CN107941961A - The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer - Google Patents
The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer Download PDFInfo
- Publication number
- CN107941961A CN107941961A CN201711468667.4A CN201711468667A CN107941961A CN 107941961 A CN107941961 A CN 107941961A CN 201711468667 A CN201711468667 A CN 201711468667A CN 107941961 A CN107941961 A CN 107941961A
- Authority
- CN
- China
- Prior art keywords
- reducer
- polycarboxylate water
- sample
- detection method
- sodium oxide
- 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.)
- Pending
Links
- 239000003638 chemical reducing agent Substances 0.000 title claims abstract description 38
- 229920005646 polycarboxylate Polymers 0.000 title claims abstract description 37
- KKCBUQHMOMHUOY-UHFFFAOYSA-N sodium oxide Chemical compound [O-2].[Na+].[Na+] KKCBUQHMOMHUOY-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 229910001948 sodium oxide Inorganic materials 0.000 title claims abstract description 31
- JKQOBWVOAYFWKG-UHFFFAOYSA-N molybdenum trioxide Chemical compound O=[Mo](=O)=O JKQOBWVOAYFWKG-UHFFFAOYSA-N 0.000 title claims abstract description 30
- CHWRSCGUEQEHOH-UHFFFAOYSA-N potassium oxide Chemical compound [O-2].[K+].[K+] CHWRSCGUEQEHOH-UHFFFAOYSA-N 0.000 title claims abstract description 30
- 229910001950 potassium oxide Inorganic materials 0.000 title claims abstract description 30
- 238000001514 detection method Methods 0.000 title claims abstract description 17
- 238000012360 testing method Methods 0.000 claims abstract description 26
- 150000002500 ions Chemical class 0.000 claims abstract description 20
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 16
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 15
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 14
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 12
- 239000000243 solution Substances 0.000 claims description 9
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 9
- 239000012498 ultrapure water Substances 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 8
- 238000005070 sampling Methods 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000001103 potassium chloride Substances 0.000 claims description 6
- 235000011164 potassium chloride Nutrition 0.000 claims description 6
- 239000000126 substance Substances 0.000 claims description 6
- 235000006408 oxalic acid Nutrition 0.000 claims description 5
- 239000012086 standard solution Substances 0.000 claims description 5
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 claims description 4
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003153 chemical reaction reagent Substances 0.000 claims description 4
- 239000012528 membrane Substances 0.000 claims description 4
- 230000002572 peristaltic effect Effects 0.000 claims description 4
- 239000011975 tartaric acid Substances 0.000 claims description 4
- 235000002906 tartaric acid Nutrition 0.000 claims description 4
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 claims description 3
- 235000015165 citric acid Nutrition 0.000 claims description 3
- 238000001816 cooling Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 238000002347 injection Methods 0.000 claims description 3
- 239000007924 injection Substances 0.000 claims description 3
- 238000005374 membrane filtration Methods 0.000 claims description 3
- -1 polytetrafluoroethylene Polymers 0.000 claims description 3
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims description 3
- 239000004810 polytetrafluoroethylene Substances 0.000 claims description 3
- 150000007524 organic acids Chemical class 0.000 claims description 2
- 150000001336 alkenes Chemical class 0.000 claims 1
- 239000003086 colorant Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 229920002521 macromolecule Polymers 0.000 abstract description 6
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 238000010998 test method Methods 0.000 abstract description 5
- 238000012545 processing Methods 0.000 abstract description 3
- 239000000523 sample Substances 0.000 description 31
- 238000004458 analytical method Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 2
- 230000000996 additive effect Effects 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000012417 linear regression Methods 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- 238000004611 spectroscopical analysis Methods 0.000 description 2
- 239000011550 stock solution Substances 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 235000012501 ammonium carbonate Nutrition 0.000 description 1
- 239000000908 ammonium hydroxide Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 239000006210 lotion Substances 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 239000011591 potassium Substances 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000012488 sample solution Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Landscapes
- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (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 invention discloses the detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer.The present invention is using OnC18 pretreatment columns processing polycarboxylate water-reducer sample, remove the organic macromolecule material having a great influence to solution viscosity, avoid its influence to test result, reduce test result error, and pretreated polycarboxylate water-reducer sample passes through ion chromatograph, pollution of the organic macromolecule material to chromatographic column effectively is avoided, extends the service life of chromatographic column；The content of sodium oxide molybdena and potassium oxide in pretreated polycarboxylate water-reducer is tested using ion chromatograph, effectively avoid the influence that release agent disturbs test result in traditional test methods, the accuracy of method is improved, there is the advantages of evaluated error is small, and precision is high.
