CN108918442A - A kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method - Google Patents
A kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method Download PDFInfo
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- CN108918442A CN108918442A CN201810768953.0A CN201810768953A CN108918442A CN 108918442 A CN108918442 A CN 108918442A CN 201810768953 A CN201810768953 A CN 201810768953A CN 108918442 A CN108918442 A CN 108918442A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
Abstract
The invention belongs to spectrophotometric method technical fields, and in particular to a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method.The problem of in the prior art, when testing phosphorus content using ammonium molybdate spectrophotometric method, the element silicon in water sample will form silica, influence the accuracy of test, the technical scheme is that：Include the following steps, [1] clears up water sample, obtains digestion solution；[2] ascorbic acid, antimonic salt and ammonium molybdate are added into digestion solution, obtains blue complex solution；[3] blue complex solution is tested by spectrophotometry, obtains the phosphorus content in water sample；Between step [1] and step [2], also digestion solution is handled as follows：[1-1] quantitatively pipettes digestion solution, and adjusting pH is 3-5, and MgO is added into digestion solution, is stirred to react；After the completion of [1-2] is stirred to react, the pH of digestion solution is adjusted to 1-3 and constant volume；After [1-3] stands the digestion solution after constant volume, precipitating is filtered to remove with supermicro filtration membrane.The present invention is suitable for water quality detection.
Description
Technical field
The invention belongs to spectrophotometric method technical fields, and in particular in a kind of Water by Ammonium molybdate Spectrophotometer method
Total phosphorus method.
Background technique
Ammonium molybdate spectrophotometric method is a kind of method for total phosphorus content in analysis water-like.In the prior art, ammonium molybdate
Spectrophotometry mainly includes the following steps：Make sample digestion with potassium peroxydisulfate (or nitric acid-perchloric acid) in neutral conditions, it will
The phosphorous whole of institute is oxidized to orthophosphates.In acid medium, orthophosphates and ammonium molybdate reaction generate phosphorus in the presence of antimonic salt
It after molybdenum heteropolyacid, is restored immediately by ascorbic acid, generates blue complex solution.Then it is complexed with spectrophotometry blue
The content of P elements in object solution.
But since in above-mentioned treatment process, the element silicon in water sample will form silica, silica and antimonic salt
Also it will form blue complex, cause in spectrophotomelric assay, the measurement of phosphorus element content generates error, influences the standard of result
True property.
Summary of the invention
For in the prior art, when testing phosphorus content using ammonium molybdate spectrophotometric method, the element silicon in water sample be will form
Silica, influence test accuracy the problem of, the present invention provides a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry side
Method, its object is to：Eliminate influence of the element silicon to the accuracy of ammonium molybdate spectrophotometric method test phosphorus in water sample.
The technical solution adopted by the present invention is as follows：
A kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method, includes the following steps,
[1] water sample is cleared up using potassium peroxydisulfate or nitric acid-perchloric acid, obtains digestion solution；
[2] ascorbic acid, antimonic salt and ammonium molybdate are added in the digestion solution obtained to step [1], it is molten to obtain blue complexing
Liquid；
[3] the blue complex solution obtained by spectrophotometry testing procedure [2], obtains the phosphorus content in water sample；
Between step [1] and step [2], also digestion solution is handled as follows：
[1-1] quantitatively pipettes digestion solution, and the pH for adjusting the digestion solution pipetted is 3-5, is added into digestion solution
MgO is stirred to react；
After the completion of [1-2] is stirred to react, the pH of digestion solution is adjusted to 1-3 and constant volume；
After [1-3] stands the digestion solution after constant volume, precipitating is filtered to remove with supermicro filtration membrane.
After the technical solution, silicic acid magnesium precipitate is formed first with the silicate ion in MgO and solution, is then used
Supermicro filtration membrane filters off precipitating, to realize the purpose of the silicon removal in digestion solution.In the treatment process of digestion solution,
The volume and pH of strict control solution avoid the detection that P elements are influenced on the treatment process of digestion solution.Using the technical side
Case can be improved the detection accuracy of ammonium molybdate spectrophotometric method.
Preferably, in step [1-1] and step [1-2], adjusting acid used in the pH of digestion solution is sulfuric acid, nitric acid, salt
Acid or perchloric acid.
Preferably, in step [1-1] and step [1-2], adjusting alkali used in the pH of digestion solution is sodium hydroxide or hydrogen
Potassium oxide.
The anion and cation that the bronsted lowry acids and bases bronsted lowry selected in above-mentioned preferred embodiment uses reaction system Central Plains originally to contain, keep away
Exempt to introduce new ion pair detection to have an impact.
Preferably, in step [1-1], after MgO is added, the time to digestion solution stirring is 10-30min.The time model
Enclosing can guarantee that reaction occurs completely.
Preferably, it is measured in the treatment process to digestion solution and the resolution quantitatively pipetted in recording step [1-1] is molten
The volume V of liquid1, in step [1-2] by the volume V after digestion solution constant volume2After filter operation with progress step [1-3]
The volume V of the filtered digestion solution arrived3.In order to guarantee the reliability of testing result, constant volume before filtration is needed, and filtering
After measure volume, deduct P elements caused by liquor capacity during filtering etc. loses and be lost, thus in subsequent detection process
In obtain accurate result.
It is further preferred that in the filtered digestion solution that step [1-3] obtains P elements content m2With step [1-
1] the content m of P elements in the digestion solution quantitatively pipetted in1Ratio be m2/m1=V3/V2。
It is handled it is further preferred that quantitatively pipetting 25ml digestion solution in step [1-1], it will in step [1-2]
Digestion solution constant volume is 50ml or 100ml, after measuring after the filter operation for carrying out step [1-3] and recording the filtering that is collected into
Digestion solution volume.The liquor capacity that this preferred embodiment is selected facilitates operation and can guarantee the accuracy of measurement result.
Preferably, the time of repose in step [1-3] is 30-60min.The time range can guarantee shape in digestion solution
At magnesium silicate be sufficiently precipitated out.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows：
1. forming silicic acid magnesium precipitate first with the silicate ion in MgO and solution, it is heavy then to be filtered off with supermicro filtration membrane
It forms sediment, to realize the purpose of the silicon removal in digestion solution.In the treatment process of digestion solution, strict control solution
Volume and pH avoid the detection that P elements are influenced on the treatment process of digestion solution.Molybdic acid can be improved using the technical solution
The detection accuracy of ammonium spectrophotometry.
2. anion and cation that the bronsted lowry acids and bases bronsted lowry for adjusting pH uses reaction system Central Plains originally to contain avoid introducing newly
Ion pair detection has an impact.
3. needing constant volume before filtration, and measure volume after filtration to guarantee the reliability of testing result, filtering is deducted
P elements caused by liquor capacity loses Deng during are lost, to obtain accurate result in subsequent detection process.
Specific embodiment
All features disclosed in this specification or disclosed all methods or in the process the step of, in addition to mutually exclusive
Feature and/or step other than, can combine in any way.
A kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method, includes the following steps,
[1] water sample is cleared up using potassium peroxydisulfate or nitric acid-perchloric acid, obtains digestion solution；
[2] ascorbic acid, antimonic salt and ammonium molybdate are added in the digestion solution obtained to step [1], it is molten to obtain blue complexing
Liquid；
[3] the blue complex solution obtained by spectrophotometry testing procedure [2], obtains the phosphorus content in water sample；
Between step [1] and step [2], also digestion solution is handled as follows：
[1-1] quantitatively pipettes digestion solution, and the pH for adjusting the digestion solution pipetted is 3-5, is added into digestion solution
MgO is stirred to react；
After the completion of [1-2] is stirred to react, the pH of digestion solution is adjusted to 1-3 and constant volume；
After [1-3] stands the digestion solution after constant volume, precipitating is filtered to remove with supermicro filtration membrane.
Preferably, in step [1-1] and step [1-2], adjusting acid used in the pH of digestion solution is sulfuric acid, nitric acid, salt
Acid or perchloric acid.
Preferably, in step [1-1] and step [1-2], adjusting alkali used in the pH of digestion solution is sodium hydroxide or hydrogen
Potassium oxide.
Preferably, in step [1-1], after MgO is added, the time to digestion solution stirring is 10-30min.
Preferably, it is measured in the treatment process to digestion solution and the resolution quantitatively pipetted in recording step [1-1] is molten
The volume V of liquid1, in step [1-2] by the volume V after digestion solution constant volume2After filter operation with progress step [1-3]
The volume V of the filtered digestion solution arrived3。
It is further preferred that in the filtered digestion solution that step [1-3] obtains P elements content m2With step [1-
1] the content m of P elements in the digestion solution quantitatively pipetted in1Ratio be m2/m1=V3/V2。
It is handled it is further preferred that quantitatively pipetting 25ml digestion solution in step [1-1], it will in step [1-2]
Digestion solution constant volume is 50ml or 100ml, after measuring after the filter operation for carrying out step [1-3] and recording the filtering that is collected into
Digestion solution volume.
Preferably, the time of repose in step [1-3] is 30-60min.
Below by specific detection embodiment, further description of the technical solution of the present invention.
Embodiment 1
In the present embodiment, step [1], step [2] and step [3] are according to national standard GB 11893-89《Total phosphorus yield-molybdenum
Sour ammonium spectrophotometry》In regulation operated.
Between step [1] and step [2], unspecified treatment process in GB 11893-89 additionally joined, specifically such as
Under：After the resolution of pernitric acid-perchloric acid, digestion solution is diluted to 25ml, and 25ml digestion solution is completely used for connecing down
In the processing come.Resolution is fitted into conical flask, the pH of solution is adjusted to 3-5 with perchloric acid and sodium hydroxide, at this time solution
Volume should be within the scope of 27-32m l.Then will 0.01g MgO be added solution in, be stirred to react (stirring can also with ultrasound shake
Swing replacement), reaction time 30min.Then by the solution perchloric acid and sodium hydroxide adjusting pH to 1-3 after reaction, at this point,
The volume of digestion solution should be within the scope of 32-37ml.Digestion solution is settled to 50ml and stands 30min.It finally will resolution
Solution is filtered with supermicro filtration membrane.After the filtrate being obtained by filtration carries out stereometry, continue to carry out step according to GB 11893-89
[2] and the continuous mode of step [3].
Using the method for the present embodiment, the standard water sample that the phosphorus content to preparation is 0.510mg/L is measured, is surveyed
Determining result phosphorus content is 0.504mg/L.The method according to as defined in GB 11893-89 is measured completely, obtains measurement result phosphorus
Content is 0.506mg/L.
Using the method for the present embodiment, the standard that the phosphorus content to preparation is 0.510mg/L, silicone content is 0.120mg/L
Water sample is measured, and obtaining measurement result phosphorus content is 0.512mg/L, which substantially eliminates the influence of silicon.Completely
Be measured according to method as defined in GB 11893-89, obtain measurement result phosphorus content be 0.598mg/L, the result obviously by
The influence of silicone content is arrived.
Embodiment 2
The treatment process of the present embodiment is substantially the same manner as Example 1, and difference is that the resolution of water sample using potassium peroxydisulfate, disappears
Solving the reaction time after MgO is added in solution is 10min, and the time of repose after the completion of constant volume is 60min.
Using the method for the present embodiment, the standard water sample that the phosphorus content to preparation is 0.510mg/L is measured, is surveyed
Determining result phosphorus content is 0.508mg/L.The method according to as defined in GB 11893-89 is measured completely, obtains measurement result phosphorus
Content is 0.507mg/L.
Using the method for the present embodiment, the standard that the phosphorus content to preparation is 0.510mg/L, silicone content is 0.120mg/L
Water sample is measured, and obtaining measurement result phosphorus content is 0.514mg/L, which substantially eliminates the influence of silicon.Completely
Be measured according to method as defined in GB 11893-89, obtain measurement result phosphorus content be 0.607mg/L, the result obviously by
The influence of silicone content is arrived.
