CN110455981A - The measuring method of total alumina content in a kind of water treatment agent polyaluminium chloride - Google Patents
The measuring method of total alumina content in a kind of water treatment agent polyaluminium chloride Download PDFInfo
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- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 title claims abstract description 53
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 49
- 238000000034 method Methods 0.000 title claims abstract description 46
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 20
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 title claims abstract description 13
- KCXVZYZYPLLWCC-UHFFFAOYSA-N EDTA Chemical compound OC(=O)CN(CC(O)=O)CCN(CC(O)=O)CC(O)=O KCXVZYZYPLLWCC-UHFFFAOYSA-N 0.000 claims abstract description 20
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 34
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 18
- 239000012086 standard solution Substances 0.000 claims description 16
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 15
- 239000011701 zinc Substances 0.000 claims description 14
- 229910052725 zinc Inorganic materials 0.000 claims description 14
- 239000007853 buffer solution Substances 0.000 claims description 11
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000003995 emulsifying agent Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 9
- 239000000243 solution Substances 0.000 claims description 9
- 238000001354 calcination Methods 0.000 claims description 8
- ORZHVTYKPFFVMG-UHFFFAOYSA-N xylenol orange Chemical compound OC(=O)CN(CC(O)=O)CC1=C(O)C(C)=CC(C2(C3=CC=CC=C3S(=O)(=O)O2)C=2C=C(CN(CC(O)=O)CC(O)=O)C(O)=C(C)C=2)=C1 ORZHVTYKPFFVMG-UHFFFAOYSA-N 0.000 claims description 8
- 239000011521 glass Substances 0.000 claims description 7
- 239000000155 melt Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 5
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 238000011017 operating method Methods 0.000 claims description 4
- 229910052709 silver Inorganic materials 0.000 claims description 4
- 239000004332 silver Substances 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 3
- 239000004677 Nylon Substances 0.000 claims description 3
- 229910019142 PO4 Inorganic materials 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 239000012153 distilled water Substances 0.000 claims description 3
- 238000002844 melting Methods 0.000 claims description 3
- 230000008018 melting Effects 0.000 claims description 3
- 239000004570 mortar (masonry) Substances 0.000 claims description 3
- 229920001778 nylon Polymers 0.000 claims description 3
- 239000010452 phosphate Substances 0.000 claims description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 3
- 238000002604 ultrasonography Methods 0.000 claims description 3
- 229920002554 vinyl polymer Polymers 0.000 claims description 3
- 238000005070 sampling Methods 0.000 claims description 2
- 238000003892 spreading Methods 0.000 claims description 2
- 238000010926 purge Methods 0.000 claims 2
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims 1
- 238000004945 emulsification Methods 0.000 claims 1
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims 1
- 239000007974 sodium acetate buffer Substances 0.000 claims 1
- BHZOKUMUHVTPBX-UHFFFAOYSA-M sodium acetic acid acetate Chemical compound [Na+].CC(O)=O.CC([O-])=O BHZOKUMUHVTPBX-UHFFFAOYSA-M 0.000 claims 1
- 229910052782 aluminium Inorganic materials 0.000 abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 abstract description 11
- 239000004411 aluminium Substances 0.000 abstract description 10
- 239000003513 alkali Substances 0.000 abstract description 7
- 238000004448 titration Methods 0.000 abstract description 6
- -1 EDTA zinc salt Chemical class 0.000 abstract description 4
- 238000001914 filtration Methods 0.000 abstract description 3
- 239000012535 impurity Substances 0.000 abstract description 3
- 238000012360 testing method Methods 0.000 abstract description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 abstract description 2
- 230000000536 complexating effect Effects 0.000 abstract description 2
- 238000001514 detection method Methods 0.000 abstract description 2
- 230000004927 fusion Effects 0.000 abstract description 2
- 229910052751 metal Inorganic materials 0.000 abstract description 2
- 239000002184 metal Substances 0.000 abstract description 2
- 230000001376 precipitating effect Effects 0.000 abstract description 2
- 238000011084 recovery Methods 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 abstract description 2
- 229910052708 sodium Inorganic materials 0.000 abstract description 2
- 150000003751 zinc Chemical class 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 abstract 1
- 239000002585 base Substances 0.000 description 10
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 4
