CN1766555A - Manganese determination solution and colorimetric determination tube therefor - Google Patents
Manganese determination solution and colorimetric determination tube therefor Download PDFInfo
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- CN1766555A CN1766555A CN 200510048465 CN200510048465A CN1766555A CN 1766555 A CN1766555 A CN 1766555A CN 200510048465 CN200510048465 CN 200510048465 CN 200510048465 A CN200510048465 A CN 200510048465A CN 1766555 A CN1766555 A CN 1766555A
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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 bivalent manganese content in water mass. The bivalent manganese analyzing liquid comprises 0.05% pyridylazo phenol 1-20 unit volume, 0.01% surface active agent 1-20 unit volume, and pH buffer liquid 5-30 unit volume, the analyzing tube contains uniform cross-section vacuum sealed glass tube, the glass tube is equipped with bivalent manganese 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 = 1:2-15. 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 manganese Determination on content liquid and colorimetric cylinder thereof in a kind of fast measuring water quality.
Two. background technology: manganese has the metallic luster of iron and steel sample, and its compound has multiple valence state, and the main valence state of manganese has divalence, trivalent, tetravalence, sexavalence and septivalency.Manganese mainly is that form with divalence, trivalent or tetravalence exists in underground water basin or the surface water.Manganese is one of biological necessary trace element, is the composition or the activator of some enzyme, participates in the generation of chondroitin sulfate in the bone matrix, and manganese prevents ataxic effect in addition, and the hematopoietic function of it and animal is closely related.But the manganese of excess intake can cause feed intake to descend, and grows and is obstructed, skeleton deformity etc., even can cause nerve dysfunction and cancer.Therefore, general industry water manganese content does not allow to surpass 0.1mg/L.The primary pollution source of manganese is the discharging of ferrous metal mine, metallurgical industry, battery industry and chemical engineering sewage.
Traditional manganese method of testing is a potassium metaperiodate oxidation photometry, and its operation steps is:
(1) 0mL is drawn in the drafting of typical curve respectively, 0.50mL, 1.00mL, 1.50mL, 2.00mL, 2.50mL the manganese standard uses liquid to place six 50mL color comparison tubes, add water to 25mL, add 10mL potassium pyrophosphate-sodium acetate buffer, add 2% potassium metaperiodate solution 3mL after shaking up again, be diluted with water to scale, shake up.Place after 10 minutes, at the 525nm place, make the reference measurement absorbance, by the absorbance of gained amount drawing standard curve behind blank correction manganese with water with the 50mm cuvette.
(2) the waste water water sample that the mensuration of sample is more with suspension or colourity is darker is got the 25mL mixing and is placed the 100mL beaker for two parts, adds 5mL nitric acid and (1+1) sulfuric acid or perchloric acid 2mL, and heating is cleared up until Mao Baiyan, is evaporated near doing, and takes off.Cold slightly back adds low amounts of water, and the low-grade fever dissolving quantitatively moves in the 50mL color comparison tube, regulate the nearly neutrality of pH value with (1+9) ammoniacal liquor, a copy of it is pressed the same steps as colour developing that typical curve is drawn, and another part replaces water sample with pure water, by same operation, measure absorbance at the 525nm place.
The problem that potassium metaperiodate oxidation photometry exists: (1) this method is to utilize potassium metaperiodate that the bivalent manganese of lower valency etc. is oxidized to the potassium permanganate of high valence state, and oxidation reaction causes result error not exclusively easily, and error is big; (2) contain the sewage of strong oxidizer or reductive agent, test is disturbed big, must measure complicated operating process again after acid is cleared up; (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:
Purpose of the present invention: simplify the manganese testing procedure, shorten minute greatly, alleviate intensity of workers, make manganese determination solution and colorimetric cylinder thereof.
Technical solution of the present invention:
A kind of manganese determination solution, represent with unit volume, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, 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 increase.
