CN106706808B - The morphological analysis method of organic matter in a kind of sodium aluminate solution - Google Patents
The morphological analysis method of organic matter in a kind of sodium aluminate solution Download PDFInfo
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- CN106706808B CN106706808B CN201611111974.2A CN201611111974A CN106706808B CN 106706808 B CN106706808 B CN 106706808B CN 201611111974 A CN201611111974 A CN 201611111974A CN 106706808 B CN106706808 B CN 106706808B
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of morphological analysis method of organic matter in sodium aluminate solution, include the following steps: that (1) solution extracts；(2) extract liquor is esterified；(3) it is esterified fluid dewatering；(4) GC/MS is analyzed.The present invention keeps test sample structure more single, the organic form in test sample is more stable by extracting, being esterified to sodium aluminate solution and dehydration pre-process, detection effect is more preferable, meanwhile, corrosivity is smaller, weaker to the corrosiveness of equipment, service life of equipment is longer；Meanwhile suitable HCL concentration regulator being selected, and optimization enzymatic synthesis condition separates the organic phase in sodium aluminate solution more completely, detection effect is more preferably.
Description
Technical field
It is organic in especially a kind of sodium aluminate solution the present invention relates to a kind of analysis method of organic matter in sodium aluminate solution
The morphological analysis method of object.
Background technique
The alumina-producing method industrially applied mainly has Bayer process, sintering process, Bayer sintering combination method, due to China
Bauxite resource with high alumina, high silicon, low iron diaspore based on, therefore the alumina producing in China be mainly Bayer sintering
Combination method.Combination method leaching temperature is high, diaspore content of organics used is low, sintering process accounting weight is larger in process, raw
Organic matter during production can be removed directly substantially, therefore the organic matter accumulation problem in process flow does not protrude.
Alumina producing Bayer process has many advantages, such as that process is short, low energy consumption, at low cost, quality is high, China's aluminum oxide industry
Just Bayer process gradually is turned to from traditional Bayer sintering combination method.But compared to combination method, face one of Bayer process is important to be wanted
Problem is the accumulation and harm of organic matter.
Due to raw material and technologic difference, the organism kinds in sodium aluminate solution are more, study according to C.Sato et al.
Report, the carbon in sodium aluminate solution, there are about 96% to derive from bauxite, remaining 4% derives from unclassified stores.Wherein there are about 26%
It is sodium carbonate, 18% is sodium oxalate, and 56% is Organic Sodium Salt.And the lower fatty acid of relative molecular mass in these Organic Sodium Salts
Salt [2] includes mainly oxalates, formates and acetate, accounts for 44% of total organic carbon or so；Relative molecular mass is greater than
500 humate, accounts for 25% of total organic carbon or so；Katolysis product terephthalic acid sodium and phenol etc., Zhan is always organic
22% or so of carbon.
In alumina producing Bayer process process, the organic matter that ore, additive etc. are brought into can be during process cycles not
The normal production of disconnected cumulative effect aluminium oxide, the granularity for such as reducing corrosion, reducing product aluminium hydroxide reduce product matter
Amount etc., it is therefore necessary to the organic matter in Bayer process sodium aluminate solution be studied, theoretically seek to remove organic matter
Effective ways, to reduce the harm of organic matter bring.
The type of organic matter and structure is complicated, analyzes its form, can from it is microcosmic it is upper understand organic matter in technique
Specific existing forms in the process and Morphological Transitions rule are the research essential links of organic matter, therefore by organic matter
Morphological analysis method standardization, standardization have practical significance.
Organic matter detection means mainly has a gas chromatography-mass spectrometry at present, liquid chromatography mass combined instrument, and nuclear-magnetism is total
Vibration etc., but detected both for conventional known organic matter greatly.Structure is complicated for sodium aluminate solution, and the form of organic matter exists
Wherein constantly transformation, and solution is strong basicity, for most detecting instrument intolerant to alkali corrosion, testing result is also sufficiently complete.Cause
This targetedly must carry out pre-processing to sodium aluminate solution, could obtain good detection effect.
Summary of the invention
To solve the above problems, the present invention provides a kind of morphological analysis method of organic matter in sodium aluminate solution.