According to the verifying of embodiment 1 and embodiment 2, illustrate that method of the invention can actually not influence phosphorus detection
Under the premise of, eliminate influence of the element silicon to phosphorus detection.
The specific embodiment of the application above described embodiment only expresses, the description thereof is more specific and detailed, but simultaneously
The limitation to the application protection scope therefore cannot be interpreted as.It should be pointed out that for those of ordinary skill in the art
For, under the premise of not departing from technical scheme design, various modifications and improvements can be made, these belong to this
The protection scope of application.
Claims (8)
1. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method, includes the following steps,
[1] water sample is cleared up using potassium peroxydisulfate or nitric acid-perchloric acid, obtains digestion solution；
[2] ascorbic acid, antimonic salt and ammonium molybdate are added in the digestion solution obtained to step [1], obtains blue complex solution；
[3] the blue complex solution obtained by spectrophotometry testing procedure [2], obtains the phosphorus content in water sample；
It is characterized in that,
Between step [1] and step [2], also digestion solution is handled as follows：
[1-1] quantitatively pipettes digestion solution, and the pH for adjusting the digestion solution pipetted is 3-5, and MgO is added into digestion solution, stirs
Mix reaction；
After the completion of [1-2] is stirred to react, the pH of digestion solution is adjusted to 1-3 and constant volume；
After [1-3] stands the digestion solution after constant volume, precipitating is filtered to remove with supermicro filtration membrane.
2. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method described in accordance with the claim 1, it is characterised in that：Step
In [1-1] and step [1-2], adjusting acid used in the pH of digestion solution is sulfuric acid, nitric acid, hydrochloric acid or perchloric acid.
3. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method described in accordance with the claim 1, it is characterised in that：Step
In [1-1] and step [1-2], adjusting alkali used in the pH of digestion solution is sodium hydroxide or potassium hydroxide.
4. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method described in accordance with the claim 1, it is characterised in that：Step
In [1-1], after MgO is added, the time to digestion solution stirring is 10-30min.
5. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method described in accordance with the claim 1, it is characterised in that：Right
The volume V of digestion solution for measuring in the treatment process of digestion solution and quantitatively being pipetted in recording step [1-1]1, in step [1-
2] by the volume V after digestion solution constant volume in2The filtered digestion solution obtained after filter operation with progress step [1-3]
Volume V3。
6. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method according to claim 5, it is characterised in that：Step
The content m of P elements in the filtered digestion solution that [1-3] is obtained2With in the digestion solution that is quantitatively pipetted in step [1-1]
The content m of P elements1Ratio be m2/m1=V3/V2。
7. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method according to claim 5, it is characterised in that：Step
25ml digestion solution is quantitatively pipetted in [1-1] to be handled, in step [1-2] by digestion solution constant volume be 50ml or 100ml,
The volume for the filtered digestion solution being collected into is measured and recorded after the filter operation for carrying out step [1-3].
8. a kind of Judgment of Determination of Total Phosphorus In Water With Ammonium Molybdate Spectrophotometry method described in accordance with the claim 1, it is characterised in that：Step
Time of repose in [1-3] is 30-60min.
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Cited By (3)
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| CN109827918A (en) * | 2019-04-03 | 2019-05-31 | 广西壮族自治区冶金产品质量检验站 | The measuring method of silicone content in tin-doped indium oxide powder |
| CN111912797A (en) * | 2019-12-17 | 2020-11-10 | 南开大学 | Method for measuring total phosphorus content in water |
| WO2024066180A1 (en) * | 2022-09-28 | 2024-04-04 | 广东邦普循环科技有限公司 | Method for measuring total phosphorus content of non-ferrous metal extraction waste liquid |
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| CN109827918A (en) * | 2019-04-03 | 2019-05-31 | 广西壮族自治区冶金产品质量检验站 | The measuring method of silicone content in tin-doped indium oxide powder |
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