CN106645561B - A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution - Google Patents
A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution Download PDFInfo
- Publication number
- CN106645561B CN106645561B CN201710135211.XA CN201710135211A CN106645561B CN 106645561 B CN106645561 B CN 106645561B CN 201710135211 A CN201710135211 A CN 201710135211A CN 106645561 B CN106645561 B CN 106645561B
- Authority
- CN
- China
- Prior art keywords
- solution
- content
- magnesium
- calcium
- ion
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- JLVVSXFLKOJNIY-UHFFFAOYSA-N Magnesium ion Chemical compound [Mg+2] JLVVSXFLKOJNIY-UHFFFAOYSA-N 0.000 title claims abstract description 51
- 229910001425 magnesium ion Inorganic materials 0.000 title claims abstract description 51
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 title claims abstract description 44
- 229910001424 calcium ion Inorganic materials 0.000 title claims abstract description 44
- 238000000034 method Methods 0.000 title claims abstract description 37
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 32
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 16
- 238000005259 measurement Methods 0.000 title claims abstract description 16
- 239000000243 solution Substances 0.000 claims abstract description 92
- 239000002253 acid Substances 0.000 claims abstract description 21
- 239000012086 standard solution Substances 0.000 claims abstract description 18
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 claims abstract description 14
- 229910052804 chromium Inorganic materials 0.000 claims abstract description 14
- 239000011651 chromium Substances 0.000 claims abstract description 14
- 239000003109 Disodium ethylene diamine tetraacetate Substances 0.000 claims abstract description 13
- 239000007853 buffer solution Substances 0.000 claims abstract description 13
- 235000019301 disodium ethylene diamine tetraacetate Nutrition 0.000 claims abstract description 13
- 239000007986 glycine-NaOH buffer Substances 0.000 claims abstract description 6
- -1 ethylene glycol diethyl ether diammonium Chemical compound 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 52
- 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 description 25
- 239000007788 liquid Substances 0.000 claims description 20
- 238000004448 titration Methods 0.000 claims description 6
- 235000009508 confectionery Nutrition 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- DHMQDGOQFOQNFH-UHFFFAOYSA-N Glycine Chemical compound NCC(O)=O DHMQDGOQFOQNFH-UHFFFAOYSA-N 0.000 claims description 4
- 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 claims description 4
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 4
- 239000011734 sodium Substances 0.000 claims description 4
- 229910052708 sodium Inorganic materials 0.000 claims description 4
- QBZIEGUIYWGBMY-FUZXWUMZSA-N (5Z)-5-hydroxyimino-6-oxonaphthalene-2-sulfonic acid iron Chemical compound [Fe].O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O.O\N=C1/C(=O)C=Cc2cc(ccc12)S(O)(=O)=O QBZIEGUIYWGBMY-FUZXWUMZSA-N 0.000 claims description 2
- 239000004471 Glycine Substances 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000004570 mortar (masonry) Substances 0.000 claims description 2
- 239000001103 potassium chloride Substances 0.000 claims description 2
- 235000011164 potassium chloride Nutrition 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 4
- 229910021529 ammonia Inorganic materials 0.000 claims 2
- 229960001484 edetic acid Drugs 0.000 claims 1
