CN100510707C - Cobalt determination solution and colorimetric determination tube therefor - Google Patents
Cobalt determination solution and colorimetric determination tube therefor Download PDFInfo
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- CN100510707C CN100510707C CNB2005100485060A CN200510048506A CN100510707C CN 100510707 C CN100510707 C CN 100510707C CN B2005100485060 A CNB2005100485060 A CN B2005100485060A CN 200510048506 A CN200510048506 A CN 200510048506A CN 100510707 C CN100510707 C CN 100510707C
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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 cobalt content in water mass. The cobalt analyzing liquid comprises 0.005% nitroso compound solution 0-30 unit volume, and pH buffer liquid 0-20 unit volume, the analyzing tube contains uniform cross-section vacuum sealed glass tube, the glass tube is equipped with cobalt 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 = 1:2-20. The invention can realize quick-speed simplified measurement, higher accuracy, and longer retention time.
Description
One. technical field: the present invention relates to contain in a kind of water quality the assay method and the measuring appliance thereof of trace level chemical substance, particularly relate to cobalt determination solution and colorimetric cylinder thereof in a kind of water quality.
Two. background technology: cobalt (Co
2+) be one of human body and plant trace elements necessary.Cobalt content is very low in the natural water, and concentration is many at 0.002～1 μ g/L, can not produce toxic action to human body and animals and plants.The cobalt that often contains high concentration in the enterprise wastewater such as coloured smelting factory and processing factory, cobalt surpasses when a certain amount of in the water, can be to the look of water, smell, proterties such as flavor exerts an influence, and have and poison and carcinogenesis.The water that cobalt content surpasses 7.0～15.0mg/L can cause fish kills.To the harmful concentration of causing of the self-purification of water is 0.9mg/L.
At present, the assay method of cobalt has atomic absorption method, spectrophotometric method etc.
5-CL-PADAB spectrophotometric method basic step:
1. the drafting of calibration curve:
Get that to contain the cobalt amount be that the standard of 2.0mg/L uses liquid in the 25ml volumetric flask, add 5.0mlHAc-NaAc buffer solution, thin up is to the 10ml mixing; Place boiling water bath to heat 5min, take off.Add (1+1) HCL solution 10ml after being cooled to room temperature, water water is diluted to graticule, and mixing in 570nm wavelength place, is a reference with the blank reagent solution with the 20mm cuvette, measures absorbance.
2. sample analysis:
In the 25ml volumetric flask, following steps are with the drafting of calibration curve to draw clean surface water water sample 2～10ml (deciding on cobalt ions content in the water sample); If iron-holder height in the water sample should suitably be added sodium pyrophosphate solution, the consumption of sodium pyrophosphate solution should be identical with the mensuration water sample when drew calibration curve this moment.
For containing organic higher surface water and industrial waste water: draw water sample 2～20ml (deciding) in the 100ml beaker on cobalt ions content in the water sample, add 2ml nitric acid, cover surface plate, heated and boiled 1～5min on heating plate, take off cold slightly, add 1～2ml perchloric acid (deciding), continue to be heated to and emit white cigarette on the content of organic matter, and continue to solution do not have black residue transparent till.Be transferred in the 25ml volumetric flask after taking off cooling, add 1～2 paranitrophenol indicator, drip 20%NaOH and present yellow to solution, following steps are with the drafting of calibration curve.
3. for surface water and the industrial waste water of cobalt content below 0.02ml/L, carry out pre-service by following method.
(1) Sulfhydryl Cotton method: water sampling 500ml (deciding) on cobalt ions content in the water sample, add 10% ammonium tartrate solution 2.5ml, regulate PH to 8.5～9.5, adding PH is ammonium chloride-ammoniacal liquor buffer solution 10ml of 10, flow velocity with 1～4ml/min carries out wash-out at twice, and eluent is accepted with the 25ml volumetric flask, adds 1～2 paranitrophenol to eluent, drip 20%NaOH and present yellow to solution, following steps are with the drafting of calibration curve.
(2) AmbreliteXAD-2 type resin preenrichment:
Water sampling 500ml (deciding) on cobalt ions content in the water sample, transfer PH to 5～6, add the acetate-sodium acetate buffer solution 10ml of PH5～6,5-CL-PADAB solution 1.5ml heats 5min in boiling water bath, PH to 10 is regulated with 20% sodium hydroxide solution in the cooling back, flow velocity with 1～2ml/min passes through the adsorbent equipment enrichment, and the ethanolic solution 10ml with 95% is wash-out at twice, puts into water-bath behind the wash-out, be evaporated to about 5ml cooling; Add (1+1) HCL solution 10ml, be diluted with water to graticule, shake up, following steps are with the drafting of calibration curve.
