CN100538342C - Hardness measurement reagent - Google Patents
Hardness measurement reagent Download PDFInfo
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- CN100538342C CN100538342C CNB2005100627057A CN200510062705A CN100538342C CN 100538342 C CN100538342 C CN 100538342C CN B2005100627057 A CNB2005100627057 A CN B2005100627057A CN 200510062705 A CN200510062705 A CN 200510062705A CN 100538342 C CN100538342 C CN 100538342C
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- hardness
- water
- variable color
- pigment
- measurement reagent
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- 239000003153 chemical reaction reagent Substances 0.000 title claims abstract description 62
- 238000007542 hardness measurement Methods 0.000 title claims abstract description 48
- 239000000049 pigment Substances 0.000 claims abstract description 41
- -1 alkali metal salt Chemical class 0.000 claims abstract description 35
- 229910052783 alkali metal Inorganic materials 0.000 claims abstract description 25
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 16
- VBRNLOQCBCPPHL-UHFFFAOYSA-N calmagite Chemical compound CC1=CC=C(O)C(N=NC=2C3=CC=CC=C3C(=CC=2O)S(O)(=O)=O)=C1 VBRNLOQCBCPPHL-UHFFFAOYSA-N 0.000 claims abstract description 6
- 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 claims abstract description 4
- KXDHJXZQYSOELW-UHFFFAOYSA-N Carbamic acid Chemical compound NC(O)=O KXDHJXZQYSOELW-UHFFFAOYSA-N 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 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 5
- RPACBEVZENYWOL-XFULWGLBSA-M sodium;(2r)-2-[6-(4-chlorophenoxy)hexyl]oxirane-2-carboxylate Chemical compound [Na+].C=1C=C(Cl)C=CC=1OCCCCCC[C@]1(C(=O)[O-])CO1 RPACBEVZENYWOL-XFULWGLBSA-M 0.000 claims 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 87
- 239000003352 sequestering agent Substances 0.000 abstract description 29
- AMMWFYKTZVIRFN-UHFFFAOYSA-M chembl2028442 Chemical compound [Na+].C1=CC=CC2=C(O)C(N=NC3=C4C=CC(=CC4=C(C=C3O)S([O-])(=O)=O)[N+]([O-])=O)=CC=C21 AMMWFYKTZVIRFN-UHFFFAOYSA-M 0.000 abstract description 14
- 239000013522 chelant Substances 0.000 description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 9
- 238000011161 development Methods 0.000 description 7
- 230000018109 developmental process Effects 0.000 description 7
- 239000000203 mixture Substances 0.000 description 6
- 238000006243 chemical reaction Methods 0.000 description 5
- 238000000034 method Methods 0.000 description 5
- 238000002360 preparation method Methods 0.000 description 5
- UEUXEKPTXMALOB-UHFFFAOYSA-J tetrasodium;2-[2-[bis(carboxylatomethyl)amino]ethyl-(carboxylatomethyl)amino]acetate Chemical compound [Na+].[Na+].[Na+].[Na+].[O-]C(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O UEUXEKPTXMALOB-UHFFFAOYSA-J 0.000 description 5
- NWUYHJFMYQTDRP-UHFFFAOYSA-N 1,2-bis(ethenyl)benzene;1-ethenyl-2-ethylbenzene;styrene Chemical compound C=CC1=CC=CC=C1.CCC1=CC=CC=C1C=C.C=CC1=CC=CC=C1C=C NWUYHJFMYQTDRP-UHFFFAOYSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 239000003456 ion exchange resin Substances 0.000 description 4
- 229920003303 ion-exchange polymer Polymers 0.000 description 4
- 239000011734 sodium Substances 0.000 description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 3
- 239000002671 adjuvant Substances 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 239000000470 constituent Substances 0.000 description 3
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 3
- 238000007710 freezing Methods 0.000 description 3
- 230000008014 freezing Effects 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- RGHNJXZEOKUKBD-SQOUGZDYSA-N D-gluconic acid Chemical compound OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C(O)=O RGHNJXZEOKUKBD-SQOUGZDYSA-N 0.000 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 description 2
- 244000061458 Solanum melongena Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 150000001340 alkali metals Chemical class 0.000 description 2
- 238000003556 assay Methods 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000002738 chelating agent Substances 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000008929 regeneration Effects 0.000 description 2