- XHCCWBJFZUXJBV-UHFFFAOYSA-K trisodium 2-[(2-oxido-5-sulfophenyl)diazenyl]-3,6-disulfonaphthalene-1,8-diolate Chemical compound C1=CC(=C(C=C1S(=O)(=O)O)N=NC2=C(C3=C(C=C(C=C3C=C2S(=O)(=O)O)S(=O)(=O)O)[O-])[O-])[O-].[Na+].[Na+].[Na+] XHCCWBJFZUXJBV-UHFFFAOYSA-K 0.000 claims 1
- 229910019142 PO4 Inorganic materials 0.000 abstract description 8
- 239000010452 phosphate Substances 0.000 abstract description 8
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 abstract description 4
- AFDBFFXBFLGWHB-UHFFFAOYSA-N azane ethoxyethane Chemical compound N.N.CCOCC AFDBFFXBFLGWHB-UHFFFAOYSA-N 0.000 abstract description 2
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 abstract description 2
- ZGTMUACCHSMWAC-UHFFFAOYSA-L EDTA disodium salt (anhydrous) Chemical compound [Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC(O)=O)CC([O-])=O ZGTMUACCHSMWAC-UHFFFAOYSA-L 0.000 abstract 2
- 229940071106 ethylenediaminetetraacetate Drugs 0.000 description 13
- 238000012360 testing method Methods 0.000 description 8
- 238000004458 analytical method Methods 0.000 description 7
- 239000011575 calcium Substances 0.000 description 7
- 238000001514 detection method Methods 0.000 description 7
- 239000011777 magnesium Substances 0.000 description 6
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 5
- 229910052791 calcium Inorganic materials 0.000 description 5
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 4
- 229910052749 magnesium Inorganic materials 0.000 description 4
- 229910052760 oxygen Inorganic materials 0.000 description 4
- KUQNVBOOZFTKOW-ILKKLZGPSA-M [OH-].[Na+].C(CC)N[C@@H](CCO)C(=O)O Chemical compound [OH-].[Na+].C(CC)N[C@@H](CCO)C(=O)O KUQNVBOOZFTKOW-ILKKLZGPSA-M 0.000 description 3
- 239000002585 base Substances 0.000 description 3
- BRPQOXSCLDDYGP-UHFFFAOYSA-N calcium oxide Chemical compound [O-2].[Ca+2] BRPQOXSCLDDYGP-UHFFFAOYSA-N 0.000 description 3
- 239000000292 calcium oxide Substances 0.000 description 3
- ODINCKMPIJJUCX-UHFFFAOYSA-N calcium oxide Inorganic materials [Ca]=O ODINCKMPIJJUCX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 229940079593 drug Drugs 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- DEFVIWRASFVYLL-UHFFFAOYSA-N ethylene glycol bis(2-aminoethyl)tetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)CCOCCOCCN(CC(O)=O)CC(O)=O DEFVIWRASFVYLL-UHFFFAOYSA-N 0.000 description 3
- 239000001301 oxygen Substances 0.000 description 3
- CPLXHLVBOLITMK-UHFFFAOYSA-N Magnesium oxide Chemical compound [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 2
- ZRBROGSAUIUIJE-UHFFFAOYSA-N azanium;azane;chloride Chemical compound N.[NH4+].[Cl-] ZRBROGSAUIUIJE-UHFFFAOYSA-N 0.000 description 2
- ZFXVRMSLJDYJCH-UHFFFAOYSA-N calcium magnesium Chemical compound [Mg].[Ca] ZFXVRMSLJDYJCH-UHFFFAOYSA-N 0.000 description 2
- KMQAPZBMEMMKSS-UHFFFAOYSA-K calcium;magnesium;phosphate Chemical compound [Mg+2].[Ca+2].[O-]P([O-])([O-])=O KMQAPZBMEMMKSS-UHFFFAOYSA-K 0.000 description 2
- 239000003795 chemical substances by application Substances 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- CIJQGPVMMRXSQW-UHFFFAOYSA-M sodium;2-aminoacetic acid;hydroxide Chemical compound O.[Na+].NCC([O-])=O CIJQGPVMMRXSQW-UHFFFAOYSA-M 0.000 description 2
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonia chloride Chemical compound [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 description 1
- 239000004254 Ammonium phosphate Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 239000004375 Dextrin Substances 0.000 description 1
- QXNVGIXVLWOKEQ-UHFFFAOYSA-N Disodium Chemical compound [Na][Na] QXNVGIXVLWOKEQ-UHFFFAOYSA-N 0.000 description 1
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 1