If contain organic matter or other impurity and suspension etc. in the water sample, should clear up in advance or filter, carry out enrichment again.
The problem that the 5-CL-PADAB spectrophotometric method exists:
(1) to water sample pre-service and enrichment program complexity, deals with improperly and cause the cobalt data of being surveyed inaccurate easily.
(2) use of plurality of reagents causes secondary pollution easily, and to operation accuracy requirement height, some reagent needs now with the current.
(3) drafting of typical curve, operating process is tediously long, complexity, labour intensity is big.
(4) need to use the Instrument measuring absorbance, and, operator quality is required height, testing cost costliness with formula calculating concentration value.
Three. summary of the invention:
The objective of the invention is to simplify the cobalt testing procedure, shorten the test duration greatly, alleviate staff's labour intensity, make cobalt determination solution and colorimetric cylinder thereof.
The technical solution adopted in the present invention: a kind of cobalt determination solution, contain 0.005% nitroso compound 1～30 unit volume, PH damping fluid 0～20 unit volume, mixed preparing forms; Measure when each concentration of component improves in the liquid, its volume is corresponding to be reduced, when each concentration of component reduces, and the then corresponding increase of its volume.
Described cobalt determination solution, wherein 0.005% nitroso compound is 1～10 unit volume, the PH damping fluid is 0～20 unit volume.
Described cobalt determination solution, wherein 0.005% nitroso compound is 10～20 unit volumes, the PH damping fluid is 0～20 unit volume.
Described cobalt determination solution, wherein 0.005% nitroso compound is 20～30 unit volumes, the PH damping fluid is 0～20 unit volume.
Described cobalt determination solution, wherein 0.005% nitroso compound is 1～30 unit volume, the PH damping fluid is 0～8 unit volume.
Described cobalt determination solution, wherein 0.005% nitroso compound is 1～30 unit volume, the PH damping fluid is 8～15 unit volumes.
Described cobalt determination solution, wherein 0.005% nitroso compound is 1～30 unit volume, the PH damping fluid is 15～20 unit volumes.
Described cobalt determination solution, wherein nitroso compound is 1-nitroso--2 hydroxy naphthalene-3,6-sodium disulfonate, 2-nitroso--4-DMAP, 1-Nitroso-2-naphthol-6-sulfonic acid, the PH damping fluid is Na
2HPO
4-citric acid, KH
2PO
4-borax, Na
2HPO
4-citric acid.
A kind of cobalt colorimetric cylinder contains uniform cross section vacuum seal glass tube, is provided with one section sealing at glass tube one end and is communicated with capillary tube segment, adorns described aluminium determination solution 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=2～20.
Described mensuration pipe, the height H of mensuration liquid in glass tube
1With the glass tube uniform cross section height H of leaving a blank
2Ratio be H
1: H
2=1:4～15.
Described mensuration pipe contains 0.005% nitroso compound 1～30 unit volume in the cobalt determination solution, damping fluid 0～20 unit volume, the mensuration liquid that mixed preparing forms; Measure when concentration of component improves in the liquid, its volume is corresponding to be reduced; When concentration of component reduces, the then corresponding increase of its volume.
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 testing tube makes in the water sample automatic ration tail pipe to be measured and measures liquid generation metachromasia, with the contrast of standard color range, just can draw cobalt content more accurately behind the colour stable.Need not preparing standard solution, reagent when each test, can simplify the detection step greatly, save the test duration, reduce labor intensity.
2. to measure formula of liquid reasonable in the present invention, advanced technology, and stable performance is used simple.Can adopt standard sample liquid to react with it in advance, the fixing back of color forms permanent colour code standard, and encapsulation forms the contrast color range.The on-the-spot detection need not other any reagent, and testing result accurately and reliably.The standard colour code can be made by standard color range pipe, also can adopt other physical medium material such as computer color atlas, autochion printing paper, colour plastic plate or stained glass goods, uses very convenient.
3. compare with traditional 5-CL-PADAB spectrophotometry, the present invention need not to use large-scale instrument, has reduced measuring process, has accelerated finding speed.
4. the present invention measures liquid and determinand (cobalt) metachromasia, be to carry out automatically in the glass tube with vacuum under specific pH value condition, can effectively avoid accidental error and personal error, testing result accurately and reliably, detection limit meets national sewage comprehensive emission standard, and testing result meets the requirement of water analysis error precision.
