CN1310028C - Fluoride assaying liquid and its colorimeteric estimation tube - Google Patents
Fluoride assaying liquid and its colorimeteric estimation tube Download PDFInfo
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- CN1310028C CN1310028C CNB2004100101352A CN200410010135A CN1310028C CN 1310028 C CN1310028 C CN 1310028C CN B2004100101352 A CNB2004100101352 A CN B2004100101352A CN 200410010135 A CN200410010135 A CN 200410010135A CN 1310028 C CN1310028 C CN 1310028C
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Abstract
The present invention relates to a method and a device for measuring a microchemistrical material, particularly to a measuring solution for rapidly measuring fluoride in water quality and a colorimetric measuring pipe. The measuring solution for rapidly measuring fluoride in water quality is prepared by mixing 18 to 38 unit volume of fluoron of 0.001 mol/l, 5 to 15 unit volume of sodium acetate trihydrate of 3.5%, 18 to 38 unit volume of lanthanum nitrate 99.9% of 0.001 mol/l and 18 to 38 unit volume of acetone as a solvent. The colorimetric measuring pipe comprises a vacuum sealing glass pipe with uniform section. One end of the vacuum sealing glass pipe is provided with a sealing and communicating capillary pipe section, and a certain fluoride measuring solution is packed. The ratio of the height H1 of the certain fluoride measuring solution to the space height H2 of the vacuum sealing glass pipe is 1: 7 to 12. The present invention carries out product forming and commercialization for measuring technology. Thus, a standard solution and a relevant reagent do not need to be prepared when in measurement each time. When in use, only the sealing and communicating capillary pipe section of the colorimetric measuring pipe is fractured in a water sample to be measured, and then, the water sample is automatically be sucked into the colorimetric measuring pipe in a quantitative way to generate discoloring reaction with the measuring solution. The present invention has the advantages of simple and quick measurement, no relevant step, such as pretreatment, interference suppress, etc., and low workload; the colorimetric measuring pipe and the measuring solution have the advantages of long retention time, good using value and easy popularization.
Description
One. technical field: the present invention relates to contain the assay method of the relevant chemical substance of trace in a kind of water quality and measure utensil, particularly relate to the Fluoride Determination Liquid And Its Colorimetric Determination Tube of content of fluoride in a kind of fast measuring water quality.
Two. background technology: fluoride (F
-) be one of trace element of needed by human, fluorine content has certain suitable concentration in the potable water, crosses low meeting and suffers from dental caries, and spot tooth disease even fluorosis of bone are suffered from too high meeting.Usually contain excessive fluorine in the waste water of industrial and mining enterprises such as coke, iron and steel, glass, electronics, agricultural chemicals and the underground water of certain areas, the fluoride poisoning incident happens occasionally.Enhancing along with people's environmental consciousness; people are to oneself living environment and also growing interest of the earth ecology of whole mankind's activity; strengthen environmental protection; love is green, pays close attention to the objective of the struggle that life and health has become whole world society, in recent years; China is when concentrating one's energy to develop national economy; also strengthened environmental improvement, firmly banned some with serious pollution factories and miness, enterprise, never starting, those are harmful to, are unfavorable for the project that the common people are healthy to environmental protection.But still have some lawless persons,, put state's laws, people ' s health in ignoring for economic interests at the moment, steal effluent, waste gas, waste residue etc., bring sizable difficulty to environment protection treating, many times, efforts at environmental protection personnel's work likes and is doing surprise attack, and some analytical instrument or carry, use inconvenience, be complicated operation, calculate loaded down with trivial detailsly, strong scientific basis can not be provided at the scene, weaken the dynamics that the environmental protection law-breaker is administered greatly, influenced government's law enforcement image.
