CN100543454C - Indium determining liquid and colorimetric cylinder thereof - Google Patents
Indium determining liquid and colorimetric cylinder thereof Download PDFInfo
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- CN100543454C CN100543454C CNB2005100485272A CN200510048527A CN100543454C CN 100543454 C CN100543454 C CN 100543454C CN B2005100485272 A CNB2005100485272 A CN B2005100485272A CN 200510048527 A CN200510048527 A CN 200510048527A CN 100543454 C CN100543454 C CN 100543454C
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Abstract
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 indium Determination on content liquid and colorimetric cylinder thereof in a kind of fast measuring water quality.Indium determining liquid of the present invention contains 0.005% azo-compound 1～40 unit volume, pH damping fluid 1～60 unit volume, and mixed preparing forms.Its mensuration pipe contains uniform cross section vacuum seal glass tube, and indium determining 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: 2～20.The present invention is with the detection technique commercialization, and commercialization is loaded on the mensuration fluid-tight for preparing in advance in the glass tube with vacuum, can be directly used in mensuration, carries, and is easy to use, measures simply fast, and accurately, the holding time is long.Detection limit meets national sewage comprehensive discharge control and requires standard, testing result to meet the requirement of water analysis error precision.
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 indium Determination on content liquid and colorimetric cylinder thereof in a kind of fast measuring water quality.
Two. background technology:
Indium is not animals and plants and necessary for human body trace element, it in animal body physiological action it be unclear that.The white mouse test of indium shows, sucks 30mg/d and produces poisoning, and sucking 200mg/d can cause death.The abundance value of indium in the earth's crust is 0.1mg/kg.The content range of indium is 0.7～3mg/kg in world's soil, and median is 1mg/kg.The concentration of indium is about 0.00011mg/L in the seawater.In nonferrous metal mine exploitation and smelting process, often there is a large amount of indiums to be discharged in the water environment, thus the accident of polluting.
Classical indium assay method is the extraction graphite oven atomic absorption, and its operation steps is:
1. water sample is cleared up
(1) accurately pipette an amount of water sample (indium content is less than 0.4 μ g) in beaker, add liquor ferri trichloridi 0.5mL, concentrated hydrochloric acid 5mL, when on electric hot plate, being evaporated to about 5mL, adding (1+1) sulfuric acid 15mL, low-grade fever is dissolved issuable residue.Change in the 50mL color-comparison tube, be cooled to room temperature, add pure water 15mL, potassium bromide solution 2mL placed 5 minutes, added 5mL phosphoric acid, added water and was settled to 50mL.Accurately add methyl isobutyl ketone (MIBK) 5mL, jolting 3 minutes, standing demix.
(2) organic phase is to be measured, replaces water sample with pure water simultaneously, carries out blank test.
2. the drafting of typical curve
(1) in six 50mL beakers, adds 0mL, 0.05mL, 0.10mL, 0.20mL, 0.30mL, 0.40mL indium standard operation solution respectively, add liquor ferri trichloridi 0.5mL and concentrated hydrochloric acid 1mL again, put and steam on the electric hot plate near doing, add (1+1) sulfuric acid 15mL, the low-grade fever dissolving changes in the 50mL color-comparison tube, be cooled to room temperature, add water to about 35mL, add potassium bromide solution 2mL again, shake up.Below operation is cleared up with step 1 water sample.
(2) get organic phase and advance the absorbance that graphite furnace is measured indium, behind blank correction, draw absorbance-concentration curve.
(3) measure simultaneously that water sample is cleared up after the organic phase that extracts.Deduct the absorbance of omnidistance preface blank by the absorbance of sample, find the content of indium the sample, calculate the concentration of indium in the water sample from calibration curve.
The problem that the extraction graphite oven atomic absorption exists:
(1) must use indium standard solution, a large amount of sulfuric acid and organic reagent, the people is for causing environmental pollution.
(2) 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) must measure absorbance and, operator quality be required height, testing cost costliness by the use large-scale instrument with formula calculating concentration value.
