CN107247046A - A kind of ammonia nitrogen detection method of low mercury salt - Google Patents
A kind of ammonia nitrogen detection method of low mercury salt Download PDFInfo
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- CN107247046A CN107247046A CN201710377371.5A CN201710377371A CN107247046A CN 107247046 A CN107247046 A CN 107247046A CN 201710377371 A CN201710377371 A CN 201710377371A CN 107247046 A CN107247046 A CN 107247046A
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Abstract
A kind of ammonia nitrogen detection method of low mercury salt belongs to chemical technology field, it is nessler reagent including preparing mercuric chloride-KI-potassium hydroxide solution, potassium sodium tartrate solution is prepared, ammonia nitrogen solution is configured in colorimetric cylinder and obtains ammonia nitrogen standard series and draws the big step of calibration curve four.When the present invention determines ammonia nitrogen in waste water, HgCl is used2Prepare nessler reagent to produce without precipitation, the measurement result degree of accuracy and precision are all higher, can be used for control analysis.Reality of issuing licence is studied by contrast, passes through KI, KOH and HgCl2Potassium sodium tartrate solution detection ammonia nitrogen after the nessler reagent of preparation and optimization, both ensures low levels of mercury, and the fast and convenient detection of energy, and the calibration curve sensitivity made of this method is higher.
Description
Technical field
The invention belongs to chemical technology field, a kind of ammonia nitrogen detection method of low mercury salt is especially related to.
Background technology
Ammonia nitrogen is one of leading indicator of evaluating water quality, and the ammonia nitrogen for determining water and waste water is more often done in water analysis
Project.Generally there are reagent colorimetric method, the hypochlorite colorimetric method of phenol one and electrode method etc. in assay method.Nessler reagent light
Degree method is generally to determine one of standard method of ammonia nitrogen in water and waste water in current environmental monitoring work.
Nessler reagent has two kinds of compound methods:First method utilizes KI, HgI2Prepared with NaOH, second method is utilized
KI, KOH and HgCl2Prepare.Prepare more using first method at present, its method is simple to operate but has precipitation to produce, and needs quiet
Put or just can be used after filtering.And second method does not provide HgCl accurately2Consumption, it is necessary to during according to preparation of reagents
Phenomenon is judged, empirical strong.
Common metal ion has Ca in water body2+、Mg2+、Fe2+、Mn2+Deng if content is higher, easily with OH in nessler reagent-Or
I-Reaction generation precipitation is muddy, influences colorimetric.Thus before nessler reagent is added, sodium potassium tartrate tetrahydrate need to be first added, to shelter
These metal ions, it is as follows that it shelters principle:The alkaline solution of mercuric iodixde and KI and the light red brown colloidal state of ammonia reaction generation
Compound, this color is strongly absorbed in wider wave-length coverage, generally measurement wavelength 410~425n m scopes.The party
Method takes dilution nessler reagent, and reduces article colorimetric cumulative volume and analyzed, and the consumption of mercury is reduced with this, reduces chemistry point
In the basic conditions, ammonia is with nessler reagent reaction generation yellow compound, the absorption maximum of this compound for secondary pollution in analysis
Wavelength is 420nm, can carry out colorimetric estimation.
No matter in which kind of method nessler reagent containing hypertoxic composition, it is improper to reclaim, can severe contamination environment, mercury can pass through
Breathing and skin contact enter human body, and great threat is caused to health, therefore under the premise of guarantee test result is accurate,
Nessler reagent consumption is controlled and reduces as far as possible, it is significant to the health of operator and environmental protection.
The content of the invention
The technical problems to be solved by the invention are：It is traditional for solving to provide a kind of ammonia nitrogen detection method of low mercury salt
Containing the hypertoxic composition such as mercury in nessler reagent, it is improper to reclaim, and meeting severe contamination environment causes the skill of great threat to health
Art problem.
