CN2831106Y - Se colorimetric estimation tube - Google Patents

Se colorimetric estimation tube Download PDF

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Publication number
CN2831106Y
CN2831106Y CN 200520032636 CN200520032636U CN2831106Y CN 2831106 Y CN2831106 Y CN 2831106Y CN 200520032636 CN200520032636 CN 200520032636 CN 200520032636 U CN200520032636 U CN 200520032636U CN 2831106 Y CN2831106 Y CN 2831106Y
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selenium
glass tube
tube
determination
liquid
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CN 200520032636
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刘五一
崔纪周
徐恺
唐翠莲
朱思羽
白莉
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白莉
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Abstract

The utility model relates to a selenium determination device, particularly a selenium colorimetric determination tube. The selenium colorimetric determination tube is a vacuum sealed tube, which comprises an equal cross-section glass tube of which one end is closed, the opening of the glass tube is communicated with a capillary pipe of which one end is closed and a transition section, and the ratio of the height H1 of determination liquid in the glass tube and the equal cross-section airborne height H2 of the glass tube is from 1/1 to 1/20. The product forming and the commercialization of the determination technology are realized by the utility model, and the prepared determination liquid is sealed in the vacuum glass tube and is packaged for use. When the utility model is used, the capillary tube segment of the colorimetric tube is broken in a water sample to be measured, the water sample is automatically and quantitatively sucked into the glass tube, the discoloration reaction between the water sample and the determination liquid occurs, and relatively precise selenium content can be obtained by the contrast of the color of the water sample and the standard color levels. The determination device has the advantages of long retention period, and simple, fast and correct determination, and also has the advantage that the determination steps can be simplified, the determination time can be saved, and the workload can be reduced.