Technical solution of the present invention: the morphological analysis method of organic matter in a kind of sodium aluminate solution includes the following steps:
(1) solution extracts: taking sodium aluminate solution to be placed in separatory funnel A, is diluted with water, then shakes when concentrated hydrochloric acid is added dropwise
It shakes to there is white precipitate precipitation, precipitating dissolution is then rocked into solution when hydrochloric acid (1+1) is added dropwise completely, is rinsed with water liquid separation
Inner wall of hopper；Then it is added extractant into separatory funnel A, lower layer's solution is put into liquid separation leakage after stratification by oscillation extraction
It struggles against in B, extractant, then oscillation extraction is added into separatory funnel B, stratification will be in separatory funnel A and separatory funnel B
Upper solution takes out mixing to get extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid is added into extract liquor made from step (1), is esterified；Then solution is moved into and is divided
In liquid funnel C, it is rinsed with water flask inner wall, and washing lotion is incorporated to separatory funnel C, lower layer's solution is released after solution left standstill layering, so
After be rinsed with water separatory funnel C inner wall, to stratification after shaking up, lower part solution is released, the upper layer in separatory funnel C is molten
Liquid takes out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rock sufficiently mixed to solution
It closes, is shaken up again after standing, repetition shakes up-stands at least 3 times, is then allowed to stand at least 12 hours, finally by the solution after standing
It shakes up and carries out natural filtration to get dehydration test sample；
(4) GC/MS is analyzed: dehydration test sample obtained in step (3) is detected using gas chromatography mass spectrometer
Analysis result can be measured the degree of each organic matter component in sodium aluminate solution by analysis using area normalization method.
The morphological analysis method of organic matter, includes the following steps: in sodium aluminate solution above-mentioned
(1) solution extracts: taking sodium aluminate solution to be placed in separatory funnel A, is diluted with water, then shakes when concentrated hydrochloric acid is added dropwise
It shakes to there is white precipitate precipitation, precipitating dissolution is then rocked into solution when hydrochloric acid (1+1) is added dropwise completely, is rinsed with water liquid separation
Inner wall of hopper；Then extractant is added into separatory funnel A, oscillation extraction 5 minutes or more, puts lower layer's solution after stratification
Enter in separatory funnel B, extractant, then oscillation extraction 5 minutes or more, stratification, by separatory funnel are added into separatory funnel B
Upper solution in A and separatory funnel B takes out mixing to get extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid is added into extract liquor made from step (1), carries out being esterified at 70-90 DEG C anti-
It answers 40-60 hours；Then solution is moved into separatory funnel C, is rinsed with water flask inner wall 1-2 times, washing lotion is incorporated to separatory funnel
Lower layer's solution is released after solution left standstill layering, is then rinsed with water separatory funnel C inner wall 1 time by C, to stratification after shaking up,
Lower part solution is released, the upper solution in separatory funnel C is taken out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rock sufficiently mixed to solution
It closes, shakes up, at least 3 times repeatedly, be then allowed to stand at least 12 hours, finally by the solution after standing again after standing at least 1 hour
It shakes up and carries out natural filtration to get dehydration test sample；
(4) GC/MS is analyzed: dehydration test sample obtained in step (3) is detected using gas chromatography mass spectrometer
Analysis result can be measured the degree of each organic matter component in sodium aluminate solution by analysis using area normalization method.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, in the step (1), the oscillation extraction time is 10
Minute.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, in the step (1), concentrated hydrochloric acid is mass fraction
For 37% commercially available excellent pure grade concentrated hydrochloric acid, hydrochloric acid (1+1) is that the commercially available concentrated hydrochloric acid for being 37% by 500ml mass fraction is diluted with water
It is made after to 1L.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, in the step (2), dilute hydrochloric acid refers to mole dense
Degree is the hydrochloric acid of 8mol/L.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, in the step (2), esterification temperature is 80 DEG C,
Esterification time is 48 hours.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned in the step (3), is added anhydrous in esterifying liquid
Magnesium sulfate is rocked to solution after being sufficiently mixed, and need to be stood 1 hour, then be shaken up again, 3 times repeatedly, is then allowed to stand 12 hours.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, the extractant are n-butanol.
The morphological analysis method of organic matter in sodium aluminate solution above-mentioned, water used in the method is that resistivity is
The ultrapure water of 18.3M Ω .cm.