The present invention carry, easy to use, measure simply, quick and precisely, the holding time is long.The on-the-spot detection do not need other equipment and instruments, uses manpower and material resources sparingly greatly, reduces integrated cost.The present invention is easy to promotion and implementation, has good social and economic benefit.
The present invention measures Guan Fayu 5-CL-PADAB spectrophotometric method data comparison sheet:
Four. description of drawings: Fig. 1: cobalt colorimetric cylinder structural representation
Five. embodiment:
Embodiment one; 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 cobalt determination solution.H
1For measuring liquid height, H
2For the uniform cross section glass tube with vacuum is left a blank highly.Uniform cross section glass tube with vacuum internal diameter 7.0mm in this example, overall height is 12cm, measures the liquid height H in the glass tube
1Be 1.5cm, the height H of leaving a blank
2Be 8.0cm, capillary tube segment length is 2.5cm.
The mensuration formula of liquid is: contain 1-nitroso--2 hydroxy naphthalene-3 of 0.005%, 6-sodium disulfonate 8L, Na
2HPO
4-citric acid 13L is hybridly prepared into the cobalt determination solution of 21L, makes the mensuration pipe of some by demand can vacuum seal.
Make the series standard colour code that detects cobalt content, the method that forms color range: for example make 10 the color range pipes of standard colour code that detect low concentration cobalt content in the water quality, cobalt content is respectively 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, the standard colour code of 3.0mg/L.At first get 1-nitroso--2 hydroxy naphthalene-3 of 0.005%, 6-sodium disulfonate 8L, Na
2HPO
4-citric acid 13L is hybridly prepared into mensuration liquid; Making cobalt content then respectively is 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.4mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, 3.0mg/L 10 kinds of normal concentration cobalt aqueous solution, to measure liquid and various normal concentration cobalt aqueous solution in the 1:10 ratio, pour into reaction solution in 10 charomatrons respectively, and constant color, seal charomatron then, form non-fading serial color range standard colors mark pipe.Should be noted in the discussion above that and only measuring and its height H of mensuration liquid of measuring the Guan Zhongtong proportioning in measuring the colour code that liquid and normal concentration cobalt aqueous solution 1:10 ratio are made
1With the uniform cross section glass tube with vacuum height H of leaving a blank
2Ratio just meaningful when being 1:10.
Can make the high concentration cobalt content with quadrat method and be respectively 0.0mg/L, 1.0mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L, 5.0mg/L, 6.0mg/L, 8.0mg/L, 9 standard charomatron colour codes of 10.0mg/L specifically no longer describe in detail.Certainly measure the formula of liquid difference, the color range of corresponding standard colour code of making and formation is also different, only illustrates standard colors target compound method at this.
The capillary tube segment that to measure pipe during use immerses in the analyte sample fluid, kapillary fractures, be filled the uniform cross section glass tube with vacuum section of leaving a blank Deng analyte sample fluid, take out to be inverted repeatedly and mix, make it fully to carry out chromogenic reaction, with the contrast of standard colour code, the pairing cobalt concentration numerical value of the colour code that is near the mark most is the cobalt content that records behind about 1～5min colour stable; If measure the pipe color between two standard colour codes, then get its mean value.
Embodiment two: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 8mm in this example, and overall height is 10.0cm, measures the liquid height H in the glass tube
1Be 1.0cm, the height H of leaving a blank
2Be 7.0cm, capillary tube segment length is 2.0cm.
The mensuration formula of liquid is: contain 1-nitroso--2 hydroxy naphthalene-3 of 0.005%, 6-sodium disulfonate 17L, Na
2HPO
4-citric acid 10L is hybridly prepared into the cobalt determination solution of 27L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment three: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 8mm in this example, and overall height is 14.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 10.0cm, capillary tube segment length is 2.0cm.
The mensuration formula of liquid is: contain 1-nitroso--2 hydroxy naphthalene-3 of 0.005%, 6-sodium disulfonate 10L, Na
2HPO
4-citric acid is 0L, is mixed with the cobalt determination solution of 10L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment four: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 6mm in this example, and overall height is 20.0cm, measures the liquid height H in the glass tube
1Be 2.5cm, the height H of leaving a blank
2Be 15.0cm, capillary tube segment length is 2.5cm.
The cobalt determination solution prescription is: contain 2-nitroso--4-DMAP 8L of 0.005%, KH
2PO
4-borax 18L is hybridly prepared into the cobalt determination solution of 26L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment five: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 8mm in this example, and overall height is 11.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 7.0cm, capillary tube segment length is 2.0cm.