Description
Technical field
The invention belongs to construction material detection technology field, and in particular to sodium oxide molybdena and oxidation in a kind of polycarboxylate water-reducer
The detection method of potassium content.
Background technology
Concrete admixture is a kind of material filled to improve and adjust the performance of concrete, the addition of additive
Improvement to concrete performance plays certain effect.Polycarboxylate water-reducer is a kind of very important concrete admixture,
And a kind of concrete admixture that research is relatively broad.The complicated component of polycarboxylate water-reducer, brand is various, and manufacturer is many
It is more.Certain requirement that the addition and use of polycarboxylate water-reducer have, the content of some components are such as not under control, may
Different degrees of influence can be caused to the concrete works in later stage.Sodium oxide molybdena and potassium oxide are exactly that one kind has in polycarboxylate water-reducer
The content height of evil component, sodium oxide molybdena and potassium oxide is possible to that alkali-aggregate reaction can be produced, and causes concrete that volumetric expansion occurs,
Cause crack, deteriorate its mechanical property, cause engineering structure to be destroyed, seriously affect the durability of engineering.Therefore, polycarboxylic acids subtracts
The content of sodium oxide molybdena and potassium oxide needs stringent control in aqua, measures the content of sodium oxide molybdena and potassium oxide in polycarboxylate water-reducer
Have very important significance.
The test method of sodium oxide molybdena and potassium oxide alkali content is to use standard test side in test concrete admixture at present
Method, first with hot water dissolving's sample, separates iron and aluminium with release agent ammonium hydroxide, with release agent ammonium carbonate separating calcium and magnesium, then adopts
With the sodium oxide molybdena and potassium oxide in flame photometer filtrates tested.The method can have certain deficiency during test
Place, such as release agent may bring larger blank into when separating coexisting ion, and the ammonia that excess of ammonia water produces can be to surveying
Determine result to affect, using dramatically increasing time for entirely testing when boiling and excluding ammonia again；Concrete admixture
Generally organic macromolecule material, has a great influence solution viscosity, does not remove organic macromolecule material by pretreatment, adopts
When testing the content of sodium oxide molybdena and potassium oxide in additive with flame spectrometry, liquid absorption amount and materialization efficiency meeting to sample solution
Large effect is produced, measurement result is produced certain error.Therefore using in flame spectrometry test concrete admixture
There are certain evaluated error, accuracy be not high during the content of sodium oxide molybdena and potassium oxide.
The content of the invention
It is an object of the invention to overcome prior art defect, there is provided sodium oxide molybdena and potassium oxide in a kind of polycarboxylate water-reducer
The detection method of content.
Technical scheme is as follows：
The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer, includes the following steps：
(1) polycarboxylate water-reducer sample 0.1000g~0.5000g accurately is weighed, ultra-pure water is settled to after being completely dissolved
VmL, obtains prepare liquid, then crosses OnC18 pretreatment columns after prepare liquid is diluted n times, and gained liquid passes through membrane filtration, treated again
Sample；
(2) it is accurate to weigh the mark for through drying top pure grade NaCl after cooling and KC1 reagents, being prepared into that concentration is 100mg/mL
Quasi- stock solution, then takes the standard reserving solution of 0.0mL, 1.0mL, 2.0mL, 3.0mL and 4.0mL in 50mL volumetric flasks respectively
In, scale is diluted to ultra-pure water, is configured to a series of standard solution of various concentrations, shakes up and is placed on ion chromatograph progress
Test, using peak area and the relation of solution concentration, draws standard working curve；
(3) sample to be tested made from step (1) is placed in ion chromatograph and is tested, parallel testing takes afterwards several times
Average value, brings into step (2) obtained standard curve, obtains the potassium oxide and sodium oxide molybdena of polycarboxylate water-reducer sample to be measured
Concentration C 1 and C2, then according to formulaObtain
The content of sodium oxide molybdena and potassium oxide in polycarboxylate water-reducer to be measured, the unit of wherein W1 and W2 are that the unit of %, C1 and C2 are mg/
ML, n are the diluted multiples of prepare liquid, and dimensionless, V is the volume of prepare liquid, and unit is mL, and m is polycarboxylate water-reducer sample to be measured
The sampling amount of product, unit are g,It is the conversion coefficient that sodium chloride is scaled sodium oxide molybdena,It is that potassium chloride is scaled potassium oxide
Conversion coefficient, dimensionless factor；
In above-mentioned ion chromatograph, the guard column used is for Metrosep C6-100/2.0 guard columns, chromatographic column
Metrosep C6-100/2.0 splitters, the granular size of the internal diameter of chromatographic column is 5 μm, and the temperature of chromatographic column is 20~30 DEG C,
Sample size is 10~30 μ L, and leacheate used is organic acid, is at least one in citric acid, oxalic acid, tartaric acid and aromatic acid
Kind, the flow velocity of leacheate is 0.5~1.0mL/min.