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- 238000001816 cooling Methods 0.000 description 3
- 238000004090 dissolution Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- 239000007788 liquid Substances 0.000 description 3
- 229910052759 nickel Inorganic materials 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical group [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000005259 measurement Methods 0.000 description 2
- 229910001388 sodium aluminate Inorganic materials 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910020264 Na2TiO3 Inorganic materials 0.000 description 1
- 239000004698 Polyethylene Substances 0.000 description 1
- 229910020453 SiO2+2NaOH Inorganic materials 0.000 description 1
- VMHLLURERBWHNL-UHFFFAOYSA-M Sodium acetate Chemical compound [Na+].CC([O-])=O VMHLLURERBWHNL-UHFFFAOYSA-M 0.000 description 1
- 241001062472 Stokellia anisodon Species 0.000 description 1
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 238000004364 calculation method Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000002242 deionisation method Methods 0.000 description 1
- 239000002019 doping agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000005518 electrochemistry Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- FLTRNWIFKITPIO-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe] FLTRNWIFKITPIO-UHFFFAOYSA-N 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide Inorganic materials 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 238000010309 melting process Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920000573 polyethylene Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 239000001632 sodium acetate Substances 0.000 description 1
- 235000017281 sodium acetate Nutrition 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229910052911 sodium silicate Inorganic materials 0.000 description 1
- 241000894007 species Species 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000000967 suction filtration Methods 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- 239000004408 titanium dioxide Substances 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N31/00—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods
- G01N31/16—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using titration
Landscapes
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Molecular Biology (AREA)
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
Abstract
The present invention provides a kind of measuring methods of alumina content total in water treatment agent polyaluminium chloride, and sample is used alkali fusion at high temperature, and aluminium is made to generate sodium metaaluminate soluble easily in water, and common metal impurity generates hydroxide precipitating, and by filtering removal；Since aluminium and EDTA complexing be not complete, then excess EDTA is added using zinc salt back titration and is sufficiently complexed with aluminium, remaining EDTA zinc salt residual titration acquires alumina content by calculating.Measuring method of the invention, reproducibility is high, and precision is good, and accuracy is high, and testing cost is low, and detection speed is fast and easily operated, and recovery of standard addition is between 98%-102%.
Description
Technical field
The invention belongs to total aluminium oxide in chemical analysis technology field more particularly to a kind of water treatment agent polyaluminium chloride
The measuring method of content.
Background technique
Water treatment agent is a kind of water-soluble inorganic high molecular polymer, with electrochemistry, cohesion, suction during dissolution
Echo precipitating etc. physicochemical changes, floccule body formed it is fast and coarse, cause analyze result preci-sion and accuracy it is poor.Water process
For agent aluminium polychloride iron product since dopant species are excessive, PAFC system is complicated, and disturbing factor is more, it is therefore desirable to its feature
Parameter aluminium oxide is furtherd investigate, to determine the feasibility of method.
Currently, the usual actual total content of aluminium oxide is up to standard, but test specimens in the water treatment agent polyaluminium chloride of production
Due to preparation process difference when product, aluminum feedstock source is different, and long-distance transport, permanent storage make the originals such as properties of product variation
Cause is not achieved the variation of water solubility existing for national standard, especially principal component aluminium oxide, causes its assay result seriously inclined
Low, poor accuracy.
Summary of the invention
The technical problem to be solved by the present invention is to overcome the shortcomings of to mention in background above technology and defect, provide one
The measuring method of total alumina content in kind water treatment agent polyaluminium chloride.
