CN105866110A - Detection agent for determining content of silica in water - Google Patents
Detection agent for determining content of silica in water Download PDFInfo
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- CN105866110A CN105866110A CN201610181876.XA CN201610181876A CN105866110A CN 105866110 A CN105866110 A CN 105866110A CN 201610181876 A CN201610181876 A CN 201610181876A CN 105866110 A CN105866110 A CN 105866110A
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- G—PHYSICS
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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
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Abstract
The invention relates to a detection agent for determining the content of silica in water, and belongs to the technical field of environment detection. Ammonium sulfate or ammonium chloride, ammonium bisulfate and ammonium molybdate are weighed according to a mass ratio of (30-100):(10-50):(1-10), and are uniformly mixed, the obtained ammonium mixture is ground to form powder which is soluble silica detection powder I; oxalic acid or sodium oxalate and sodium sulfite are weighed according to a mass ratio of (10-60):(50-100) and are uniformly mixed, and the obtained sodium mixture is ground to form powder which is soluble silica detection powder II; and the detection powder I is added to 4ml of a water sample to be detected and is dissolved through shaking, chromogenic treatment is carried out for 5min, the detection powder II is added and is dissolved through shaking, the obtained solution stands for 5min, and the concentration of soluble silica is measured through a colorimeter or a spectrophotometer. The soluble silica detection agent has the advantages of high sensitivity, good selectivity, wide detection range, stable quality, convenient carrying, simple operation, and suitableness for detecting the concentration of soluble silica in surface water, underground water, seawater and drinking water.
Description
Technical field
The present invention relates to a kind of measure the detection agent of soluble silica content in water body, belong to environment measuring skill
Art field.
Background technology
Silicon is the important component part of the earth's crust, widely distributed in nature.Silicon in water body mainly has solubilised state
Silicate (DSi), biogenic opal (PBSi) and three kinds of forms of diagenesis silicon (LSi), wherein Dissolved Silicon is mainly with H4SiO4
Form exists, can be the most bioavailable, is also the limiting factor determining growth of diatom algae breeding.Silicate is floated
It is mainly used to synthesize amorphous silicon (SiO after trip plant absorption2·nH2O), the silicon of the phytoplanktons such as diatom is formed
Mass shell, a small amount of biosynthesis being used for regulating phytoplankton.In the case of silicon lacks, in frustule wall
Silicone content reduces, and wall is thinning, and then affects growth and breeding and the structure of community of diatom.Soluble silicon in water body
Accurate Determining is prediction and differentiates that growth of diatom algae or even wawter bloom form the important prerequisite of probability.Diatom group change and
In deposit preserve recorded information become research whole world change important content, it is therefore desirable to more
Understand the level of silicon in water body exactly.
The detection method of dioxide-containing silica routine has: gravimetric method, potassium fluoride volumetry, colorimetric method, X penetrate
Line fluorescent spectrometry, inductively coupled plasma emission spectrography etc..The complex operation that these methods have, analyzes
Cycle is long, and liquid reagent colour developing is slowly；Some need the huge and instrument of costliness, to operating personnel's specialty skill
Can require higher, can only complete in laboratory, it is impossible to meet the requirement of fast-field evaluation.To this end, it is numerous
Researcher has carried out many effort.Zheng Yasha improves silica sample-smelting method, adds boric acid and carbon with sodium carbonate
Acid potassium makees mixed flux, and the method is easy quickly, and the operating time is shortened to 30-40min by original 3-4h.
(Zheng Yasha；Quickly measure the improvement [J] of silica sample-smelting method；Assay laboratory；1987,6(11):57).