A kind of ammonia nitrogen detection method of low mercury salt, comprises the following steps, and following steps are sequentially carried out,
Step 1: it is nessler reagent to prepare mercuric chloride-KI-potassium hydroxide solution
15.0g potassium hydroxide is weighed, is dissolved in 50ml water, is cooled to room temperature stand-by；
5.0g KIs are weighed, are dissolved in 10ml water, under agitation, by 2.50g mercuric chloride powder point plural number
Add in liquor kalii iodide, until there is micro mercury chloride to precipitate in liquor kalii iodide, two are added dropwise dropwise into the liquor kalii iodide
Mercury chloride saturated solution, is not redissolved until occurring a small amount of vermilion precipitation in liquor kalii iodide, stops being added dropwise, form dichloride
The mixed liquor of mercury and KI；
Under agitation, the potassium hydroxide solution of cooling is added to the mixed liquor of above-mentioned mercuric chloride and KI
In, and add be diluted to 100ml without ammoniacal liquor, in dark place stand 24h, take supernatant be nessler reagent, store in polyethylene bottle, use rubber
Leather plug or polyethylene lid covers are preserved；
Step 2: preparing potassium sodium tartrate solution
Weigh 50.0g sodium potassium tartrate tetrahydrates to be dissolved in 100ml water, (about 20min) is boiled in heating, be cooled to after room temperature plus without ammonia
Water is diluted to 100ml, instills the nessler reagent being made in 5ml steps one, and acquisition mass concentration is 50% potassium sodium tartrate solution；
Step 3: ammonia nitrogen solution is configured in colorimetric cylinder obtains ammonia nitrogen standard series
In 7 50ml colorimetric cylinders, 0ml, 0.5ml, 1.0ml, 3.0ml, 5.0ml, 7.0ml and 10.0ml ammonia are separately added into
Nitrogen concentration is 10 μ g/ml ammonia nitrogen standard working solution, and 7 colorimetric cylinders add water to graticule,
Corresponding ammonia nitrogen mass concentration is respectively 0.00mg/L, 0.2mg/L, 0.6mg/L, 1.00mg/L, 1.40mg/L and
2.00mg/L, obtains ammonia nitrogen standard series；
Step 4: drawing calibration curve
The potassium sodium tartrate solution prepared in 1.0ml step 2 is added into 7 colorimetric cylinders of ammonia nitrogen standard series respectively,
Rock up and down 5~7 times, add the nessler reagent 1.0ml prepared in step one, rock up and down 5~7 times,
10min is placed at room temperature, under wavelength 420nm, 20mm cuvettes are used, reference is made with water, measures absorbance, and with
Absorbance after blank correction is ordinate, using ammonia-nitrogen content as abscissa, draws calibration curve.
2.50g mercuric chloride powder point plural number time adds concretely comprising the following steps in liquor kalii iodide in the step one：
Mercuric chloride powder adds 0.8g first, and dissolution time is 1min, second of addition 0.5g, and dissolution time is
1.5min, third time adds 0.5g, and dissolution time is 3min, the 4th addition 0.3g, and dissolution time is 5min, the 5th addition
0.2g, dissolution time is 5min, the 6th addition 0.1g, and dissolution time is 8min, the 7th addition 0.05g, and dissolution time is
15min, the 8th addition 0.05g, dissolution time is 30min, and mercuric chloride powder is not completely dissolved, and mercuric chloride powder stops adding
Enter.
By above-mentioned design, the present invention can bring following beneficial effect：
When the present invention determines ammonia nitrogen in waste water, HgCl is used2Prepare nessler reagent without precipitation produce, the measurement result degree of accuracy and
Precision is all higher, can be used for control analysis.Research is confirmed by contrast, passes through KI, KOH and HgCl2The Na Shi examinations of preparation
Potassium sodium tartrate solution detection ammonia nitrogen after agent and optimization, both ensures low levels of mercury, and the fast and convenient detection of energy, and use the party
The calibration curve sensitivity that method makes is higher.
Embodiment
Embodiment one,
Sodium potassium tartrate tetrahydrate is prepared using national standard：Weigh 50g sodium potassium tartrate tetrahydrates to be dissolved in 100ml water, heating boils to remove
Ammonia, lets cool to room temperature, adds water and be settled to 100ml.The mass concentration of the sodium potassium tartrate tetrahydrate made is ρ=500g/l.
