CN106645343A - Device and method for measuring concentration of ammonia nitrogen in water sample - Google Patents
Device and method for measuring concentration of ammonia nitrogen in water sample Download PDFInfo
- Publication number
- CN106645343A CN106645343A CN201611190363.1A CN201611190363A CN106645343A CN 106645343 A CN106645343 A CN 106645343A CN 201611190363 A CN201611190363 A CN 201611190363A CN 106645343 A CN106645343 A CN 106645343A
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- China
- Prior art keywords
- water sample
- holding part
- small beaker
- water
- ammonia
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 112
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 26
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims abstract description 86
- 229910021529 ammonia Inorganic materials 0.000 claims abstract description 41
- 239000003153 chemical reaction reagent Substances 0.000 claims abstract description 30
- 238000005259 measurement Methods 0.000 claims abstract description 15
- 239000007788 liquid Substances 0.000 claims abstract description 13
- 238000006243 chemical reaction Methods 0.000 claims abstract description 10
- 238000001514 detection method Methods 0.000 claims description 14
- 239000003513 alkali Substances 0.000 claims description 10
- 230000008569 process Effects 0.000 claims description 5
- 230000008859 change Effects 0.000 claims description 4
- 230000008676 import Effects 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 239000000463 material Substances 0.000 claims description 3
- 239000004033 plastic Substances 0.000 claims description 3
- 229920003023 plastic Polymers 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 3
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 3
- 239000012498 ultrapure water Substances 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 238000003756 stirring Methods 0.000 claims description 2
- 239000007789 gas Substances 0.000 claims 2
- 230000005611 electricity Effects 0.000 claims 1
- 239000003795 chemical substances by application Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- -1 standard specimen Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 238000005273 aeration Methods 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000002894 chemical waste Substances 0.000 description 1
- 238000004939 coking Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000012895 dilution Substances 0.000 description 1
- 238000010790 dilution Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 239000010842 industrial wastewater Substances 0.000 description 1
- 230000000813 microbial effect Effects 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000010841 municipal wastewater Substances 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000010865 sewage Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/26—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating electrochemical variables; by using electrolysis or electrophoresis
- G01N27/28—Electrolytic cell components
- G01N27/30—Electrodes, e.g. test electrodes; Half-cells
- G01N27/31—Half-cells with permeable membranes, e.g. semi-porous or perm-selective membranes
Landscapes
- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Physics & Mathematics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Electrochemistry (AREA)
- Molecular Biology (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The invention relates to a device and a method for measuring concentration of ammonia nitrogen in a water sample. The device comprises a water bath kettle and measurement components arranged in the water bath kettle, wherein the water bath kettle is a constant-temperature water bath kettle; the measurement components comprise an ammonia-sensitive electrode, a small beaker serving as a reaction container, a support plate, a plane mirror, a support, a reagent accommodating part, a standard sample accommodating part and a water sample accommodating part; the support is located at the bottom of the constant-temperature water bath kettle; the reagent accommodating part, the standard sample accommodating part and the water sample accommodating part are arranged on the support side by side; the ammonia-sensitive electrode is placed in the small beaker, and the small beaker is nested in the support plate and floats on the liquid surface of the constant-temperature water bath kettle; the plane mirror is located on the support below the oblique side of the small beaker. Compared with the prior art, the device and the method are simple, effective and easy to implement; a reagent, a standard sample and the water sample are at the same temperature, and errors caused by temperature difference are avoided; the condition that bubbles are produced and affect the measurement accuracy and stability is prevented.
Description
Technical field
The present invention relates to a kind of apparatus and method for determining pollutant load concentration in water sample, more particularly, to one kind
The apparatus and method for determining ammonia nitrogen concentration in water sample.
Background technology
The source of ammonia nitrogen is mainly the catabolite that itrogenous organic substance in sanitary sewage receives microbial action, some works in water
Industry waste water, such as coking chemical waste water and synthesis ammonia chemical fertilizer factory waste water, and agricultural drain.Ammonia nitrogen concentration is too high, can cause to have
Evil is biological, causes fish dead, determines ammonia nitrogen in water, contributes to evaluating water pollution situation.