In order to solve the above technical problems, technical solution proposed by the present invention are as follows:
The measuring method of total alumina content in a kind of water treatment agent polyaluminium chloride, comprising the following steps:
(1) to water treatment agent polyaluminium chloride random sampling to be checked, take 0.2000-0.5000g sample spare；It will examination
Sample and 2-3g mixed base are added in crucible, then instill 2-5 drop pure water, and low-temperature heat avoids lye from splashing, and starts to melt to sample
It heats up again, melts sample completely, crucible is then placed in calcination in Muffle furnace, it is ensured that sample decomposes completely, takes out after calcination
Crucible simultaneously rotates, and is adhered to melt on sidewall of crucible；The melt being adhered on sidewall of crucible is purged in volumetric flask with hot water, is shaken
Even constant volume, is filtered, make solution and insoluble matter quickly, efficiently separate；
(2) 25ml sample is pipetted in conical flask, and the EDTA that 25ml concentration is 0.0500mol/L is added and (uses benchmark EDTA
Prepare), 2-3 drop xylenol orange phthalein indicator is added, is adjusted to yellow with hydrochloric acid, is adjusted to red with sodium hydroxide solution, use is dilute
Hydrochloric acid is adjusted to yellow, and (aluminium ion has sealing process to indicator such as xylenol orange, and xylenol orange is often made into 0.2% as indicator
Aqueous solution use, when pH > 6.3, present red；When pH < 6.3, yellow is presented；When pH=pka=6.3, intermediate face is presented
Color), then be added 5-10mL buffer solution adjust pH value, add 2-4 drop emulsifier, shake up, boil, cool down after add 2- again
3 drop xylenol orange phthalein indicators and 5-10ml buffer solution, so that the pH value of strict control solution is in OK range, it is ensured that network
It closes sufficiently, being titrated to blush with the Zinc standard solution of 0.05mol/L is terminal, the volume of the Zinc standard solution consumed；
(3) content of total aluminium oxide is calculated.
Above-mentioned measuring method, it is preferred that in the step (3), the calculation formula of the content of total aluminium oxide such as formula (1) institute
Show:
---indicates Al in formula: W2O3Percentage composition, %；
C1 ---indicates the concentration of EDTA standard solution, mol/L；
C2 ---indicates the concentration of Zinc standard solution, mol/L；
V1 ---indicates the volume of EDTA standard solution, ml；
V2 ---indicates the volume of Zinc standard solution, ml；
W ---indicates the percentage composition of PAC/PAFC, %；
M ---expression weighs sample mass, g；
0.05098 ---indicates 1/2 aluminium oxide mM quality.
Conventional method demarcates zinc by preparing mark EDTA titer, and calibration process is cumbersome, is easy error, and the present invention uses
The direct configuration standard liquid of benchmark EDTA, can effectively reduce error.
Above-mentioned measuring method, it is preferred that in the step (1), the method for sample and mixed base is added in silver crucible
Including operating procedure in detail below: first uniformly spreading in crucible bottom into 0.5-1g mixed base, whole samples are then covered on paving
On good mixed base, then the remaining mixed base of uniform fold on sample.The prior art is often when weighing directly by sample
It mixes, and is stirred evenly with polyethylene stick, or sample and alkali are added separately in crucible with alkali, these addition manners all can not
With degree influence the measurement of alumina content.And addition manner of the invention, it effectively prevents sample and sinks to bottom or float on
Loss caused by reacting incomplete caused by lye surface and being adhered on mixing tool, ensure that subsequent oxidation aluminium content measures
Accuracy.
Above-mentioned measuring method, it is preferred that the mixed base is the mixture of sodium hydroxide and potassium hydroxide.With single alkali
It compares, the melting effect for the mixed base that the present invention selects is more preferable, and smelt flow is bigger, is adhered to convenient for the melt in crucible
On sidewall of crucible.The present invention can eliminate the huge sum of money such as main chaff interferent iron and copper, manganese, magnesium, tin, chromium, nickel by the way that flux alkali is added
The interference of category, without taking other physically or chemically means again.
Above-mentioned measuring method, it is preferred that the crucible is silver crucible or nickel crucible.
