CN100535640C - Antimony determination solution and colorimetric determination tube therefor - Google Patents
Antimony determination solution and colorimetric determination tube therefor Download PDFInfo
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- CN100535640C CN100535640C CNB2005100485253A CN200510048525A CN100535640C CN 100535640 C CN100535640 C CN 100535640C CN B2005100485253 A CNB2005100485253 A CN B2005100485253A CN 200510048525 A CN200510048525 A CN 200510048525A CN 100535640 C CN100535640 C CN 100535640C
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- naphthols
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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 antimony content in water mass. The antimony analyzing liquid comprises 0.005% pyridine azocompound 1-30 unit volume, 0.5mol/L inorganic acid 1-50 unit volume, the analyzing tube contains uniform cross-section vacuum sealed glass tube, the glass tube is equipped with antimony 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 = 1:1-20. 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 the mensuration liquid and the colorimetric cylinder thereof of antimony content in a kind of fast measuring water quality.
Two. background technology:
Antimony Sb is silvery white metal, at occurring in nature mainly with Sb
3+, Sb
5+And Sb
3-Form exists, and the antimony hydride toxicity of negative trivalent is violent, in the occurring in nature instability, easily is decomposed into metal and water.And Sb
3+And Sb
5+In faintly acid facile hydrolysis precipitation to the neutral medium, therefore the concentration of antimony is extremely low in natural water, on average is about 0.2 μ g/L.The quality standard of water environment regulation antimony of Japan must be below 0.002mg/L.The waste water that the pollution of antimony is mainly discharged from industries such as ore dressing, metallurgy, plating, pharmacy, font printing, leathers in the water.
The conventional test methodologies of antimony is the 5-Br-PADAP photometry, and its operation steps is:
1. the drafting of typical curve
(1) takes place to add 0mL, 0.50mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL, 3.00mL, 3.50mL antimony standard solution respectively in the bottle in 8, add 25% tartrate 4mL, 5% thiocarbamide 4mL, (1+1) hydrochloric acid 12mL is diluted with water to 25mL, shakes up.
(2) in absorption tube, add the 5mL absorption liquid, put into 2 potassium borohydride tablets at the reagent storage place that bottle takes place, install wireway, the jam-pack rubber stopper, bottle will take place gently to lopsidedness, allow wherein a slice " tablet " falls into solution, after question response stops, again another tablet is fallen into solution, to drive residual gas.
(3) after reaction stops, washing wireway with low amounts of water, add 0.5mol/L hydrochloric acid 2.5mL in absorption liquid, 3 of 5% thiocarbamides shake up.Treat that purple takes off, add 20% potassium iodide 0.5mL, acetone 12mL accurately adds the 5-Br-PADAP ethanolic solution 2mL of 0.002mol/L, is diluted with water to graticule, shakes up.
(4) using the 10mm cuvette, at 600nm wavelength place, is reference with blank sample, measures absorbance, draws absorbance one concentration curve.
2. sample determination
The problem that tradition antimony method of testing 5-Br-PADAP photometry exists:
1. must use the antimony standard solution, artificial cause environmental pollution.
2. the operating process such as drafting of the preparation of sample, typical curve are tediously long, loaded down with trivial details, and labour intensity is big.
3. institute's use instrument and equipment complexity, complicated operation requires highly to operating personnel's specialized capability, and labour intensity is big.
Three. summary of the invention:
Purpose of the present invention: simplify the determination step of antimony content in the water, shorten minute greatly, alleviate intensity of workers, reduce environmental pollution, make antimony determination solution and colorimetric cylinder thereof.
Technical solution of the present invention:
A kind of antimony determination solution contains 0.005% pyridine-azo compound 1～30 unit volume, mineral acid 1～50 unit volume of 0.5mol/L, and mixed preparing forms, and measures the rising or the reduction of each components and concentration in the liquid, and its volume is corresponding to be dwindled or increases.
Described antimony determination solution, 0.005% pyridine-azo compound 1～9 unit volume wherein, mineral acid 1～50 unit volume of 0.5mol/L.
Described antimony determination solution, 0.005% pyridine-azo compound 9～21 unit volumes wherein, mineral acid 1～50 unit volume of 0.5mol/L.
Described antimony determination solution, 0.005% pyridine-azo compound 21～30 unit volumes wherein, mineral acid 1～50 unit volume of 0.5mol/L.