- 241001536374 Indicator indicator Species 0.000 description 1
- 241001062009 Indigofera Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- MSKSOBAQMWJYTJ-UHFFFAOYSA-N [Mg].OP(O)(O)=O Chemical compound [Mg].OP(O)(O)=O MSKSOBAQMWJYTJ-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 229910052784 alkaline earth metal Inorganic materials 0.000 description 1
- 239000012670 alkaline solution Substances 0.000 description 1
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 description 1
- 229910000148 ammonium phosphate Inorganic materials 0.000 description 1
- 235000019289 ammonium phosphates Nutrition 0.000 description 1
- 239000000872 buffer Substances 0.000 description 1
- 230000003139 buffering effect Effects 0.000 description 1
- 239000001506 calcium phosphate Substances 0.000 description 1
- 229910000389 calcium phosphate Inorganic materials 0.000 description 1
- 235000011010 calcium phosphates Nutrition 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- SXYCCJAPZKHOLS-UHFFFAOYSA-N chembl2008674 Chemical compound [O-][N+](=O)C1=CC=C2C(N=NC3=C4C=CC=CC4=CC=C3O)=C(O)C=C(S(O)(=O)=O)C2=C1 SXYCCJAPZKHOLS-UHFFFAOYSA-N 0.000 description 1
- MVQBFZXBLLMXGS-UHFFFAOYSA-N chembl331220 Chemical compound C1=CC=C2C(N=NC=3C4=CC=CC=C4C=C(C=3O)C(=O)O)=C(O)C=C(S(O)(=O)=O)C2=C1 MVQBFZXBLLMXGS-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- MNNHAPBLZZVQHP-UHFFFAOYSA-N diammonium hydrogen phosphate Chemical compound [NH4+].[NH4+].OP([O-])([O-])=O MNNHAPBLZZVQHP-UHFFFAOYSA-N 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 238000009616 inductively coupled plasma Methods 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 230000000873 masking effect Effects 0.000 description 1
- 150000003891 oxalate salts Chemical class 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000002686 phosphate fertilizer Substances 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- QORWJWZARLRLPR-UHFFFAOYSA-H tricalcium bis(phosphate) Chemical compound [Ca+2].[Ca+2].[Ca+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O QORWJWZARLRLPR-UHFFFAOYSA-H 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 method of calcium ions and magnesium ions content is, using acid chromium blue k-naphthol green B as indicator, the total content of calcium ion and magnesium ion to be measured with disodium ethylene diamine tetraacetate standard solution in the buffer solution that pH value is 10 in a kind of measurement phosphoric acid solution；Again in the Glycine-NaOH buffer solution that pH value is 10, enough ethylene glycol diethyl ether diammonium tetrem acid solutions are added and measure the content of magnesium ion with the quasi- solution of disodium ethylene diamine tetraacetate using acid chromium blue k-naphthol green B as indicator；Calcium ion content can be obtained with the content that the total content of calcium ion and magnesium ion subtracts magnesium ion.The present invention measures calcium ions and magnesium ions content in the Glycine-NaOH buffer solution that pH value is 10, avoid influence of the phosphate radical to measurement result, and spent glycol diethyl ether diammonium tetraacethyl shelters calcium ion, and then the content of magnesium ion in solution is measured, accurate, quick, simplicity it can measure calcium ion and magnesium ion content in phosphoric acid solution.
Description
Technical field
The invention belongs to technical field of analysis and detection, and in particular to a kind of side for measuring calcium ions and magnesium ions content in phosphoric acid solution
Method.