Above-mentioned measuring method, it is preferred that in the step (2), emulsifier be OP emulsifier, the OP emulsifier be by
Ammonium alcohol polyvinyl phosphate and water are prepared to obtain according to volume ratio for 2-4:50.Aluminium ion hydrolysis can generate a series of multicore hydroxys
Complex compound, the present invention are used as sensitizer by the way that OP emulsifier is added, further eliminate and interfere, and effectively increase each interionic connect
Contacting surface promotes aluminium ion to be complexed rapidly and is complexed completely, increases the stability of complex compound, increase the acumen of titration end-point
Property.
Above-mentioned measuring method, it is preferred that in the step (1), heating rate is 50 DEG C/30min, and the temperature of calcination is
750 DEG C, time 30min.
Above-mentioned measuring method, it is preferred that in the step (1), water treatment agent polyaluminium chloride to be checked is placed in
It is ground in agate mortar, all crosses 100 mesh nylon mesh.
Above-mentioned measuring method, it is preferred that in the step (2), buffer solution is NaAc_HAc buffer solution, is added
Enter buffer solution and pH value is adjusted to 5.4-5.6.
Above-mentioned measuring method, it is preferred that in the step (2), the volume fraction of hydrochloric acid is 50%, sodium hydroxide solution
Mass fraction is 1%, and the volume fraction of dilute hydrochloric acid is 10%.
Above-mentioned measuring method, it is preferred that in the step (1), in order to guarantee sample clean up and shift completely, use
The melt being adhered on sidewall of crucible is purged the method in volumetric flask and includes operating procedure in detail below by hot water: clear with distilled water
Crucible outer wall is washed, hot water is added in crucible, crucible is directly put into ultrasonic cleaning motor spindle, or crucible is put into glass and is burnt
In cup, then glass beaker is put into ultrasonic cleaning motor spindle, is added in supersonic cleaning machine and is no more than 2/3 height water of crucible height
Booting ultrasound 10 minutes, fusant is washed in volumetric flask.
The method of total alumina content is mainly based upon following principle in analysis water treatment agent of the invention:
Sample is used into alkali fusion at high temperature, aluminium is made to generate sodium metaaluminate soluble easily in water, and common metal impurity generates hydrogen
Oxide precipitation, and by filtering removal；Excess EDTA is added since aluminium and EDTA complexing be not complete, then using zinc salt back titration
It is sufficiently complexed with aluminium, remaining EDTA zinc salt residual titration, acquires alumina content by calculating.
The reaction equation of main chemical reaction involved in melting process is following (by taking alkali is sodium hydroxide as an example):
(1) aluminium oxide: Al2O3·nH2O+2NaOH→2NaAlO2+nH2O；
(2) silica: SiO2+2NaOH→Na2SiO3+H2O；
(3) iron oxide: the Fe of dissolution2O3It is not reacted with NaOH, iron ion and hydroxyl, which generate, in sample precipitates: Fe3++OH
→Fe(OH)3；
(4) titanium dioxide: TiO2+ 2NaOH=Na2TiO3+H2O；
(5) carbonate: mainly there is CaCO3+2NaOH→Na2CO3+Ca(OH)2；
MgCO3+2NaOH→Na2CO3+Mg(OH)2。
The reaction equation of main chemical reaction involved in titration process is as follows:
HCl+NaAlO2+H2O=NaCl+Al (OH)3；
4HCl+NaAlO2=AlCl3+NaACl+2H2O；
Al3++ Y=AlY (Y indicates EDTA).
Compared with the prior art, the advantages of the present invention are as follows:
Measuring method of the invention, reproducibility is high, and precision is good, and accuracy is high, and testing cost is low, and detection speed is fast, and
Easily operated, recovery of standard addition is between 98%-102%.
Measuring method of the invention is suitable for analysis and measures various technique such as plate and frame type filter-press filter press techniques, natural subsidence
Total alumina content in the water treatment agent of the productions such as method, can analyze the aluminium for determining various forms in sample, including α and β etc.
The aluminium of form can be used for the alumina content in measurement water treatment agent aluminium chloride.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is the present invention
Some embodiments for those of ordinary skill in the art without creative efforts, can also basis
These attached drawings obtain other attached drawings.
