CN100498291C - Beryllium determination solution and colorimetric determination tube therefor - Google Patents
Beryllium determination solution and colorimetric determination tube therefor Download PDFInfo
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- CN100498291C CN100498291C CNB2005100484706A CN200510048470A CN100498291C CN 100498291 C CN100498291 C CN 100498291C CN B2005100484706 A CNB2005100484706 A CN B2005100484706A CN 200510048470 A CN200510048470 A CN 200510048470A CN 100498291 C CN100498291 C CN 100498291C
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- sodium salt
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Abstract
The invention relates to a method for measuring the trace amount chemicals in water mass and related analyzer, in particular an analyzing liquid and colorimetric analyzing tube for quick measurement of beryllium content in water mass. The beryllium analyzing liquid comprises 0.01% azo napsylate 1-15 unit volume, and pH buffer liquid 1-50 unit volume, the analyzing tube contains uniform cross-section vacuum sealed glass tube, the glass tube is equipped with beryllium analyzing liquid, The ratio of the height H1 of the analyzing liquid in the glass tube and the height H2 of the glass tube uniform cross-section vacancy is H1:H2 =1:2-25. The invention can realize quick-speed simplified measurement, higher accuracy, and longer retention time.
Description
One. technical field: the present invention relates to the assay method of trace level chemical substance in a kind of water quality and measure utensil, particularly relate to beryllium Determination on content liquid and colorimetric cylinder thereof in a kind of fast measuring water quality.
Two. background technology: beryllium and toxicity of compound thereof are extremely strong, even also can conjunctiva, cornea are inflamed owing to local excitation injures skin, mucous membrane on a small quantity, cause diseases such as pulmonary emphysema, pneumonia.Because the toxicity of beryllium is extremely strong and continuous action is also very strong, even if suck the trace beryllium people is poisoned, suck more beryllium people's death by poisoning is died.The industrial pollution source of beryllium mainly comes from the factory effluent of industries such as smelting, mining and feature material, radio component parts and instrument part.
The method of traditional test beryllium content is the chrome azurol S photometry, and its operation steps is:
(1) the sample pretreatment water sample that will contain large amount of organic is cleared up with nitric acid-sulfuric acid, has interfering material to exist or the extremely low water sample of beryllium content activated charcoal separation and concentration.
(2) sample determination is got an amount of water sample in color comparison tube, is adjusted to faintly acid, adds Na successively
2-EDTA solution 2mL, 0.1% chrome azurol S 2mL, ammonia buffer 5mL, cetylpyridinium chloride 1mL adds the 150mg activated charcoal behind the mixing, stir evenly the back and placed 10 minutes, with the filtration of bleeding of the speed of 10mL/min, discards filtrate.The 25mL color comparison tube is put into bottle,suction, and the hydrochloric acid 6mL that seethes with excitement with 2mol/L divides dropping detergent active charcoal three times, uses low amounts of water detergent active charcoal again, gives suction filtration after every dropping once.Take out color comparison tube, add 1 of phenolphthalein solution in pipe, be neutralized to the micro-redness of solution with 1:1 ammoniacal liquor, the HCl residual titration with 2mol/L just disappears to red again.Heating is 5 minutes in 60 ℃ of water-baths, takes out and places 30 minutes.Measure absorbance at the 618nm place with the 20mm cuvette.After the absorbance by the absorbance deduction blank sample of measuring gained, find the content of beryllium, by formula calculate beryllium content in the sample then from typical curve.
(3) a drawing standard curve peek color comparison tube adds the beryllium standard solution respectively, by the above-mentioned steps operation, and draws through the absorbance of the blank correction typical curve to beryllium content.
The problem that the chrome azurol S photometry exists: (1) needs to use the beryllium standard solution, and artificial pollutes, and harmful; (2) in the mensuration process, use varieties of reagent many, palpus separation, enrichment and heat treated, complex operation, complexity; (3) need with the Instrument measuring absorbance and with formula calculating concentration value, high to the operator quality requirement, the testing cost costliness.