Beneficial effects of the present invention:
1, the present invention makes test sample structure more by being extracted, being esterified to sodium aluminate solution and dehydration pre-process
Single, the organic form in test sample is more stable, and detection effect is more preferable.
2, in the prior art, due to the step of not being dehydrated, map stability is bad.Increase dehydration in the present invention
Afterwards, test map is shown, as a result more stable.
3, in the prior art, due to the step of not being dehydrated, detection the results show that siliceous organic matter in test sample
Content is high, causes test sample larger to the corrosion impact of equipment.And the present invention is by reducing test sample after dehydration
In siliceous organic matter content, reduce the corrosivity of test sample, reduce corruption of the test sample to detection device chromatographic column
Erosion influences, and weaker to the corrosiveness of equipment, service life of equipment is longer, and testing result is more acurrate, still, after common dehydration
Test sample can have an adverse effect to testing result, and the detection method of this hair is after dewatering, does not find to test sample
Have an adverse effect.
4, the present invention is by " anhydrous magnesium sulfate being added, rocks to solution and is sufficiently mixed, after standing at least 1 hour again
Shake up, at least 3 times repeatedly, be then allowed to stand at least 12 hours, finally the solution after standing is shaken up and carries out natural filtration ", research
Display after being dehydrated in this way, influences minimum to the testing result of sample to be tested, the result of detection is more accurate.
5, suitable HCL concentration regulator, and optimization enzymatic synthesis condition is selected to keep the organic phase in sodium aluminate solution more complete
Ground is separated, and detection effect is more preferably.
Experimental example
The sodium aluminate solution extract liquor and dehydration each portion of test sample that the method for the present invention of learning from else's experience respectively is prepared, as
Test sample is detected using 5977N type mass spectrometer detector, and operating condition is as follows:
Chromatographic column: Agilent HP-5MS (5%)-diphenyl (95%)-dimethyl arlydene silicone copolymers；
Quartz capillary column: 30mx0.25mmx025mm；
Column flow: 1mL/min；
Injector temperature: 250 DEG C；
Temperature programming: 50 DEG C -1min-10 DEG C/min-220 DEG C -1min-5 DEG C/min-315 DEG C -2min of column temperature；
Split ratio: it does not shunt；
Sample volume: 1uL；
Carrier gas: high-pure helium (99.999%)；
Ionization mode: EI；
Electron energy: 70eV；
Emission current: 100mA；
Ion source temperature: 230 DEG C；
Mass scan range: 30-350m/z；
Retrieve mass spectral database: U.S. NIST Library；
Wherein organic matter testing result difference is as shown in Table 1 and Table 2, total ion chromatogram such as attached drawing 1 and attached in sample
Shown in Fig. 2.
The content of organic matter in 1 esterifying liquid sample of table
Table 2 is dehydrated the content of organic matter in test sample
Through comparison Tables 1 and 2 it is found that compared with the type of the organic matter detected in esterifying liquid sample, dehydration detection
The organism kinds detected in sample are more, more complete, illustrate the shape that organic matter is more advantageous to after the method for the present invention processing
Body analysis.
In addition, from the testing result of Tables 1 and 2 it can also be seen that, dehydrated sample detection in siliceous ingredient organic matter (such as two
Butoxy silane, ten prestoxs-ring nonyl siloxanes etc.) percentage contents and the esterifying liquid result phase not Jing Guo dehydration
Than decreasing, illustrates sample detection after dehydration, the corrosiveness of equipment chromatographic column is reduced, making for chromatographic column is conducive to extend
Use the service life.
Detailed description of the invention
Attached drawing 1 is the total ion chromatogram of esterifying liquid sample detection after dehydration；
Attached drawing 2 is the total ion chromatogram of esterifying liquid sample detection before being dehydrated.
Before being dehydrated it can be seen from attached drawing 1 and attached drawing 2, the starting end of the total ion chromatogram of esterifying liquid sample detection
Curve float up and down larger, illustrate that testing result is undesirable, and after being dehydrated, the total ion chromatogram of esterifying liquid sample detection
The curve of starting end float up and down smaller, be the change curve to tend towards stability.Illustrate after dehydration, test sample
It more conducively detects, testing result is more preferable.