- 238000011069 regeneration method Methods 0.000 description 2
- 238000012216 screening Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- CHHHXKFHOYLYRE-UHFFFAOYSA-M 2,4-Hexadienoic acid, potassium salt (1:1), (2E,4E)- Chemical compound [K+].CC=CC=CC([O-])=O CHHHXKFHOYLYRE-UHFFFAOYSA-M 0.000 description 1
- ARZSRJNMSIMAKS-UHFFFAOYSA-N 4-aminobutane-1,2-diol Chemical compound NCCC(O)CO ARZSRJNMSIMAKS-UHFFFAOYSA-N 0.000 description 1
- FCKYPQBAHLOOJQ-UHFFFAOYSA-N Cyclohexane-1,2-diaminetetraacetic acid Chemical compound OC(=O)CN(CC(O)=O)C1CCCCC1N(CC(O)=O)CC(O)=O FCKYPQBAHLOOJQ-UHFFFAOYSA-N 0.000 description 1
- RGHNJXZEOKUKBD-UHFFFAOYSA-N D-gluconic acid Natural products OCC(O)C(O)C(O)C(O)C(O)=O RGHNJXZEOKUKBD-UHFFFAOYSA-N 0.000 description 1
- QZKRHPLGUJDVAR-UHFFFAOYSA-K EDTA trisodium salt Chemical compound [Na+].[Na+].[Na+].OC(=O)CN(CC([O-])=O)CCN(CC([O-])=O)CC([O-])=O QZKRHPLGUJDVAR-UHFFFAOYSA-K 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- UEZVMMHDMIWARA-UHFFFAOYSA-N Metaphosphoric acid Chemical compound OP(=O)=O UEZVMMHDMIWARA-UHFFFAOYSA-N 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 208000034189 Sclerosis Diseases 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000035614 depigmentation Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- XPPKVPWEQAFLFU-UHFFFAOYSA-N diphosphoric acid Chemical compound OP(O)(=O)OP(O)(O)=O XPPKVPWEQAFLFU-UHFFFAOYSA-N 0.000 description 1
- 238000010494 dissociation reaction Methods 0.000 description 1
- 230000005593 dissociations Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 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 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000002440 hepatic effect Effects 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 230000002452 interceptive effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002736 nonionic surfactant Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 229920000137 polyphosphoric acid Polymers 0.000 description 1
- 229910052700 potassium Inorganic materials 0.000 description 1
- 229940069338 potassium sorbate Drugs 0.000 description 1
- 235000010241 potassium sorbate Nutrition 0.000 description 1
- 239000004302 potassium sorbate Substances 0.000 description 1
- 229940005657 pyrophosphoric acid Drugs 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- MNCGMVDMOKPCSQ-UHFFFAOYSA-M sodium;2-phenylethenesulfonate Chemical compound [Na+].[O-]S(=O)(=O)C=CC1=CC=CC=C1 MNCGMVDMOKPCSQ-UHFFFAOYSA-M 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/18—Water
- G01N33/1813—Specific cations in water, e.g. heavy metals
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/75—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated
- G01N21/77—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator
- G01N21/78—Systems in which material is subjected to a chemical reaction, the progress or the result of the reaction being investigated by observing the effect on a chemical indicator producing a change of colour
-
- 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
- G01N31/22—Investigating or analysing non-biological materials by the use of the chemical methods specified in the subgroup; Apparatus specially adapted for such methods using chemical indicators
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Pathology (AREA)
- Immunology (AREA)
- General Physics & Mathematics (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Plasma & Fusion (AREA)
- Biophysics (AREA)
- Molecular Biology (AREA)
- Food Science & Technology (AREA)
- Medicinal Chemistry (AREA)
- Investigating Or Analyzing Non-Biological Materials By The Use Of Chemical Means (AREA)
- Investigating Or Analysing Materials By The Use Of Chemical Reactions (AREA)
Abstract
Near a kind of hardness measurement reagent that management hardness, makes determined water variable color observantly.It contains the alkali metal salt that is selected from pigment, triethanolamine, diol compound and sequestrant in eriochrome black T (EBT) or the calmagite.
Description
Technical field
The present invention relates to be used for measuring the hardness measurement reagent of contained hardness such as process water, domestic water.