In a preferred embodiment of the invention, the filter membrane is 0.05~0.5 μm of polytetrafluoroethylene film.
It is further preferred that the filter membrane is 0.22 μm of polytetrafluoroethylene film.
In a preferred embodiment of the invention, the temperature of the chromatographic column is 25 DEG C, and sample size is 20 μ L.
In a preferred embodiment of the invention, the flow velocity of the leacheate is 0.8mL/min.
In a preferred embodiment of the invention, the ion chromatograph leads to 883 ion chromatographs for Switzerland ten thousand, its
Include mobile phase, automatic sampling apparatus, peristaltic pump, chromatographic column, suppressor and detection cell, automatic sampling apparatus by automatically into
Sample sample disc device is connected with peristaltic pump carries out auto injection, and suppressor is MSM II chemical suppressors, and detection cell is examined for conductance
Survey pond.
The beneficial effects of the invention are as follows：
1st, the present invention is removed and had a great influence to solution viscosity using OnC18 pretreatment columns processing polycarboxylate water-reducer sample
Organic macromolecule material, avoid its influence to test result, reduce test result error, and pretreated poly-
Carboxylic acid water reducer sample passes through ion chromatograph, effectively avoids pollution of the organic macromolecule material to chromatographic column, extends
The service life of chromatographic column.
2nd, the present invention using OnC18 pretreatment columns processing polycarboxylate water-reducer sample to its sodium oxide molybdena and potassium oxide content into
Row test, solves the shortcomings that traditional test methods pre-treatment step is cumbersome, time-consuming, and the method for the present invention pretreatment is simple, quick,
Time cost is reduced, substantially increases the efficiency of analysis test.
3rd, the present invention uses ion chromatograph to the content of sodium oxide molybdena and potassium oxide in pretreated polycarboxylate water-reducer
Tested, effectively avoid the influence that release agent disturbs test result in traditional test methods, improve the standard of method
Exactness, has the advantages of evaluated error is small, and precision is high.
4th, ion chromatograph is applied to the test of sodium oxide molybdena and potassium oxide content in polycarboxylate water-reducer by the present invention, is widened
The test method of potassium oxide and sodium oxide content, the test for sodium oxide molybdena in polycarboxylate water-reducer and potassium oxide content provide
A kind of new means of testing.
Embodiment
Technical scheme is further detailed and described below by way of embodiment.
Embodiment 1
1.1 instruments and reagent
883 ion chromatograph systems are led in ten thousand Switzerland of Tong Zhong Co., Ltd ten thousand of Switzerland；Metrosep C6-100/2.0 are protected
Column；Metrosep C6-100/2.0 splitters；MSM II chemical suppressors；Conductance detecting pool；Mei Teletuo benefits instrument (on
Sea) Co., Ltd's electronic analytical balance；KCl (top pure grade)；NaCl (top pure grade)；Citric acid (analysis is pure)；Oxalic acid (analysis is pure)；
Tartaric acid (analysis is pure)；Aromatic acid (analysis is pure)；Use for laboratory water is ultra-pure water；Specimen in use is polycarboxylate water-reducer sample
1#, 2#, 3#, purchased from Fujian company
1.2 sample pretreatment
It is accurate to weigh polycarboxylate water-reducer sample 1#0.1005g, after ultra-pure water dissolving, it is settled in 100mL volumetric flasks, so
After the sample after constant volume is diluted 2 times afterwards, after OnC18 pretreatment columns (being purchased from Tianjin Mai Sike Chemical Co., Ltd.s),
Gained liquid passes through 0.22 μm of membrane filtration, obtains sample to be tested；
1.3 standard solution are prepared and Specification Curve of Increasing
10.000g accurately is weighed through drying top pure grade NaCl after cooling and KC1 reagents, is prepared into concentration 100.0mg/mL
Standard Stock solutions, then take the standard reserving solution of 0.0mL, 1.0mL, 2.0mL, 3.0mL and 4.0mL respectively in 50mL capacity
In bottle, scale is diluted to ultra-pure water, it is respectively 0mg/mL, 2mg/mL, 4mg/mL, 6mg/mL, 8mg/mL to be configured to concentration
Standard solution, shakes up rear spare.Ion chromatograph is opened, after instrument stabilizer, the standard solution of various concentrations is placed in ion
Chromatograph is tested, and using peak area and the relation of solution concentration, draws standard working curve.Obtained sodium chloride it is linear
Regression equation, that is, standard curve is：Y=0.74*C1+0.22, related coefficient 0.991, the equation of linear regression of potassium chloride are marked
Directrix curve is：Y=0.7*C2+0.04, related coefficient 0.994.