Traditional fluoride method of testing has Fluoride ion selective electrode method and spectrophotometric method.Electrode method selectivity is good, and the scope of application is wide, its shortcoming be the electrode film surface be subject to stain and reduction of service life cost higher, and this method temperature influence is bigger, each test must be carried out slope correction with standard solution, complex operation calculates trouble.Spectrophotometric method must be prepared plurality of reagents and standard solution, complex operation, and must use instrument, can't test at the water quality scene.
Fairly simple a kind of method of testing is an alizarin sulfonic acid zirconium visual colorimetry at present, utilization is in acid solution, sodium alizarine sulphonate and zirconates generate red complex, when having fluorine ion to exist in the sample, can capture zirconium ion in this complex compound, generate colourless zirconium fluoride ion, discharge yellow sodium alizarine sulphonate.By the red colourity difference that takes off to yellow, relatively come the quantitative measurement fluorine according to solution with the standard colors row.This method is used simpler, measures liquid and can stablize preservation six months, and concentration limit is 0.05mg/L F
-
But the shortcoming that alizarin sulfonic acid zirconium visual colorimetry exists is, this method does not have commercialization, and standardization all needs preparation related standards liquid and contrast colour code earlier when each measurement operation, be unable to do without reference instrument, container during detection; Need in addition some is treated that sample measuring liquid need carry out pre-service, to eliminate chlorine residue in the sample, total alkalinity, sulfate, phosphate, interference and influence that iron, aluminium etc. produce can increase the workload of measurement undoubtedly, increase labour intensity, the lengthening minute requires operating personnel's professional qualities higher simultaneously, and this detection method cost is higher.
Three. summary of the invention: the object of the invention: at the background technology deficiency, for simplifying the fluoride measurement step, accelerate detection speed, reduce and detect cost, the present invention uses lambert-Beer law, proposes a kind of Fluoride Determination Liquid And Its Colorimetric Determination Tube.
The technical solution adopted in the present invention: a kind of fluoride measurement liquid, with the unit volume is unit, contain 0.001mol/L fluorine reagent 18～38 unit volumes, 3.5% sodium acetate, 5～15 unit volumes, 0.001mol/L lanthanum nitrate 18～38 unit volumes, solvent acetone 18～38 unit volumes, mixed preparing forms, and the concentration of fluorine reagent, sodium acetate, lanthanum nitrate and acetone improves or reduces its volume and can correspondingly dwindle or enlarge.
Fluorine reagent 25～30 unit volumes of 0.001mol/L in the described fluoride measurement liquid, 3.5% sodium acetate 8～10 unit volumes, lanthanum nitrate 25～30 unit volumes of 0.001mol/L, organic solvent-acetone 25～30 unit volumes.
A kind of fluoride colorimetric cylinder, contain uniform cross section vacuum seal glass tube, be provided with one section sealing at glass tube one end and be communicated with capillary tube segment, in uniform cross section vacuum seal glass tube, be packaged with fluoride measurement liquid as claimed in claim 1, measure the height H of liquid in the vacuum seal glass tube
1With measure the pipe uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 7～12.
Measure the fluoride measurement liquid in the pipe, with the unit volume is unit, fluorine reagent 18～38 unit volumes that contain 0.001mol/L, 3.5% sodium acetate 5～15 unit volumes, 0.001mol/L lanthanum nitrate 18～38 unit volumes, acetone 18～38 unit volumes, mixed preparing forms, and the concentration of fluorine reagent, sodium acetate, lanthanum nitrate and acetone improves or reduces its volume and can correspondingly dwindle or enlarge.
Described fluoride colorimetric cylinder, fluorine reagent 25～30 unit volumes of 0.001mol/L wherein, 3.5% sodium acetate 8～10 unit volumes, lanthanum nitrate 25～30 unit volumes of 0.001mol/L, acetone 25～30 unit volumes.
Positive beneficial effect of the present invention:
1. the present invention's mensuration fluid-tight that will prepare is loaded in the glass tube with vacuum, package spare together with the permanent standard color range of preparing in advance, mensuration liquid is mixed with quantitative sample liquid, treat contrast standard colour code behind abundant reaction, the colour stable, just can draw content of fluoride more accurately.This product can be directly used in on-the-spot the detection, and disturbing factor is few, uses simply, simplifies greatly and detects step, saves minute, reduces labor intensity, and testing result accurately and reliably.
