CN103926242A - Method for rapidly detecting borate in drinking water - Google Patents
Method for rapidly detecting borate in drinking water Download PDFInfo
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- CN103926242A CN103926242A CN201410160188.6A CN201410160188A CN103926242A CN 103926242 A CN103926242 A CN 103926242A CN 201410160188 A CN201410160188 A CN 201410160188A CN 103926242 A CN103926242 A CN 103926242A
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Abstract
The invention discloses a method for rapidly detecting borate in drinking water. The method comprises the following steps: adsorbing borate in a large-volume water sample through a high-efficiency adsorption column for detecting multiple harmful negative ions in the drinking water (the packing is layered magnesium aluminum hydroxide), and eluting the borate attached to an adsorbent by using a small-volume eluent, so that high-rate concentration is realized; developing the concentrated borate and an indicator under the condition that a certain amount of buffer solution is added, comparing with colors on a color chart, judging whether the borate in the water sample exceeds the standard, and thus finishing preliminary screening of the water sample. According to the method for rapidly detecting borate in drinking water, detection of the borate in the water sample can be finished on site, and the method has the advantages of low time consumption, high sensitivity, simple and convenient operation, low cost and the like. According to the method, the detection limit can reach 0.05mg/L.
Description
Technical field
The invention belongs to technical field of analytical chemistry, be specifically related to a kind of method for quick of potable water mesoboric acid salt.
Background technology
Boron is a kind of special inorganic non-metallic element, is typical lacked electron atom.In the Nature, general and oxygen coordination, forms boron oxygen acid or Borate.In food service industry, boric acid is through being often used as the antiseptic of breast, dairy products, meat or bean product; Particularly borax, can be used for food antiseptic, increases food elasticity, fragility, makes the effects such as food expansion; And in chemical industry, boric acid is the primary raw material of manufacturing the various borides such as boron nitride, boron carbide, boric acid also can be used for the manufacture of leather industry, photograph and jewel; In agricultural, boric acid can be used for doing fertilizer and pesticide; In medical treatment, be usually used in sanitizer and anti-corruption dose, visible boric acid and borate have been prevalent among the mankind's productive life.But in recent years, water pollution condition is day by day serious, many enterprises directly enter the factory effluent of undressed boracic in drinking water source, cause boron pollution.
Although the boron of trace is useful to human body, can enhance metabolism, will cause serious harm to human body but go beyond the limit.Research shows, absorbs continuously borate and can make it in internal organs, accumulate, and the high toxicity symptom that there will be of content, severe patient even there will be shock and stupor.
Borate detection technique mainly concentrates on ICP-MS (single sample only needs 12 minutes detection time), spectrophotometric method and test paper method etc. both at home and abroad at present.ICP-MS method need possess stronger professional knowledge, and hardware requirement is high, can not be used for Site Detection; Spectrophotometric method spent time is longer; Test paper method have sensitivity low, easily the problem such as be disturbed.Simultaneously, China's water quality detection ability is also troubling, and national Jin You minority mechanism has the detectability of 106 full indexs, and most detectability is lower than 51, average detected ability only has 33, and the water quality detection ability of most of county-level city is lower than average national level.In some rural area of China, even city does not also possess borate detectability, is therefore badly in need of a kind of simple to operate, highly sensitive, boratory method of fast detecting short, that cost is low consuming time.
Summary of the invention
The object of the present invention is to provide a kind of method for quick of potable water mesoboric acid salt, can on-the-spot complete the detection of water sample mesoboric acid salt, there is short, low cost and other advantages simple to operate, highly sensitive, consuming time.
For achieving the above object, the present invention adopts following technical scheme:
A method for quick for potable water mesoboric acid salt, adopts the borate in efficient adsorption post absorption water sample with bulk mass, then with eluant, eluent by the borate wash-out in adsorption column, realize high multiple concentrated; Borate after concentrated is added in damping fluid, after indicator colour developing, by with colorimetric card on color contrast judge that whether water sample mesoboric acid salt exceeds standard, and completes the primary dcreening operation of water sample.