Three. summary of the invention:
The object of the invention: simplify the beryllium testing procedure, shorten minute greatly, alleviate intensity of workers, reduce or the eliminating secondary pollution, make beryllium determination solution and colorimetric cylinder thereof.
Technical solution of the present invention:
The invention provides a kind of beryllium determination solution, represent with unit volume, described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume and pH damping fluid 1～50 unit volume, and mixed preparing forms; Described Anazolene Sodium salt is (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt or 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt, described PH damping fluid is KCl-NaOH damping fluid or borax-sodium hydrate buffer solution.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～6 unit volume, pH damping fluid 1～50 unit volume.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 6～11 unit volumes, pH damping fluid 1～50 unit volume.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 11～15 unit volumes, pH damping fluid 1～50 unit volume.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 1～18 unit volume.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 18～36 unit volumes.
Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 36～50 unit volumes.
A kind of beryllium colorimetric testing tube is vacuum sealing tube, contains the uniform cross section glass tube of end sealing, and the opening part of glass tube is communicated with the kapillary and the transition section of end sealing, and beryllium determination solution is housed in glass tube, measures the height H of liquid in glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1:2～25; Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume and pH damping fluid 1～50 unit volume, forms through mixed preparing; Described Anazolene Sodium salt is (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt or 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt, described PH damping fluid is KCl-NaOH damping fluid or borax-sodium hydrate buffer solution.
Described beryllium colorimetric testing tube, the height H of mensuration liquid in glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1:10～19.
Positive beneficial effect of the present invention:
1. the present invention is with the detection technique commercialization, and commercialization is loaded on the mensuration fluid-tight for preparing in the glass tube with vacuum, can directly use.Only need during operation to fracture in the water sample to be measured capillary tube segment of test tube makes in the water sample automatic ration tail pipe to be measured and measures liquid generation metachromasia, just can draw beryllium content more accurately with the contrast of standard color range behind the colour stable.Need not be when each test preparing standard solution, reagent, can simplify the detection step greatly, save minute, reduce workload, reduce labor intensity.
2. to measure formula of liquid reasonable in the present invention, advanced technology, and stable performance is used simple.Adopt standard sample liquid to react with it in advance, constant color forms permanent colour code standard, and encapsulation forms the contrast color range, carries out the scene and detects, and need not to prepare other any reagent, and testing result accurately and reliably.The standard colour code can be made by standard color range pipe of the present invention and form, also can be, or the colored printing cardboard, or the colored plastic rod by the computer color atlas, or other physical medium material such as stained glass goods forms, and uses very convenient.
3. compare with the method for traditional chrome azurol S spectrphotometric method for measuring beryllium, the present invention has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand beryllium be to carry out automatically under given conditions the glass tube with vacuum in the present invention, can effectively avoid accidental error and personal error, testing result meets the requirement of water analysis error precision accurately and reliably, and detection limit meets national sewage comprehensive emission standard.
The present invention carry, easy to use, measure simple fast, accurately, the holding time is long.The on-the-spot detection do not need the miscellaneous equipment instrument, saves human and material resources greatly, reduces integrated cost.The present invention is easy to promotion and implementation, has good social and economic benefit.