2. compare with alizarin sulfonic acid zirconium visual colorimetry, the present invention is with the detection technique commercialization, standardization, need not preparing standard solution and relevant reagent when each test, the capillary tube segment of testing tube only needs during use to fracture in water sample to be measured, water sample be in the automatic ration tail pipe with measure liquid generation metachromasia, measure simple, fast.And exempt relevant steps such as pre-service, eliminating interference, workload is low; Mensuration is managed, the mensuration liquid holding time is longer, is easy to promote, and use value is better.
3. to measure the chromogenic reaction of liquid and determinand (fluoride) be to carry out automatically in the glass tube with vacuum under specific pH value condition in the present invention, can effectively avoid stochastic error or personal error, helps improving accuracy of detection.
The present invention carry, easy to use, carry out the scene and detect and need not the miscellaneous equipment instrument, economize on the use of funds, save human and material resources.River, lake, plant effuent, waste water quality are detected very convenient, help environmental protection.Experiment showed, that the present invention measures the pipe test result and meets the requirement of water analysis error precision, detection limit meets national potable water requirement standard.
Testing tube of the present invention and iodimetric titration data comparison sheet:
Four. description of drawings;
Fig. 1: fluoride colorimetric cylinder structural representation
Five. embodiment:
Embodiment one:
Make the series standard colour code that detects content of fluoride in advance, form color range.For example make 13 the color range pipes of standard colour code that detect content of fluoride in the water quality, content of fluoride is respectively 0mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.7mg/L, 0.8mg/L, 0.9mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, the standard colour code of 2.5mg/L.At first get the fluorine reagent 30ml of 0.001mol/L, 3.5% sodium acetate 10ml, 0.001mol/L lanthanum nitrate 30ml, be mixed and made into mensuration liquid with organic solvent-acetone 30ml, make content of fluoride then respectively and be respectively 0mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.7mg/L, 0.8mg/L, 0.9mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, 2.5mg/L 13 kinds of normal concentration fluoride aqueous solutions, will measure liquid and various normal concentration fluoride aqueous solution and pour into reaction solution in 13 charomatrons respectively, and constant color in 1: 7 ratio, 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, measures the ratio of mensuration liquid and normal concentration fluoride aqueous solution volume when measuring the long-pending corresponding formulation standard of the ratio color range pipe with the volume of leaving a blank of liquid in the pipe.
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 fluoride measurement liquid.H
1For measuring liquid height, H
2For the uniform cross section vacuum tube is left a blank highly.The mensuration liquid of the corresponding preparation standard colour code of present embodiment is promptly measured liquid and aqueous solution volume ratio to be measured by 1: 7.7.5 millimeters of uniform cross section vacuum glass external diameter of pipe, 10 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 0.9 centimetre, the height H of leaving a blank
2Be 6.3 centimetres, capillary tube segment length is 2.8 centimetres.
To measure pipe during use and immerse analyte sample fluid, capillary tube segment fractures, be filled the uniform cross section glass tube with vacuum pipeline section of leaving a blank Deng analyte sample fluid, take out to be inverted repeatedly and mix, make it fully to carry out chromogenic reaction, with the contrast of standard colour code, be the content of fluoride that records behind about 5～10 minutes colour stables with the pairing fluoride concentration numerical value of the colour code that is near the mark most, if measure the pipe color between two standard colour codes, then get its mean value.
Fluoride colorimetric cylinder of the present invention is measured formula of liquid or is: with the unit volume is example, contains the sodium acetate 8 of the fluorine reagent 25,3.5% of 0.001mol/L, the lanthanum nitrate 25 of 0.001mol/L, organic solvent-acetone 25.