Nessler reagent is prepared using the method for Standard：Mercuric chloride-KI-potassium hydroxide (HgC12-KI-
KOH) solution：15.0g potassium hydroxide (KOH) is weighed, is dissolved in 50ml water, is cooled to room temperature；5.0g KIs (KI) are weighed, it is molten
In 10ml water, under agitation, by 2.50g mercuric chloride (HgCl2) powder adds in liquor kalii iodide, add first several times
0.8gHgCl2Powder dissolution time is 1min, is completely dissolved, second of 0.5gHgCl2Powder, dissolution time is 1.5min, the 3rd
Secondary addition 0.5gHgCl2Powder dissolution time is 3min, is completely dissolved, then adds 0.3gHgCl2Powder dissolution time is
5min, is completely dissolved, and adds 0.2gHgCl2Powder dissolution time is 5min, is completely dissolved, then adds 0.1gHgCl2Powder
Dissolution time is 8min, is completely dissolved, and then adds 0.05gHgCl2Powder dissolution time is 15min, is completely dissolved, and is added
0.05gHgCl2Powder dissolution time is 30min, HgCl2Powder is not completely dissolved, there is microprecipitation, is thoroughly mixed, and is dripped
Plus mercuric chloride saturated solution, when a small amount of vermilion precipitation occur behind about 3 drop left and right and not being redissolved, stop being added dropwise；In stirring
Under, in the mixed liquor that the potassium hydroxide solution of cooling is slowly added into above-mentioned mercuric chloride and KI, and it is diluted to
100ml, stands 24h in dark place, pours out supernatant, store in polyethylene bottle, with rubber stopper or polyethylene lid covers.
Examined with the nessler reagent of this proportions through many experiments, sensitivity can reach requirement of experiment.In 7 50ml
In colorimetric cylinder, 0ml, 0.5ml, 1.0ml, 3.0ml, 5.0ml, 7.0ml and 10.0ml ammonia nitrogen standard working solution, ammonia are separately added into
Nitrogen standard working solution mass concentration is ρ N=10 μ g/ml, and it adds water to graticule, corresponding to be configured to ammonia-nitrogen content concentration difference
For 0.00mg/L, 0.2mg/L, 0.6mg/L, 1.00mg/L, 1.40mg/L and 2.00mg/L ammonia nitrogen standard series.
The potassium sodium tartrate solution of 1.0ml Standards preparation is separately added into 7 50ml colorimetric cylinders, is shaken up, then is added
Enter the nessler reagent 1.5ml configured by Standard, shake up.Room temperature is placed after 10min, under wavelength 420nm, uses 20mm colorimetrics
Ware, reference is made with water, measures absorbance.Using the absorbance after blank correction as ordinate, with its corresponding ammonia-nitrogen content (mg)
For abscissa, calibration curve L1-L6. is drawn
Embodiment two,
Sodium potassium tartrate tetrahydrate is prepared using Standard：50g sodium potassium tartrate tetrahydrates are weighed to be dissolved in 100ml water, heating boil with
Except deammoniation, let cool to room temperature, add water and be settled to 100ml.The mass concentration of the sodium potassium tartrate tetrahydrate made is ρ=500g/l.
Nessler reagent is prepared, and is prepared using fast method nessler reagent：16g sodium hydroxides are weighed, is dissolved in 50ml water, fills
Divide and be cooled to room temperature.Separately weigh 7g KIs and 10g mercuric iodixdes (HgI2) water is dissolved in, then this solution is noted slowly under agitation
Enter in sodium hydroxide solution, be diluted with water to 100ml, store in polyethylene bottle, close plug is preserved.
In 7 50ml colorimetric cylinders, 0ml, 0.5ml, 1.0ml, 3.0ml, 5.0ml, 7.0ml and 10.0ml ammonia are separately added into
Nitrogen standard working solution, ammonia nitrogen standard working solution mass concentration is ρ N=10 μ g/ml, and it adds water to graticule, corresponding configuration
It is respectively 0.00mg/L, 0.2mg/L, 0.6mg/L, 1.00mg/L, 1.40mg/L and 2.00mg/L ammonia into ammonia-nitrogen content concentration
Nitrogen standard series.