Specific embodiment
The embodiment of the present invention:
Embodiment 1: the morphological analysis method of organic matter in a kind of sodium aluminate solution includes the following steps:
A, prepared by reagent:
(1) extractant: taking 500mL n-butanol to mix with 500mL water, vibrates 10min, takes upper layer water saturation after standing for 1 night
N-butanol is to get extractant；
(2) concentrated hydrochloric acid: taking commercial quality score is 37% excellent pure grade HCl；
(3) the commercially available concentrated hydrochloric acid that 500mL mass fraction is 37% hydrochloric acid (1+1): is diluted to 1L；
B, sample pretreatment:
(1) solution extracts: taking sodium aluminate solution to be placed in separatory funnel A, is diluted with water, then shakes when concentrated hydrochloric acid is added dropwise
It shakes to there is a large amount of white precipitates to be precipitated, precipitating dissolution is then rocked into solution when hydrochloric acid (1+1) is added dropwise completely, is rinsed with water
Separatory funnel inner wall；Then it is added extractant into separatory funnel A, oscillation extraction 10 minutes, by lower layer's solution after stratification
It is put into separatory funnel B, extractant, then oscillation extraction 10 minutes, stratification, by separatory funnel A is added into separatory funnel B
Mixing is taken out with the upper solution in separatory funnel B to get extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid (molar concentration 8mol/L) is added into extract liquor made from step (1), in
It is carried out esterification 48 hours at 80 DEG C；Then solution is moved into separatory funnel C, is rinsed with water flask inner wall 1 time, washing lotion is simultaneously
Enter separatory funnel C, lower layer's solution is released after solution left standstill layering, separatory funnel C inner wall is then rinsed with water 1 time, after shaking up
To stratification, lower part solution is released, the upper solution in separatory funnel C is taken out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rock sufficiently mixed to solution
It closes, is shaken up again after standing 1 hour, 3 times repeatedly, be then allowed to stand 12 hours, the solution after standing is finally shaken up into carry out nature
Filtering is to get dehydration test sample；
C, GC/MS is analyzed: dehydration test sample obtained in sample pretreatment is examined using gas chromatography mass spectrometer
Analysis is surveyed, analysis result can be measured to the degree of each organic matter component in sodium aluminate solution using area normalization method.
Embodiment 2: the morphological analysis method of organic matter in a kind of sodium aluminate solution includes the following steps:
A, prepared by reagent:
(1) extractant: taking 500mL n-butanol to mix with 500mL water, vibrates 10min, takes upper layer water saturation after standing for 1 night
N-butanol is to get extractant；
(2) concentrated hydrochloric acid: taking commercial quality score is 37% excellent pure grade HCl；
(3) the commercially available concentrated hydrochloric acid that 500mL mass fraction is 37% hydrochloric acid (1+1): is diluted to 1L；
B, sample pretreatment:
(1) solution extracts: taking sodium aluminate solution to be placed in separatory funnel A, is diluted with water, then shakes when concentrated hydrochloric acid is added dropwise
It shakes to there is a large amount of white precipitates to be precipitated, precipitating dissolution is then rocked into solution when hydrochloric acid (1+1) is added dropwise completely, is rinsed with water
Separatory funnel inner wall；Then extractant is added into separatory funnel A, oscillation extraction 5 minutes, puts lower layer's solution after stratification
Enter in separatory funnel B, be added extractant, then oscillation extraction 5 minutes into separatory funnel B, stratification, by separatory funnel A and
Upper solution in separatory funnel B takes out mixing to get extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid (molar concentration 8mol/L) is added into extract liquor made from step (1), in
It is carried out esterification 60 hours at 70 DEG C；Then solution is moved into separatory funnel C, is rinsed with water flask inner wall 2 times, washing lotion is simultaneously
Enter separatory funnel C, lower layer's solution is released after solution left standstill layering, separatory funnel C inner wall is then rinsed with water 2 times, after shaking up
To stratification, lower part solution is released, the upper solution in separatory funnel C is taken out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rock sufficiently mixed to solution
It closes, is shaken up again after standing 3 hours, 5 times repeatedly, be then allowed to stand 18 hours, the solution after standing is finally shaken up into carry out nature
Filtering is to get dehydration test sample；
C, GC/MS is analyzed: dehydration test sample obtained in sample pretreatment is examined using gas chromatography mass spectrometer
Analysis is surveyed, analysis result can be measured to the degree of each organic matter component in sodium aluminate solution using area normalization method.