Embodiment two: 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 fluoride measurement liquid.H
1For measuring liquid height, H
2For the uniform cross section vacuum tube is left a blank highly.Uniform cross section glass tube with vacuum external diameter is 6 millimeters in the present embodiment, 12.5 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 10 centimetres, capillary tube segment length is 1.5 centimetres.
Present embodiment fluoride colorimetric cylinder, the fluoride measurement formula of liquid is: the sodium acetate 9 of the fluorine reagent 28,3.5% of 0.001mol/L, the lanthanum nitrate 27 of 0.001mol/L, and organic solvent-acetone 27.The preparation of standard colors target no longer is described in detail with embodiment one.
Embodiment three: 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 fluoride measurement liquid.H
1For measuring liquid height, H
2For the uniform cross section vacuum tube is left a blank highly.Uniform cross section glass tube with vacuum external diameter is 8 millimeters in the present embodiment, 12 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 0.8 centimetre, the height H of leaving a blank
2Be 9.6 centimetres, capillary tube segment length is 1.6 centimetres.
Present embodiment is measured pipe, and the fluoride measurement formula of liquid is: the sodium acetate 10 of the fluorine reagent 30,3.5% of 0.001mol/L, and the lanthanum nitrate 30 of 0.001mol/L, and organic solvent-acetone 25, concrete compound method no longer is described in detail.Standard colors standard configuration system as described above.
In concrete enforcement, improve or reduce according to the concentration of measuring each active principle in the liquid, the volume of uniform cross section sealed glass tube can correspondingly dwindle or increase, measuring the height of liquid in the uniform cross section vacuum seal glass tube and measuring that pipe leaves a blank highly also is according to measuring liquid and treat that sample measuring liquid is concrete and fixed with suitable volume mixture ratio, and the making of colour code should with measure measure liquid concentration in the pipe and mixing ratio consistent.
Claims (5)
1. fluoride measurement liquid, it is characterized in that: be unit with the unit volume, contain 0.001mol/L fluorine reagent 18～38 unit volumes, 3.5% sodium acetate, 5～15 unit volumes, 0.001mol/L lanthanum nitrate 18～38 unit volumes, solvent acetone 18～38 unit volumes, mixed preparing forms, and the concentration of fluorine reagent, sodium acetate, lanthanum nitrate and acetone improves or reduces its volume and can correspondingly dwindle or enlarge.
2. fluoride measurement liquid according to claim 1, it is characterized in that: fluorine reagent 25～30 unit volumes of 0.001mol/L wherein, 3.5% sodium acetate 8～10 unit volumes, lanthanum nitrate 25～30 unit volumes of 0.001mol/L, organic solvent-acetone 25～30 unit volumes.
3. fluoride colorimetric cylinder, contain uniform cross section vacuum seal glass tube, be provided with one section sealing at glass tube one end and be communicated with capillary tube segment, it is characterized in that: in uniform cross section vacuum seal glass tube, be packaged with fluoride measurement liquid as claimed in claim 1, measure the height H of liquid in the vacuum seal glass tube
1With measure the pipe uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 7～12.
4. fluoride colorimetric cylinder according to claim 3, it is characterized in that: described fluoride measurement liquid, with the unit volume is unit, fluorine reagent 18～38 unit volumes that contain 0.001mol/L, 3.5% sodium acetate 5～15 unit volumes, lanthanum nitrate 18～38 unit volumes of 0.001mol/L, acetone 18～38 unit volumes, mixed preparing forms, and the concentration of fluorine reagent, sodium acetate, lanthanum nitrate and acetone improves or reduces its volume and can correspondingly dwindle or enlarge.