Testing tube of the present invention and chrome azurol S photometry data comparison sheet:
Four. description of drawings
Fig. 1: beryllium colorimetric testing tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects beryllium content in advance, form color range.For example make 9 the color range pipes of standard colour code that detect beryllium content in the water quality, beryllium content is respectively 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.04mg/L, 0.05mg/L, 0.06mg/L, 0.08mg/L, the standard colour code of 0.10mg/L.At first get 0.01% (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt 90mL, KCl-NaOH damping fluid 252mL is mixed and made into mensuration liquid.Making beryllium content then respectively is 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.04mg/L, 0.05mg/L, 0.06mg/L, 0.08mg/L, 0.10mg/L 9 kinds of normal concentration beryllium aqueous solution, will measure liquid and various normal concentration beryllium aqueous solution pours into reaction solution in 9 charomatrons respectively in 1: 10 ratio, and constant color, seal charomatron then, form non-fading serial color range standard colors mark pipe.The mensuration liquid concentration of production standard color range pipe is identical with the mensuration liquid concentration of supporting mensuration pipe, the ratio of mensuration liquid and normal concentration beryllium aqueous solution volume when measuring the corresponding formulation standard of the ratio color range pipe of liquid volume and the volume of leaving a blank in the pipe.Measure formula of liquid not simultaneously, the corresponding standard colour code of making, the color range of formation is also different.Only use the compound method of method description standard colour code for example at this.
Measure the pipe implementation method: referring to Fig. 1,1 is the uniform cross section glass tube with vacuum among the figure, and 2 is capillary tube segment, and 3 is beryllium determination solution.H
1For measuring liquid height, H
2For the uniform cross section glass tube with vacuum is left a blank highly.The mensuration liquid of the corresponding preparation standard colour code of present embodiment, promptly measuring liquid and aqueous solution volume ratio to be measured is 1:10.6.5 millimeters of uniform cross section vacuum glass external diameter of pipe, 14.2 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.1 centimetres, the height H of leaving a blank
2Be 11 centimetres, capillary tube segment length is 2.1 centimetres.
During use, the capillary tube segment of measuring pipe is immersed in the water sample to be measured, capillary tube segment fractures, be filled the uniform cross section glass tube with vacuum pipeline section of leaving a blank etc. water sample to be measured, take out to be inverted repeatedly and mix, make it fully to carry out chromogenic reaction, contrast with the standard colour code behind about 1～5 minute colour stable, be the beryllium content that records with the pairing beryllium concentration of the colour code numerical value that is near the mark most,, then get its mean value if measure the pipe color between two standard colour codes.
Beryllium colorimetric testing tube of the present invention is measured formula of liquid or is: represent with unit volume, contain 0.01% (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt 15 unit volumes, KCl-NaOH damping fluid 42 unit volumes.
Embodiment two: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 6.5 millimeters in the present embodiment, 21.8 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1 centimetre, the height H of leaving a blank
2Be 19 centimetres, capillary tube segment length is 1.8 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt 11 unit volumes, KCl-NaOH damping fluid 50 unit volumes.
Embodiment three: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 7.5 millimeters in the present embodiment, 28 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1 centimetre, the height H of leaving a blank
2Be 25 centimetres, capillary tube segment length is 2.0 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt 15 unit volumes, KCl-NaOH damping fluid 36 unit volumes.
Embodiment four: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 7 millimeters in the present embodiment, 18.8 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1 centimetre, the height H of leaving a blank
2Be 16 centimetres, capillary tube segment length is 1.8 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt 6 unit volumes, KCl-NaOH damping fluid 18 unit volumes.
Embodiment five: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 7 millimeters in the present embodiment, 12.7 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.2 centimetres, the height H of leaving a blank
2Be 9.6 centimetres, capillary tube segment length is 1.9 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt 1 unit volume, borax-sodium hydrate buffer solution 27 unit volumes.
Embodiment six: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 6.5 millimeters in the present embodiment, 23.1 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1 centimetre, the height H of leaving a blank
2Be 20 centimetres, capillary tube segment length is 2.1 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt 15 unit volumes, borax-sodium hydrate buffer solution 1 unit volume.
Embodiment seven: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.Standard colors target method for making, the making of measuring pipe and using method no longer are described in detail with embodiment one.Difference is:
Uniform cross section glass tube with vacuum external diameter is 7 millimeters in the present embodiment, 6.9 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.6 centimetres, the height H of leaving a blank
2Be 3.8 centimetres, capillary tube segment length is 1.5 centimetres.