Embodiment 3: the morphological analysis method of organic matter in a kind of sodium aluminate solution includes the following steps:
A, prepared by reagent:
(1) extractant: taking 500mL n-butanol to mix with 500mL water, vibrates 10min, takes upper layer water saturation after standing for 1 night
N-butanol is to get extractant；
(2) concentrated hydrochloric acid: taking commercial quality score is 37% excellent pure grade HCl；
(3) the commercially available concentrated hydrochloric acid that 500mL mass fraction is 37% hydrochloric acid (1+1): is diluted to 1L；
B, sample pretreatment:
(1) solution extracts: taking sodium aluminate solution to be placed in separatory funnel A, is diluted with water, then shakes when concentrated hydrochloric acid is added dropwise
It shakes to there is a large amount of white precipitates to be precipitated, precipitating dissolution is then rocked into solution when hydrochloric acid (1+1) is added dropwise completely, is rinsed with water
Separatory funnel inner wall；Then it is added extractant into separatory funnel A, oscillation extraction 20 minutes, by lower layer's solution after stratification
It is put into separatory funnel B, extractant, then oscillation extraction 20 minutes, stratification, by separatory funnel A is added into separatory funnel B
Mixing is taken out with the upper solution in separatory funnel B to get extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid (molar concentration 8mol/L) is added into extract liquor made from step (1), in
It is carried out esterification 40 hours at 90 DEG C；Then solution is moved into separatory funnel C, is rinsed with water flask inner wall 2 times, washing lotion is simultaneously
Enter separatory funnel C, lower layer's solution is released after solution left standstill layering, separatory funnel C inner wall is then rinsed with water 1 time, after shaking up
To stratification, lower part solution is released, the upper solution in separatory funnel C is taken out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rock sufficiently mixed to solution
It closes, is shaken up again after standing 10 hours, 8 times repeatedly, be then allowed to stand 30 hours, the solution after standing is finally shaken up into carry out nature
Filtering is to get dehydration test sample；
C, GC/MS is analyzed: dehydration test sample obtained in sample pretreatment is examined using gas chromatography mass spectrometer
Analysis is surveyed, analysis result can be measured to the degree of each organic matter component in sodium aluminate solution using area normalization method.
Water used in above embodiments is the ultrapure water that resistivity is 18.3M Ω .cm.
Claims (7)
1. the morphological analysis method of organic matter in a kind of sodium aluminate solution, which comprises the steps of:
(1) solution extract: take sodium aluminate solution to be placed in separatory funnel A, be diluted with water, then rocked when concentrated hydrochloric acid is added dropwise to
Have white precipitate precipitation, then side be added dropwise the commercially available concentrated hydrochloric acid that 500ml mass fraction is 37% be diluted with water to it is obtained dilute after 1L
Precipitating dissolution is rocked into solution completely in hydrochloric acid side, is rinsed with water separatory funnel inner wall；Then positive fourth is added into separatory funnel A
Lower layer's solution is put into separatory funnel B after stratification, n-butanol is added into separatory funnel B, then shake by alcohol, oscillation extraction
Extraction is swung, the upper solution in separatory funnel A and separatory funnel B is taken out mixing to get extract liquor by stratification；
(2) extract liquor is esterified: dilute hydrochloric acid is added into extract liquor made from step (1), is esterified；Then solution is moved into liquid separation leakage
It struggles against in C, is rinsed with water flask inner wall, washing lotion is incorporated to separatory funnel C, releases lower layer's solution after solution left standstill layering, then use
Water rinses separatory funnel C inner wall and releases lower part solution to stratification after shaking up, and the upper solution in separatory funnel C is taken
Out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rocks to solution and is sufficiently mixed, it is quiet
It postpones and shakes up again, repetition shakes up-stands at least 3 times, is then allowed to stand at least 12 hours, finally shakes up the solution after standing
Natural filtration is carried out to get dehydration test sample；
(4) GC/MS is analyzed: dehydration test sample obtained in step (3) is tested and analyzed using gas chromatography mass spectrometer,
Analysis result can be measured to the degree of each organic matter component in sodium aluminate solution using area normalization method；The detection
It is as follows to analyze operating condition: chromatographic column: -95% dimethyl arlydene silicone copolymers of Agilent HP-5MS-5% diphenyl；
Quartz capillary column: 30mm*0.25mm*0.25mm；Column flow: 1mL/min；Injector temperature: 250 DEG C；Temperature programming: column temperature
50℃-1min-10℃/min-220℃-1min-5℃/min-315℃-2min；Split ratio: it does not shunt；Sample volume: 1uL；It carries
Gas: 99.999% high-pure helium；Ionization mode: EI；Electron energy: 70eV；Emission current: 100mA；Ion source temperature: 230 DEG C；Matter
Measure scanning range: 30-350m/z；Retrieve mass spectral database: U.S. NIST Library.