Background technique
Calcium and magnesium is two kinds of common alkali earth metals, in nature mostly with compounds such as carbonate, sulfate, phosphate
In the presence of in quantitative analysis process, the detection and analysis of calcium-magnesium content account for critically important status.Currently, the side of measurement calcium-magnesium content
Method mainly has compleximetry, atomic absorption spectrography (AAS), inductively coupled plasma emission spectrography, spectrophotometry etc..Its
In, compleximetry is a kind of analysis method of common measurement calcium ions and magnesium ions content, and this method is simple and easy to do, can be quickly quasi-
Really detect that calcium ions and magnesium ions content in solution, detection process include the following steps, take solution to be measured, adjust pH value to 13 with
On, calcon-carboxylic acid is added, the content of calcium ion is measured with EDTA standard solution；The solution to be measured of same volume is taken again, is added one
Determine ammonia-ammonium chloride buffer solution that the pH value of volume is 10, eriochrome black T or acid chromium blue k-naphthol green B indicator is added, uses EDTA
Solution measures the total content of calcium ions and magnesium ions；Magnesium ion can be obtained with the content that the total content of calcium ions and magnesium ions subtracts calcium ion to contain
Amount.
But in practical applications, compleximetry usually will receive the influence of many disturbing factors, for example, phosphate radical
Calcium ions and magnesium ions content detection can be had a huge impact.The author has found during the experiment, in measurement phosphoric acid magnesium solution
Magnesium ion content when, pH value be 10 ammonia-ammonium chloride buffer solution in, part magnesium ion will generate ammonium phosphate in solution
Magnesium, this indissoluble object can not react with EDTA, and then keep the measured value of magnesium ion content relatively low；In measurement calcium phosphate solution
Calcium ion content when, after pH value is transferred to 13, titrated with EDTA standard solution, find in prepare liquid there is no free calcium from
Son, and EDTA can not also react with insoluble calcium salt；When measuring the calcium ions and magnesium ions content in calcium phosphate magnesium solution, to institute
The calcium phosphate magnesium standard solution titration results of configuration are analyzed, and calcium ion content measured by discovery EDTA standard solution will
Greater than its theoretical value, and it is less than the theoretical value of calcium ions and magnesium ions total content, this phenomenon shows in the presence of phosphate radical, adjusts solution
To after 13, the magnesium salts that EDTA will be insoluble with part reacts pH value, and then keeps surveyed calcium ion content higher.
Currently, what the detection method of calcium ions and magnesium ions content in phosphoric acid solution was mostly used is precipitation and separation-complexometry
Method.For example, calcium oxide content and content of magnesia are adopted respectively in GB/T1871.4-1995 and GB/T1871.5-1995
With oxalates separation-EDTA volumetric method (arbitration law) and precipitation and separation-EDTA volumetric method, this two methods pass through by it is to be measured from
Son precipitating, separation, dissolution, and then influence of other interfering ions to measurement result is avoided, but its analytic process step is many and diverse,
Analytic process is longer, easily causes error and keeps measurement result accuracy poor.In addition, in GB/T1871.4-1995, it is another
The method of kind measurement calcium oxide content is the interference made protective agent with dextrin and inhibit phosphate radical and magnesium, with calcein-methyl hundred
In fragrant phenol indigo plant be indicator Indicator Reaction terminal, but interference of this indicator vulnerable to sodium salt and indicator dosage, end point fluorescence disappear
It loses unobvious, it is difficult to determine, usually will cause the larger [calcium oxide content in Yang Yuqiong Phosphorus in Yunnan Province ore of analysis result error
Improvement in determination method [J] phosphate fertilizer and compound fertilizer, 2010,01:60- 61.].
Therefore, a kind of simple, fast method is found to the influence during calcium ions and magnesium ions complexometry for phosphate radical
Carrying out calcium ions and magnesium ions content in Accurate Determining phosphoric acid solution becomes present invention problem in the urgent need to address.
Summary of the invention
To avoid phosphate radical influence caused by calcium ions and magnesium ions content detection in alkaline solution, this method is 10 with pH value
Glycine-NaOH solution is buffer solution, using EGTA as screening agent, provides calcium ions and magnesium ions in a kind of measurement phosphoric acid solution and contains
The method of amount goes out the content of calcium ions and magnesium ions in phosphoric acid solution for Accurate Determining.