Background technology
As everyone knows, in the water supply line of cold and hot instrument class such as boiler, water heater or refrigeratory, need prevent that incrustation scale from cold and hot instrument built-in, therefore be connected with and be used for removing the hardness components (Ca that former water such as process water, domestic water contain
2+And Mg
2+) device, for example will use the water-softening equipment of ion exchange resin to be connected on the water supply line, with the hardness components (Ca in the former water
2+And Mg
2+) be substituted by Na
+, the softening processing water that obtains is supplied with to cold and hot instrument class as supplying water.
Used under the situation of aforementioned water-softening equipment, the ion exchange resin deterioration that is equipped with when the inside of this device, when perhaps regeneration of ion-exchange resin was insufficient, the hardness components in then supplying water was to Na
+Conversion insufficient.Therefore, need be according to the former water hardness of region that cold and hot instrument class is set and position etc., preestablish the hardness of permission, measure by the hardness in the water supply of water-softening equipment termly.And, when the hardness in the water supply surpasses the upper limit (below be called management hardness) of permissible value, be judged as and hardness takes place leak, dispose so that ion exchange resin exchanges or regeneration etc., making supplies water is in specific durometer level.
The method of the hardness in judge supplying water is disclosed following method (with reference to patent documentation 1,2,3), be about to the hardness measurement reagent of the non-water system that eriochrome black T (EBT) for example contains as pigment, be added on from the determined water that water supply is taked to obtain, with the tone of determined water as index.The tone of determined water by the pigment that contains in hardness components and the hardness measurement reagent react generate chelate and the pigment of unreacted (dissociating) have a ratio, measure qualitatively.Specifically be to use under the situation of EBT as pigment, raising along with the hardness in the determined water, the tone of determined water becomes bluish violet (following hardness will present hepatic tone the time is called " variable color starting point ") from initial blueness, and (following hardness will present red tone the time is called the variable color terminal point to become redness through aubergine again.)。
Therefore, judge under the situation that hardness leaks in the tonal variation that is conceived to take place with the hardness in this determined water, determine management hardness in advance, determine simultaneously after the condition determination of the cooperation ratio of the EBT in the hardness measurement reagent, the addition of the hardness measurement reagent when measuring and the capacity of determined water etc., carry out the measurement operation of reagent, so that this management hardness enters between color development starting point and the color development terminal point.
As mentioned above, under the situation of tonal variation as the index of hardness leakage with the hardness in the determined water of correspondence, the assay method of the tone that adopts is that the people estimates by observation usually, perhaps uses Instrument measuring transmittance or absorbance.Under situation about estimating, the tone of determined water is judged as and hardness occurs and leak when bluish violet changes redness into.In addition, when Instrument measuring, according to the typical curve of the relation of representing hardness and transmittance (or absorbance), hardness directly is shown on analyzer, when hardness reaches management hardness, judges that hardness occurring leaks.No matter adopt which kind of assay method,, wish near management hardness, to make determined water that variable color take place observantly in order positively to carry out the judgement that hardness is leaked.
But, former hardness measurement reagent, the amplitude of variable color starting point and variable color terminal point (below be called " variable color amplitude ") is wide, near management hardness variable color blunt, so when utilizing colorimetric to estimate, difference appears in the individual when the judgement of hardness leakage.
Patent documentation 1 spy opens flat 11-64323 communique
Patent documentation 2 spies open the 2002-181802 communique
Patent documentation 3 spies open the 2002-181803 communique
Summary of the invention
The problem to be solved in the present invention is to find out near a kind of hardness measurement reagent of the sharp variable color of determined water-sensitive management hardness.
The present inventor has carried out research in depth in order to solve above-mentioned problem, found that, the pigment that contains in hardness components and the hardness measurement reagent reacts the compound of the chelate that generates and unreacted pigment when existing with specific ratio, grasping determined water begins variable color and presents this a certain amount of relation of bluish violet, use the hardness measurement reagent after cooperating with the alkali metal salt that the hardness components preferential reaction generates the specific sequestrant of chelate simultaneously, can solve foregoing problems, until finishing the present invention.
Just, the present invention 1 is characterised in that, contains the alkali metal salt that is selected from pigment, triethanolamine, diol compound and sequestrant in eriochrome black T (EBT) or the calmagite (calmagite).
