CN1773252A - Arsenic assaying liquid and colorimetric cylinder thereof - Google Patents
Arsenic assaying liquid and colorimetric cylinder thereof Download PDFInfo
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- CN1773252A CN1773252A CN 200510048503 CN200510048503A CN1773252A CN 1773252 A CN1773252 A CN 1773252A CN 200510048503 CN200510048503 CN 200510048503 CN 200510048503 A CN200510048503 A CN 200510048503A CN 1773252 A CN1773252 A CN 1773252A
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Abstract
The present invention relates to a determination method of trace chemical substance in the water quality and its determination device. In particular, it relates to determination liquor for quickly determining arsenium content in the water quality and its colorimetric determination tube. The invented determination liquor is made up by mixing 0.01% dithiocarbamic acid compound 1-50 unit volume, organic solvent 1-30 unit volume and pH regulating agent 1-50 unit volume. Its determination tube contains an uniform-section vacuum sealed glass tube in which the determination liquor is held, the ratio of the height H1 of the determination liquor level in the glass tube and the glass tube uniform-section space-remained height H2 is H1:H2=1:2-20.
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 arsenic Determination on content liquid and colorimetric cylinder thereof in a kind of fast measuring water quality.
Two. background technology: arsenic (AS) is the human body non-essential element, and the compound of arsenic is all poisonous, and the trivalent arsenic compound is stronger than pentavalent arsenic toxicity of compound, and organo-arsenic all has severe toxicity to human body and biology.Arsenic contacts by respiratory tract, alimentary canal and skin and enters human body.If intake surpasses excretion, arsenic will particularly be accumulated in hair, nail, thereby cause arsenicalism at positions such as the liver of human body, kidney, lung, uterus, placenta, bone, muscle, is latent period several years even decades.Arsenicalism has gastrointestinal symptom, neurological symptom and cutaneous lesions etc.Arsenic also has carcinogenesis, can cause cutaneum carcinoma.In the ordinary course of things, soil, water, air, plant and human body all contain the arsenic of denier, can not constitute harm to human body.Arsenic is one of index of China's enforcement total emission volumn control.
Arsenic content has very big-difference in the surface water because of the water source is different with geographical conditions.Fresh water is 0.2～230 μ g/L, and average out to 0.5 μ g/L, seawater are 3.7 μ g/L.The pollution source of arsenic are mainly derived from the industrial waste water of departments such as mining, metallurgy, chemical industry, chemical pharmacy, pesticide producing, textile industry, glass, process hides.
The conventional test methodologies of arsenic is lignocaine two a bamic acids silver photometry, and its operation steps is:
1. specimen preparation is at first got the 50mL sample, or with an amount of diluted sample to 50mL (arsenic content is less than 25 μ g), place arsenic hydride that bottle takes place, add 4mL sulfuric acid and 5mL nitric acid, in ventilating kitchen, clear up to producing white smoke, do not clarify, can add the 5mL red fuming nitric acid (RFNA) again as solution, continue to be heated to the generation white smoke, clarify until solution.After the cooling, add 25mL water, be heated to the generation white smoke again, drive most nitric acid.Add water then, making cumulative volume is 50mL, is equipped with to measure to use.
2. the measurement of sample
(1) colour developing: take place to add 4mL liquor kalii iodide and 2mL stannous chloride solution in the bottle in above-mentioned arsenic hydride, shake up, placed 15 minutes.Get the 5mL absorption liquid and place dry absorption tube, insert wireway, add the 4g arsenic-free zinc granule rapidly in arsenic hydride generation bottle, exist side by side soon wireway is connected (it is air tight to guarantee to connect bottle) with the generation bottle.At room temperature reacted 1 hour, arsenic is disengaged fully, and add methenyl choloride the absorption liquid volume is supplied 5mL.Entire reaction is in ventilating kitchen or draughty indoor carrying out.
(2) measure: use the 10mm cuvette, be that reference is measured the absorbance of absorption liquid at 510nm wavelength place with the methenyl choloride, and make blank correction.
3. 8 arsenic hydrides that are drawn on of typical curve take place to add 0 μ g, 1.00 μ g, 2.50 μ g, 5.00 μ g, 10.00 μ g, 15.00 μ g, 20.00 μ g, 25.00 μ g arsenic standard solutions respectively in the bottle, add water to 50mL.Add the 4mL concentrated sulphuric acid respectively, below develop the color and measure, and draw through the absorbance of blank correction typical curve to arsenic content by the operation of said sample.
The problem that lignocaine two bamic acids silver photometry exists:
(1) uses a large amount of arsenic titer, nitric acid, sulfuric acid, hydrochloric acid and perchloric acid, artificial cause chemical contamination.
(2) arsenide severe toxicity has the danger of effusion in the evaporation operation process.
(3) 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.
(4) need with the Instrument measuring absorbance and with formula calculating concentration value, high to the operator quality requirement, the testing cost costliness.
(5) in test, disturbing factor is many, gets rid of trouble, deals with improperly and causes measured data inaccurate easily, and error is big.
Three. summary of the invention:
Purpose of the present invention: simplify arsenic Determination on content step in the water, shorten minute greatly, alleviate intensity of workers, reduce environmental pollution, make arsenic assaying liquid and colorimetric cylinder thereof.
Technical solution of the present invention:
A kind of arsenic assaying liquid contains 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume, 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 arsenic assaying liquid, 0.01% dithiocarbamic acid compound 1～17 unit volume wherein, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 17～36 unit volumes, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 36～50 unit volumes, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume.
Described arsenic assaying liquid, 0.01% dithiocarbamic acid compound 1～50 unit volume wherein, pH regulator agent 1～17 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 17～36 unit volumes, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 36～50 unit volumes, organic solvent 1～30 unit volume.
Described arsenic assaying liquid, 0.01% dithiocarbamic acid compound 1～50 unit volume wherein, pH regulator agent 1～50 unit volume, organic solvent 1～9 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 9～21 unit volumes; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 21～30 unit volumes.
A kind of arsenic 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 arsenic 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: 2～20.
Arsenic assaying liquid in the glass tube contains 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume, 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.
Measure the height H of liquid in the glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1: 9～13.
Positive beneficial effect of the present invention is:
1. the present invention is with the detection technique commercialization, and commercialization is loaded on the mensuration fluid-tight for preparing in the glass tube with vacuum, can directly use.Only needing during operation fracture in water sample to be measured measures the capillary tube segment of pipe, makes in the water sample automatic ration tail pipe to be measured and measures liquid generation metachromasia, just can draw arsenic content more accurately with the contrast of standard color range behind the colour stable.Need not be when each mensuration preparing standard solution, reagent, can simplify the detection step greatly, save minute, reduce workload, reduce labor intensity, reduce environmental pollution.
2. to measure formula of liquid reasonable in the present invention, advanced technology, and stable performance is used simple.Adopt standard sample liquid to react with it in advance, constant color forms permanent colour code, and encapsulation forms the contrast color range, carries out the scene and detects, and need not to prepare other any reagent, and testing result accurately and reliably.The standard colour code can be made by standard color range pipe of the present invention and form, also can be, or the colored printing cardboard, or the colored plastic rod by the computer color atlas, or other physical medium material such as stained glass goods forms, and uses very convenient.
3. compare with the method for traditional lignocaine two bamic acids silver spectrphotometric method for measuring arsenic content, the present invention has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand arsenic 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 lignocaine two bamic acids silver photometry data comparison sheet:
Four. description of drawings
Fig. 1: arsenic colorimetric test tube structural representation
Five. embodiment
Embodiment one:
Make the series standard colour code that detects arsenic content in advance, form color range.For example make 9 the color range pipes of standard colour code that detect arsenic content in the water quality, arsenic content is respectively 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.04mg/L, 0.06mg/L, 0.08mg/L, 0.10mg/L, the standard colour code of 0.20mg/L.At first get 0.01% diethyl amino dithioacid diethyl ammonium 85mL, 1.0mol/L sulfuric acid 180mL, carbon tetrachloride solvent 45mL, be mixed and made into mensuration liquid, making arsenic content then respectively is 0.0mg/L, 0.01mg/L, 0.02mg/L, 0.03mg/L, 0.04mg/L, 0.06mg/L, 0.08mg/L, 0.10mg/L, 0.20mg/L 9 kinds of normal concentration arsenic aqueous solution, will measure liquid and various normal concentration arsenic aqueous solution pours into reaction solution in 9 charomatrons respectively in 1: 9 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 arsenic 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 arsenic 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 arsenic concentration numerical value of the colour code that is near the mark most is the arsenic content that records, if measure the pipe color between two standard colour codes, then gets its mean value.
Arsenic colorimetric test tube of the present invention is measured formula of liquid: contain 0.01% diethyl amino dithioacid diethyl ammonium 17 unit volumes, 1.0mol/L sulfuric acid 36 unit volumes, carbon tetrachloride solvent 9 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, 7.8 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 4.2 centimetres, capillary tube segment length is 1.5 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% diethyl amino dithioacid diethyl ammonium 36 unit volumes, 1.0mol/L sulfuric acid 1 unit volume, carbon tetrachloride solvent 21 unit volumes.
