CN106855504A - A kind of method of quick measure sulfate radical content - Google Patents
A kind of method of quick measure sulfate radical content Download PDFInfo
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- CN106855504A CN106855504A CN201610976826.0A CN201610976826A CN106855504A CN 106855504 A CN106855504 A CN 106855504A CN 201610976826 A CN201610976826 A CN 201610976826A CN 106855504 A CN106855504 A CN 106855504A
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- sulfate radical
- radical content
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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 discloses a kind of method of quick measure sulfate radical content, so that H can be provided+And produce acid solution and gumwater in addition to precipitating as stabilizer except anion can be combined with barium ions, add stabilizer, chlorination titanate particle to be measured light absorption value in testing sample.The method that the present invention determines sulfate radical content, simplified operational procedure, testing conditions are easy to control, and sulfate radical content is less than in the range of 40mg/L, and linear relationship is good, reproducible；The present invention can also be detected by dilution for sample of the sulfate radical content more than 40mg/L suitable for the low sample of sulfate radical content with the inventive method；The present invention is under the conditions of without the advanced precision equipment of outfit, with relatively low testing cost, it is ensured that determine precision with accuracy well, relative coefficient is up to 99.9%, and detection efficiency is high, for laboratory provides a kind of reliable method that sulfate radical content is determined suitable for batch sample.
Description
Technical field
The present invention relates to a kind of detection method, more particularly to a kind of method of quick measure sulfate radical content.
Background technology
The common method for determining sulfate radical at present has chromatography of ions, barium sulfategravimetry, turbidimetry, volumetric method, barium chromate
AAS etc..The chromatography of ions needs large-scale instrument, relatively costly, and many laboratories cannot be equipped with；Classical gravimetric method behaviour
Make cumbersome, detection efficiency is low；The testing conditions requirement of turbidimetry described in GB is harsh, linear not good enough, poor repeatability；Volumetric method is grasped
Make time-consuming, the irritant smell of ammoniacal liquor used, Ca in sample2+、Mg2+Content meeting high influences the Accurate Determining of sulfate radical；Chromic acid
The trivial operations such as heating, tune pH value, filtering are time-consuming in barium photometry, and error is larger, and in sulfate radical content in 8~120mg/L
In the range of meet law of Beer, be not suitable for the relatively low sample of sulfate radical content.In order to ensure accurately and efficiently to determine sulfate radical
Content, the existing turbid method of investigation and comparison, Barium Chromate Spectrophotometry propose many improvement.As in barium sulfate turbidimetry with gelatin,
The stabilizers such as PVA replace the glycerine and ethanol mixed stabilizer described in GB；The filtering improvement of Barium Chromate Spectrophotometer is centrifugation
Removal precipitation.But it is poor that above-mentioned improvement is not fully solved turbidimetry linear relationship, testing result is unstable and barium chromate luminosity
Method is cumbersome, be not suitable for sulfate radical low content sample the problems such as.So far, for being not equipped with the experiment of advanced precision instrument
For room, still without a kind of proper method for accurately and efficiently determining the different samples of sulfate radical content height.
The information for being disclosed in the background section is merely intended to increase the understanding to general background of the invention, without answering
In being considered as recognizing or imply in any form that the information structure has been the prior art well known to persons skilled in the art.
The content of the invention
The present invention is directed to above-mentioned technical problem, invents a kind of method for determining sulfate radical content, simplified operational procedure, detection
Condition is easy to control, and linear relationship is good, reproducible, testing result precise and high efficiency, and sulfate radical content is less than in the range of 40mg/L
Meet law of Beer, the range of linearity is big.The sample of sulfate radical low content can be determined directly, and the sample of sulfate radical high content is by dilute
Can also be determined after releasing, therefore the present invention is applied widely.
To achieve the above object, the technical scheme that the present invention is provided is as follows：
A kind of method of quick measure sulfate radical content, so that H can be provided+And sunk except anion can be combined generation with barium ions
Acid solution and gumwater beyond shallow lake adds stabilizer, chlorination titanate particle to carry out as stabilizer in testing sample
Determine light absorption value.