The present invention 2 is characterised in that, on the basis of the present invention 1 formation, sequestrant is the organic system amino carboxylic acid.
The present invention 3 is characterised in that the present invention 1 or 2 described hardness measurement reagents are made of a kind of liquid.
The present invention makes the variable color observantly of determined water near management hardness, can positively differentiate hardness thus and leak.In more detail, the hardness components that the alkali metal salt of sequestrant has precedence in pigment and the determined water generates the chelate compound, and residual hardness components and pigment reaction generate chelate, so the variable color amplitude narrows down, near determined water variable color observantly management hardness thus.And, owing to this hardness measurement reagent is made of a kind of liquid, so can handle and use reagent easily.
Embodiment
Below, embodiments of the present invention are described.Hardness measurement reagent of the present invention is characterised in that, is a kind of liquid and is non-aqueous, except that containing the pigment that is selected from EBT or the calmagite, triethanolamine, diol compound, also contains the alkali metal salt of sequestrant.
EBT or calmagite are to make itself and hardness components form chelate by the pH zone at alkali, and to the redness pigment of variable color significantly, they can use or mix the back individually and use from blueness.The cooperation ratio of pigment is not particularly limited, consider near management hardness, making the viewpoint that variable color takes place determined water observantly, be 0.24 weight % in order to make the hardness measurement reagent concentration in the determined water during interpolation, preferred hardness is measured with it is 0.1～1.0 weight % in the reagent, more preferably 0.1～0.5 weight %.
Triethanolamine is used for pH is maintained near 10, makes the color development of pigment stable.The cooperation ratio of triethanolamine is not particularly limited, and from inhibition triethanolamine freezing reagent, and keeps the viewpoint of the suitable viscosity of reagent to consider that preferred hardness is measured with it is 10～80 weight % in the reagent, more preferably 30～50 weight %.
Diol compound is as the solvent of hardness measurement reagent.Diol compound for example has ethylene glycol, propylene glycol, diethylene glycol etc., and it can use or mix two or more uses separately.Wherein, consider preferred especially ethylene glycol from decomposition that suppresses pigment and the aspect of freezing that prevents triethanolamine.The cooperation ratio of diol compound is not particularly limited, and plays the viewpoint of non freezing solution effect and consider that preferably it is 10～80 weight % in hardness measurement reagent, more preferably 30～50 weight % from reagent.
The sequestrant that constitutes the alkali metal salt of sequestrant can use organic system sequestrant or inorganic chelating agent.The organic system sequestrant for example has ethylenediamine tetraacetic acid (EDTA), anti-form-1,2-diamino-cyclohexane tetraacethyl (CyDTA), neighbour, neighbour-two (2-amino-ethyl) ethylene glycol tetraacetic amino carboxylic acids such as (GEDTA), citric acid, gluconic acid etc., these can use or mix two or more uses separately.Inorganic chelating agent for example has known phosphate cpds such as pyrophosphoric acid, polyphosphoric acid, metaphosphoric acid.Wherein, from considering preferred organic system sequestrant, preferred amino carboxylic acid in the organic system sequestrant with viewpoint more preferential than pigment and the chelating formation ability that hardness components is reacted.Form ability and economic viewpoint consideration from aforementioned chelating, preferred especially EDTA in the amino carboxylic acid.
The alkaline metal that constitutes the alkali metal salt of sequestrant for example has Na and K.The alkali metal salt of EDTA for example has EDTA-Na, EDTA-K, EDTA-2Na, BDTA-3Na, BDTA-3K, BDTA-4Na, EDTA-4K etc.Wherein, the good deliquescent viewpoint when being added on determined water is considered, preferred especially EDTA-2Na, EDTA-3Na and BDTA-4Na.The alkali-metal cooperation ratio of sequestrant is not particularly limited, from near management hardness, making the viewpoint consideration of variable color observantly of determined water, preferably in hardness measurement reagent, contain it so that can equivalence add " management hardness-0.1～2.0ppm " in the determined water.
In addition, can replace the alkali metal salt of sequestrant in the hardness measurement reagent of the present invention, or mixing contains the cationite with alkali-metal gegenion.Described cationite preferably has the little functional group of dissociation constant of hardness components, for example Sodium styrene sulfonate etc.The cooperation ratio of this cationite is preferably to cooperate with the same ratio of the alkaline metal of sequestrant.