Fig. 1 is that step (3) uses the photo for filtering device progress dry tap filter in the embodiment of the present invention 1.
Specific embodiment
To facilitate the understanding of the present invention, invention herein is done below in conjunction with Figure of description and preferred embodiment more complete
Face meticulously describes, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter are generally understood meaning phase with those skilled in the art
Together.Technical term used herein is intended merely to the purpose of description specific embodiment, and it is of the invention to be not intended to limitation
Protection scope.
Unless otherwise specified, various raw material, reagent, the instrument and equipment etc. used in the present invention can pass through city
Field is commercially available or can be prepared by existing method.
Embodiment 1:
The measuring method of total alumina content in a kind of water treatment agent polyaluminium chloride of the invention, including following step
It is rapid:
(1) 0.0500mol/l EDTA standard liquid is configured with benchmark EDTA: claiming 18.625 grams of EDTA, it is soluble in water, it is settled to
In 1000ml volumetric flask, shake up；
(2) it prepares 0.0500mol/l zinc standard liquid: claiming 3.2685 grams of arsenic-free zinc granules, 1:1 hydrochloric acid 35ml, cap upper surface is added
Ware, micro- heating, dissolution cooling are settled in 1000ml volumetric flask, shake up；
(3) water treatment agent polyaluminium chloride to be checked is placed in agate mortar and is ground, all cross 100 mesh nylon mesh,
It is spare that 0.5000g sample is weighed with difference assay；Nickel crucible or silver crucible bottom uniformly spread into 0.7g mixed base (sodium hydroxide and
The mixture of potassium hydroxide), then 0.5000g sample is covered on the mixed base completed, then uniform fold is surplus on sample
2 drop pure water are added in remaining 1.4g mixed base, in low-temperature heat on electric furnace, start melting to sample and are gradually warmed up, every half an hour
50 DEG C are risen, to sample whole melt stability, crucible is placed in 750 DEG C of Muffle furnaces calcination 30 minutes, calcination is taken out crucible and turned
Melt is adhered on sidewall of crucible by dynamic crucible, cooling, washes away impurity outside crucible with distilled water, and 30ml hot water is added in crucible,
Crucible is directly put into ultrasonic cleaning motor spindle, or crucible is put into 250ml glass beaker, then glass beaker is put into super
Sound cleans motor spindle, is added in supersonic cleaning machine and is no more than the booting of 2/3 height water of crucible height ultrasound 10 minutes, reusable heat water
Fusant is purged in 100ml volumetric flask, constant volume is shaken up, carries out dry tap filter (as shown in Figure 1) with Suction filtration device, filtrate is not necessarily to
It has filtered entirely, has had 30-50ml sample that can divide and take 25ml for analyzing；
(4) 25ml sample is pipetted in conical flask, and the EDTA that 25ml concentration is 0.0500mol/L, 25ml deionization is added
2-3 drop xylenol orange phthalein indicator is added in water, is adjusted to yellow with the hydrochloric acid that volume fraction is 50%, is 1% with mass fraction
Sodium hydroxide is adjusted to red, is adjusted to yellow with the dilute hydrochloric acid that volume fraction is 10%, 10ml NaAc_HAc buffer solution is added
(the 46g sodium acetate weighed up and 5.7mL glacial acetic acid are dissolved in 1000mL water and obtained), control solution ph are 5.5, are added
2 drop OP emulsifiers (are prepared to obtain) according to volume ratio by ammonium alcohol polyvinyl phosphate and water for 3:50, shake up, boil, flowing water cooling
2 drop xylenol orange phthalein indicators and 10ml NaAc_HAc buffer solution are added again afterwards, with the quasi- solution of the zinc of 0.0500mol/L
Being titrated to blush is terminal, and the volume of the zinc titer of consumption is 13.5ml；
4, the content of total aluminium oxide is calculated:
---indicates Al in formula: W2O3Percentage composition, %；
C1 ---indicates the concentration of EDTA standard solution, mol/L；
C2 ---indicates the concentration of Zinc standard solution, mol/L；
V1 ---indicates the volume of EDTA standard solution, ml；
V2 ---indicates the volume of Zinc standard solution, ml；
W ---indicates the percentage composition of PAC/PAFC, %；
M ---expression weighs sample mass, g；
0.05098 ---indicates 1/2 aluminium oxide mM quality.