Wherein, the method that sulfate radical content is determined as described above, comprising following operating procedure：
(1) testing sample is taken, sequentially adding can provide H+And in addition to anion can be combined generation precipitation with barium ions
Acid solution, gumwater, chlorination titanate particle, rock 5~6 times, must treat test sample, stand 15min；Wherein, described water is
The deionized water that the same day newly produces；
(2) repeat step (1) operation, water is substituted for by testing sample, and other are identical, obtains blank sample, stands 15min；Its
In, described water is the same day new deionized water produced；
(3) step (2) gained blank sample is returned to zero at specific wavelength 420nm, then determination step (1) gained treats that test sample is inhaled
Light value, obtains final product.
Wherein, testing sample and salpeter solution in step (1), gumwater, chlorination titanate particle are into 5~25:0.25
~1:0.25~1:0.15~0.8 mass ratio.
Wherein, testing sample and salpeter solution in step (1), gumwater, chlorination titanate particle are into 25:0.5:0.5:
0.2 mass ratio.
Wherein, it is described that H can be provided+And except the acid solution that anion can be combined in addition to producing precipitation with barium ions is nitric acid
One kind in solution, hydrochloric acid solution, acetic acid solution.
Wherein, described salpeter solution, hydrochloric acid solution or acetic acid solution volumetric concentration are all 0.2%~5%.
Wherein, testing sample pH value is 2~6.
Wherein, described gumwater mass concentration 0.1%~1%, consumption 0.2mL~5mL.
Wherein, described gumwater mass concentration is 0.5%.
Wherein, described barium chloride grain diameter is 0.25~1mm.
Compared with prior art, the present invention has the advantages that：
(1) method that the present invention determines sulfate radical content, simplified operational procedure, testing conditions are easy to control, sulfate radical content
In the range of 40mg/L, linear relationship is good, reproducible；
(2) suitable for the low sample of sulfate radical content, the sample for sulfate radical content more than 40mg/L passes through the present invention
Dilution can also be detected with the inventive method；
(3) extensively, half working day detectable more or less a hundred sample, is test in laboratory batch sample sulfuric acid to applicability of the present invention
The proper method of radical content；
(4) it is of the invention under the conditions of without the advanced precision equipment of outfit, with relatively low testing cost, it is ensured that determine precision
Good with accuracy, relative coefficient is up to 99.9%, and detection efficiency is high, and batch sample is applied to for laboratory provides one kind
Product determine the reliable method of sulfate radical content.
Specific embodiment
It is described in detail with reference to specific embodiment, it is to be understood that protection scope of the present invention is not by specific
The limitation of implementation method.The collection of the sample employed in embodiment and treatment：Guangxi friendship closes forest ecosystem positioning view
Research station's 1~No. 7 Atmospheric precipitation of sample point of field experiment of ripple in volt is surveyed, 7 sample points respectively take 1 water sample, and water sample numbering is same to be taken
1, No. 2 sample point water samplings 2 of sampling point number, i.e., No. 1 sample point water sampling, by that analogy.Sample is deposited in 0~4 DEG C of refrigerator,
As water sample to be measured.The present invention is also applied for the detection of other class solution sulfate radicals except can detect water sample.
1st, salpeter solution：Pipette extracts desired amount of nitric acid (HNO3, analyzing pure, Lianjiang City likes that honest and clean chemical reagent has
Limit company), add deionized water to prepare and obtain final product；
2nd, gumwater：Weigh desired amount of Arabic gum and (analyze pure, Chengdu Kingsoft limited public affairs of chemical reagent
Department；), deionized water is added, heating is boiled to Arabic gum dissolving, and cooling and standings are overnight used afterwards；Gumwater can
, such as there is muddy, transparent blob of viscose or mildew in reagent bottle in normal temperature sealing storage more than 2 weeks, should discard and prepare again；
3rd, 0.1mg/mL sulfate radicals standard liquid：1.4788g is weighed in 105 DEG C of anhydrous sodium sulfate (Na of drying2SO4, analyze pure,
Tianjin Bo Di chemical inc) it is soluble in water, 1L is settled to, the sulfate radical standard liquid with prepared 1mg/m L/.Take out
10mL is taken, plus deionized water is settled to 100m L and obtains final product 0.1mg/mL sulfate radical standard liquids；
4th, chlorination titanate particle (BaCl2, analyze pure, Chengdu Ke Long chemical reagents factory)：After barium chloride is rolled or ground,
Pour into combination sieve upper (being above 18 mesh sieves, be above 60 mesh sieves), sieve and take crystal grain of the particle size in 0.25-1mm；
Above reagent is the pure rank of analysis, is all commercially available；
5th, balance；
6th, adjustable electric cooking stove；
7th, 722 spectrophotometer；
8th, baking oven；
9th, 18 mesh standard sieve；
10th, 60 mesh standard sieve；
11st, deionized water.