In the hardness measurement reagent of the present invention in the scope that does not influence effect of the present invention, beyond the alkaline metal of depigmentation, triethanolamine, diol compound and sequestrant, can also suitably cooperate adjuvants such as screening agent, sensitizer, deterioration preventing agent, defoamer.Screening agent forms part by making the interfering ion (for example Fe, Mn, Al etc.) in itself and the determined water, makes the color development stabilization of determined water, and triethanolamine is for example arranged, KCN etc., and wherein triethanolamine is preferably used in the security consideration after the draining.Sensitizer passes through the Ca in the determined water
2+Be substituted by Mg
2+, make the color emissivity enhanced sensitivity of determined water.For example, preferably use EDTA-Mg.The cooperation ratio of sensitizer is not particularly limited, and from make the viewpoint consideration of variable color observantly of determined water near management hardness, preferred hardness is measured and contained in the reagent so that can add in determined water more than the equivalent of management hardness.Deterioration preventing agent is that hardness measurement reagent places under the situation of the high temperature more than 50 ℃ and can prevent the pigment deterioration, for example preferably uses potassium sorbate.Defoamer is to eliminate the material that is contained in the bubble in the determined water of measuring in the container, preferably uses non-ionic surfactant (for example NONIN HS 240).
Hardness measurement reagent of the present invention can be by making the alkali metal salt of pigment, triethanolamine, diol compound and sequestrant, and the adjuvant that adds as required evenly mixes, and makes.For example, diol compound and triethanolamine are mixed equably, then, the adjuvant that adds successively and mix the alkali metal salt of chelant compounds, add as required by adding pigment and mixing, can be made uniform hardness measurement reagent at last.
And hardness measurement reagent of the present invention mixes by the alkali metal salt that makes pigment, triethanolamine, diol compound and sequestrant, as a kind of liquid, can measure the hardness in the determined water.The reagent of described a kind of liquid is to contain the required constituent of hardness measurement, as a kind of hardness measurement reagent of solution.Therefore, when using this hardness measurement reagent, than adding each constituent respectively and mix when using, operation and easy to use does not need the determination step of complexity.
Then, when being added on the hardness measurement reagent of the former alkali metal salt that does not cooperate sequestrant in the determined water, the tonal variation of relevant determined water, the fact known to the present inventor is described, and on the basis of this fact, effect of the present invention and the preferred method of using are described.At first, in not having the determined water of hardness components, add and use under the situation of EBT as the hardness measurement reagent of pigment, the pigment that contains in the hardness measurement reagent is because to exist under the state that does not generate chelate, do not react, so determined water presents blueness.And, at the chelate that generates and unreacted pigment with chelate: unreacted pigment=20～30: in the presence of 80～70 the mol ratio, determined water changes to bluish violet from blueness.And along with the ratio that exists of the relative unreacted pigment of chelate increases, determined water changes to aubergine from bluish violet, the unreacted pigment fully and hardness components react, and only exist under the situation of chelate, determined water presents redness, arrives the variable color terminal point.
Consider aforementioned viewpoint from the amount of pigment this respect that determined water, adds, as can be known, in the pigment after the interpolation, 20～30% (metachromism ratios) and hardness components react, when generating chelate, determined water begins variable color, present bluish violet, in the pigment that adds, during 100% generation chelate, determined water variable color finishes, and presents redness.Therefore, to manage hardness when for example being set at 1mg/L (1ppm just), if in determined water, add the pigment that is equivalent to hardness 1ppm, be the variable color starting point then with hardness 0.2～0.3ppm, determined water presents bluish violet, the beginning variable color is so (hardness 0.2～0.3ppm) is equivalent to hardness 0.7～0.8ppm part to the variable color amplitude of variable color terminal point (hardness 1ppm) from the variable color starting point.
Just, when the pigment of the amount that will be equivalent to manage hardness is added in the determined water, under 20～30% the hardness that management hardness is, determined water begins variable color, when so the hardness in the determined water is in the variable color amplitude, when measuring the tone of determined water, be difficult to hardness to judge whether near management hardness or whether much lower than management hardness.Therefore, in order positively to carry out above-mentioned judgement, the variable color amplitude that need narrow perhaps can positively be judged the hardness leakage by the variable color amplitude that narrows.