Ammonia Gas Sensor Electrode Method is a kind of simple, quick, accurate, detection range width, the method for measuring ammonia nitrogen in water of environmental protection.
For the water sample for having certain turbidity and colourity etc. can be determined directly, strong antijamming capability, without the need for additional compensation, can be used for
The measurement of ammonia nitrogen in the water samples such as surface water, running water, municipal wastewater and industrial wastewater.
Ammonia Gas Sensor Electrode Method accuracy of measurement and the factor of stability is affected mainly to have temperature and bubble.
The measurement of standard specimen and water sample should be in same temperature environment, for 1 DEG C of the temperature deviation meeting of some ammonia gas-sensing electrodes
Cause 2% measure error.
Ammonia gas-sensing electrode can form detection liquid film when water sample is measured at pellicle and liquid knot circle.Due to pellicle
It is hydrophobic, the bubble that the bubble or water sample itself that water sample is brought into is produced is liable to stick to pellicle and ties at boundary with liquid.Such as
Fruit detection liquid film contains bubble, and speed of the ammonia caused in water sample through liquid film is interfered, and affects electrode measurement current potential,
Further affect the degree of accuracy of ammonia nitrogen measurement data and stability in water sample.
The content of the invention
Based on the deficiencies in the prior art, present invention is primarily targeted at providing one kind can ensure that reagent, standard specimen, water sample
The apparatus and method that temperature is consistent, avoid ammonia nitrogen concentration accuracy of measurement and stability in aeration water sample.
In order to achieve the above object, the present invention provide it is a kind of determine water sample in ammonia nitrogen concentration device, including water-bath with
And the measure component being placed in the water-bath, wherein the water-bath is thermostat water bath, the measure component includes ammonia
Gas sensing electrode, the small beaker as reaction vessel, supporting plate, level crossing, support, reagent holding part, standard specimen holding part, water sample are housed
Portion, wherein the support is located at the bottom of thermostat water bath, the reagent holding part, standard specimen holding part, water sample holding part are by simultaneously
Row is placed on support, and the ammonia gas-sensing electrode is placed in small beaker, and small beaker is nested in supporting plate, floats on thermostat water bath
Liquid level on, the level crossing be located at the oblique side-lower of small beaker support on.
Preferably, there is provided the temperature of the thermostat water bath of isoperibol is set as 38 DEG C.
Preferably, reagent, standard specimen, water sample accommodating respectively in the reagent holding part, standard specimen holding part, water sample holding part
It is in 38 DEG C.
Preferably, the volume of the small beaker as reaction vessel being nested in the supporting plate is 25ml.
Preferably, the material of the supporting plate is foamed plastics.
The method that the present invention also provides ammonia nitrogen concentration in a kind of measure water sample, wherein methods described comprises the steps：It is permanent
Temperature/sampling procedure：The small beaker being nested in supporting plate is positioned on the liquid level of thermostat water bath, by reagent holding part, standard specimen
Holding part, water sample holding part are positioned over support, wait thermostat water bath to be heated to 38 DEG C, and constant temperature starts to hold water sample after 5 minutes
The water sample put in portion is imported in small beaker, is then entered ammonia gas-sensing electrode slow oblique cutting in small beaker, makes the half of ammonia gas-sensing electrode
Permeable membrane is completely submerged in water sample；Observation bubble step：In measurement process, the water sample in the water sample holding part imports to little
After beaker, the slow oblique cutting of ammonia gas-sensing electrode is entered in the water sample in small beaker so as to which pellicle is completely submerged in water sample, if
Bubble is observed on the pellicle of ammonia gas-sensing electrode, ammonia gas-sensing electrode is taken out, bubble is rinsed out using wash bottle, continue slow
Pellicle is rinsed, after forming water membrane on pellicle, is again put ammonia gas-sensing electrode in small beaker into；Reaction/detection：
After adhering to without bubble on observation pellicle, the reagent in alkali lye reagent holding part is imported in small beaker, while rotating ammonia
Quick electrode stirring, mixing water sample and alkali lye reagent, after the stable reading of electrode potential, record the potential value of detection.