Above-mentioned mentioned nitric acid (HNO3, analyze pure), Arabic gum (analysis pure), anhydrous sodium sulfate (Na2SO4, analysis
It is pure), chlorination titanate particle (BaCl2, analyze pure) all buy in Nanning Hui Xinhua glass Instrument Ltd..
Embodiment 1
A kind of method of quick measure sulfate radical content, operating procedure is as follows：
(1) extract in the supernatant 25ml injection 25mL colorimetric cylinders after water sample 1 to be measured stands, addition volumetric concentration is
1% salpeter solution, the gumwater that 0.5ml mass concentrations are 0.5%, the barium chloride that 0.2g particle diameters are 0.25~1mm
Particle；Rocking 5~6 times makes each material mixing in it uniform, adds salpeter solution to make water sample pH value to be measured be 4, must treat test sample, quiet
Detected after putting 15min；
(2) repeat step (1) operation, deionized water is substituted for by the clarified solution of water sample to be measured 1：Remove ionized water 25mL notes
Enter in 25mL colorimetric cylinders, sequentially add the salpeter solution that volumetric concentration is 1%, the Arabic gum that 0.5ml mass concentrations are 0.5%
The chlorination titanate particle of solution, 0.2g particle diameters between 0.25~1mm, rocking 5~6 times makes each material mixing in it uniform, adds
Salpeter solution causes that water sample pH value to be measured is 4, obtains blank sample, is detected after standing 15min；
(3) step (2) gained blank sample is returned to zero at spectrophotometer wavelength 420nm, then determination step (1) gained is treated
Test sample light absorption value, obtains final product.
The sulfate radical in water sample 2, water sample 3, water sample 4, water sample 5, water sample 6, water sample 7 is determined in above-mentioned same method to contain
Amount, each water sample to be measured repeats the above steps 6 times, takes the average value of measurement gained light absorption value, and the data obtained is as shown in table 1.
Embodiment 2
A kind of method of quick measure sulfate radical content, operating procedure is as follows：
(1) extract in the supernatant 25ml injection 25mL colorimetric cylinders after water sample 1 to be measured stands, addition volumetric concentration is
0.2% hydrochloric acid solution, the gumwater that 0.1ml mass concentrations are 1%, the barium chloride that 0.2g particle diameters are 0.25~1mm
Particle；Rocking 5~6 times makes each material mixing in it uniform, adds hydrochloric acid solution to make water sample pH value to be measured be 2, must treat test sample, quiet
Detected after putting 15min；
(2) repeat step (1) operation, deionized water is substituted for by the clarified solution of water sample to be measured 1：Remove ionized water 25mL notes
Enter in 25mL colorimetric cylinders, sequentially add the hydrochloric acid solution that volumetric concentration is 0.2%, the Arabic gum that 0.1ml mass concentrations are 1%
The chlorination titanate particle of solution, 0.2g particle diameters between 0.25~1mm, rocking 5~6 times makes each material mixing in it uniform, adds
Hydrochloric acid solution causes that water sample pH value to be measured is 2, obtains blank sample, is detected after standing 15min；
(3) step (2) gained blank sample is returned to zero at spectrophotometer wavelength 420nm, then determination step (1) gained is treated
Test sample light absorption value, obtains final product.
Repeat the above steps 6 times, take the average value of measurement gained light absorption value.
Embodiment 3
A kind of method of quick measure sulfate radical content, operating procedure is as follows：
(1) extract in the supernatant 25ml injection 25mL colorimetric cylinders after water sample 1 to be measured stands, addition volumetric concentration is
5% acetic acid solution, the gumwater that 5ml mass concentrations are 0.1%, the barium chloride that 0.2g particle diameters are 0.25~1mm
Grain；Rocking 5~6 times makes each material mixing in it uniform, adds acetic acid solution to make water sample pH value to be measured be 6, must treat test sample, stands
Detected after 15min；
(2) repeat step (1) operation, deionized water is substituted for by the clarified solution of water sample to be measured 1：Remove ionized water 25mL notes
Enter in 25mL colorimetric cylinders, sequentially add the Arabic peptization that the acetic acid solution, 5ml mass concentrations that volumetric concentration is 5% are 0.1%
The chlorination titanate particle of liquid, 0.2g particle diameters between 0.25~1mm, rocking 5~6 times makes each material mixing in it uniform, adds second
Acid solution causes that water sample pH value to be measured is 6, obtains blank sample, is detected after standing 15min；
(3) step (2) gained blank sample is returned to zero at spectrophotometer wavelength 420nm, then determination step (1) gained is treated
Test sample light absorption value, obtains final product.