Embodiment three: referring to Fig. 1, numbering is identical with embodiment one among the figure, represents same meaning.The using method of standard colors target method for making, the method for making of measuring pipe and testing tube no longer is 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.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: represent with unit volume, contain 0.01% diethyl amino dithioacid diethyl ammonium 1 unit volume, 1.0mol/L sulfuric acid 17 unit volumes, carbon tetrachloride solvent 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, 22.7 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 20 centimetres, capillary tube segment length is 1.7 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% diethyl amino dithioacid silver 50 unit volumes, 0.1% cinchonine, 11 unit volumes, methenyl choloride solvent 6 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, 13.8 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 10.8 centimetres, capillary tube segment length is 1.8 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% diethyl amino dithioacid silver 42 unit volumes, 0.1% cinchonine, 50 unit volumes, methenyl choloride solvent 15 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 6.5 millimeters in the present embodiment, 10.2 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.2 centimetres, the height H of leaving a blank
2Be 7.2 centimetres, capillary tube segment length is 1.8 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% diethyl amino dithioacid silver 25 unit volumes, 0.1% cinchonine, 43 unit volumes, methenyl choloride solvent 1 unit volume.
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 7.0 millimeters in the present embodiment, 15.6 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.0 centimetres, the height H of leaving a blank
2Be 13 centimetres, capillary tube segment length is 1.6 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% ammonium pyrrolidine dithiocarbamate 11 unit volumes, 0.2mol/L sulfuric acid 25 unit volumes, methenyl choloride 13 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, 12.8 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 10 centimetres, capillary tube segment length is 1.8 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% ammonium pyrrolidine dithiocarbamate 13 unit volumes, 0.2mol/L sulfuric acid 39 unit volumes, methenyl choloride 25 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, 17.8 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 15 centimetres, capillary tube segment length is 1.8 centimetres.
Arsenic colorimetric test tube in the present embodiment, the arsenic assaying liquid prescription is: contain 0.01% ammonium pyrrolidine dithiocarbamate 46 unit volumes, 0.2mol/L sulfuric acid 11 unit volumes, methenyl choloride 18 unit volumes.
Claims (7)
1. an arsenic assaying liquid is characterized in that: contain 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume, 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. arsenic assaying liquid according to claim 1 is characterized in that: 0.01% dithiocarbamic acid compound 1～17 unit volume wherein, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 17～36 unit volumes, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 36～50 unit volumes, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume.
3. arsenic assaying liquid according to claim 1 is characterized in that: 0.01% dithiocarbamic acid compound 1～50 unit volume wherein, pH regulator agent 1～17 unit volume, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 17～36 unit volumes, organic solvent 1～30 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 36～50 unit volumes, organic solvent 1～30 unit volume.
4. arsenic assaying liquid according to claim 1 is characterized in that: 0.01% dithiocarbamic acid compound 1～50 unit volume wherein, pH regulator agent 1～50 unit volume, organic solvent 1～9 unit volume; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 9～21 unit volumes; Or 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 21～30 unit volumes.
5. arsenic 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: arsenic 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: 2～20.
6. arsenic colorimetric test tube according to claim 5, arsenic assaying liquid in the glass tube, contain 0.01% dithiocarbamic acid compound 1～50 unit volume, pH regulator agent 1～50 unit volume, organic solvent 1～30 unit volume, 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.
7. arsenic colorimetric test tube according to claim 5 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.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100485037A CN100510706C (en) | 2005-11-08 | 2005-11-08 | Arsenic assaying liquid and colorimetric cylinder thereof |
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|---|---|---|---|
| CNB2005100485037A CN100510706C (en) | 2005-11-08 | 2005-11-08 | Arsenic assaying liquid and colorimetric cylinder thereof |
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|---|---|
| CN1773252A true CN1773252A (en) | 2006-05-17 |
| CN100510706C CN100510706C (en) | 2009-07-08 |
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|---|---|---|---|
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102262087A (en) * | 2011-04-27 | 2011-11-30 | 杭州慕迪科技有限公司 | On-line monitoring device for total arsenic in water quality |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1265373A (en) * | 2000-02-18 | 2000-09-06 | 李兴德 | Yellow phosphorus de-oiling and dearsenicating method |
| JP4170189B2 (en) * | 2003-10-02 | 2008-10-22 | 株式会社アペレ | Measuring cell such as a colorimeter and method of using the same |
| CN2704840Y (en) * | 2004-03-12 | 2005-06-15 | 白莉 | Chlorinedioxide colorimetric determining tubes |
| CN2840021Y (en) * | 2005-11-08 | 2006-11-22 | 白莉 | Arsenic colorimetric estimation cylinder |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102262087A (en) * | 2011-04-27 | 2011-11-30 | 杭州慕迪科技有限公司 | On-line monitoring device for total arsenic in water quality |
| CN102262087B (en) * | 2011-04-27 | 2013-01-16 | 杭州慕迪科技有限公司 | On-line monitoring device for total arsenic in water quality |
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| CN100510706C (en) | 2009-07-08 |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract record no.: 2012410000012 Denomination of invention: Arsenic assaying liquid and colorimetric cylinder thereof Granted publication date: 20090708 License type: Exclusive License Open date: 20060517 Record date: 20120306 |
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