Preferably, the level crossing is mounted with the support of the oblique side-lower of small beaker, ammonia is observed by level crossing quick
Whether the pellicle of electrode has bubble to produce in detection.
Preferably, if bubble is observed on the pellicle of ammonia gas-sensing electrode by the level crossing, should be quick by ammonia
Electrode is taken out, and with the wash bottle equipped with ultra-pure water bubble is rinsed out.
Preferably, it is rapid to be stirred by the way of rotation ammonia gas-sensing electrode after importing the alkali lye reagent in measurement process
Mix, mix water sample and alkali lye reagent.
Preferably, when the electrode potential reading of the ammonia gas-sensing electrode changes less than 1mV in 40 seconds, it is considered as reading steady
It is fixed, record the potential value of detection.
Compared with prior art, the present invention is simple effectively, it is easy to accomplish；Ensure that reagent, standard specimen, water sample are in same temperature
Degree, it is to avoid the error that the temperature difference is brought；Prevent bubble from producing the degree of accuracy and stability for affecting measurement.
Description of the drawings
Fig. 1 is a kind of structural representation for determining the device of ammonia nitrogen concentration in water sample of the present invention.
Fig. 2 is a kind of schematic flow sheet for determining the method for ammonia nitrogen concentration in water sample of the present invention.
Specific embodiment
The specific embodiment of the present invention is further detailed below in conjunction with accompanying drawing.
As shown in figure 1, a kind of embodiment that the present invention determines the device of ammonia nitrogen concentration in water sample is illustrated therein is, it is described
Device includes thermostat water bath 1, ammonia gas-sensing electrode 2, the small beaker 3 as reaction vessel, supporting plate 4, level crossing 5, support 6, examination
Agent holding part 7, standard specimen holding part 8, water sample holding part 9.Wherein, the support 6 is located at the bottom of thermostat water bath 1, the examination
Agent holding part 7, standard specimen holding part 8, water sample holding part 9 are located on support 6.The ammonia gas-sensing electrode 2 is placed in small beaker 3, little
Beaker 3 is nested in supporting plate 4, is floated on the liquid level of thermostat water bath 1.The level crossing 5 is located at the oblique side-lower of small beaker 3
Support 6 on.Supporting plate 4 provides buoyancy for the liquid level that small beaker 3 floats on thermostat water bath 1.The perseverance of isoperibol is provided
The temperature of warm water bath 1 is set as 38 DEG C, it is ensured that during detection, and the temperature of water sample is 38 DEG C in small beaker.The reagent holding part
7th, reagent accommodating respectively in standard specimen holding part 8, water sample holding part 9, standard specimen, water sample are in 38 DEG C.It is nested in the support
The volume of the small beaker 3 as reaction vessel in plate 4 is 25ml.The material of the supporting plate 4 is foamed plastics.
As shown in Fig. 2 illustrated therein is a kind of embodiment that the present invention determines the method for ammonia nitrogen concentration in water sample.
Constant temperature/sampling：The small beaker 3 being nested in supporting plate 4 is positioned on the liquid level of thermostat water bath 1.Reagent is held
Put portion 7, standard specimen holding part 8, water sample holding part 9 to be positioned on support 6.Thermostat water bath 1 is waited to be heated to 38 DEG C, 5 points of constant temperature
Zhong Hou, starts the water sample in water sample holding part 9 to be imported in small beaker 3.Then, the slow oblique cutting of ammonia gas-sensing electrode 2 is entered into little burning
In cup 3, the pellicle for making ammonia gas-sensing electrode 2 is completely submerged in water sample.
Observation bubble：In measurement process, the water sample in the water sample holding part 9 is imported to after small beaker 3, and ammonia is quick
The slow oblique cutting of electrode 2 enters in the water sample in small beaker 3 so as to which pellicle is completely submerged in water sample.