The purpose of the present invention is achieved through the following technical solutions.
The method of calcium ions and magnesium ions content, the specific detecting step of the method are as follows in a kind of measurement phosphoric acid solution:
1) take solution 0.2-3mL to be measured, it is neutrality that sodium hydroxide solution, which is added dropwise, and adjusts prepare liquid, be added pH value be 10 it is sweet
Acid chromium blue k-naphthol green B indicator 0.5-2g is added, with ethylenediamine tetrem in propylhomoserin-sodium hydroxide buffer solution 50-200mL
The titration of acid disodium standard solution, obtains the total content of calcium ion and magnesium ion；
2) take solution 0.2-3mL to be measured, it is neutrality that sodium hydroxide solution, which is added dropwise, and adjusts prepare liquid, be added pH value be 10 it is sweet
Propylhomoserin-sodium hydroxide buffer solution 50-200mL is added acid chromium blue k-naphthol green B indicator 0.5-2g, enough second is added
Glycol diethyl ether diammonium tetrem acid solution is titrated with disodium ethylene diamine tetraacetate standard solution, obtains the content of magnesium ion；
3) content of the resulting magnesium ion of step 2 is subtracted i.e. with the total content of the resulting calcium ion of step 1) and magnesium ion
Calcium ion content can be obtained.
In the above-mentioned technical solutions, the concentration of the sodium hydroxide solution is 0.5-2mol/L；The pH value be 10 it is sweet
Propylhomoserin-sodium hydroxide buffer solution configuration method are as follows: weigh 1.875g glycine, 0.64gNaOH adds water to release to 500ml, mixes
It is even；The acid chromium blue k-naphthol green B indicator configuration method are as follows: weigh 0.1g acid chromium blue k, 0.1g naphthol green B and 20g
Dry potassium chloride is placed in finely ground mixing in mortar, stores in port grinding bottle；The concentration of the disodium ethylene diamine tetraacetate standard solution
For 0.01-0.03mol/L；The concentration of the ethylene glycol diethyl ether diammonium tetrem acid solution is 0.01-0.03mol/L, is added
Volume is 1-2 times of disodium ethylene diamine tetraacetate standard solution volume consumed by step 1).
Compared with the method for calcium ions and magnesium ions content in existing measurement phosphoric acid solution, embody the advantages of this method as follows.
This method by improve detection process used in buffer solution, indicator and screening agent, accurately measure calcium from
Son and the total content of magnesium ion and the content of magnesium ion, and then obtain the content of calcium ion, realize in phosphoric acid solution calcium and magnesium from
The Accurate Determining of sub- content.
This method replaces ammonia-chloride buffer that pH value is 10 by 10 Glycine-NaOH buffer solution with pH value
Solution avoids the generation of ammonium magnesium phosphate, can accurately measure magnesium ion content in solution.
Excess EGTA solution, masking solutions are added in the Glycine-NaOH buffer solution that pH value is 10 in this method
In measurement of the calcium ion without influencing magnesium ion, magnesium ion content in accurately measure solution.
In the Glycine-NaOH buffer solution that pH value is 10, EDTA can generate steady this method with calcium ions and magnesium ions
Fixed complex compound is not influenced by phosphate radical in solution, can accurately measure calcium ions and magnesium ions total content in solution.
Specific embodiment
Specific embodiment is as follows.
Embodiment 1
Accurately weigh the Ca (NO of 0.59g, 1.18g, 2.36g, 3.54g, 4.72g3)2•4H2The burning of five 100mL is added in O
Cup；The phosphoric acid solution of 5mL85% is added into each beaker, the deionized water of 20mL is added, shakes up；Solution is added 50mL's
Volumetric flask, constant volume.