The potassium sodium tartrate solution that 1.0ml national standards are prepared is added, shakes up, adds by KI, mercuric iodixde and hydroxide
The nessler reagent 1.0ml of sodium rapid configuration, shakes up.Place after 10min (room temperature), under wavelength 420nm, use 20mm cuvettes,
Reference is made with water, absorbance is measured.It is horizontal stroke with its corresponding ammonia-nitrogen content (μ g) using the absorbance after blank correction as ordinate
Coordinate, draws calibration curve L9-L14；
Summarized the experience by above-mentioned many experiments：It is to use KI, dichloro in the preparation method of nessler reagent, embodiment one
Change mercury and potassium hydroxide is formulated；It is that mercuric iodixde and potassium hydroxide are directly prepared in embodiment two.Blank assay result shows:
The blank assay value of embodiment two is than one high 1 times or so of embodiment.KI, HgI in embodiment two2The nessler reagent prepared with NaOH
The content of ammonia nitrogen is detected with sodium potassium tartrate tetrahydrate, the method is simple and efficient, is only limitted to the Preliminary detection of Instructing manufacture, data are not advised
Model；
It may thus be appreciated that it is preferred scheme to be formulated nessler reagent with KI, mercuric chloride and potassium hydroxide.This Na Shi
Preparation of reagents meets Standard.
Embodiment three,
Step 1: it is nessler reagent to prepare mercuric chloride-KI-potassium hydroxide solution
15.0g potassium hydroxide is weighed, is dissolved in 50ml water, is cooled to room temperature stand-by；
5.0g KIs are weighed, are dissolved in 10ml water, under agitation, 2.50g mercuric chloride powder is added several times
Enter in liquor kalii iodide, mercuric chloride powder adds 0.8g first, dissolution time is 1min, second of addition 0.5g, during dissolving
Between be 1.5min, third time add 0.5g, dissolution time is 3min, the 4th time addition 0.3g, dissolution time is 5min, the 5th time
0.2g is added, dissolution time is 5min, the 6th addition 0.1g, dissolution time is 8min, the 7th addition 0.05g, during dissolving
Between be 15min, the 8th time addition 0.05g, dissolution time is 30min, and mercuric chloride powder is not completely dissolved, and mercuric chloride powder stops
Only add；Mercuric chloride saturated solution is added dropwise dropwise into the liquor kalii iodide, until occurring in liquor kalii iodide a small amount of bright red
Color precipitation is not redissolved, and is stopped being added dropwise, is formed the mixed liquor of mercuric chloride and KI；
Under agitation, the potassium hydroxide solution of cooling is added to the mixed liquor of above-mentioned mercuric chloride and KI
In, and water of the addition without ammonium ion is diluted to 100ml, and 24h is stood in dark place, it is nessler reagent to take supernatant, stores in poly- second
In alkene bottle, preserved with rubber stopper or polyethylene lid covers；
Step 2: optimization potassium sodium tartrate solution
Weigh 50.0g sodium potassium tartrate tetrahydrates to be dissolved in 100ml water, heating is boiled about 20 minutes, is cooled to after room temperature and is added not
Water containing ammonium ion is diluted to 100ml, instills the nessler reagent being made in 5ml steps one, and acquisition mass concentration is 50% winestone
Sour potassium sodium solution, the step paratartaric acid potassium sodium solution has done further correction, and the potassium sodium tartrate solution after correction can
Ensure masking effect, antijamming capability during detection ammonia-nitrogen content is ensure that to greatest extent；
Step 3: ammonia nitrogen solution is configured in colorimetric cylinder obtains ammonia nitrogen standard series
In 7 50ml colorimetric cylinders, 0ml, 0.5ml, 1.0ml, 3.0ml, 5.0ml, 7.0ml and 10.0ml ammonia are separately added into
Nitrogen concentration is 10 μ g/ml ammonia nitrogen standard working solution, and 7 colorimetric cylinders add water to graticule, and corresponding ammonia nitrogen quality is dense
Degree is respectively 0.00mg/L, 0.2mg/L, 0.6mg/L, 1.00mg/L, 1.40mg/L and 2.00mg/L, obtains ammonia nitrogen standard system
Row；
Step 4: drawing calibration curve
The potassium sodium tartrate solution added respectively into 7 colorimetric cylinders of ammonia nitrogen standard series after 1.0ml present invention optimizations,
Shake up, add the nessler reagent 1.0ml for preferably going out in step one and complying with the national standard requirements, shake up, place at room temperature
10min, under wavelength 420nm, uses 20mm cuvettes, and reference is made with water, measures absorbance, using the absorbance after blank correction as
Ordinate, with its corresponding ammonia-nitrogen content (μ g) for abscissa, draws calibration curve L15-L22.