Repeat the above steps 6 times, take the average value of measurement gained light absorption value.
The foundation of standard curve
Concentration is extracted for 0.1mg/mL sulfate radicals titer 0,0.5,1,2,4,8,10mL is injected separately into 7 colorimetric cylinders, is gone
Ionized water is settled to 25mL, obtains the standard liquid series of sulfate radical content 0,0.05,0.1,0.2,0.4,0.8,1mg.Each
Sequentially add salpeter solution, the Arabic gum that 0.5mL mass concentrations are 0.5%, 0.2g particle diameters that 0.25mL volumetric concentrations are 1%
Chlorination titanate particle between 0.25~1mm, fluctuates 5~6 times, and the salpeter solution of addition makes standard liquid pH value be 4, quiet
Light absorption value is determined at spectrophotometer wavelength 420nm after putting 15min.With the titer of sulfate radical content 0mg to spectrophotometric
Meter zeroing, then the light absorption value of other standards liquid is determined, the regression equation of sulfate radical content and light absorption value is set up according to measurement result,
Content for calculating sulfate radical in sample.
W=(k × A+b)/V × 1000
W：Sulfate radical content mg/L；
k：The slope of standard curve (regression equation)；
A：The light absorption value of testing sample；
b：The intercept of standard curve (regression equation)；
V：Extract prepare liquid volume mL；
1000：Units conversion factor.
The experiment of accuracy
Extract concentration and be injected separately into 6 colorimetric cylinders for 0.1mg/mL sulfate radicals titer 0,0.5,1,1.5,2,6mL, go from
Sub- water is settled to 25mL, obtains sulfate radical content 0,2,4,6,8,24mg/L standard liquids.Each sequentially add 0.25mL volumes
Chlorine of the gumwater, 0.2g particle diameters that concentration is 1% nitric acid, 0.5mL mass concentrations are 0.5% between 0.25~1mm
Change titanate particle, fluctuate 5~6 times, the salpeter solution of addition makes prepare liquid pH value be 4, in spectrophotometer after standing 15min
Light absorption value is determined at wavelength 420nm.Spectrophotometer is returned to zero with the titer of sulfate radical content 0mg, then determines sulfate radical and contained
Amount 2,4,6, the 8, light absorption value of 24mg/L solution.Process gained regression equation is set up according to above-mentioned standard curve, sulfate radical is calculated
Content, above experiment is repeated 6 times, and takes the average value of gained measured value, and the data obtained is as shown in table 2.
Table 1 quickly determines the precision test of sulfate radical content method
From table 1, the sulfate radical content of sample 1,2,3 is relatively low, and less than 5mg/L, SD (standard deviation) is less than 0.3, sulfuric acid
The CV (coefficient of variation) of radical content is less than 10%；Between 5-11mg/L, SD is less than 0.5, sulphur to the sulfate radical content of sample 4,5,6,7
The CV of acid group content is less than 5%.Between 20-40mg/L, SD is less than 1.5, sulfate radical content CV to the sulfate radical content of sample 6,7
Less than 5%.Thus illustrate, detection method proposed by the present invention is to sulfate radical content less than 5mg/L and sulfate radical content in 5-
Sample between 40mg/L can ensure that testing result dispersion is small, and precision is good.Quick measure sulfate radical proposed by the present invention
The precision of content method can meet the different sample detection requirement of sulfate radical content height.
Table 2 quickly determines the Test of accuracy of sulfate radical content method
From table 2, between 95%-104%, RSD (relative standard deviation) is in 2%- for the rate of recovery of the inventive method
Between 5%, the accuracy that this explanation present invention determines sulfate radical content is higher, and deviation is smaller.As can be seen here, the present invention is quick surveys
The method precision for determining sulfate radical content is good with accuracy, meets test in laboratory requirement.