The solution to be measured that 1mL is configured is taken, sodium hydroxide solution is added dropwise, measures prepare liquid acid-base property with pH test paper, and remember
Record prepare liquid is adjusted to the volume of consumed sodium hydroxide solution when neutrality；Take the solution to be measured that 1mL is configured again, be added with
Glycine-hydrogen-oxygen that the pH value of 50mL is 10 is added to adjust prepare liquid as neutrality in the sodium hydroxide solution of upper step same volume
Change sodium buffer solution, acid chromium blue k-naphthol green B indicator of 0.1g is added, shakes up, with disodium ethylene diamine tetraacetate (EDTA)
Standard solution titration, record consumed volume when solution colour becomes blue from red, calculates calcium ion in prepare liquid
Content.The following table 1 is the testing result of the embodiment of the present invention 1.
Table 1
| Testing result (mol/L) of the present invention | Actual concentrations (mol/L) | |
| Solution one | 0.052 | 0.05 |
| Solution two | 0.1014 | 0.1 |
| Solution three | 0.2004 | 0.2 |
| Solution four | 0.2994 | 0.3 |
| Solution five | 0.3984 | 0.4 |
Drug used is that analysis is pure in above-described embodiment 1.
Embodiment 2
Accurately weigh the Mg (NO of 0.64g, 1.28g, 2.56g, 3.84g, 5.12g3)2•6H2The burning of five 100mL is added in O
Cup；The phosphoric acid solution of 5mL85% is added into each beaker, the deionized water of 20mL is added, shakes up；Solution is added 50mL's
Volumetric flask, constant volume.
The solution to be measured that 1mL is configured is taken, sodium hydroxide solution is added dropwise, measures prepare liquid acid-base property with pH test paper, and remember
Record prepare liquid is adjusted to the volume of consumed sodium hydroxide solution when neutrality；Take the solution to be measured that 1mL is configured again, be added with
Glycine-hydrogen-oxygen that the pH value of 50mL is 10 is added to adjust prepare liquid as neutrality in the sodium hydroxide solution of upper step same volume
Change sodium buffer solution, acid chromium blue k-naphthol green B indicator of 0.1g is added, shakes up, with disodium ethylene diamine tetraacetate (EDTA)
Standard solution titration, record consumed volume when solution colour becomes blue from red, calculates magnesium ion in prepare liquid
Content.
The following table 2 is the testing result of the embodiment of the present invention 2.
Table 2
| Testing result (mol/L) of the present invention | Actual concentrations (mol/L) | |
| Solution one | 0.0516 | 0.05 |
| Solution two | 0.101 | 0.1 |
| Solution three | 0.2008 | 0.2 |
| Solution four | 0.2996 | 0.3 |
| Solution five | 0.3988 | 0.4 |
Drug used is that analysis is pure in above-described embodiment 2.
Embodiment 3
Accurately weigh the Ca (NO of certain mass3)2·4H2O and Mg (NO3)2·6H2O is put into the beaker of five 100mL,
Weighed quality be respectively 0.59g and 0.64g, 1.18g and 1.28g, 2.36g and 2.56g, 1.18g and 0.64g, 2.36g and
The phosphoric acid solution of 5mL85% is added into each beaker, the deionized water of 20mL is added, shakes up by 0.64g；Solution is added
The volumetric flask of 50mL, constant volume.