Described its filler of efficient adsorption post is particle diameter 80-200 object stratiform magaldrate, and quality is 0.5-5g, and specification is: internal diameter 10-30mm, and volume 50-100mL, sieve plate material is glass core, and aperture is 20-120 μ m, and nylon cloth order number is 100-500 order.
Its volume of described water sample with bulk mass is 100-1000mL.
Its consumption of described eluant, eluent is 1-10ml, eluant, eluent is one or both in NaCl aqueous solution, NaOH solution, the volume ratio of NaCl aqueous solution, NaOH aqueous solution is 0:11-11:0, and wherein the concentration of NaCl aqueous solution is 1-5mol/L, and the concentration of NaOH aqueous solution is 0.1-1mol/L.
Described damping fluid is one or more in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, ammonium acetate, and pH is 5.2-5.9,
Described indicator is one or several of azomethine-H ﹑ Jiang Huang Su ﹑ famille rose, and its solution concentration is 1-10g/L, and consumption is 0.5mL-2mL.
Described colorimetric khaki manufacturing conditions is: will be the borate titer of concentration gradient and damping fluid, indicator reaction, be made according to the borate of each concentration and the corresponding relation of color after reaction.
Remarkable advantage of the present invention is: potable water mesoboric acid salt method for quick of the present invention can on-the-spot complete the detection of water sample mesoboric acid salt, has short, low cost and other advantages simple to operate, highly sensitive, consuming time.The method detectability can reach 0.05mg/L.
Specific embodiment
Following embodiment further sets forth the present invention, but the present invention is not limited only to this.
Colorimetric card method for making
Compound concentration is the borate standard solution of 0mg/L, 0.02mg/L, 0.5mg/L, 1mg/L, 5mg/L, 10mg/L, getting respectively 100ml crosses " the efficient adsorption post that in potable water, multiple harmful anion detects " and carries out enrichment, with the borate on 5ml eluant, eluent wash-out adsorbent, after twice of wash-out, the damping fluid and the 1ml indicator that add 1ml, mix, and leaves standstill 20min, use cameras record color developing effect, make colorimetric card.
embodiment 1
The inventive method is to the different water sample mesoboric acid salt recovery
Efficient adsorption post: filler is particle diameter 80-200 object stratiform magaldrate, and quality is 0.5g, and specification is: internal diameter 10mm, volume 50mL, sieve plate material is glass core, and aperture is 20 μ m, and nylon cloth order number is 500 orders.
Collect several frequently seen potable water water sample, add respectively the mark liquid of containing borate, making boratory concentration is limitation concentration 0.5mg/L and the 5mg/L specifying in GB, then respectively get 100mL aqueous sample stream through adsorption column, adsorbed rear with the borate in the NaCl aqueous solution wash-out adsorption column of 5mL 3mol/L, by spectrophotometry eluent mesoboric acid salinity.The parallel survey of each sample 3 times, calculates average recovery rate, standard deviation and relative standard deviation, the different water samples that record the results are shown in Table 1:
The recovery of standard addition (n=3) of the different potable water samples of table 1
Result shows that the recovery of different water samples stabilizes to 55% left and right, has proved the stability of the inventive method, has ensured the reliability of testing result.Although the recovery is not high, the boratory concentration under this recovery can meet the requirement that makes indicator colour developing.
embodiment 2
Tap water testing result and the comparison of interpolation borate testing result
Experimental selection tap water, testing result shows in tap water not containing borate.
Its filler of efficient adsorption post is particle diameter 80-200 object stratiform magaldrate, and quality is 5g, and specification is: internal diameter 30mm, and volume 100mL, sieve plate material is glass core, and aperture is 60 μ m, and nylon cloth order number is 100 orders.
With method of the present invention adsorb, wash-out, process color.Get the 100mL tap water water sample adsorption column of flowing through, adsorb rear with the borate on 5mL 0.5 mol/L NaOH aqueous solution wash-out adsorbent, collect eluent and 1ml acetic acid, ammonium acetate buffer that 5mL flows out, the curcumin that pH is 5.4,1ml concentration is 5g/L reacts.