Described antimony determination solution, 0.005% pyridine-azo compound 1～30 unit volume wherein, mineral acid 1～18 unit volume of 0.5mol/L.
Described antimony determination solution, 0.005% pyridine-azo compound 1～30 unit volume wherein, mineral acid 18～36 unit volumes of 0.5mol/L.
Described antimony determination solution, 0.005% pyridine-azo compound 1～30 unit volume wherein, mineral acid 36～50 unit volumes of 0.5mol/L.
A kind of antimony colorimetric test 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 transition section with the kapillary of end sealing, and antimony 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: 1～20.
Antimony determination solution in the glass tube contains 0.005% pyridine-azo compound 1～30 unit volume, mineral acid 1～50 unit volume of 0.5mol/L, and mixed preparing forms, and measures the rising or the reduction of each components and concentration in the liquid, and its volume is corresponding to be dwindled or increases.
Measure the height H of liquid in the glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 9～13.
Positive beneficial effect of the present invention is:
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 needing during operation fracture in water sample to be measured measures the capillary tube segment of pipe, makes in the water sample automatic ration tail pipe to be measured and measures liquid generation metachromasia, just can draw antimony content more accurately with the contrast of standard color range behind the colour stable.Need not be when each mensuration preparing standard solution, reagent, can simplify the detection step greatly, save minute, reduce workload, reduce labor intensity, reduce environmental pollution.
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, 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 5-Br-PADAP spectrphotometric method for measuring antimony content, the present invention has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand antimony 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 accurately and reliably, meet the requirement of water analysis error precision, detection limit meets national sewage comprehensive discharge control and requires 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 5-Br-PADAP photometry data comparison sheet:
Four. description of drawings
Fig. 1: antimony colorimetric test tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects antimony content in advance, form color range.For example make 13 the color range pipes of standard colour code that detect antimony content in the water quality, antimony content is respectively 0.0mg/L, 0.05mg/L, 0.10mg/L, 0.15mg/L, 0.20mg/L, 0.25mg/L, 0.30mg/L, 0.35mg/L, 0.40mg/L, 0.50mg/L, 0.60mg/L, 0.80mg/L, the standard colour code of 1.00mg/L.At first get 4-(5-bromo-2-pyridylazo)-1-naphthols 105mL of 0.005%, 0.5mol/L sulfuric acid 55mL, be mixed and made into mensuration liquid, making antimony content then respectively is 0.0mg/L, 0.05mg/L, 0.10mg/L, 0.15mg/L, 0.20mg/L, 0.25mg/L, 0.30mg/L, 0.35mg/L, 0.40mg/L, 0.50mg/L, 0.60mg/L, 0.80mg/L, 13 kinds of normal concentration antimony aqueous solution of 1.00mg/L, to measure liquid and various normal concentration antimony aqueous solution pours into reaction solution in 13 color range pipes respectively in 1: 9 ratio, and constant color, seal the color range pipe 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 antimony aqueous solution volume when measuring the corresponding production standard color range of the ratio 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 antimony 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: 9.7 millimeters of uniform cross section vacuum glass external diameter of pipe, 13.6 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 10.8 centimetres, capillary tube segment length is 1.6 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, the pairing antimony concentration of the color range that is near the mark most numerical value is the antimony content that records, if measure the pipe color between two standard color ranges, then gets its mean value.
Measure formula of liquid in the present embodiment or be: contain 4-(5-bromo-2-pyridylazo)-1-naphthols 21 unit volumes of 0.005%, sulfuric acid 11 unit volumes of 0.5mol/L.
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, 22.9 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 1.9 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(5-bromo-2-pyridylazo)-1-naphthols 30 unit volumes of 0.005%, sulfuric acid 17 unit volumes of 0.5mol/L.
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 millimeters in the present embodiment, 11.2 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 8.4 centimetres, capillary tube segment length is 1.6 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(5-bromo-2-pyridylazo)-1-naphthols 9 unit volumes of 0.005%, sulfuric acid 25 unit volumes of 0.5mol/L.
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 6.5 millimeters in the present embodiment, 18.9 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 1.9 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1 unit volume of 0.005%, sulfuric acid 41 unit volumes of 0.5mol/L.