1.4 polycarboxylate water-reducer sample tests
Chromatographic condition is：Metrosep C6-100/2.0 guard columns, Metrosep C6-100/2.0 splitters, MSM II
Chemical suppressor, conductance detecting pool, column temperature are 20 DEG C, and sample size is 10 μ L, using citric acid and oxalic acid mixed liquor as leacheate, leaching
The flow velocity of washing lotion is 0.6mL/min.Take and treat test sample, ion chromatograph parallel determination 10 times is placed under above-mentioned chromatographic condition, survey
Test result is brought into standard curve obtained above after removing average value, obtains the concentration C 1 of sodium oxide molybdena and potassium oxide in sample to be tested
And C2, according to formula and then according to formula Treated
The content of sodium oxide molybdena and potassium oxide in polycarboxylate water-reducer is surveyed, the unit of wherein W1 and W2 is that the unit of %, C1 and C2 are mg/
ML, n are the diluted multiples of prepare liquid, and dimensionless, V is the volume of prepare liquid, and unit is mL, and m is polycarboxylate water-reducer sample to be measured
The sampling amount of product, unit are g,It is the conversion coefficient that sodium chloride is scaled sodium oxide molybdena,It is that potassium chloride is scaled potassium oxide
Conversion coefficient, dimensionless factor, the sodium oxide molybdena and the content of potassium oxide measured is respectively 0.0382% and 0.0029%, relatively
Standard deviation is respectively 0.27% and 1.96%.
Embodiment 2
Polycarboxylate water-reducer sample 2#0.2502g is accurately weighed in 2.2, after ultra-pure water dissolving, is settled to 100mL volumetric flasks
In, the sample after constant volume is then diluted 5 times.
Polycarboxylate water-reducer sample test in 2.4, chromatographic condition are：Metrosep C6-100/2.0 guard columns,
Metrosep C6-100/2.0 splitters, MSM II chemical suppressors, conductance detecting pool, column temperature are 25 DEG C, and sample size is 20 μ
L, using citric acid, oxalic acid and tartaric acid mixed liquor as leacheate, the flow velocity of leacheate is 0.8mL/min.
Other are same as Example 1.
Embodiment 3
Polycarboxylate water-reducer sample 3#0.5012g is accurately weighed in 3.2, after ultra-pure water dissolving, is settled to 100mL volumetric flasks
In, the sample after constant volume is then diluted 10 times.
Polycarboxylate water-reducer sample test in 3.4, chromatographic condition are：Metrosep C6-100/2.0 guard columns,
Metrosep C6-100/2.0 splitters, MSM II chemical suppressors, conductance detecting pool, column temperature are 30 DEG C, and sample size is 30 μ
L, using aromatic acid as leacheate, the flow velocity of leacheate is 1.0mL/min.
Other are same as Example 1.
The foregoing is only a preferred embodiment of the present invention, therefore cannot limit the scope that the present invention is implemented according to this, i.e.,
The equivalent changes and modifications made according to the scope of the claims of the present invention and description, all should still belong in the range of the present invention covers.