2. the morphological analysis method of organic matter in sodium aluminate solution according to claim 1, which is characterized in that including as follows
Step:
(1) solution extract: take sodium aluminate solution to be placed in separatory funnel A, be diluted with water, then rocked when concentrated hydrochloric acid is added dropwise to
Have white precipitate precipitation, then side be added dropwise the commercially available concentrated hydrochloric acid that 500ml mass fraction is 37% be diluted with water to it is obtained dilute after 1L
Precipitating dissolution is rocked into solution completely in hydrochloric acid side, is rinsed with water separatory funnel inner wall；Then positive fourth is added into separatory funnel A
Lower layer's solution oscillation extraction 5 minutes or more, is put into separatory funnel B after stratification, is added just into separatory funnel B by alcohol
Butanol, then oscillation extraction 5 minutes or more, the upper solution in separatory funnel A and separatory funnel B is taken out mixing by stratification,
Up to extract liquor；
(2) extract liquor is esterified: dilute hydrochloric acid is added into extract liquor made from step (1), esterification is carried out at 70-90 DEG C
40-60 hours；Then solution being moved into separatory funnel C, is rinsed with water flask inner wall 1-2 times, washing lotion is incorporated to separatory funnel C,
Lower layer's solution is released after solution left standstill layering, is then rinsed with water separatory funnel C inner wall 1 time, it, will to stratification after shaking up
Lower part solution is released, and the upper solution in separatory funnel C is taken out to get esterifying liquid；
(3) it is esterified fluid dewatering: anhydrous magnesium sulfate is added into esterifying liquid made from step (2), rocks to solution and is sufficiently mixed, it is quiet
Shaken up again after setting at least 1 hour, at least 3 times repeatedly, be then allowed to stand at least 12 hours, finally by the solution after standing shake up into
Row natural filtration is to get dehydration test sample；
(4) GC/MS is analyzed: being analyzed using GC/MS analysis method described in claim 1 step (4).
3. the morphological analysis method of organic matter in sodium aluminate solution according to claim 2, it is characterised in that: the step
(1) in, the oscillation extraction time is 10 minutes.
4. the morphological analysis method of organic matter in sodium aluminate solution according to claim 2, it is characterised in that: the step
(2) in, dilute hydrochloric acid refers to that molar concentration is the hydrochloric acid of 8mol/L.
5. the morphological analysis method of organic matter in sodium aluminate solution according to claim 2, it is characterised in that: the step
(2) in, esterification temperature is 80 DEG C, and esterification time is 48 hours.
6. the morphological analysis method of organic matter in sodium aluminate solution according to claim 2, it is characterised in that: the step
(3) in, anhydrous magnesium sulfate is added in esterifying liquid, rocks to solution after being sufficiently mixed, 1 hour need to be stood, then shaken up again, instead
It is 3 times multiple, it is then allowed to stand 12 hours.
7. the morphological analysis method of organic matter in sodium aluminate solution according to claim 2, it is characterised in that: the method
Used in water be resistivity be 18.3 M Ω .cm ultrapure water.
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| CN106093019A (en) * | 2016-05-31 | 2016-11-09 | 贵州大学 | A kind of method analyzing content of organics in sodium aluminate solution |
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2016
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|---|---|---|---|---|
| US3899571A (en) * | 1972-12-06 | 1975-08-12 | Sumitomo Chemical Co | Method for the removal of organic substances from sodium aluminate solution |
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