Closing Xi'an etc. and have studied in the presence of oxalic acid, in hydrochloric acid medium, silicon-molybdenum heteropoly acid develops the color with rhodamine B (KB),
And then establish the highly sensitive method of one of aqueous phase direct chromogenic assay silica；This method developing time stablizes 24h
Above, Si02Content meets Beer-Lambert Law in the range of 0～3.5ug/50ml, and molar absorption coefficient is 1.8
×105(L·mol-1·cm-1), the rate of recovery 99%～103%, trace in high purity aluminium oxide and aluminium hydroxide
The mensuration of amount silica, result is satisfied.(close Xi'an, Wang Yonghui, Xue Shulin；Measuring Method for Trace Silica
Research [J]；Shanxi science and technology；2002,5:58-59).Wang Yuxin etc. are in Silicon Molybdenum Blue Spectrophotometry mensuration aluminum oxide two
The method of silica content improves, and overcomes complex compound colour developing instability, or the phenomenons such as muddy occurs；With
Ascorbic acid makees reducing agent, measures at 810nm；When the silicon molybdenum blue complex compound formed in improved method is stablized
Between long, can be measured within 20min to 2h after colour developing, the relative deviation that 3 sample parallel measure is only
3%, recovery of standard addition is 95%～103%, and maximum relative error is 5.0%；Phosphorus, arsenic and concentration of iron are respectively
The mensuration of silicon is not disturbed at 10,100 and 250 below μ g/mL；Wanting of general industry analysis can be fully met
Ask.(Wang Yuxin etc.；The improvement [J] of Silica Determination in Alumina with Spectrophotometr of Silica-molybdenum；Non-ferrous metal；
2003,55(3):147-148).Animal glue is condensed gravimetric detemination silica by Zhang Qun etc. and molybdenum blue spectrophotometry is surveyed
The method determining silica combines, and establishes silicon dioxide content test animal glue cohesion weight in apatite
The new method of method filtrate molybdenum blue spectrophotometric method, the method has higher than original gravimetric method, volumetric method
Preci-sion and accuracy.(Zhang Qun etc.；The new method [J] of the silicon dioxide content test in apatite；Guizhou
Work；2007,32(2):33-34).But the most not yet find the development report of relevant dioxide-containing silica detection pulvis
Road.
Summary of the invention
It is an object of the invention to open one and be suitable for various water bodies such as surface water, underground water, seawater, drinking water
Etc. the preparation method of soluble silica content detection agent, another object of the present invention is to provide one and makes
Use method.
In order to achieve the above object, the present invention is according to quilt after soluble silica and ammonium molybdate generation chromogenic reaction
The principle of sodium sulfite reduction prepares soluble silica detection agent, and this detection agent is examined by soluble silica
Surveying powder I and soluble silica detection II two kinds of powder detection powder composition, wherein, soluble silica detects
The preparation method of powder I is, first weighs ammonium sulfate or ammonium chloride according to mass ratio: ammonium hydrogen sulfate: ammonium molybdate=
Then they are mixed, pulverize by (30～100): (10～50): (1～10), and obtaining can
Dissolubility silica detection powder I；The preparation method of soluble silica detection powder II is to claim according to mass ratio
Take oxalic acid or sodium oxalate: sodium sulfite=(10～60): (50～100), they are mixed, grind
Cheng Fen, obtains soluble silica detection powder II；
The using method of the detection agent of a kind of soluble silica content measured in water body, takes 5ml water to be measured
Sample, in plastics chromoscope, adds soluble silica detection powder I 0.1～0.3g, after shake is dissolved, stands
5min, adds soluble silica detection powder II 0.1～0.5g, after shake is dissolved, stands 5min, utilize
Colorimeter or spectrophotometer measurement, obtain soluble silica content in water sample to be measured；
Above-mentioned water sample to be measured is surface water, underground water, seawater, drinking water.
The invention have the advantage that
1. the detection agent of the present invention has that preparation method is simple, steady quality, easy to carry, processing ease etc.
Feature, layman can use.
2. the detection agent of the present invention is the best: in detected water sample during below phosphate-containing 3mg/L, do not disturb
Measure.
3, the detection agent detection range width of the present invention, it is applicable to silica in detected water sample
0.05～7.0mg/L, highly sensitive, and, it is suitable for the water bodys such as surface water, underground water, seawater, drinking water
Middle soluble silica Concentration Testing.
Detailed description of the invention
Embodiment 1
Measure the preparation of the detection agent of soluble silica content in water body
Weighing 1g ammonium hydrogen sulfate, mix with 7g ammonium chloride, 0.5g ammonium molybdate, grind into powder, obtaining can
Dissolubility silica detection powder I, standby；
Weigh 1g oxalic acid and 5g sodium sulfite, mix, obtain soluble silica detection powder II, standby.
Embodiment 2
Measure the preparation of the detection agent of soluble silica content in water body
Weigh 1g ammonium hydrogen sulfate, mix with 10g ammonium sulfate, 0.5g ammonium molybdate, grind into powder,
Soluble silica detection powder I, standby；
Weigh 1g sodium oxalate and 5g sodium sulfite, mix, obtain soluble silica detection powder II, standby
With.