Claims (6)
- A kind of 1. detection method of sodium oxide molybdena and potassium oxide content in polycarboxylate water-reducer, it is characterised in that：Include the following steps：(1) polycarboxylate water-reducer sample 0.1000g~0.5000g accurately is weighed, ultra-pure water is settled to VmL after being completely dissolved, obtains Prepare liquid, then OnC18 pretreatment columns are crossed after prepare liquid is diluted n times, gained liquid passes through membrane filtration, obtains treating test sample again Product；(2) it is accurate to weigh the standard storage for through drying top pure grade NaCl after cooling and KCl reagents, being prepared into that concentration is 100mg/mL Standby solution, then takes the standard reserving solution of 0.0mL, 1.0mL, 2.0mL, 3.0mL and 4.0mL in 50mL volumetric flasks respectively, with Ultra-pure water is diluted to scale, is configured to a series of standard solution of various concentrations, shakes up and is placed on ion chromatograph and is tested, Using peak area and the relation of solution concentration, standard working curve is drawn；(3) sample to be tested made from step (1) is placed in ion chromatograph and is tested, parallel testing is averaged afterwards several times Value, bring into step (2) obtained standard curve, obtain polycarboxylate water-reducer sample to be measured potassium oxide and sodium oxide molybdena it is dense C1 and C2 is spent, then according to formulaObtain to be measured The content of sodium oxide molybdena and potassium oxide in polycarboxylate water-reducer, the unit of wherein W1 and W2 are that the unit of %, C1 and C2 are mg/mL, n It is the diluted multiple of prepare liquid, dimensionless, V is the volume of prepare liquid, and unit is mL, and m is polycarboxylate water-reducer sample to be measured Sampling amount, unit are g,It is the conversion coefficient that sodium chloride is scaled sodium oxide molybdena,It is that potassium chloride is scaled changing for potassium oxide Calculate coefficient, dimensionless factor；In above-mentioned ion chromatograph, the guard column used is Metrosep C6-100/2.0 guard columns, chromatographic column Metrosep C6-100/2.0 splitters, the granular size of the internal diameter of chromatographic column is 5 μm, and the temperature of chromatographic column is 20~30 DEG C, and sample size is 10~30 μ L, leacheate used are organic acid, at least one of citric acid, oxalic acid, tartaric acid and aromatic acid, leacheate Flow velocity be 0.5~1.0mL/min.
- 2. detection method as claimed in claim 1, it is characterised in that：The filter membrane is 0.05~0.5 μm of polytetrafluoroethyl-ne Alkene film.
- 3. detection method as claimed in claim 2, it is characterised in that：The filter membrane is 0.22 μm of polytetrafluoroethylene film.
- 4. detection method as claimed in claim 1, it is characterised in that：The temperature of the chromatographic column is 25 DEG C, and sample size is 20 μ L。
- 5. detection method as claimed in claim 1, it is characterised in that：The flow velocity of the leacheate is 0.8mL/min.
- 6. detection method as claimed in claim 1, it is characterised in that：The ion chromatograph leads to 883 ion colors for Switzerland ten thousand Spectrometer, including mobile phase, automatic sampling apparatus, peristaltic pump, chromatographic column, suppressor and detection cell, automatic sampling apparatus leads to Cross auto injection sample disc device and be connected with peristaltic pump and carry out auto injection, suppressor is MSM II chemical suppressors, detection cell For conductance detecting pool.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711468667.4A CN107941961A (en) | 2017-12-28 | 2017-12-28 | The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201711468667.4A CN107941961A (en) | 2017-12-28 | 2017-12-28 | The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107941961A true CN107941961A (en) | 2018-04-20 |
Family
ID=61937885
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201711468667.4A Pending CN107941961A (en) | 2017-12-28 | 2017-12-28 | The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107941961A (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001174446A (en) * | 1999-12-20 | 2001-06-29 | Seimi Chem Co Ltd | Cation quantitatively analyzing method by ion chromatography |
| US20030172850A1 (en) * | 2002-03-13 | 2003-09-18 | Byong-Wa Chun | Beneficiated water reducing compositions |
| CN102128900A (en) * | 2010-12-15 | 2011-07-20 | 中国铝业股份有限公司 | Method for detecting components of alumyte |
| CN102590383A (en) * | 2012-02-13 | 2012-07-18 | 河北中烟工业有限责任公司 | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously |
| CN106248862A (en) * | 2016-10-17 | 2016-12-21 | 湖北鑫统领万象科技有限公司 | A kind of chloride ion conductor method in polycarboxylate water-reducer |
| CN110395935A (en) * | 2018-04-25 | 2019-11-01 | 信越化学工业株式会社 | Preparation, diminishing composition and the hydraulic-composition of diminishing composition |
-
2017
- 2017-12-28 CN CN201711468667.4A patent/CN107941961A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001174446A (en) * | 1999-12-20 | 2001-06-29 | Seimi Chem Co Ltd | Cation quantitatively analyzing method by ion chromatography |
| US20030172850A1 (en) * | 2002-03-13 | 2003-09-18 | Byong-Wa Chun | Beneficiated water reducing compositions |
| CN102128900A (en) * | 2010-12-15 | 2011-07-20 | 中国铝业股份有限公司 | Method for detecting components of alumyte |
| CN102590383A (en) * | 2012-02-13 | 2012-07-18 | 河北中烟工业有限责任公司 | Method for determining content of potassium, sodium, calcium and magnesium in cigarette paper simultaneously |
| CN106248862A (en) * | 2016-10-17 | 2016-12-21 | 湖北鑫统领万象科技有限公司 | A kind of chloride ion conductor method in polycarboxylate water-reducer |
| CN110395935A (en) * | 2018-04-25 | 2019-11-01 | 信越化学工业株式会社 | Preparation, diminishing composition and the hydraulic-composition of diminishing composition |
Non-Patent Citations (6)
| Title |
|---|
| LILIA BASILIO DE CALAND ET AL.: "Determination of sodium, potassium, calcium and magnesium cations in biodiesel by ion chromatography", 《ANALYTICA CHIMICA ACTA》 * |
| 刘功斌 等: "离子色谱法分析土壤水溶性盐中的阳离子", 《干旱环境监测》 * |
| 国家质量技术监督局: "《GB/T 8077-2000 中华人民共和国国家标准 混凝土外加剂均质性试验方法》", 18 December 2000 * |
| 张显安 等: "非抑制型离子色谱法同时测定矿泉水中6种阳离子", 《食品工业》 * |
| 朱彬和 等: "离子色谱法测定减水剂中的阴离子", 《浙江大学学报（理学版）》 * |
| 杨学灵 等: "离子色谱法测定减水剂中硫酸钠含量", 《广州化学》 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN108956815B (en) | Method for testing chloride ion content in sea sand | |
| CN106872595A (en) | The assay method of the chiral molecules content based on circular dichroism technology | |
| CN106526062B (en) | The ion chromatographic method of trace chloro ion in a kind of measure triethyl aluminum | |
| CN102353668A (en) | Method for determining anionic surfactant in surface water | |
| CN102830116A (en) | Detection device and detection method for continuous flow of total cyanide in water | |
| CN107478591A (en) | The content assaying method of polyoxyethylene sorbitan monoleate in a kind of traditional Chinese medicine | |
| CN108279274A (en) | The detection method of calcium oxide and content of magnesia in a kind of portland cement | |
| CN104655473B (en) | Enrichment and the method for detection Determination of Trace Mercury In Water | |
| CN103760273A (en) | Analysis method for trace oxalic acid root in mother liquor of plutonium oxalate precipitation | |
| CN106483157B (en) | Method for measuring total chlorine in desulfurization solution | |
| CN104849335A (en) | Method for detecting ionic calcium content of blood sample | |
| CN107941961A (en) | The detection method of sodium oxide molybdena and potassium oxide content in a kind of polycarboxylate water-reducer | |
| CN112578071A (en) | Quantitative analysis method for inorganic acid salt in electrolytic stripping powder | |
| CN104569214B (en) | The assay method of low concentration xylol in metal ion and Organic substance compound wastewater | |
| Ping et al. | Determination of organic acids exuded from plant roots by high performance liquid chromatography | |
| CN102841093B (en) | Continuous flow test system for chloride in water and test method | |
| CN111007194A (en) | Method for quantifying sodium ion content in nylon monomer by using ion chromatography | |
| CN110220856A (en) | The method that Flow Injection Analysis detects chloride ion content in the electrodeposit liquid of electrolytic copper foil | |
| CN101051027A (en) | Method for water phase detecting micro mercury in water or waste water by spectrophotometry | |
| CN113884459B (en) | A kind of direct determination method and application of nitrate content in seawater | |
| CN108802234A (en) | The assay method of ammonium ion content in a kind of flyash | |
| CN104280368A (en) | Method for efficiently and accurately detecting main content of industrial magnesium oxide | |
| JP2005069746A (en) | Back extraction method of silicomolybdic acid and silicon quantifying method using silicomolybdic acid (blue) absorptiometric method | |
| CN105319301B (en) | A kind of assay method of the indigo middle non-pigmented organic matter of food additives | |
| CN113325118A (en) | Method for measuring sodium content in parecoxib sodium |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20180420 |