Measuring respectively 100mL deionized water, 100mL tap water, 100mL adds boratory tap water (borate concentration is limitation concentration 0.5mg/L and 5mg/L and the lowest detectable limit 0.05mg/L specifying in GB) and completes absorption, wash-out, process color by the inventive method.Result shows that 100mL deionized water, the chromogenic reaction color that 100mL tap water is corresponding are close, do not demonstrate obvious yellow, in the time using the inventive method to detect, there is not interference problem in visible tap water, and 100mL adds the eluent that boratory tap water is corresponding and can show obvious yellow, borate and curcumin produce yellow complex.
Embodiment 3
Drinking pure water testing result and the comparison of interpolation borate testing result
The happy precious drinking pure water in experimental selection China Resources, testing result shows the happy precious drinking pure water in China Resources.
Its filler of efficient adsorption post is particle diameter 80-200 object stratiform magaldrate, and quality is 2.5g, and specification is: internal diameter 20mm, and volume 75mL, sieve plate material is glass core, and aperture is 120 μ m, and nylon cloth order number is 300 orders.
With method of the present invention adsorb, wash-out, process color.Get 100mL aqueous sample stream through adsorption column, adsorbed the rear 5mLNaCl of using and NaOH mixed solution, the volume ratio of NaCl aqueous solution, NaOH aqueous solution is 4:11, and wherein the concentration of NaCl aqueous solution is 5mol/L, the concentration of NaOH aqueous solution is 0.1 mol/L, the borate on wash-out adsorbent.Collect eluent and 1ml sulfuric acid and hydrochloride buffer that 5mL flows out, pH is the carmine reaction of 5.2-5.9,2ml 10g/L.
Measuring respectively 100mL deionized water, the happy precious drinking pure water in 100mL China Resources, 100mL adds the happy precious drinking pure water in boratory China Resources (borate concentration is limitation concentration 0.5mg/L and 5mg/L and the lowest detectable limit 0.05mg/L specifying in GB) and completes absorption, wash-out, process color by the inventive method.Result shows that 100mL deionized water, the chromogenic reaction color that the happy precious drinking pure water in 100mL China Resources is corresponding are close, do not demonstrate blueness, in the time using the inventive method to detect, there is not interference problem in the happy precious drinking pure water in visible China Resources, and 100mL adds boratory China Resources eluent corresponding to happy precious drinking pure water and can show blueness, i.e. borate and the carmine blue complex that produces.
Embodiment 4
Mineral water testing result and the comparison of interpolation borate testing result
Experimental selection NongFuShanQuan mineral water.Testing result shows not containing borate of NongFuShanQuan mineral water.
Its filler of efficient adsorption post is particle diameter 80-200 object stratiform magaldrate, and quality is 4g, and specification is: internal diameter 25mm, and volume 80mL, sieve plate material is glass core, and aperture is 100 μ m, and nylon cloth order number is 300 orders.
With method of the present invention adsorb, wash-out, process color.Get 100mL aqueous sample stream through adsorption column, having adsorbed rear is the mixed solution of NaCl and NaOH with 5mL eluant, eluent, the volume ratio of NaCl aqueous solution, NaOH aqueous solution is 11:1, and wherein the concentration of NaCl aqueous solution is 1 mol/L, and the concentration of NaOH aqueous solution is 1mol/L.Borate on wash-out adsorbent, the damping fluid of the eluent that collection 5mL flows out and 1ml hydrochloric acid, phosphoric acid, pH is 5.2-5.9,1ml 1g/L azomethine-H reaction.
Measuring respectively 100mL deionized water, 100mL NongFuShanQuan mineral water, 100mL adds boratory NongFuShanQuan mineral water (borate concentration is limitation concentration 0.5mg/L and 5mg/L and the lowest detectable limit 0.05mg/L specifying in GB) and completes absorption, wash-out, process color by the inventive method.Result shows that 100mL deionized water, the chromogenic reaction color that 100mL tap water is corresponding are close, do not demonstrate obvious yellow, in the time using the inventive method to detect, there is not interference problem in visible NongFuShanQuan mineral water, can show obvious yellow and 100mL adds the eluent that boratory tap water is corresponding, borate and azomethine-H produces yellow complex.