5. fluoride colorimetric cylinder according to claim 4, it is characterized in that: fluorine reagent 25～30 unit volumes of 0.001mol/L wherein, 3.5% sodium acetate 8～10 unit volumes, lanthanum nitrate 25～30 unit volumes of 0.001mol/L, acetone 25～30 unit volumes.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100101352A CN1310028C (en) | 2004-03-17 | 2004-03-17 | Fluoride assaying liquid and its colorimeteric estimation tube |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2004100101352A CN1310028C (en) | 2004-03-17 | 2004-03-17 | Fluoride assaying liquid and its colorimeteric estimation tube |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1563974A CN1563974A (en) | 2005-01-12 |
| CN1310028C true CN1310028C (en) | 2007-04-11 |
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ID=34477816
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|---|---|---|---|
| CNB2004100101352A Expired - Fee Related CN1310028C (en) | 2004-03-17 | 2004-03-17 | Fluoride assaying liquid and its colorimeteric estimation tube |
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| CN (1) | CN1310028C (en) |
Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101029327B (en) * | 2006-11-30 | 2010-10-06 | 白莉 | Acetony methyl generating test fluid and testing tube |
| CN103558168A (en) * | 2013-10-31 | 2014-02-05 | 大连大公环境检测有限公司 | Detection method for fluoride content |
| CN109238984A (en) | 2018-09-06 | 2019-01-18 | 哈尔滨医科大学 | It is a kind of for detecting the detection method of content of fluoride ion in trace sample |
| CN109238983A (en) * | 2018-09-06 | 2019-01-18 | 哈尔滨医科大学 | It is a kind of for detecting the kit of content of fluoride ion in trace sample |
| CN113484260A (en) * | 2021-07-07 | 2021-10-08 | 山东中节能天融环保技术有限公司 | Method for measuring fluoride in water by spectrophotometry |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071757A (en) * | 1991-10-19 | 1993-05-05 | 山东省地方病防治研究所 | Survey fluorine reagent and color board fast |
| JPH07198704A (en) * | 1993-12-28 | 1995-08-01 | Shimadzu Corp | Method for analyzing fluorine ion |
| JPH1026588A (en) * | 1996-07-12 | 1998-01-27 | Nec Corp | Analyzing method for fluoride ion and analyzing reagent |
| JP2003043025A (en) * | 2001-07-26 | 2003-02-13 | Tohoku Techno Arch Co Ltd | Plate for detecting fluoride ion, and method for judging concentration of fluoride ion using the plate |
| CA2426476A1 (en) * | 2002-04-27 | 2003-10-27 | Prominent Dosiertechnik Gmbh | Fluoride-sensitive electrode |
-
2004
- 2004-03-17 CN CNB2004100101352A patent/CN1310028C/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1071757A (en) * | 1991-10-19 | 1993-05-05 | 山东省地方病防治研究所 | Survey fluorine reagent and color board fast |
| JPH07198704A (en) * | 1993-12-28 | 1995-08-01 | Shimadzu Corp | Method for analyzing fluorine ion |
| JPH1026588A (en) * | 1996-07-12 | 1998-01-27 | Nec Corp | Analyzing method for fluoride ion and analyzing reagent |
| JP2003043025A (en) * | 2001-07-26 | 2003-02-13 | Tohoku Techno Arch Co Ltd | Plate for detecting fluoride ion, and method for judging concentration of fluoride ion using the plate |
| CA2426476A1 (en) * | 2002-04-27 | 2003-10-27 | Prominent Dosiertechnik Gmbh | Fluoride-sensitive electrode |
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|---|---|
| CN1563974A (en) | 2005-01-12 |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract fulfillment period: 2009.3.25 to 2014.3.25 Contract record no.: 2009410000016 Denomination of invention: Fluoride assaying liquid and its colorimeteric estimation tube Granted publication date: 20070411 License type: Exclusive license Record date: 20090326 |
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| LIC | Patent licence contract for exploitation submitted for record |
Free format text: EXCLUSIVE LICENSE; TIME LIMIT OF IMPLEMENTING CONTACT: 2009.3.25 TO 2014.3.25; CHANGE OF CONTRACT Name of requester: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Effective date: 20090326 |
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Granted publication date: 20070411 Termination date: 20210317 |