In embodiment three in ammonia nitrogen in determining waste water, HgCl is used2Prepare nessler reagent to produce without precipitation, measurement result is accurate
Exactness and precision are all higher, can be used for control analysis.Pass through the mercury content to two kinds of nessler reagents of three kinds of embodiments
Make one to compare, prepare 400m lHgCl2Method nessler reagent about needs HgCl282g, being computed the 15m nessler reagent mercury contents is
0.0227g, and prepare 100ml HgI2Method nessler reagent about needs HgI2100g, 15ml the nessler reagent mercury content are 0.0662g,
The latter be the former 25 times of in summary experimental results demonstrate, it is considered to environmental requirement, reduce the detection method of mercury content；KI、
KOH and HgCl2The potassium sodium tartrate solution detection ammonia nitrogen after nessler reagent and optimization is prepared, low levels of mercury is both ensured, and can be fast
Fast easy detection.
Blank absorbency uses HgCl respectively2Method nessler reagent and HgI2Method nessler reagent enters line blank test, 2/d, continuously
Determine 3d, HgCl2Method nessler reagent enters line blank test, 2/d, METHOD FOR CONTINUOUS DETERMINATION 5d, HgCl with the sodium potassium tartrate tetrahydrate after correction2
Method nessler reagent blank absorbency is in 0.012~0.028 fluctuation；HgI2The blank absorbency of method nessler reagent 0.038~
0.045 fluctuation；HgCl2Sodium potassium tartrate tetrahydrate after method nessler reagent and correction measures blank absorbency in 0.006~0.011 ripple
It is dynamic.Therefore HgCl is used2The calibration curve sensitivity made with sodium potassium tartrate tetrahydrate method nessler reagent after correction is higher.
Points for attention：From testing and discussing, Nessler's reagent photometer measure ammonia nitrogen should be noted that and solve 6 kinds and common asks
Topic：(1) it should be noted that main agents character, chooses qualified reagent.(2) the correct preparation of reagent decides method sensitivity, especially
It is noted that understanding nessler reagent preparation principle, correct nessler reagent of grasping prepares main points.(3) reduction blank assay value can improve reality
Precision is tested, to experimental water, reagent blank and filtering filter paper it is noted that checking.
Claims (2)
1. a kind of ammonia nitrogen detection method of low mercury salt, it is characterized in that：Comprise the following steps, and following steps are sequentially carried out,
Step 1: it is nessler reagent to prepare mercuric chloride-KI-potassium hydroxide solution
15.0g potassium hydroxide is weighed, is dissolved in 50ml water, is cooled to room temperature stand-by；
5.0g KIs are weighed, are dissolved in 10ml water, under agitation, 2.50g mercuric chloride powder point plural number time is added
In liquor kalii iodide, until there is micro mercury chloride to precipitate in liquor kalii iodide, dichloride is added dropwise dropwise into the liquor kalii iodide
Mercury saturated solution, is not redissolved until occurring a small amount of vermilion precipitation in liquor kalii iodide, stops being added dropwise, formed mercuric chloride and
The mixed liquor of KI；
Under agitation, the potassium hydroxide solution of cooling is added in the mixed liquor of above-mentioned mercuric chloride and KI, and
Plus 100ml is diluted to without ammoniacal liquor, 24h is stood in dark place, it is nessler reagent to take supernatant, stores in polyethylene bottle, uses rubber stopper
Or polyethylene lid covers are preserved；
Step 2: preparing potassium sodium tartrate solution
Weigh 50.0g sodium potassium tartrate tetrahydrates to be dissolved in 100ml water, heating is boiled 20 minutes, be cooled to after room temperature plus without ammoniacal liquor dilution
To 100ml, the nessler reagent being made in 5ml steps one is instilled, acquisition mass concentration is 50% potassium sodium tartrate solution；
Step 3: ammonia nitrogen solution is configured in colorimetric cylinder obtains ammonia nitrogen standard series
In 7 50ml colorimetric cylinders, 0ml, 0.5ml, 1.0ml, 3.0ml, 5.0ml, 7.0ml and 10.0ml ammonia nitrogen matter are separately added into
The ammonia nitrogen standard working solution that concentration is 10 μ g/ml is measured, 7 colorimetric cylinders add water to graticule,
Corresponding ammonia nitrogen mass concentration is respectively 0.00mg/L, 0.2mg/L, 0.6mg/L, 1.00mg/L, 1.40mg/L and
2.00mg/L, obtains ammonia nitrogen standard series；
Step 4: drawing calibration curve
The potassium sodium tartrate solution prepared in 1.0ml step 2 is added into 7 colorimetric cylinders of ammonia nitrogen standard series respectively, up and down
Rock 5~7 times, add the nessler reagent 1.0ml prepared in step one, rock up and down 5~7 times,
10min is placed at room temperature, under wavelength 420nm, 20mm cuvettes are used, reference is made with water, measures absorbance, and with blank
Absorbance after correction is ordinate, using ammonia-nitrogen content as abscissa, draws calibration curve.