Therefore, among the present invention, constituent as hardness measurement reagent, by cooperating the alkali metal salt of sequestrant, the hardness components that sequestrant is had precedence in pigment and the determined water generates chelate, residual hardness components and pigment reaction generate chelate, and the variable color amplitude that can narrow like this makes near the variable color observantly management hardness of determined water.
Particularly, management hardness is with aforementioned identical, be set at 1ppm, hardness being equivalent to the alkali metal salt of sequestrant of 0.5ppm and the pigment that hardness is equivalent to 0.5ppm is added in the determined water, at this moment the preferential and hardness of the alkali metal salt of the sequestrant hardness components that is equivalent to 0.5ppm is reacted, generate chelate, residual then hardness components and pigment reaction.At this moment variable color starting point is 0.6～0.65ppm, and the variable color terminal point is 1ppm.Therefore, variable color amplitude is 0.35～0.4ppm part.If relatively have or not aforementioned two examples of the alkali metal salt of sequestrant, when then cooperating the alkali metal salt of sequestrant in hardness measurement reagent, the variable color amplitude narrows to 0.37～0.42ppm.Just, identical with the former in the example by the aforementioned latter by the variable color terminal point is set, under this state, make the variable color starting point near variable color terminal point side, the variable color amplitude is narrowed.As mentioned above, the alkali metal salt that the present invention can be by suitably changing sequestrant and the cooperation ratio of pigment are freely set the variable color amplitude, can make the variable color observantly of determined water near management hardness thus.To manage hardness and set highly more, effect of the present invention is remarkable more, compares with former hardness measurement reagent, and the use level of pigment is few more.
In order to use hardness measurement reagent of the present invention to improve the mensuration precision of hardness, preferably pre-determine after the condition determinations such as capacity of determined water of addition, collection of concentration, the hardness measurement reagent when measuring of the alkali metal salt of the pigment concentration that contains in the hardness measurement reagent and sequestrant, measure.Concrete is when adding hardness measurement reagent in determined water, operate, make pigment contain 0.00024～0.0024 weight % in determined water, triethanolamine contains more than the 0.05 weight %, and the alkali metal salt of sequestrant contains 0.00006～0.0012 weight %.In addition, the concentration preferably calculated of the concentration in the hardness measurement reagent of pigment with following formula.
Several 1
As mentioned above, use hardness measurement reagent of the present invention, can near management hardness, make the variable color observantly of determined water,, use but be suitable for Instrument measuring too so be particularly suitable for estimating by colorimetric.In addition, among the present invention, can be with the determination object as hardness such as water in all water supply of supplying with Heating and cooling instrument device class, the cold warm water system or boiler water.Therefore, for example be not only limited to softening processing water by aforementioned sclerosis softening plant, also can with by the former water before the water-softening equipment as the hardness measurement object.
Embodiment
Below, the present invention is illustrated in further detail that the present invention is not subjected to any restriction of embodiment by embodiment.
Detect the preparation of water
As shown in table 1, hardness is set at 9 levels of 0mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.2mg/L, 1.4mg/L, 1.6mg/L, 2.0mg/L and 4.0mg/L, M basicity is set at 5mg/L, 40mg/L and 120mg/L three levels, and preparation detects water.In addition, when adjusting hardness, observe Ca
2+And Mg
2+The asynchronous tone difference that compares, the mol ratio that makes each is Ca
2+: Mg
2+=4:1,1:2, Ca under the preparation same rigidity
2+And Mg
2+Compare different 2 kinds detect water.When preparation detected water, hardness utilized ICP to confirm, M basicity uses 1/50N sulfuric acid to confirm by titration.
The preparation of hardness measurement reagent
Composition as shown in table 2 cooperates EBT, triethanolamine, ethylene glycol, EDTA-Mg and EDTA-4Na respectively, stirs fully and dissolves, and prepares 4 kinds of hardness measurement reagents.