If by the level crossing 5, bubble is observed on the pellicle of ammonia gas-sensing electrode 2, should be by ammonia gas-sensing electrode 2
Take out, with the wash bottle equipped with ultra-pure water bubble is rinsed out.Continue slow flushing pellicle, water membrane is formed on pellicle
Afterwards, ammonia gas-sensing electrode 2 is put into again the appearance that bubble can be avoided in small beaker 3.The volume of micro moisture film is compared to concrete water quality
Can with or slightly, be not result in the dilution of water sample.
Reaction/detection：After the level crossing 5 is observed and adhered to without bubble on pellicle, by alkali lye reagent holding part 7
In reagent import small beaker 3 in.Meanwhile, it is rapid to be stirred by the way of rotation ammonia gas-sensing electrode 2, mix water sample and alkali lye examination
Agent.Avoiding may produce the problem that heat causes solution temperature to change using electromagnetic agitation.In the stable reading of electrode potential
After (change in 40 seconds is less than 1mV), the potential value of detection is recorded.
Above specific embodiment has been described in detail to the present invention, but these not constitute the limit to the present invention
System.Protection scope of the present invention is not limited with above-mentioned embodiment, as long as those of ordinary skill in the art are according to institute of the present invention
Equivalent modification or change that disclosure is made, all should include in the protection domain described in claims.
Claims (10)
1. a kind of device for determining ammonia nitrogen concentration in water sample, including water-bath and the measure group being placed in the water-bath
Part, it is characterised in that：The water-bath is thermostat water bath, and the measure component is including ammonia gas-sensing electrode, as reaction vessel
Small beaker, supporting plate, level crossing, support, reagent holding part, standard specimen holding part, water sample holding part, wherein the support be located at perseverance
The bottom of warm water bath, the reagent holding part, standard specimen holding part, water sample holding part are disposed side by side on support, the ammonia
Gas sensing electrode is placed in small beaker, and small beaker is nested in supporting plate, is floated on the liquid level of thermostat water bath, the level crossing position
On the support of the oblique side-lower of small beaker.
2. it is according to claim 1 it is a kind of determine water sample in ammonia nitrogen concentration device, it is characterised in that：Isoperibol is provided
The temperature of the thermostat water bath be set as 38 DEG C.
3. it is according to claim 1 it is a kind of determine water sample in ammonia nitrogen concentration device, it is characterised in that：The reagent is housed
Portion, standard specimen holding part, the interior reagent accommodating respectively of water sample holding part, standard specimen, water sample are in 38 DEG C.
4. it is according to claim 1 it is a kind of determine water sample in ammonia nitrogen concentration device, it is characterised in that：It is nested in described
The volume of the small beaker as reaction vessel in supporting plate is 25ml.
5. it is according to claim 1 it is a kind of determine water sample in ammonia nitrogen concentration device, it is characterised in that：The material of the supporting plate
Expect for foamed plastics.
6. it is a kind of determine water sample in ammonia nitrogen concentration method, it is characterised in that methods described comprises the steps：Constant temperature/sampling
Step：The small beaker being nested in supporting plate is positioned on the liquid level of thermostat water bath, by reagent holding part, standard specimen holding part,
Water sample holding part is positioned over support, waits thermostat water bath to be heated to 38 DEG C, and constant temperature starts in water sample holding part after 5 minutes
Water sample import small beaker in, then the slow oblique cutting of ammonia gas-sensing electrode is entered in small beaker, make the pellicle of ammonia gas-sensing electrode complete
It is immersed in entirely in water sample；Observation bubble step：In measurement process, the water sample in the water sample holding part imports to small beaker
Afterwards, the slow oblique cutting of ammonia gas-sensing electrode is entered in the water sample in small beaker so as to which pellicle is completely submerged in water sample, if in ammonia
Bubble is observed on the pellicle of gas sensing electrode, ammonia gas-sensing electrode is taken out, bubble is rinsed out using wash bottle, continue slow flushing
Pellicle, after forming water membrane on pellicle, again puts ammonia gas-sensing electrode in small beaker into；Reaction/detection：In observation
After adhering to without bubble on pellicle, the reagent in alkali lye reagent holding part is imported in small beaker, while rotating the quick electricity of ammonia
Pole stirring, mixing water sample and alkali lye reagent, after the stable reading of electrode potential, record the potential value of detection.