2. a kind of ammonia nitrogen detection method of low mercury salt according to claim 1, it is characterized in that：2.50g in the step one
Mercuric chloride powder point plural number time adds concretely comprising the following steps in liquor kalii iodide：
Mercuric chloride powder adds 0.8g first, and dissolution time is 1min, second of addition 0.5g, and dissolution time is 1.5min,
Third time add 0.5g, dissolution time is 3min, the 4th time addition 0.3g, dissolution time is 5min, the 5th time addition 0.2g, it is molten
The solution time is 5min, the 6th addition 0.1g, and dissolution time is 8min, the 7th addition 0.05g, and dissolution time is 15min, the
Eight addition 0.05g, dissolution time is 30min, and mercuric chloride powder is not completely dissolved, and mercuric chloride powder stops adding.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001196A (en) * | 2018-10-10 | 2018-12-14 | 闫宏涛 | A kind of solid powder detection agent measuring ammonium nitrogen content |
| CN110308103A (en) * | 2019-07-04 | 2019-10-08 | 江苏天宇检测技术有限公司 | A kind of kit and its detection method detecting water body ammonia-nitrogen content |
| CN111912800A (en) * | 2020-08-11 | 2020-11-10 | 深圳市泛邦建设工程咨询有限公司 | Method for detecting low-concentration ammonia nitrogen in drinking water |
| CN112683823A (en) * | 2020-12-17 | 2021-04-20 | 飞鸣科学仪器（武汉）有限公司 | Detection reagent for detecting total nitrogen content in wastewater and preparation method |
| CN113607725A (en) * | 2021-07-30 | 2021-11-05 | 云南铜业股份有限公司西南铜业分公司 | Method for determining ammonia nitrogen content in wastewater |
-
2017
- 2017-05-25 CN CN201710377371.5A patent/CN107247046A/en active Pending
Non-Patent Citations (1)
| Title |
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| No relevant documents disclosed * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109001196A (en) * | 2018-10-10 | 2018-12-14 | 闫宏涛 | A kind of solid powder detection agent measuring ammonium nitrogen content |
| CN110308103A (en) * | 2019-07-04 | 2019-10-08 | 江苏天宇检测技术有限公司 | A kind of kit and its detection method detecting water body ammonia-nitrogen content |
| CN111912800A (en) * | 2020-08-11 | 2020-11-10 | 深圳市泛邦建设工程咨询有限公司 | Method for detecting low-concentration ammonia nitrogen in drinking water |
| CN111912800B (en) * | 2020-08-11 | 2023-07-18 | 深圳市泛邦建设工程咨询有限公司 | Method for detecting low-concentration ammonia nitrogen in drinking water |
| CN112683823A (en) * | 2020-12-17 | 2021-04-20 | 飞鸣科学仪器（武汉）有限公司 | Detection reagent for detecting total nitrogen content in wastewater and preparation method |
| CN113607725A (en) * | 2021-07-30 | 2021-11-05 | 云南铜业股份有限公司西南铜业分公司 | Method for determining ammonia nitrogen content in wastewater |
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Application publication date: 20171013 |