Embodiment 1～5 and comparative example 1～3
50 milliliters detection water is put into 100 milliliters beaker, utilize micro syringe that 121 microlitre hardness measurement reagents are splashed into and detect in the water, beaker gently vibrates.Detect water color development at once.Observe tone from color development after 1 minute.The results are shown in table 1.In addition, the variable color starting point of each test site that obtains according to table 1 result, variable color terminal point and variable color amplitude are shown in table 3.In this test, splash into the hardness equipotent concentration of EBT and EDTA-4Na in the hardness measurement reagent that respectively detects behind the water, use CaCO
3Convert, reagent 1 is 2.2mg/L (EDTA-4Na is 0.7mg/L, and EBT is 1.5mg/L), and reagent 2 is 3.5mg/L (EDTA-4Na is 1.0mg/L, and EBT is 2.5mg/L), and reagent 3 and reagent 4 are 2.5mg/L (EBT is 2.5mg/L).
Table 1
Table 2
Table 3
As known from Table 3, embodiment 1～4 is narrower than the variable color amplitude of comparative example 1～3.Hence one can see that, for this embodiment, for example will manage hardness when being set at 2.0mg/L, by contain EDTA-4Na in hardness measurement reagent, can make and detect near water variable color observantly hardness 2.0mg/L, can judge positively that thus hardness leaks.In addition, compare reagent 1 (embodiment 1～3) and reagent 2 (embodiment 5), variable color starting point as can be known is all different with the variable color terminal point, and the variable color amplitude of reagent 1 is narrow.Therefore, for this embodiment,, can freely control color development starting point and variable color amplitude by changing the cooperation ratio of BDTA-4Na and EBT.
Claims (2)
1, a kind of hardness measurement reagent that is made of a kind of liquid is characterized in that, contains the alkali metal salt of the pigment, triethanolamine, diol compound, EDTA-Mg and the amino carboxylic acid that are selected from eriochrome black T or the calmagite.
2, hardness measurement reagent as claimed in claim 1 is characterized in that, the alkali metal salt of described amino carboxylic acid is the Na salt of EDTA.
Applications Claiming Priority (6)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP99173/04 | 2004-03-30 | ||
| JP2004099173 | 2004-03-30 | ||
| JP99173/2004 | 2004-03-30 | ||
| JP2005059226A JP4222327B2 (en) | 2004-03-30 | 2005-03-03 | Reagent for hardness measurement |
| JP59226/05 | 2005-03-03 | ||
| JP59226/2005 | 2005-03-03 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1677090A CN1677090A (en) | 2005-10-05 |
| CN100538342C true CN100538342C (en) | 2009-09-09 |
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|---|---|---|---|
| CNB2005100627057A Expired - Fee Related CN100538342C (en) | 2004-03-30 | 2005-03-30 | Hardness measurement reagent |
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|---|---|
| JP (1) | JP4222327B2 (en) |
| KR (1) | KR20060044816A (en) |
| CN (1) | CN100538342C (en) |
| TW (1) | TW200538733A (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007263632A (en) * | 2006-03-28 | 2007-10-11 | Miura Co Ltd | Method and kit for measuring chelating agent |
| JP5002418B2 (en) * | 2007-11-02 | 2012-08-15 | 野村マイクロ・サイエンス株式会社 | Leak monitoring device |
| CN102539329A (en) * | 2011-11-24 | 2012-07-04 | 沈阳理工大学 | Method for measuring total hardness of industrial water |
| JP5949822B2 (en) | 2014-03-28 | 2016-07-13 | 栗田工業株式会社 | Hardness measuring composition, hardness measuring reagent kit, hardness measuring method, and antifouling method in hardness measuring apparatus |
| CN104267144B (en) * | 2014-10-16 | 2016-05-18 | 天津农学院 | Total hardness of water test fluid and preparation method thereof and using method for aquaculture and the Shui nationality |
| CN108333296A (en) * | 2018-01-26 | 2018-07-27 | 山东五洲检测有限公司 | A kind of determining total hardness of water detection agent and preparation method thereof |
| CN114441524A (en) * | 2022-02-14 | 2022-05-06 | 上海蓝长自动化科技有限公司 | Water hardness determination reagent combined with continuous flow analyzer |
-
2005
- 2005-03-03 JP JP2005059226A patent/JP4222327B2/en active Active
- 2005-03-28 KR KR1020050025322A patent/KR20060044816A/en not_active Application Discontinuation
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| JP4222327B2 (en) | 2009-02-12 |
| JP2005315857A (en) | 2005-11-10 |
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