Described manganese determination solution, described mensuration liquid is the divalence manganese determination solution.
Described manganese determination solution, contain 0.005% PAP 2 phenol 1～7 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 7～13 unit volumes, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 13～20 unit volumes, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes.
Described manganese determination solution, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～7 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 7～13 unit volumes, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 13～20 unit volumes, pH buffer solution 5～30 unit volumes.
Described manganese determination solution, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～13 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 13～22 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 22～30 unit volumes.
A kind of manganese 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 the kapillary and the transition section of end sealing, and the divalence manganese 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: 2～15.
Described manganese colorimetric test tube, manganese determination solution in the glass tube, be the divalence manganese determination solution, represent with unit volume, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, 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 increase.
In glass tube, measure the height H of liquid
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 7～10.
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 manganese 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. method of testing of the present invention is compared with changing photometry, has obviously reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand manganese 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 potassium metaperiodate oxidation photometry data comparison sheet:
Four. description of drawings
Fig. 1: manganese colorimetric test tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects manganese content in advance, form color range.For example make 13 the color range pipes of standard colour code that detect manganese content in the water quality, manganese content is respectively 0.0mg/L, 0.5mg/L, and 1.0mg/L,
1.5mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 8.0mg/L, 10mg/L, 15.0mg/L, the standard colour code of 20.0mg/L.At first get pyridylazo-4-chloro-1-phenol 65mL of 0.005%, 0.01% Tritonx-100 surfactant 100mL, borax-sodium hydroxide buffer solution 110mL is mixed and made into mensuration liquid.Making manganese content then respectively is 0.0mg/L, 0.5mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 8.0mg/L, 10mg/L, 15.0mg/L, 20.0mg/L 13 kinds of normal concentration manganese aqueous solution, will measure liquid and various normal concentration manganese aqueous solution pours into reaction solution in 13 charomatrons respectively in 1: 8 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 manganese 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 manganese 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: 8.6.5 millimeters of uniform cross section vacuum glass external diameter of pipe, 12 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 8.8 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, the pairing manganese concentration of colour code that is near the mark most numerical value is the manganese content that records, if measure the pipe color between two standard colour codes, then gets its mean value.
Manganese colorimetric test tube of the present invention is measured formula of liquid: be example with the unit volume, contain pyridylazo-4-chloro-1-phenol 13 unit volumes of 0.005%, 0.01% Tritonx-100 surfactant 20 unit volumes, borax-sodium hydroxide buffer solution 22 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 7 millimeters in the present embodiment, 9.5 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 7 centimetres, capillary tube segment length is 15 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain pyridylazo-4-chloro-1-phenol 20 unit volumes of 0.005%, 0.01% Tritonx-100 surfactant 7 unit volumes, borax-sodium hydroxide buffer solution 13 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 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.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain pyridylazo-4-chloro-1-phenol 7 unit volumes of 0.005%, 0.01% Tritonx-100 surfactant 1 unit volume, borax-sodium hydroxide buffer solution 30 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, 6 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.5 centimetres, the height H of leaving a blank
2Be 3 centimetres, capillary tube segment length is 1.5 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain pyridylazo-4-chloro-1-phenol 1 unit volume of 0.005%, 0.01% Tritonx-100 surfactant 7 unit volumes, borax-sodium hydroxide buffer solution 5 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, 17.6 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 15 centimetres, capillary tube segment length is 1.6 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain 0.005% pyridine-azo maphthol 17 unit volumes, 0.01% Tritonx-100 surfactant 8 unit volumes, borax-sodium hydroxide buffer solution 18 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 7 millimeters in the present embodiment, 11.8 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 9 centimetres, capillary tube segment length is 1.8 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain 0.005% pyridine-azo maphthol 5 unit volumes, 0.01% Tritonx-100 surfactant 6 unit volumes, borax-sodium hydroxide buffer solution 9 unit volumes.