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 6.5 millimeters in the present embodiment, 5.6 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 2.6 centimetres, the height H of leaving a blank
2Be 2.6 centimetres, capillary tube segment length is 1.4 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 13 unit volumes of 0.005%, sulfuric acid 1 unit volume of 0.5mol/L.
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, 15.8 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 13 centimetres, capillary tube segment length is 1.8 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 50 unit volumes of 0.005%, sulfuric acid 17 unit volumes of 0.5mol/L.
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 6.5 millimeters in the present embodiment, 14.6 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 12 centimetres, capillary tube segment length is 1.6 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(2-pyridylazo)-1-naphthols 25 unit volumes of 0.005%, sulfuric acid 18 unit volumes of 0.5mol/L.
Embodiment eight: 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, 10 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 7.2 centimetres, capillary tube segment length is 1.6 centimetres.
Antimony colorimetric test tube in the present embodiment, the antimony determination solution prescription is: contain 4-(2-pyridylazo)-1-naphthols 7 unit volumes of 0.005%, sulfuric acid 36 unit volumes of 0.5mol/L.
Claims (9)
1. antimony determination solution is characterized in that: contain 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1～30 unit volume of 0.005%, and sulfuric acid 1～50 unit volume of 0.5mol/L, mixed preparing forms.
2. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1～9 unit volume wherein, sulfuric acid 1～50 unit volume of 0.5mol/L.
3. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 9～21 unit volumes wherein, sulfuric acid 1～50 unit volume of 0.5mol/L.
4. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 21～30 unit volumes wherein, sulfuric acid 1～50 unit volume of 0.5mol/L.
5. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1～30 unit volume wherein, sulfuric acid 1～18 unit volume of 0.5mol/L.
6. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1～30 unit volume wherein, sulfuric acid 18～36 unit volumes of 0.5mol/L.
7. antimony determination solution according to claim 1 is characterized in that: 0.005% 4-(3,5-two bromo-2-pyridylazos)-1-naphthols 1～30 unit volume wherein, sulfuric acid 36～50 unit volumes of 0.5mol/L.
8. antimony colorimetric test tube, be vacuum sealing tube, contain the uniform cross section glass tube of end sealing, the opening part of glass tube is communicated with transition section with the kapillary of end sealing, it is characterized in that: the described antimony determination solution of claim 1 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: 1～20.
9. antimony colorimetric test tube according to claim 8 is characterized in that: the height H of measuring liquid in the glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 9～13.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100485253A CN100535640C (en) | 2005-11-14 | 2005-11-14 | Antimony determination solution and colorimetric determination tube therefor |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100485253A CN100535640C (en) | 2005-11-14 | 2005-11-14 | Antimony determination solution and colorimetric determination tube therefor |
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|---|---|
| CN1766567A CN1766567A (en) | 2006-05-03 |
| CN100535640C true CN100535640C (en) | 2009-09-02 |
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|---|---|---|---|
| CNB2005100485253A Expired - Fee Related CN100535640C (en) | 2005-11-14 | 2005-11-14 | Antimony determination solution and colorimetric determination tube therefor |
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Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107247050A (en) * | 2017-06-27 | 2017-10-13 | 同济大学 | The preparation of the quick detection agent of antimony and application method in a kind of measure water body |
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2005
- 2005-11-14 CN CNB2005100485253A patent/CN100535640C/en not_active Expired - Fee Related
Non-Patent Citations (4)
| Title |
|---|
| 2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚在光度分析应用中的新进展. 金伟.理化检验－化学分册，第31卷第1期. 1995 |
| 2-(5-溴-2-吡啶偶氮)-5-二乙氨基酚在光度分析应用中的新进展. 金伟.理化检验－化学分册，第31卷第1期. 1995 * |
| 锑的野外快速分析方法－－锑－5－Br－PADAP光导比色法. 白金峰，卢荫庥.岩矿测试，第24卷第3期. 2005 |
| 锑的野外快速分析方法－－锑－5－Br－PADAP光导比色法. 白金峰，卢荫庥.岩矿测试，第24卷第3期. 2005 * |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract record no.: 2012410000012 Denomination of invention: Antimony determination solution and colorimetric determination tube therefor Granted publication date: 20090902 License type: Exclusive License Open date: 20060503 Record date: 20120306 |
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