The detectability of the inventive method can reach 0.05mg/L.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (7)
1. a method for quick for potable water mesoboric acid salt, is characterized in that: adopt the borate in efficient adsorption post absorption water sample with bulk mass, then with eluant, eluent by the borate wash-out in adsorption column, realize high multiple concentrated; Borate after concentrated is added in damping fluid, after indicator colour developing, by with colorimetric card on color contrast judge that whether water sample mesoboric acid salt exceeds standard, and completes the primary dcreening operation of water sample.
2. the method for quick of potable water mesoboric acid salt according to claim 1, it is characterized in that: described its filler of efficient adsorption post is particle diameter 80-200 object stratiform magaldrate, quality is 0.5-5g, specification is: internal diameter 10-30mm, volume 50-100mL, sieve plate material is glass core, and aperture is 20-120 μ m, and nylon cloth order number is 100-500 order.
3. the method for quick of potable water mesoboric acid salt according to claim 1, is characterized in that: its volume of described water sample with bulk mass is 100-1000mL.
4. the method for quick of potable water mesoboric acid salt according to claim 1, it is characterized in that: its consumption of described eluant, eluent is 1-10ml, eluant, eluent is one or both in NaCl aqueous solution, NaOH solution, the volume ratio of NaCl aqueous solution, NaOH aqueous solution is 0:11-11:0, wherein the concentration of NaCl aqueous solution is 1-5mol/L, and the concentration of NaOH aqueous solution is 0.1-1mol/L.
5. the method for quick of potable water mesoboric acid salt according to claim 1, is characterized in that: described damping fluid is one or more in sulfuric acid, hydrochloric acid, phosphoric acid, acetic acid, ammonium acetate, and pH is 5.2-5.9, and consumption is 0.5mL-2mL.
6. the method for quick of potable water mesoboric acid salt according to claim 1, is characterized in that: described indicator is one or several of azomethine-H ﹑ Jiang Huang Su ﹑ famille rose, and its solution concentration is 1-10g/L, and consumption is 0.5mL-2mL.
7. the method for quick of potable water mesoboric acid salt according to claim 1, it is characterized in that: described colorimetric khaki manufacturing conditions is: will be the borate titer of concentration gradient and damping fluid, indicator reaction, be made according to the borate of each concentration and the corresponding relation of color after reaction.
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Cited By (2)
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CN104297234A (en) * | 2014-10-11 | 2015-01-21 | 北京华益精点生物技术有限公司 | Preparation methods of color developing agent and test paper for testing boric acid and borax |
CN104730071A (en) * | 2015-03-27 | 2015-06-24 | 河南中烟工业有限责任公司 | Reactive extraction colorimetric device and measuring method for measuring boric acid content in water-based adhesive |
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CN102507465A (en) * | 2011-10-17 | 2012-06-20 | 攀钢集团江油长城特殊钢有限公司 | Novel turmeric direct photometry for determining boron content in steel |
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CN1766561A (en) * | 2005-10-31 | 2006-05-03 | 白莉 | Boron determination solution and colorimetric determination tube therefor |
CN102507465A (en) * | 2011-10-17 | 2012-06-20 | 攀钢集团江油长城特殊钢有限公司 | Novel turmeric direct photometry for determining boron content in steel |
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104297234A (en) * | 2014-10-11 | 2015-01-21 | 北京华益精点生物技术有限公司 | Preparation methods of color developing agent and test paper for testing boric acid and borax |
CN104730071A (en) * | 2015-03-27 | 2015-06-24 | 河南中烟工业有限责任公司 | Reactive extraction colorimetric device and measuring method for measuring boric acid content in water-based adhesive |
CN104730071B (en) * | 2015-03-27 | 2018-05-01 | 河南中烟工业有限责任公司 | Measure the reaction, extraction colorimetric device and measuring method of boric acid content in water base adhesive |
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