7. it is according to claim 6 it is a kind of determine water sample in ammonia nitrogen concentration method, it is characterised in that：In the oblique side of small beaker
The level crossing is mounted with the support of lower section, whether the pellicle for observing ammonia gas-sensing electrode by level crossing has gas in detection
Bubble is produced.
8. it is according to claim 6 it is a kind of determine water sample in ammonia nitrogen concentration method, it is characterised in that：If by described
Level crossing observes bubble on the pellicle of ammonia gas-sensing electrode, should take out ammonia gas-sensing electrode, with the wash bottle equipped with ultra-pure water
Rinse out bubble.
9. it is according to claim 6 it is a kind of determine water sample in ammonia nitrogen concentration method, it is characterised in that：In measurement process
In, it is rapid to be stirred by the way of rotation ammonia gas-sensing electrode after importing the alkali lye reagent, mix water sample and alkali lye reagent.
10. it is according to claim 6 it is a kind of determine water sample in ammonia nitrogen concentration method, it is characterised in that：The ammonia is quick
When change is less than 1mV in the electrode potential reading 40 seconds of electrode, it is considered as stable reading, records the potential value of detection.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190363.1A CN106645343A (en) | 2016-12-21 | 2016-12-21 | Device and method for measuring concentration of ammonia nitrogen in water sample |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611190363.1A CN106645343A (en) | 2016-12-21 | 2016-12-21 | Device and method for measuring concentration of ammonia nitrogen in water sample |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN106645343A true CN106645343A (en) | 2017-05-10 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201611190363.1A Pending CN106645343A (en) | 2016-12-21 | 2016-12-21 | Device and method for measuring concentration of ammonia nitrogen in water sample |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106645343A (en) |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1267246A1 (en) * | 1985-03-20 | 1986-10-30 | Белорусский Ордена Трудового Красного Знамени Научно-Исследовательский Институт Почвоведения И Агрохимии | Method of potentiometric determining of nitrogen of grain mineralizates |
| CN201740756U (en) * | 2010-03-08 | 2011-02-09 | 华北电力科学研究院有限责任公司 | On-line ammonia nitrogen monitoring system |
| CN102834964A (en) * | 2010-02-10 | 2012-12-19 | 迪奥尼克斯公司 | Electrochemical detection cell for liquid chromatography system |
| CN203941133U (en) * | 2014-07-02 | 2014-11-12 | 华北电力科学研究院有限责任公司 | Ammonia content on-line monitoring system in a kind of boiler water of electric power plant |
| CN204044165U (en) * | 2014-06-25 | 2014-12-24 | 施小龙 | A kind of electrode method flow injection ammonia nitrogen water quality automatic analyzer |
-
2016
- 2016-12-21 CN CN201611190363.1A patent/CN106645343A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1267246A1 (en) * | 1985-03-20 | 1986-10-30 | Белорусский Ордена Трудового Красного Знамени Научно-Исследовательский Институт Почвоведения И Агрохимии | Method of potentiometric determining of nitrogen of grain mineralizates |
| CN102834964A (en) * | 2010-02-10 | 2012-12-19 | 迪奥尼克斯公司 | Electrochemical detection cell for liquid chromatography system |
| CN201740756U (en) * | 2010-03-08 | 2011-02-09 | 华北电力科学研究院有限责任公司 | On-line ammonia nitrogen monitoring system |
| CN204044165U (en) * | 2014-06-25 | 2014-12-24 | 施小龙 | A kind of electrode method flow injection ammonia nitrogen water quality automatic analyzer |
| CN203941133U (en) * | 2014-07-02 | 2014-11-12 | 华北电力科学研究院有限责任公司 | Ammonia content on-line monitoring system in a kind of boiler water of electric power plant |
Non-Patent Citations (1)
| Title |
|---|
| 黄伟星 等: "氨离子选择性电极法测定污水中的氨氮含量", 《同济大学学报》 * |
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Application publication date: 20170510 |