Claims (10)
1. the measuring method of total alumina content in a kind of water treatment agent polyaluminium chloride, which is characterized in that including following step
It is rapid:
(1) to water treatment agent polyaluminium chloride random sampling to be checked, take 0.2000-0.5000g sample spare；By sample and
2-3g mixed base is added in crucible, then instills 2-5 drop pure water, and heating starts melting to sample and heats up again, melts sample completely
Afterwards, crucible is then placed in calcination in Muffle furnace, crucible is taken out after calcination and rotated, be adhered to melt on sidewall of crucible；With heat
Water purges the melt being adhered on sidewall of crucible in volumetric flask, shakes up constant volume, is filtered；
(2) 25ml sample is pipetted in conical flask, and the EDTA for accurately pipetting that 25ml or 50ml concentration is 0.0500mol/L is added,
2-3 drop xylenol orange phthalein indicator is added, yellow is adjusted to hydrochloric acid, is adjusted to red with sodium hydroxide solution, with dilute hydrochloric acid tune
To yellow, 5-10mL buffer solution is then added and adjusts pH value, adds 2-4 drop emulsifier, shake up, boil, cool down after mend again
Add 2-3 drop xylenol orange phthalein indicator 5-10ml buffer solution, being titrated to blush with the Zinc standard solution of 0.0500mol/L is
Terminal, the volume of the Zinc standard solution consumed；
(3) content of total aluminium oxide is calculated.
2. measuring method according to claim 1, which is characterized in that in the step (3), the meter of the content of total aluminium oxide
It calculates shown in formula such as formula (1):
---indicates Al in formula: W2O3Percentage composition, %；
C1 ---indicates the concentration of EDTA standard solution, mol/L；
C2 ---indicates the concentration of Zinc standard solution, mol/L；
V1 ---indicates the volume of EDTA standard solution, ml；
V2 ---indicates the volume of Zinc standard solution, ml；
W ---indicates the percentage composition of PAC/PAFC, %；
M ---expression weighs sample mass, g；
0.05098 ---indicates 1/2 aluminium oxide mM quality.
3. measuring method according to claim 1 or 2, which is characterized in that in the step (1), be added in silver crucible
The method of sample and mixed base includes operating procedure in detail below: first uniformly spreading into 0.5-1g mixed base, then in crucible bottom
Whole samples are covered on the mixed base completed, then the remaining mixed base of uniform fold on sample.
4. measuring method according to claim 3, which is characterized in that the mixed base is sodium hydroxide and potassium hydroxide
Mixture.
5. measuring method according to claim 1 or 2, which is characterized in that in the step (2), emulsifier is OP emulsification
Agent, the OP emulsifier are to prepare to obtain for 2-4:50 according to volume ratio by ammonium alcohol polyvinyl phosphate and water.
6. measuring method according to claim 1 or 2, which is characterized in that in the step (1), heating rate be 50 DEG C/
30min, the temperature of calcination are 750 DEG C, time 30min.
7. measuring method according to claim 1 or 2, which is characterized in that in the step (1), by water process to be checked
Agent polyaluminum ferric chloride, which is placed in agate mortar, grinds, and all crosses 100 mesh nylon mesh.
8. measuring method according to claim 1 or 2, which is characterized in that in the step (2), buffer solution is acetic acid-
Sodium acetate buffer is added buffer solution for pH value and is adjusted to 5.4-5.6.
9. measuring method according to claim 1 or 2, which is characterized in that in the step (2), the volume fraction of hydrochloric acid
It is 50%, the mass fraction of sodium hydroxide solution is 1%, and the volume fraction of dilute hydrochloric acid is 10%.
10. measuring method according to claim 1 or 2, which is characterized in that in the step (1), will be adhered to hot water
Melt on sidewall of crucible purges the method in volumetric flask and includes operating procedure in detail below: crucible outer wall wash with distilled water,
Hot water is added in crucible, crucible is directly put into ultrasonic cleaning motor spindle, or crucible is put into glass beaker, then by glass
Glass beaker is put into ultrasonic cleaning motor spindle, is added in supersonic cleaning machine and is no more than 2/3 height water of crucible height booting ultrasound 10
Minute, fusant is washed in volumetric flask.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN116754711A (en) * | 2023-08-17 | 2023-09-15 | 蓝星安迪苏南京有限公司 | Emulsifying capacity evaluation method of emulsifier for feed |
| CN117330700A (en) * | 2023-09-15 | 2024-01-02 | 凯盛君恒(蚌埠)有限公司 | Method for continuously detecting content of barium oxide and aluminum oxide in borosilicate glass tube |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226799A (en) * | 2011-06-13 | 2011-10-26 | 大冶特殊钢股份有限公司 | Detection method capable of eliminating interference in Al2O3 analysis process of metallurgy refractory |
| CN103105396A (en) * | 2012-03-06 | 2013-05-15 | 云南磷化集团有限公司 | Method for determining alumina content in iron ore |
| CN103868911A (en) * | 2014-04-03 | 2014-06-18 | 河南科技学院 | Method for dissolving aluminum oxide and determining trace metal elements in aluminum oxide |
| CN104133036A (en) * | 2014-07-31 | 2014-11-05 | 中国冶金地质总局山东局测试中心 | Analysis determining method for aluminium oxide in bauxite |
| CN106290352A (en) * | 2016-08-23 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of aluminium sesquioxide content in carbide slag |
-
2019
- 2019-08-09 CN CN201910736229.4A patent/CN110455981A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102226799A (en) * | 2011-06-13 | 2011-10-26 | 大冶特殊钢股份有限公司 | Detection method capable of eliminating interference in Al2O3 analysis process of metallurgy refractory |
| CN103105396A (en) * | 2012-03-06 | 2013-05-15 | 云南磷化集团有限公司 | Method for determining alumina content in iron ore |
| CN103868911A (en) * | 2014-04-03 | 2014-06-18 | 河南科技学院 | Method for dissolving aluminum oxide and determining trace metal elements in aluminum oxide |
| CN104133036A (en) * | 2014-07-31 | 2014-11-05 | 中国冶金地质总局山东局测试中心 | Analysis determining method for aluminium oxide in bauxite |
| CN106290352A (en) * | 2016-08-23 | 2017-01-04 | 内蒙古包钢钢联股份有限公司 | A kind of assay method of aluminium sesquioxide content in carbide slag |
Non-Patent Citations (4)
| Title |
|---|
| 中国国家标准汇编: "《中华人民共和国国家标准 GB15892-2003》", 31 December 2004, 中国国家出版社 * |
| 张伟超: "石灰石、白云石中氧化铝的快速测定", 《冶金丛刊》 * |
| 潘祖亭 等: "《分析化学》", 31 August 2011, 华中科技大学出版社 * |
| 谢炜平: "《环境监测实训指导》", 31 January 2015, 中国环境出版社.北京 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111521467A (en) * | 2020-06-04 | 2020-08-11 | 河北省地质实验测试中心 | Graphite detection method |
| CN111521467B (en) * | 2020-06-04 | 2023-08-29 | 河北省地质实验测试中心 | Graphite detection method |
| CN116754711A (en) * | 2023-08-17 | 2023-09-15 | 蓝星安迪苏南京有限公司 | Emulsifying capacity evaluation method of emulsifier for feed |
| CN116754711B (en) * | 2023-08-17 | 2023-11-07 | 蓝星安迪苏南京有限公司 | Emulsifying capacity evaluation method of emulsifier for feed |
| CN117330700A (en) * | 2023-09-15 | 2024-01-02 | 凯盛君恒(蚌埠)有限公司 | Method for continuously detecting content of barium oxide and aluminum oxide in borosilicate glass tube |
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