The solution to be measured that 1mL is configured is taken, sodium hydroxide solution is added dropwise, measures prepare liquid acid-base property with pH test paper, and remember
Record prepare liquid is adjusted to the volume of consumed sodium hydroxide solution when neutrality；Take the solution to be measured that 1mL is configured again, be added with
Glycine-hydrogen-oxygen that the pH value of 50mL is 10 is added to adjust prepare liquid as neutrality in the sodium hydroxide solution of upper step same volume
Change sodium buffer solution, acid chromium blue k-naphthol green B indicator of 0.1g is added, shakes up, with disodium ethylene diamine tetraacetate (EDTA)
Standard solution titration, record consumed volume when solution colour becomes blue from red, calculates calcium ion in prepare liquid
With the content of magnesium ion.The solution to be measured for taking 1mL to be configured again is added and above-mentioned steps same volume in the conical flask of 250mL
For long-pending sodium hydroxide solution to adjust prepare liquid as neutrality, the Glycine-NaOH buffering that the pH value that 50mL is added is 10 is molten
The ethylene glycol diethyl ether diammonium isometric with disodium ethylene diamine tetraacetate (EDTA) standard solution consumed by previous step is added in liquid
Tetraacethyl (EGTA) solution is added acid chromium blue k-naphthol green B indicator of 0.1g, shakes up, use disodium ethylene diamine tetraacetate
(EDTA) standard solution titrates, and record consumed volume when solution colour becomes blue from red calculates in prepare liquid
The content of magnesium ion.The content that the content of calculated calcium ion and magnesium ion subtracts magnesium ion through the above steps obtain calcium from
Sub- content.The following table 3 is the testing result of the embodiment of the present invention 3.
Table 3
Drug used is that analysis is pure in above-described embodiment 2.
Claims (3)
1. the method for calcium ions and magnesium ions content, the specific detecting step of the method are as follows in a kind of measurement phosphoric acid solution:
1) solution 0.2-3mL to be measured is taken, it is neutrality that sodium hydroxide solution, which is added dropwise, and adjusts prepare liquid, and the sweet ammonia that pH value is 10 is added
Acid-sodium hydroxide buffer solution 50-200mL is added acid chromium blue k-naphthol green B indicator 0.5-2g, uses ethylenediamine tetra-acetic acid
The titration of two sodium standard solutions, obtains the total content of calcium ion and magnesium ion；
2) solution 0.2-3mL to be measured is taken, it is neutrality that sodium hydroxide solution, which is added dropwise, and adjusts prepare liquid, and the sweet ammonia that pH value is 10 is added
Acid-sodium hydroxide buffer solution 50-200mL is added acid chromium blue k-naphthol green B indicator 0.5-2g, enough second two is added
Diethylene glycol diethyl ether diammonium tetrem acid solution is titrated with disodium ethylene diamine tetraacetate standard solution, obtains the content of magnesium ion；
3) it can be obtained with the content that the total content of the resulting calcium ion of step 1) and magnesium ion subtracts the resulting magnesium ion of step 2
To calcium ion content；
The concentration of the sodium hydroxide solution is 0.5-2mol/L；
The concentration of the disodium ethylene diamine tetraacetate standard solution is 0.01-0.03mol/L；
The concentration of the ethylene glycol diethyl ether diammonium tetrem acid solution is 0.01-0.03mol/L, and volume be added is step 1) institute
1-2 times of the disodium ethylene diamine tetraacetate standard solution volume of consumption.
2. the method as described in claim 1, the Glycine-NaOH buffer solution configuration method that the pH value is 10 are as follows:
1.875g glycine is weighed, 0.64gNaOH adds water to release to 500ml, mixes.