Description

Selenium colorimetric test tube
One. technical field: the utility model relates to a kind of selenium and measures utensil, particularly relates to a kind of selenium colorimetric test tube.
Two. background technology: trace selenium is the essential nutrient of biosome, but wherein between serviceability and the intoxicating boundary very narrow, excessive selenium can make the people poison, and causes alopecia, takes off nail, illness such as numb limb even hemiplegia.
Selenium exists with the form of inorganic sexavalence, tetravalence, negative divalence and some organic selenium in the water, also has extremely micro-selenium attached on the suspended particulate substance.Mainly contain sexavalence, tetravalence selenium in the general natural water, content is many below 1 μ g/L, the flow through high stratum of selenium content or contained the selenium contaminated wastewater of indivedual water bodys, and Se content can be up to every liter of hectogamma.The selenium that often contains various valence states in the waste water, content are tens to every liter of hundreds of microgram, and the quality standard of water environment regulation Se content of Japan must be below 0.01mg/L.Containing selenium waste water is mainly derived from selenium mining, metallurgy, oil refining, concise copper, makes sulfuric acid and special glass industry.
Traditional selenium method of testing is a graphite oven atomic absorption, and its operation steps is:
1. the preparation of sample
Get even recombined sample 50~200mL, add 5~10mL red fuming nitric acid (RFNA), at heating evaporation on the electric hot plate to the 1mL.If the sample muddiness, color is darker, adds 2mL nitric acid again, continues to clear up to test solution as clear as crystal, is light color or colourless, and is evaporated near doing.Take off coldly slightly, add (1+49) nitric acid 20mL, warm, dissolving solubility salt if precipitation occurs, is filtered in the 50mL container with middling speed filter paper, is diluted to graticule with deionized water, and is to be measured.
2. the preparation of blank test solution
(1) in test specimens, measures blank.
(2) get appropriate amount of deionized water and replace sample to place the 250mL beaker,, press sample digestion and determination step again and measure optionally by the step process of measuring solubilised state selenium or total selenium.
3. the preparation of standard solution series
(1) in the 10mL color-comparison tube, add the selenium standard respectively and use liquid 1.00mL, 2.00mL, 3.00mL, 4.00mL, 5.00mL, adding 0.1mL (1+1) nitric acid and concentration is the nickel nitrate solution 0.5mL of 16g/L, is settled to 10mL with deionized water.
(2) concentration of the tested element of sample should be in the standard series concentration range.
4. calibrate and measure
(1) drawing standard curve.
(2) select condition such as wavelength and the graphite furnace heating schedule is set according to instrument service condition and heating schedule, sky burns to the graphite furnace blank value stable.In graphite-pipe, inject prepared blank, working stamndard solution and sample solution.The record absorbance.
(3) with the absorbance and the corresponding concentration curve plotting that record.
(4) according to the sample absorbance behind the deduction blank absorbency, in typical curve, find selenium concentration in the sample.
The problem that graphite oven atomic absorption exists:
1. need to use selenium standard solution and a large amount of nitric acid, the people is for polluting.
2. must use the large test instrument, cost an arm and a leg.
3. when measuring, should guarantee that the selenium hollow cathode lamp has the preheating time more than 1 hour, specimen preparation is loaded down with trivial details, and the time is tediously long, and labour intensity is big.
4. before each mensuration, must the blank and working stamndard solution of replication, in time rectify an instrument and the variation of graphite furnace sensitivity, otherwise have bigger error, operator quality is required height.
Three. the utility model content:
The utility model purpose:, make a kind of easy to carry, selenium colorimetric test tube of using simple and fast at disadvantages of background technology.
The technical solution of the utility model:
A kind of selenium 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 selenium assaying liquid 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.
Selenium assaying liquid in the glass tube contains 0.1% aniline compound 1~50 unit volume, pH damping fluid 1~50 unit volume, 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 utility model is:
1. the utility model 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 Se 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. it is reasonable that the utility model is measured formula of liquid, 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 utility model 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 conventional graphite stove aas determination Se content, the utility model has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand selenium be to carry out automatically under given conditions the glass tube with vacuum to the utility model, 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 utility model 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 utility model is easy to promotion and implementation, has good social and economic benefit.
The utility model testing tube and conventional graphite stove atomic absorption method data comparison sheet:
Figure Y20052003263600051
Four. description of drawings
Fig. 1: selenium colorimetric test tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects Se content in advance, form color range.For example make 10 the color range pipes of standard colour code that detect Se content in the water quality, Se content is respectively 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.04mg/L, 0.06mg/L, 0.08mg/L, 0.10mg/L, 0.20mg/L, 0.30mg/L, the standard colour code of 0.40mg/L.At first get 0.1% 3,3 '-diaminobenzidine 85mL, KH 2PO 4-NaOH damping fluid 180mL is mixed and made into mensuration liquid, and making Se content then respectively is 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.04mg/L, 0.06mg/L, 0.08mg/L, 0.10mg/L, 0.20mg/L, 0.30mg/L, 10 kinds of normal concentration selenium aqueous solution of 0.40mg/L, to measure liquid and various normal concentration selenium aqueous solution pours into reaction solution in 10 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 selenium 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 selenium assaying liquid.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 selenium concentration numerical value of the color range that is near the mark most is the Se content that records, if measure the pipe color between two standard color ranges, then gets its mean value.
The present embodiment selenium colorimetric test tube is measured formula of liquid or is: contain 0.1% 3,3 '-diaminobenzidine, 17 unit volumes, KH 2PO 4-NaOH damping fluid 36 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, 5.7 centimetres of overall heights, the height H of mensuration liquid in the glass tube 1Be 2.1 centimetres, the height H of leaving a blank 2Be 2.1 centimetres, capillary tube segment length is 1.5 centimetres.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% 3,3 '-diaminobenzidine, 36 unit volumes, KH 2PO 4-NaOH damping fluid 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 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.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% 3,3 '-diaminobenzidine, 50 unit volumes, KH 2PO 4-NaOH damping fluid 1 unit volume.
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, 22.8 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 20 centimetres, capillary tube segment length is 1.8 centimetres.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% 3,3 '-diaminobenzidine, 11 unit volumes, KH 2PO 4-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, 18.7 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 1.7 centimetres.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% o-phenylenediamine 1 unit volume, KCl-HCl damping fluid 25 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, 13.6 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 11 centimetres, capillary tube segment length is 1.6 centimetres.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% o-phenylenediamine 23 unit volumes, KCl-HCl damping fluid 50 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, 11.6 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 1.7 centimetres.
Selenium colorimetric test tube in the present embodiment, the selenium assaying liquid prescription is: contain 0.1% o-phenylenediamine 41 unit volumes, KCl-HCl damping fluid 43 unit volumes.

Claims (3)

1. selenium 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: selenium assaying liquid 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.
2. selenium colorimetric test tube according to claim 1, it is characterized in that: the selenium assaying liquid in the glass tube contains 0.1% aniline compound 1~50 unit volume, pH damping fluid 1~50 unit volume, mixed preparing forms, measure the rising or the reduction of each components and concentration in the liquid, its volume is corresponding to be dwindled or increases.
3. selenium colorimetric test tube according to claim 1 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.
CN 200520032636 2005-11-14 2005-11-14 Se colorimetric estimation tube Expired - Fee Related CN2831106Y (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1773254B (en) * 2005-11-14 2010-08-25 白莉 Selenium assaying liquid and colour comparision tube thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1773254B (en) * 2005-11-14 2010-08-25 白莉 Selenium assaying liquid and colour comparision tube thereof

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Granted publication date: 20061025

Termination date: 20101114