Three. summary of the invention:
Purpose of the present invention: simplify indium Determination on content step in the water, shorten minute greatly, alleviate intensity of workers, reduce environmental pollution, make indium determining liquid and colorimetric cylinder thereof.
Technical solution of the present invention:
A kind of indium determining liquid, described indium determining liquid is formed by 0.005% azo-compound 1～40 unit volume and NaAc-HAc damping fluid 1～60 unit volume mixed preparing, 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 azo-compound is 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid, 2-(2-hydroxyl-3-sulfo group-5-nitrophenylazo)-7-(3-sulfophenyl azo)-1,8-dihydroxy naphthlene-3,6-disulfonic acid and 2-(2-hydroxyl-3,5-dinitroazobenzene)-7-(3-sulfophenyl azo)-1,8-dihydroxy-3, any in the 6-naphthalenedisulfonic acid.
Described indium determining liquid, 0.005% azo-compound 1～13 unit volume wherein, NaAc-HAc damping fluid 1～60 unit volume.
Described indium determining liquid, 0.005% azo-compound 13～28 unit volumes wherein, NaAc-HAc damping fluid 1～60 unit volume.
Described indium determining liquid, 0.005% azo-compound 28～40 unit volumes wherein, NaAc-HAc damping fluid 1～60 unit volume.
Described indium determining liquid, 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 1～19 unit volume.
Described indium determining liquid, 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 19～41 unit volumes.
Described indium determining liquid, 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 41～60 unit volumes.
A kind of indium 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 transition section with the kapillary of end sealing, and indium determining liquid recited above 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=1:2～20.
Described indium colorimetric testing tube, the height H of mensuration 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 indium 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 extraction graphite furnace atomic absorption spectrometry indium content, the present invention has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand indium 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 extraction graphite oven atomic absorption data comparison sheet:
Four. description of drawings
Fig. 1: indium colorimetric testing tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects indium content in advance, form color range.For example make 8 the color range pipes of standard colour code that detect indium content in the water quality, indium content is respectively 0.0mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.40mg/L, 0.60mg/L, 0.80mg/L, the standard colour code of 1.00mg/L.At first get 0.005% 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid 112mL, NaAc-HAc damping fluid 76mL is mixed and made into mensuration liquid, making indium content then respectively is 0.0mg/L, 0.05mg/L, 0.10mg/L, 0.20mg/L, 0.40mg/L, 0.60mg/L, 0.80mg/L, 8 kinds of normal concentration indium aqueous solution of 1.00mg/L, to measure liquid and various normal concentration indium aqueous solution pours into reaction solution in 8 color range pipes respectively in the 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 indium 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 indium determining 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 indium concentration of the color range that is near the mark most numerical value is the indium 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 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid 28 unit volumes, NaAc-HAc damping fluid 19 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, 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.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid 13 unit volumes, NaAc-HAc damping fluid 41 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, 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.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid 40 unit volumes, NaAc-HAc damping fluid 27 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 6.5 millimeters in the present embodiment, 8.2 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 2.2 centimetres, the height H of leaving a blank
2Be 4.4 centimetres, capillary tube segment length is 1.6 centimetres.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3-sulfo group-5-nitrophenylazo)-7-(3-sulfophenyl azo)-1,8-dihydroxy naphthlene-3,6-disulfonic acid 1 unit volume, NaAc-HAc damping fluid 12 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 6.5 millimeters in the present embodiment, 14.8 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 12 centimetres, capillary tube segment length is 1.8 centimetres.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3-sulfo group-5-nitrophenylazo)-7-(3-sulfophenyl azo)-1,8-dihydroxy naphthlene-3,6-disulfonic acid 18 unit volumes, NaAc-HAc damping fluid 1 unit volume.
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, 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.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3-sulfo group-5-nitrophenylazo)-7-(3-sulfophenyl azo)-1,8-dihydroxy naphthlene-3,6-disulfonic acid 32 unit volumes, NaAc-HAc damping fluid 21 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 6.5 millimeters in the present embodiment, 14.8 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 12 centimetres, capillary tube segment length is 1.6 centimetres.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3,5-dinitroazobenzene)-7-(3-sulfophenyl azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid 24 unit volumes, NaAc-HAc damping fluid 53 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 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.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3,5-dinitroazobenzene)-7-(3-sulfophenyl azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid 7 unit volumes, NaAc-HAc damping fluid 59 unit volumes.
Embodiment nine: 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 1.2 centimetres, the height H of leaving a blank
2Be 16 centimetres, capillary tube segment length is 1.6 centimetres.
Indium colorimetric testing tube in the present embodiment, the indium determining liquid prescription is: contain 2-(2-hydroxyl-3,5-dinitroazobenzene)-7-(3-sulfophenyl azo)-1,8-dihydroxy-3,6-naphthalenedisulfonic acid 38 unit volumes, NaAc-HAc damping fluid 11 unit volumes.
Claims (9)
1. indium determining liquid, it is characterized in that: described indium determining liquid is formed by 0.005% azo-compound 1～40 unit volume and NaAc-HAc damping fluid 1～60 unit volume mixed preparing, measure the rising or the reduction of each components and concentration in the liquid, its volume is corresponding to be dwindled or increases; Described azo-compound is 2, two (the 2-hydroxyls-3-sulfo group-5-chlorobenzene azo)-1 of 7-, 8-dihydroxy-3,6-naphthalenedisulfonic acid, 2-(2-hydroxyl-3-sulfo group-5-nitrophenylazo)-7-(3-sulfophenyl azo)-1,8-dihydroxy naphthlene-3,6-disulfonic acid and 2-(2-hydroxyl-3,5-dinitroazobenzene)-7-(3-sulfophenyl azo)-1,8-dihydroxy-3, any in the 6-naphthalenedisulfonic acid.
2. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 1～13 unit volume wherein, NaAc-HAc damping fluid 1～60 unit volume.
3. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 13～28 unit volumes wherein, NaAc-HAc damping fluid 1～60 unit volume.
4. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 28～40 unit volumes wherein, NaAc-HAc damping fluid 1～60 unit volume.
5. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 1～19 unit volume.
6. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 19～41 unit volumes.
7. indium determining liquid according to claim 1 is characterized in that: 0.005% azo-compound 1～40 unit volume wherein, NaAc-HAc damping fluid 41～60 unit volumes.
8. indium 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 transition section with the kapillary of end sealing, it is characterized in that: the described indium determining liquid 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=1:2～20.
9. indium colorimetric testing 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 |
|---|---|---|---|
| CNB2005100485272A CN100543454C (en) | 2005-11-14 | 2005-11-14 | Indium determining liquid and colorimetric cylinder thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100485272A CN100543454C (en) | 2005-11-14 | 2005-11-14 | Indium determining liquid and colorimetric cylinder thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1773255A CN1773255A (en) | 2006-05-17 |
| CN100543454C true CN100543454C (en) | 2009-09-23 |
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|---|---|---|---|
| CNB2005100485272A Expired - Fee Related CN100543454C (en) | 2005-11-14 | 2005-11-14 | Indium determining liquid and colorimetric cylinder thereof |
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| Country | Link |
|---|---|
| CN (1) | CN100543454C (en) |
-
2005
- 2005-11-14 CN CNB2005100485272A patent/CN100543454C/en not_active Expired - Fee Related
Non-Patent Citations (2)
| Title |
|---|
| 间溴偶氮羧-m测定微量铟的研究. 王玉华.辽宁大学学报 自然科学版，第25卷第4期. 1998 |
| 间溴偶氮羧-m测定微量铟的研究. 王玉华.辽宁大学学报 自然科学版，第25卷第4期. 1998 * |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract record no.: 2012410000012 Denomination of invention: Indium determining liquid and its colorimetric estimation tube Granted publication date: 20090923 License type: Exclusive License Open date: 20060517 Record date: 20120306 |
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