3. the method as described in claim 1, the acid chromium blue k-naphthol green B indicator configuration method are as follows: weigh 0.1g acid
Property chrome blue K, 0.1g naphthol green B and 20g are dry, and potassium chloride is placed in finely ground mixing in mortar, stores in port grinding bottle.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710135211.XA CN106645561B (en) | 2017-03-08 | 2017-03-08 | A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710135211.XA CN106645561B (en) | 2017-03-08 | 2017-03-08 | A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN106645561A CN106645561A (en) | 2017-05-10 |
| CN106645561B true CN106645561B (en) | 2019-03-19 |
Family
ID=58847294
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710135211.XA Expired - Fee Related CN106645561B (en) | 2017-03-08 | 2017-03-08 | A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN106645561B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106841511A (en) * | 2015-12-03 | 2017-06-13 | 北京有色金属研究总院 | The rapid analysis method of calcium, magnesium in a kind of iron ore |
| CN114019090A (en) * | 2021-11-03 | 2022-02-08 | 固安桑普生化技术有限公司 | Rapid detection method for magnesium ions |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466641A (en) * | 2010-11-18 | 2012-05-23 | 常萍 | Method for measuring content of calcium ions |
| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
-
2017
- 2017-03-08 CN CN201710135211.XA patent/CN106645561B/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102466641A (en) * | 2010-11-18 | 2012-05-23 | 常萍 | Method for measuring content of calcium ions |
| CN103512879A (en) * | 2013-09-16 | 2014-01-15 | 内蒙古包钢钢联股份有限公司 | Complexometry joint measurement method for calcium, barium and magnesium contents in silico-calcium barium magnesium alloy |
Non-Patent Citations (1)
| Title |
|---|
| 《EDTA直接滴定硅酸盐样品中镁的研究》;李春安等;《水泥技术》;20011231;"2分析步骤"、"4样品分析应用" |
Also Published As
| Publication number | Publication date |
|---|---|
| CN106645561A (en) | 2017-05-10 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104483311A (en) | Indicator for simultaneous measurement of calcium, barium and magnesium in silicon-calcium-barium-magnesium by adopting EDTA titration method | |
| CN103196880B (en) | Method for determining content of arsenic in iron ore by using hydride generation-atomic fluorescence spectroscopy | |
| CN103512879B (en) | The method of calcium, barium, Mg content in Si Si bond surveyed by a kind of complexometric titration connection | |
| KR20120085296A (en) | Method for analyzing and detecting calcium element in ore | |
| CN104458731A (en) | Method for joint measurement of calcium-barium content of silicon-barium alloy by using compleximetry | |
| CN106645561B (en) | A kind of method of calcium ions and magnesium ions content in measurement phosphoric acid solution | |
| CN103344641B (en) | Method for measuring zinc and nickel contents in zinc-nickel alloy electroplating solution | |
| CN103645188A (en) | Method for quickly measuring content of MgO by calcium-magnesium total subtraction process | |
| CN102207463A (en) | Method for determining content of phosphor and copper in ferrotitanium | |
| CN106124689A (en) | The assay method of total nitrogen content in a kind of urea ammonium nitrate solution | |
| CN103115920A (en) | Method for measuring iron/calcium ratio in iron-calcium core-spun yarn | |
| CN107247046A (en) | A kind of ammonia nitrogen detection method of low mercury salt | |
| CN105021545A (en) | Method for measuring contents of bismuth and lead ions in tin lead bismuth alloy electroplating solution | |
| CN104849400A (en) | Novel method for measuring content of zinc in alkaline zinc-nickel alloy plating solution | |
| CN104914093B (en) | The method of testing of constant cadmium and zinc in tellurium-zincium-cadmium crystal | |
| CN108845073B (en) | Novel method for determining zinc chloride in potassium chloride galvanizing solution | |
| CN102608047A (en) | Method for measuring trace content of iron in 1, 4-butanediol | |
| CN102297862A (en) | Method for rapidly measuring rare earth grade of ion absorpt deposit in field | |
| JP5120189B2 (en) | Quantitative determination of chloride ion | |
| CN106645137A (en) | Testing method for metal-calcium-ion chelating capability of chelating acid | |
| CN108008067B (en) | Method for measuring calcium content in phosphate ore by EDTA volumetric method | |
| CN103424403B (en) | The method of Zn in the Fast Measurement aluminium alloy of a kind of stokehold | |
| CN104655610B (en) | The analysis method and assay method of vanadyl oxalate oxalate ion concentration | |
| CN104267029A (en) | Quantitative analysis method for phosphate radical | |
| CN104198652B (en) | Quick determining method for magnesium oxide in high-magnesium phosphorite |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20190319 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |