nitrite nitrogen standard stock solution (100mg/L-N)：0.4926g is weighed through 110 DEG C of drying 1h and in dry
Natrium nitrosum (the NaNO cooled down in dry device2, top pure grade) water is dissolved in, 1000mL is settled to, adds 1mL chloroforms (CHCl3,
Analyze pure) be formulated, loaded in brown reagent bottle, freezer storage, at least stable half a year.
3.2nd, nitrite nitrogen standard serial solution (artificial seawater preparation)：Store by 100mg/L-N nitrite nitrogens standard
Standby liquid is so that artificial seawater dilutes step by step and obtains, its Nitrite Nitrogen (NO2 -- N) concentration is respectively 0,0.01,0.02,0.03,
0.04、0.05mg/L。
3.3rd, nitrate nitrogen standard stock solution (100mg/L-N)：0.7215g is weighed through 110 DEG C of drying 1h and in drying
Potassium nitrate (the KNO cooled down in device3, top pure grade) water is dissolved in, 1000mL is settled to, adds 1mL chloroforms (CHCl3, analysis
It is pure) be formulated, loaded in brown reagent bottle, freezer storage, at least stable half a year.
3.4th, nitrate nitrogen standard serial solution (artificial seawater preparation)：By 100mg/L-N nitrate nitrogen Standard Reserving Solutions
So that artificial seawater dilutes step by step and obtains, wherein nitrate nitrogen (NO3 -- N) concentration is respectively 0,0.04,0.08,0.12,0.16,
0.20mg/L。
3.5th, ammonia nitrogen standard stock solution (100mg/L-N)：0.4716g is weighed through 110 DEG C of drying 1h and in drier
The ammonium sulfate ((NH of cooling4)2SO4, top pure grade) water is dissolved in, 1000mL is settled to, adds 1mL chloroforms (CHCl3, analysis
It is pure) be formulated, loaded in brown reagent bottle, freezer storage, at least stable half a year.
3.6th, ammonia nitrogen standard serial solution (artificial seawater preparation)：By 100mg/L-N ammonia nitrogens Standard Reserving Solution to simulate sea
Water dilutes and obtained step by step, wherein ammonia nitrogen (NH4 +- N) concentration is respectively 0,0.01,0.02,0.04,0.06,0.08mg/L.
3.7th, hydrochloride naphthodiamide stock solution：2g/L, by the hydrochloride naphthodiamide (C for weighing certain mass12H14N2·
2HCl, analysis are pure) it is dissolved in water and is formulated, store in lucifuge, refrigerator, can about stablize one month, need to match somebody with somebody again when color is too deep
System.
3.8th, developer C1：By concentrated hydrochloric acid (HCl, analysis are pure), sulfanilamide (SN) (C6H8O2N2S, analysis it is pure), hydrochloride naphthodiamide
(C12H14N22HCl, analysis it is pure) and water mixed preparing form, wherein concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide concentration distinguish
For：2% (V/V), 4g/L, 0.05g/L.When preparing developer C1, prior to adding a certain amount of concentrated hydrochloric acid in water, then weigh a certain amount of
Sulfanilamide (SN) be dissolved in the hydrochloride naphthodiamide stock solution for wherein, then moving into certain volume, finally with water constant volume.Or prior to a small amount of
The sulfanilamide (SN) weighed is added in water, now sulfanilamide (SN) is insoluble in water, and adding concentrated hydrochloric acid is completely dissolved sulfanilamide (SN), finally moves into hydrochloric acid naphthalene
Ethylenediamine stock solution, with water constant volume, also may be used.
3.9th, developer C2：By concentrated hydrochloric acid (HCl, analysis are pure), sulfanilamide (SN) (C6H8O2N2S, analysis it is pure), hydrochloride naphthodiamide
(C12H14N22HCl, analysis it is pure) and water mixed preparing form, wherein concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide concentration distinguish
For：8% (V/V), 4g/L, 0.05g/L.Developer C2 method is prepared with developer C1.
3.10th, developer C3：By concentrated hydrochloric acid (HCl, analysis are pure), sulfanilamide (SN) (C6H8O2N2S, analysis it is pure), hydrochloride naphthodiamide
(C12H14N22HCl, analysis it is pure) and water mixed preparing form, wherein concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide concentration distinguish
For：20% (V/V), 4g/L, 0.05g/L.Developer C3 method is prepared with developer C1.
3.11st, sodium hydroxide stock solution：About 500g/L, it is molten by weighing about 250g sodium hydroxides (NaOH, analysis are pure)
In 700mL or so water, heating is boiled to 500mL or so, after being cooled to room temperature, it is stored in polyethylene bottle, obtains concentration
About 500g/L sodium hydroxide stock solution, this solution need to demarcate.
The demarcation of sodium hydroxide stock solution：First take certain volume sodium hydroxide stock solution to dilute 62.5 times, obtain dense
Degree be about 8g/L sodium hydroxide solution mark, weigh 1g in advance through 105 DEG C dry 2h and in glass desicator constant weight neighbour
Potassium hydrogen phthalate is KHP (KHC8H4O4, standard reagent) and in 250mL conical flasks, 80mL or so water is added, is rocked to molten
Solution.2 drop phenolphthalein indicators (10g/L) are added, are titrated to blush with sodium hydroxide solution to be marked, 30s colour-fast is terminal.
Parallel calibration three times, sodium hydroxide solution volume (unit to be marked used in record：ML), average.Treat sodium hydroxide in standard liquid
Concentration (unit：G/L) calculated by below equation：
It is above-mentioned to treat that standard liquid is to dilute 62.5 times of gained, therefore sodium hydroxide stock solution by matched somebody with somebody sodium hydroxide stock solution
Middle naoh concentration (unit：G/L) it is：
3.12, phenolphthalein indicator：10g/L, by the way that 1g phenolphthalein is dissolved in into about 60mL ethanol (C2H6O, analysis are pure) in, then use
Ethanol constant volume, 100mL phenolphthalein indicators are obtained, can be preserved under lucifuge, normal temperature about 3 months.
3.13rd, alkaline carbonic acid sodium solution：By sodium carbonate (Na2CO3, analysis it is pure), sodium hydroxide stock solution (about 500g/L)
Formed with water mixed preparing, wherein sodium carbonate and naoh concentration are respectively (30 ± 2) g/L and (112 ± 8) g/L.
3.14th, alkaline solution A1：14.4g/L, diluted by pipetting a certain amount of sodium hydroxide stock solution (about 500g/L)
Obtain.
3.15th, alkaline solution A2：67.5g/L, diluted by pipetting a certain amount of sodium hydroxide stock solution (about 500g/L)
Obtain.
3.16th, reducing agent R1：By hydrazine sulfate (N2H2·H2SO4, analysis it is pure), copper sulphate (CuSO4, analysis it is pure), zinc sulfate
(ZnSO4, analysis it is pure) and water mixed preparing form, wherein hydrazine sulfate, copper sulphate, sulfuric acid zinc concentration are respectively：0.36g/L、
0.22g/L、0.22g/L。
3.17th, oxidant R2：By potassium bromate (KBrO3, analysis is pure), KBr (KBr, analysis pure), concentrated hydrochloric acid (HCl, point
Analyse pure) and water mixed preparing form, wherein potassium bromate, KBr, the concentration of concentrated hydrochloric acid are respectively：0.25g/L、0.36g/L、
1.8% (V/V).
3.18th, without ammonia seawater：By collection and seawater similar in aqueous ingredient to be measured, after 0.45 μm of membrane filtration, add
Enter a little natrium carbonicum calcinatum (Na2CO3, analysis is pure) and regulation pH is about 10, and add boiling and boil to original volume, add hydrochloric acid solution and adjust
Save pH value be 7, then every liter without ammonia seawater in plus 1mL chloroforms, mix, it is closed to be stored in polyethylene bottle.
3.19th, hydrochloric acid solution is hydrochloric acid (1+9) solution：Pass through the concentrated hydrochloric acid (HCl, analysis are pure) of 1 part of volume and 9 parts of volumes
Water be mixed to get.
3.20, water：Except otherwise indicated, " water " described in experiment is ultra-pure water, can also be replaced with redistilled water.
Specifically, developer C1, C2, C3 and reducing agent R1 is colourless solution, under conditions of lucifuge, freezer storage
At least one moon can be stablized.The test of color stability is carried out respectively to developer C1, C2, C3, has as a result been shown in 35 days
When, relatively stable, in order to ensure the accuracy of experiment, developer C1, C2, C3 pot-life are 1 month.
Oxidant R2 is yellow bromine aqueous solution, after tested, its can also stablize under the conditions of lucifuge, freezer storage 1 month with
On；Alkaline solution A1, A2 are colourless solution, can be preserved for a long time at normal temperatures.
All of above solution is both needed to closed preservation.
4th, standard working curve is drawn
4.1st, the range of linearity of nitrite nitrogen standard working curve is 0-0.05mg/L, and its drafting follows following steps：
In one group of 6 10mL colorimetric bottle (being separately added into 1mL developer C1 in advance), 9mL nitrite nitrogen standards are separately added into successively
Serial solution, its Nitrite Nitrogen (NO2 -- N) concentration is respectively 0,0.01,0.02,0.03,0.04,0.05mg/L, mix,
After standing 20min, this group of colorimetric bottle is sequentially placed into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, (540
± 3) absorbance is determined under nm wavelength, finally with standard series Nitrite Nitrogen (NO2- N) concentration be abscissa, correction inhale
Luminosity (reagent blank for deducting 0 concentration) is ordinate, draws the standard working curve of nitrite nitrogen, and obtain nitrite
The equation of linear regression of nitrogen.
Nitrite nitrogen standard working curve (0-0.05mg/L) as shown in Figure 2 is：Y=6.1686x-0.0014, R2
=0.9998.
4.2nd, the range of linearity of nitrate nitrogen standard working curve is 0-0.20mg/L, and its drafting follows following steps：In
In one group of 6 colorimetric bottle (being separately added into 1mL reducing agent R1 and 1mL alkaline solutions A1 in advance, it is not necessary to mix), it is separately added into successively
7mL nitrate nitrogen standard serial solutions, wherein nitrate nitrogen (NO3 -- N) concentration is respectively 0,0.04,0.08,0.12,0.16,
0.20mg/L, it is put into after mixing in insulating box and is taken out after 40 DEG C of constant temperature 1h, be immediately placed in frozen water and cool down, taken out after 2min, so
After sequentially add 1mL developer C2, mix, stand 20min, this group of colorimetric bottle is sequentially placed into colorimetric bottle groove, with colorimetric bottle
Middle addition 10mL water makees reference, determines absorbance under (540 ± 3) nm wavelength, finally with nitrate nitrogen in standard series
(NO3- N) concentration is abscissa, the correction absorbance reagent blank of 0 concentration (deduct) is ordinate, draw the mark of nitrate nitrogen
Quasi- working curve, and obtain the equation of linear regression of nitrate nitrogen.
Nitrate nitrogen standard working curve (0-0.20mg/L) as shown in Figure 3 is：Y=4.0364x+0.0102, R2=
0.9966。
4.3rd, the range of linearity of ammonia nitrogen standard working curve is 0-0.08mg/L, and its drafting follows following steps：In one group 6
In individual colorimetric bottle (add 1mL oxidants R2 and 1mL alkaline solution A2 in advance and mix), 7mL ammonia nitrogen standard series is separately added into
Solution, wherein ammonia nitrogen (NH4 +- N) concentration is respectively 0,0.01,0.02,0.04,0.06,0.08mg/L, mix, stand 15min
Afterwards, 1mL developer C3 are sequentially added, then after mixing, standing 20min, this group of colorimetric bottle is sequentially placed into colorimetric bottle groove, with
Add 10mL water in colorimetric bottle to make reference, determine absorbance under (540 ± 3) nm wavelength, finally with ammonia nitrogen in standard series
(NH4 +- N) concentration is abscissa, the correction absorbance reagent blank of 0 concentration (deduct) is ordinate, draw the standard work of ammonia nitrogen
Make curve, and obtain the equation of linear regression of ammonia nitrogen.
Ammonia nitrogen standard working curve (0-0.08mg/L) as shown in Figure 4 is：Y=3.6316x+0.0122, R2=
0.9958。
5th, " three nitrogen " concentration is determined
5.1st, the collection and pretreatment of seawater sample：The seawater sample in marine site to be measured is gathered, divides three parts, a copy of it warp
Directly as nitrite nitrogen testing sample after 0.45 μm of membrane filtration, two parts of every 100mL additions 2mL alkaline carbonic acid sodium are molten in addition
Liquid, is mixed, stands, flocculation sediment, and precipitation is removed through 0.45 μm of membrane filtration, is added a small amount of hydrochloric acid solution and is adjusted pH into
Property, respectively as nitrate nitrogen and the testing sample of ammonia nitrogen；Gained testing sample is stored in polyethylene bottle, point of testing sample
Analysis is operated in 3h and carried out.
5.2nd, nitrite nitrogen concentration mensuration：9mL nitrous acid is added in the colorimetric bottle B1 for adding 1mL developers C1 in advance
Salt nitrogen testing sample, mix, standing 20min-2h, (generally colour developing can reach complete after 20min, and color is steady in 2h
It is fixed, be the efficiency for improving operation, can select to determine its absorbance after standing 20min, as follows) after colorimetric bottle B1 is put
Enter in colorimetric bottle groove, make reference to add 10mL water in colorimetric bottle, it is to be measured that nitrite nitrogen is determined under (540 ± 3) nm wavelength
The absorbance A of samplew1；Above-mentioned nitrite nitrogen testing sample is replaced with 9mL water, by nitrite nitrogen same steps measure point
Analyse Blank absorbance values Ab1；By Aw1Subtract Ab1Obtained value is returned by nitrite nitrogen standard working curve or corresponding linear
Equation obtains the concentration of the nitrite nitrogen in testing sample.
Nitrite nitrogen concentration in the seawater sample in the Qingdao marine site calculated is：3.5μg/L.
5.3rd, nitrate nitrogen concentration mensuration：Adding 1mL reducing agent R1 and 1mL alkaline solution A1's (need not mix) in advance
7mL nitrate nitrogen testing samples are added in colorimetric bottle B2, after (40 ± 2) DEG C constant temperature (60 ± 5) min is put into insulating box after mixing
Take out, be immediately placed in frozen water and cool down, taken out after 1-2min, then add 1mL developer C2, mix, after standing 20min-2h,
Colorimetric bottle B2 is put into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, is determined under (540 ± 3) nm wavelength
The absorbance A of nitrate nitrogenw2, above-mentioned nitrate nitrogen testing sample is replaced with 7mL water, by nitrate nitrogen same steps measure point
Analyse Blank absorbance values Ab2；By Aw2Subtract Ab2Obtained value is returned by the standard working curve or corresponding linear of nitrate nitrogen
Equation obtains including the nitrate nitrogen concentration of nitrite nitrogen, and the nitrate nitrogen concentration comprising nitrite nitrogen is subtracted into step 2
In the concentration of nitrite nitrogen that measures, obtain the nitrate nitrogen concentration in testing sample.
Nitrate nitrogen concentration in the seawater sample in the Qingdao marine site calculated is：25.7μg/L
5.4th, ammonia nitrogen concentration determines：1mL oxidants R2 and 1mL alkaline solution A2 and the colorimetric bottle B3 mixed are being added in advance
Middle addition 7mL ammonia nitrogen testing samples, mix, stand (15 ± 5) min, add 1mL developer C3, then mix, stand 20min-
2h, colorimetric bottle B3 is put into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, surveyed under (540 ± 3) nm wavelength
Determine absorbance Aw3, above-mentioned ammonia nitrogen testing sample is replaced without ammonia seawater with 7mL, analysis margin extinction is determined by ammonia nitrogen same steps
Angle value Ab3；By Aw3Subtract Ab3Obtained value by the standard working curve of ammonia nitrogen (preparing standard series using artificial seawater) or
Corresponding linear regression equation obtains the ammonia nitrogen concentration for including nitrite nitrogen, and the ammonia nitrogen concentration for including nitrite nitrogen is subtracted
The concentration of nitrite nitrogen measured in step 2 is gone, obtains ammonia nitrogen concentration in testing sample.
Ammonia nitrogen concentration in the seawater sample in the Qingdao marine site calculated is：12.8μg/L.
6th, detection limit
A small amount of nitrite nitrogen/nitrate nitrogen/Ammonia nitrogen standard liquid, lower point of the same terms are separately added into artificial seawater
Not Jian Ce 7 concentration values, and calculate standard deviation, obtain nitrite nitrogen/ammonia nitrogen/nitrate nitrogen standard deviation.According to three times
The detection limit of nitrite nitrogen/nitrate nitrogen/ammonia nitrogen is calculated in the method for standard deviation divided by slope of standard curve：
D.L.=3s/k
In formula, s：To the same sample replication standard deviation of at least 7 times,
k：The slope of standard working curve.
It is computed, the detection limit of nitrite nitrogen：S=0.0037, k=6.1686, then D.L. (nitrite nitrogen)=3s/
K=1.8 × 10-3mg/L。
And the D.L. (nitrite nitrogen)=2.9 × 10 that ocean standard law is calculated-3mg/L。
Nitrate nitrogen detection limit：S=0.0032, k=4.0364, then D.L. (nitrate nitrogen)=3s/k=2.4 × 10- 3mg/L。
And the D.L. (nitrate nitrogen) that ocean standard law is calculated：1. Cadmium reduction column, D.L. (nitrate nitrogen) 2.5 ×
10-3mg/L；Zinc Cadmium Reduction, D.L. (nitrate nitrogen)=3.1 × 10-3mg/L。
Ammonia nitrogen detection limit：S=0.0040, k=3.6316, then D.L. (ammonia nitrogen)=3s/k=3.3 × 10-3mg/L。
It should be noted that ammonia nitrogen detection limit provides in the standard law of ocean without this, and no data supplies ginseng in other people articles
Examine.
By the comparison of above-mentioned detection limit, illustrate that the present invention has the advantages of detection limit low (that is, high sensitivity), can use
In NITROGEN IN LOW CONCENTRATION nutritive salt marine site water sample detection, nitrogen nutrition salt (nitrite nitrogen, nitrate nitrogen, the ammonia nitrogen) suitable for seawater
Carry out Site Detection.
Compared with conventional method, method of the invention specifically has the advantage that：
Nitrite nitrogen detects：Method And Principle is identical with ocean standard law, but mixed preparing developer, realizes a step
Colour developing, and developer colourless (reagent blank is low), stabilization time length；Other method detection limit is lower (that is, sensitivity is higher),
On-site measurement available for NITROGEN IN LOW CONCENTRATION nutritive salt marine site water sample.
Nitrate nitrogen detects：Hydrazine sulfate reducing process is applied to the detection of Nitrate Nitrogen in Seawater, avoids traditional cadmium also
The complex operations such as cadmium post preparation in former method, method are simple, quick；Other method detection limit is low (that is, high sensitivity), can be used for
The on-site measurement of NITROGEN IN LOW CONCENTRATION nutritive salt marine site water sample.
Ammonia nitrogen detects：Method And Principle is identical with ocean standard law, but mixed preparing bromine water (property is stable), has simplified one
Individual step；It is then added to without individually preparing hypobromite solutions in reaction vessel, the oxidation of ammonia is carried out directly in colorimetric bottle
Process, it is simple to operate, quick；Other method detection limit is low (that is, high sensitivity), available for NITROGEN IN LOW CONCENTRATION nutritive salt marine site water
The on-site measurement of sample.
It was found from Fig. 5-8, the stability for the developer C1 of the present invention, developer C2, developer C3 and oxidant R2
It is good, it is not necessary to it is now with the current, greatly save the time of on-site measurement.
Claims (10)
1. a kind of method of nitrogen nutrition salinity in quick detection seawater, it is characterised in that：Comprise the following steps：
Step 1, the collection and pretreatment of seawater sample：The seawater sample in marine site to be measured is gathered, divides three parts, a copy of it is through filter membrane
Directly as the testing sample of nitrite nitrogen after filtering, two parts of addition alkaline carbonic acid sodium solutions, mix, stand, flocculation in addition
Precipitation, remove and precipitate through membrane filtration, add hydrochloric acid solution and adjust pH to neutrality, respectively as treating for nitrate nitrogen and ammonia nitrogen
Test sample product；
Step 2, nitrite nitrogen concentration mensuration：9mL nitrite is added in the colorimetric bottle B1 for adding 1mL developers C1 in advance
Nitrogen testing sample, mix, stand, colorimetric bottle B1 is put into colorimetric bottle groove, make reference to add 10mL water in colorimetric bottle,
The absorbance A of nitrite nitrogen testing sample is determined under (540 ± 3) nm wavelengthw1；Above-mentioned nitrite nitrogen is replaced with 9mL water
Testing sample, analysis margin absorbance A is determined by nitrite nitrogen same stepsb1；By Aw1Subtract Ab1Obtained value passes through Asia
Nitrate nitrogen standard working curve or corresponding linear regression equation obtain the concentration of the nitrite nitrogen in testing sample；
Step 3, nitrate nitrogen concentration mensuration：Add in the colorimetric bottle B2 for adding 1mL reducing agent R1 and 1mL alkaline solutions A1 in advance
Enter 7mL nitrate nitrogen testing samples, take out after (40 ± 2) DEG C constant temperature (60 ± 5) min is put into insulating box after mixing, put immediately
Cooled down in frozen water, then add 1mL developer C2, mixed, stand, colorimetric bottle B2 is put into colorimetric bottle groove, with colorimetric
10mL water is added in bottle and makees reference, the absorbance A of nitrate nitrogen testing sample is determined under (540 ± 3) nm wavelengthw2, with 7mL
Water replaces above-mentioned nitrate nitrogen testing sample, and analysis margin absorbance A is determined by nitrate nitrogen same stepsb2；By Aw2Subtract
Ab2Obtained value obtains including the nitre of nitrite nitrogen by the standard working curve or corresponding linear regression equation of nitrate nitrogen
Hydrochlorate nitrogen concentration, the nitrate nitrogen concentration comprising nitrite nitrogen is subtracted to the dense of the nitrite nitrogen that is measured in the step 2
Degree, obtains the nitrate nitrogen concentration in testing sample；
Step 4, ammonia nitrogen concentration determines：In the colorimetric bottle B3 for adding 1mL oxidants R2 and 1mL alkaline solution A2 in advance and mixing
7mL ammonia nitrogen testing samples are added, mixes, stand (15 ± 5) min, add 1mL developer C3, then mixes, stand, this is compared
Color bottle B3 is put into colorimetric bottle groove, makees reference to add 10mL water in colorimetric bottle, ammonia nitrogen is determined under (540 ± 3) nm wavelength and is treated
The absorbance A of test sample productw3, above-mentioned ammonia nitrogen testing sample is replaced without ammonia seawater with 7mL, it is empty to determine analysis by ammonia nitrogen same steps
White absorbance Ab3；By Aw3Subtract Ab3Obtained value is obtained by the standard working curve or corresponding linear regression equation of ammonia nitrogen
Include the ammonia nitrogen concentration of nitrite nitrogen, the ammonia nitrogen concentration for including nitrite nitrogen is subtracted what is measured in the step 2
The concentration of nitrite nitrogen, obtain ammonia nitrogen concentration in testing sample.
2. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described is aobvious
Toner C1 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, the concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide
Concentration be respectively (2.0 ± 1.2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
3. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described goes back
Former agent R1 is formed by hydrazine sulfate, copper sulphate, zinc sulfate and water mixed preparing, the hydrazine sulfate, copper sulphate, sulfuric acid zinc concentration point
Wei not (0.36 ± 0.04) g/L, (0.22 ± 0.04) g/L, (0.22 ± 0.08) g/L.
4. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described is aobvious
Toner C2 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, the concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide
Concentration be respectively (8 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
5. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described oxygen
Agent R2 is formed by potassium bromate, KBr, concentrated hydrochloric acid and water mixed preparing, the potassium bromate, KBr, the concentration point of concentrated hydrochloric acid
Wei not (0.25 ± 0.07) g/L, (0.36 ± 0.07) g/L, (1.8 ± 0.2) % (V/V).
6. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described is aobvious
Toner C3 is formed by concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide and water mixed preparing, the concentrated hydrochloric acid, sulfanilamide (SN), hydrochloride naphthodiamide
Concentration be respectively (20 ± 2) % (V/V), (4 ± 2) g/L, (0.05 ± 0.01) g/L.
7. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described people
Work seawater is 28 ‰ -35 ‰ sodium chloride solution；It is made without ammonia seawater with actual seawater.
8. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described nothing
The preparation method of ammonia seawater is：Collection and seawater similar in aqueous ingredient to be measured, after membrane filtration, add sodium carbonate regulation pH
For 10, add boiling and boil to original volume, it is 7 to add hydrochloric acid solution regulation pH value, then in without ammonia seawater plus chloroform, is mixed
It is even, it is closed to be stored in polyethylene bottle.
9. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described alkali
Property solution A 1 is sodium hydroxide solution, and the concentration of the sodium hydroxide is (14.4 ± 1.8) g/L.
10. the method for nitrogen nutrition salinity in quick detection seawater according to claim 1, it is characterised in that：Described
Alkaline solution A2 is sodium hydroxide solution, and the concentration of the sodium hydroxide is (67.5 ± 7.5) g/L.
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| CN109142249A (en) * | 2018-08-31 | 2019-01-04 | 青岛卓建海洋装备科技有限公司 | A kind of Seawater Nitrate concentration determination method |
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| CN114441519B (en) * | 2022-01-24 | 2024-04-02 | 四川为众检测科技有限公司 | Reagent for semi-quantitatively and rapidly determining iodine content in iodized salt, preparation method and application |
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