The foregoing description to specific illustrative embodiment of the invention be in order to illustrate and illustration purpose.These descriptions
It is not wishing to limit the invention to disclosed precise forms, and it will be apparent that according to above-mentioned teaching, can be much changed
And change.The purpose of selecting and describing the exemplary embodiment is that explaining that certain principles of the invention and its reality should
With so that those skilled in the art can realize and using a variety of exemplaries of the invention and
A variety of selections and change.The scope of the present invention is intended to be limited by claims and its equivalents.
Claims (10)
1. a kind of method of quick measure sulfate radical content, it is characterised in that：So that H can be provided+And except anion can be with barium ions knot
Close and produce acid solution and gumwater beyond precipitation as stabilizer, stabilizer, barium chloride are added in testing sample
Particle is measured light absorption value.
2. the method for quickly determining sulfate radical content according to claim 1, it is characterised in that quickly determine sulfate radical content
Method, comprising following operating procedure：
(1) testing sample is taken, sequentially adding can provide H+And it is sour molten in addition to anion can be combined generation precipitation with barium ions
Liquid, gumwater, chlorination titanate particle, rock, and must treat test sample, stand；
(2) repeat step (1) operation, water is substituted for by testing sample, and other are identical, obtain blank sample, is stood；
(3) step (2) gained blank sample is returned to zero in certain wave strong point, then determination step (1) gained treats test sample light absorption value, i.e.,
.
3. the method for quickly determining sulfate radical content according to claim 2, it is characterised in that：Testing sample in step (1)
With salpeter solution, gumwater, chlorination titanate particle into 5~25:0.25~1:0.25~1:0.15~0.8 mass ratio.
4. the method for quickly determining sulfate radical content according to claim 2, it is characterised in that：Testing sample in step (1)
With salpeter solution, gumwater, chlorination titanate particle into 25:0.5:0.5:0.2 mass ratio.
5. the method for quickly determining sulfate radical content according to claim 1, it is characterised in that：Described can provide H+And remove
The acid solution that anion can be combined beyond generation precipitation with barium ions is the one kind in salpeter solution, hydrochloric acid solution, acetic acid solution.
6. the method for quickly determining sulfate radical content according to claim 5, it is characterised in that：Described salpeter solution, salt
Acid solution or acetic acid solution volumetric concentration are all 0.2%~5%.
7. the method for quick measure sulfate radical content according to claim 1 or claim 2, it is characterised in that：Testing sample pH value is 2
~6.
8. the method for quick measure sulfate radical content according to claim 1 or claim 2, it is characterised in that：Described Arabic gum
Concentration of polymer solution 0.1%~1%, consumption 0.2mL~5mL.
9. the method for quick measure sulfate radical content according to claim 1 or claim 2, it is characterised in that：Described Arabic gum
Concentration of polymer solution is 0.5%.
10. the method for quick measure sulfate radical content according to claim 1 or claim 2, it is characterised in that：Described barium chloride
Grain particle diameter is 0.25~1mm.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2681855C1 (en) * | 2017-09-15 | 2019-03-13 | Общество С Ограниченной Ответственностью "Агронэт" | Method for determining sulfur in form of sulfate ion in water soil extract and device for implementing method |
| CN112924400A (en) * | 2019-12-05 | 2021-06-08 | 中粮生物科技股份有限公司 | Method for detecting sulfate content in citric acid sample |
| CN115667151A (en) * | 2020-05-27 | 2023-01-31 | 松下知识产权经营株式会社 | Barium compound structure and method for producing same |
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| CN101765772A (en) * | 2007-05-31 | 2010-06-30 | 通用电气公司 | Method for determination of polymer concentration in water systems |
| CN105388121A (en) * | 2015-12-29 | 2016-03-09 | 瓮福达州化工有限责任公司 | Detection method for sulfate radical in load solvent |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2681855C1 (en) * | 2017-09-15 | 2019-03-13 | Общество С Ограниченной Ответственностью "Агронэт" | Method for determining sulfur in form of sulfate ion in water soil extract and device for implementing method |
| CN112924400A (en) * | 2019-12-05 | 2021-06-08 | 中粮生物科技股份有限公司 | Method for detecting sulfate content in citric acid sample |
| CN115667151A (en) * | 2020-05-27 | 2023-01-31 | 松下知识产权经营株式会社 | Barium compound structure and method for producing same |
| CN115667151B (en) * | 2020-05-27 | 2024-03-12 | 松下知识产权经营株式会社 | Barium compound structure and method for producing same |
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