Embodiment 3
The detection agent using embodiments of the invention 1 to obtain measures well water soluble silica concentration
Take 5ml well water in plastics chromoscope, the soluble silica detection powder I that addition embodiment 1 prepares
0.2g, after shake is dissolved, stands 5min, adds the soluble silica detection powder II that embodiment 1 prepares
0.2g, after shake is dissolved, stands 5min, utilizes spectrophotometer at wavelength for measuring absorbance at 660nm,
Substituting into calibration curve and calculating soluble silica concentration is 28.50mg/L, with GB detection method (SL
Testing result 91.2-1994) is consistent, therefore, this detection agent measure water quality soluble silica concentration accurately,
Reliably.
Embodiment 4
The detection agent using embodiments of the invention 2 to obtain measures river soluble silica concentration
Take 5ml river in plastics chromoscope, the soluble silica detection powder I that addition embodiment 2 prepares
0.2g, after shake is dissolved, stands 5min, adds the soluble silica detection powder II that embodiment 2 prepares
0.2g, after shake is dissolved, stands 5min, utilizes spectrophotometer at wavelength for measuring absorbance at 660nm,
Substituting into calibration curve and calculating soluble silica concentration is 19.62mg/L, with GB detection method (SL
Testing result 91.2-1994) is consistent, therefore, this detection agent measure water quality soluble silica concentration accurately,
Reliably.
Claims (2)
1. one kind measures the preparation method of the detection agent of soluble silica content in water body, it is characterised in that:
It is made up of soluble silica detection powder I and soluble silica detection powder II, wherein, solubility dioxy
The preparation method of SiClx detection powder I is, first weighs ammonium sulfate or ammonium chloride according to mass ratio: ammonium hydrogen sulfate: molybdenum
Then they are mixed, pulverize by acid ammonium=(30～100): (10～50): (1～10), and obtaining can
Dissolubility silica detection powder I；The preparation method of soluble silica detection powder II is to claim according to mass ratio
Take oxalic acid or sodium oxalate: sodium sulfite=(10～60): (50～100), they mixed, pulverizes,
Obtain soluble silica detection powder II；
Above-mentioned ammonium hydrogen sulfate, ammonium sulfate, ammonium chloride, ammonium molybdate, oxalic acid, sodium oxalate and sodium sulfite are city
Sell analysis pure chemicals.
2. one kind measures the detection agent of soluble silica content in water body with what claim 1 method obtained
Using method, it is characterised in that: take 5ml water sample to be measured in plastics chromoscope, add solubility titanium dioxide
Silicon detection powder I 0.1～0.3g, after shake is dissolved, stands 5min, adds soluble silica detection powder II
0.1～0.5g, after shake is dissolved, stand 5min, utilize colorimeter or spectrophotometer measurement, obtain water to be measured
Soluble silica content in sample；
Above-mentioned water sample to be measured is surface water, underground water, seawater, drinking water.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610181876.XA CN105866110A (en) | 2016-03-28 | 2016-03-28 | Detection agent for determining content of silica in water |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610181876.XA CN105866110A (en) | 2016-03-28 | 2016-03-28 | Detection agent for determining content of silica in water |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404773A (en) * | 2016-11-03 | 2017-02-15 | 大唐东北电力试验研究所有限公司 | Detection method for measuring silicon content in water body and silicon dioxide content analysis device |
| 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 |
| CN111458330A (en) * | 2020-04-28 | 2020-07-28 | 今麦郎饮品股份有限公司 | Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof |
| CN112432941A (en) * | 2020-10-29 | 2021-03-02 | 中化地质矿山总局地质研究院 | Method for measuring silicate content in salt lake brine |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106404773A (en) * | 2016-11-03 | 2017-02-15 | 大唐东北电力试验研究所有限公司 | Detection method for measuring silicon content in water body and silicon dioxide content analysis device |
| 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 |
| CN111458330A (en) * | 2020-04-28 | 2020-07-28 | 今麦郎饮品股份有限公司 | Method for semi-quantitatively detecting content of metasilicic acid in mineral water and detection reagent thereof |
| CN112432941A (en) * | 2020-10-29 | 2021-03-02 | 中化地质矿山总局地质研究院 | Method for measuring silicate content in salt lake brine |
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