Beryllium colorimetric testing tube in the present embodiment, the beryllium determination solution prescription is: represent with unit volume, contain 0.01% 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt 9 unit volumes, borax-sodium hydrate buffer solution 23 unit volumes.
Claims (9)
1, a kind of beryllium determination solution is characterized in that: represent that with unit volume described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume and pH damping fluid 1～50 unit volume, mixed preparing forms; Described Anazolene Sodium salt is (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt or 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt, described PH damping fluid is KCl-NaOH damping fluid or borax-sodium hydrate buffer solution.
2, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 1～6 unit volume, pH damping fluid 1～50 unit volume.
3, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 6～11 unit volumes, pH damping fluid 1～50 unit volume.
4, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 11～15 unit volumes, pH damping fluid 1～50 unit volume.
5, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 1～18 unit volume.
6, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 18～36 unit volumes.
7, beryllium determination solution according to claim 1 is characterized in that: contain 0.01% Anazolene Sodium salt 1～15 unit volume, pH damping fluid 36～50 unit volumes.
8, a kind of beryllium colorimetric testing tube, be vacuum sealing tube, contain the uniform cross section glass tube of end sealing, the opening part of glass tube is communicated with the kapillary and the transition section of end sealing, it is characterized in that: beryllium determination solution is housed in glass tube, measures the height H of liquid in glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1:2～25; Described beryllium determination solution contains 0.01% Anazolene Sodium salt 1～15 unit volume and pH damping fluid 1～50 unit volume, forms through mixed preparing; Described Anazolene Sodium salt is (disulfo-8-hydroxyl naphthylazo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid tetrasodium salt or 2-(2-hydroxyl-3-carboxyl-5-sulfonic benzo azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid trisodium salt, described PH damping fluid is KCl-NaOH damping fluid or borax-sodium hydrate buffer solution.
9, beryllium colorimetric testing tube according to claim 8 is characterized in that: the height H of measuring liquid in glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1:10～19.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100484706A CN100498291C (en) | 2005-10-31 | 2005-10-31 | Beryllium determination solution and colorimetric determination tube therefor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100484706A CN100498291C (en) | 2005-10-31 | 2005-10-31 | Beryllium determination solution and colorimetric determination tube therefor |
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| CN1766560A CN1766560A (en) | 2006-05-03 |
| CN100498291C true CN100498291C (en) | 2009-06-10 |
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|---|---|---|---|
| CNB2005100484706A Expired - Fee Related CN100498291C (en) | 2005-10-31 | 2005-10-31 | Beryllium determination solution and colorimetric determination tube therefor |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102519952B (en) * | 2011-11-25 | 2015-04-08 | 佛山市中南农业科技有限公司 | Reagent and method for rapidly determining borax in food by use of reagent |
| CN104215630A (en) * | 2013-11-12 | 2014-12-17 | 张文知 | Method for rapidly measuring beryllium in mineral rocks |
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Non-Patent Citations (4)
| Title |
|---|
| 新试剂CPAH-I的合成、纯化及与铍离子显色反应的研究. 唐文彪，徐继明，吴斌才.华东师范大学学报（自然科学版），第1期. 1999 |
| 新试剂CPAH-I的合成、纯化及与铍离子显色反应的研究. 唐文彪，徐继明，吴斌才.华东师范大学学报（自然科学版），第1期. 1999 * |
| 杂多核配位荧光增敏法测定痕量铍. 吴芳英，黄坚锋，嵇志琴.分析化学研究简报，第27卷第2期. 1999 |
| 杂多核配位荧光增敏法测定痕量铍. 吴芳英，黄坚锋，嵇志琴.分析化学研究简报，第27卷第2期. 1999 * |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract record no.: 2012410000012 Denomination of invention: Beryllium determination solution and colorimetric determination tube therefor Granted publication date: 20090610 License type: Exclusive License Open date: 20060503 Record date: 20120306 |
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