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, 9.1 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 6.5 centimetres, capillary tube segment length is 1.5 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain 0.005% pyridine-azo maphthol 10 unit volumes, 0.01% Tritonx-100 surfactant 3 unit volumes, borax-sodium hydroxide buffer solution 11 unit volumes.
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 7 millimeters in the present embodiment, 9.5 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 7 centimetres, capillary tube segment length is 1.5 centimetres.
Manganese colorimetric test tube in the present embodiment, the manganese determination solution prescription is: be example with the unit volume, contain 0.005% pyridine-azo maphthol 12 unit volumes, 0.01% Tritonx-100 surfactant 17 unit volumes, borax-sodium hydroxide buffer solution 19 unit volumes.
Claims (8)
1. manganese determination solution, it is characterized in that: represent with unit volume, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, 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 increase.
2. manganese determination solution according to claim 1 is characterized in that: described mensuration liquid is the divalence manganese determination solution.
3. manganese determination solution according to claim 1, it is characterized in that: contain 0.005% PAP 2 phenol 1～7 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 7～13 unit volumes, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 13～20 unit volumes, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes.
4. manganese determination solution according to claim 1, it is characterized in that: contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～7 unit volume, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 7～13 unit volumes, pH buffer solution 5～30 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 13～20 unit volumes, pH buffer solution 5～30 unit volumes.
5. manganese determination solution according to claim 1, it is characterized in that: contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～13 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 13～22 unit volumes, or contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 22～30 unit volumes.
6. manganese 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 the kapillary and the transition section of end sealing, it is characterized in that: the divalence manganese 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: 2～15.
7. manganese colorimetric test tube according to claim 5, it is characterized in that: the manganese determination solution in the glass tube, be the divalence manganese determination solution, represent with unit volume, contain 0.005% PAP 2 phenol 1～20 unit volume, 0.01% surfactant 1～20 unit volume, pH buffer solution 5～30 unit volumes, 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 increase.
8. manganese colorimetric test tube according to claim 5 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: 7～10.
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|---|---|---|---|
| CN 200510048465 CN1766555A (en) | 2005-10-31 | 2005-10-31 | Manganese determination solution and colorimetric determination tube therefor |
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|---|---|---|---|
| CN 200510048465 CN1766555A (en) | 2005-10-31 | 2005-10-31 | Manganese determination solution and colorimetric determination tube therefor |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128836A (en) * | 2010-12-06 | 2011-07-20 | 天津钢铁集团有限公司 | Method for detecting manganese in carbon manganese alloy |
| CN104390923A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining manganese in low alloy steel by using colorimetric method |
| CN104807813A (en) * | 2015-05-13 | 2015-07-29 | 湖南瑞铨冶金有限公司 | Rapid analysis method for content of manganese in ferromanganese iron |
| CN108593571A (en) * | 2018-03-12 | 2018-09-28 | 宁夏天元锰业有限公司 | A kind of detection method of automatic detection electrolyte manganese ion |
-
2005
- 2005-10-31 CN CN 200510048465 patent/CN1766555A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102128836A (en) * | 2010-12-06 | 2011-07-20 | 天津钢铁集团有限公司 | Method for detecting manganese in carbon manganese alloy |
| CN102128836B (en) * | 2010-12-06 | 2013-02-13 | 天津钢铁集团有限公司 | Method for detecting manganese in carbon manganese alloy |
| CN104390923A (en) * | 2014-12-17 | 2015-03-04 | 内蒙古包钢钢联股份有限公司 | Method for determining manganese in low alloy steel by using colorimetric method |
| CN104807813A (en) * | 2015-05-13 | 2015-07-29 | 湖南瑞铨冶金有限公司 | Rapid analysis method for content of manganese in ferromanganese iron |
| CN108593571A (en) * | 2018-03-12 | 2018-09-28 | 宁夏天元锰业有限公司 | A kind of detection method of automatic detection electrolyte manganese ion |
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