The cobalt determination solution prescription is: contain 2-nitroso--4-DMAP 28L of 0.005%, KH
2PO
4-borax 10L is hybridly prepared into the cobalt determination solution of 38L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment six: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 8mm in this example, and overall height is 11.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 7.0cm, capillary tube segment length is 2.0cm.
The cobalt determination solution prescription is: contain 2-nitroso--4-DMAP 5L of 0.005%, KH
2PO
4-borax 15L is hybridly prepared into the cobalt determination solution of 20L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment seven: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 7.5mm in this example, and overall height is 13.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 9.0cm, capillary tube segment length is 2.0cm.
The cobalt determination solution prescription is: contain 1-Nitroso-2-naphthol-6-sulfonic acid 15L of 0.005%, Na
2HPO
4-citric acid 16L is hybridly prepared into the cobalt determination solution of 31L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment eight: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 7.5mm in this example, and overall height is 13.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 9.0cm, capillary tube segment length is 2.0cm.
The cobalt determination solution prescription is: contain 1-Nitroso-2-naphthol-6-sulfonic acid 24L of 0.005%, Na
2HPO
4-citric acid 10L is hybridly prepared into the cobalt determination solution of 34L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Embodiment nine: present embodiment and embodiment one are basic identical, and difference is: uniform cross section glass tube with vacuum internal diameter is 7.5mm in this example, and overall height is 12.0cm, measures the liquid height H in the glass tube
1Be 2.0cm, the height H of leaving a blank
2Be 8.0cm, capillary tube segment length is 2.0cm.
The cobalt determination solution prescription is: contain 1-Nitroso-2-naphthol-6-sulfonic acid 6L of 0.005%, Na
2HPO
4-citric acid 14L is hybridly prepared into the cobalt determination solution of 20L, makes the said determination pipe of some by demand can vacuum seal.
Preparation of mensuration liquid and mensuration are managed the making method, the colour code method for making is identical with embodiment one, do not repeat.
Claims (8)
1. cobalt determination solution is characterized in that: contain 0.005% nitroso compound 1～30 unit volume, and PH damping fluid 0～20 unit volume, mixed preparing forms; Described PH damping fluid is Na
2HPO
4-citric acid or KH
2PO
4-borax, described nitroso compound are 1-nitroso--2 hydroxy naphthalene-3,6-sodium disulfonate, 2-nitroso--4-DMAP or 1-Nitroso-2-naphthol-6-sulfonic acid.
2. cobalt determination solution according to claim 1 is characterized in that: wherein 0.005% nitroso compound is 1～10 unit volume, and the PH damping fluid is 0～20 unit volume.
3. cobalt determination solution according to claim 1 is characterized in that: wherein 0.005% nitroso compound is 10～20 unit volumes, and the PH damping fluid is 0～20 unit volume.
4. cobalt determination solution according to claim 1 is characterized in that: wherein 0.005% nitroso compound is 20～30 unit volumes, and the PH damping fluid is 0～20 unit volume.
5. cobalt determination solution according to claim 1 is characterized in that: wherein 0.005% nitroso compound is 1～30 unit volume, and the PH damping fluid is 0～8 unit volume.
6. cobalt determination solution according to claim 1 is characterized in that: wherein 0.005% nitroso compound is 1～30 unit volume, and the PH damping fluid is 8～15 unit volumes; Or 0.005% nitroso compound is 1～30 unit volume, and the PH damping fluid is 15～20 unit volumes.
7. a cobalt colorimetric cylinder contains uniform cross section vacuum seal glass tube, is provided with one section sealing at glass tube one end and is communicated with capillary tube segment, it is characterized in that: cobalt 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=1:2～20; Contain 0.005% nitroso compound 1～30 unit volume in the described cobalt determination solution, damping fluid 0～20 unit volume, mixed preparing forms; Described PH damping fluid is Na
2HPO
4-citric acid or KH
2PO
4-borax, described nitroso compound are 1-nitroso--2 hydroxy naphthalene-3,6-sodium disulfonate, 2-nitroso--4-DMAP or 1-Nitroso-2-naphthol-6-sulfonic acid.
8. mensuration pipe according to claim 7 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=1:4～15.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100485060A CN100510707C (en) | 2005-11-09 | 2005-11-09 | Cobalt determination solution and colorimetric determination tube therefor |
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|---|---|---|---|
| CNB2005100485060A CN100510707C (en) | 2005-11-09 | 2005-11-09 | Cobalt determination solution and colorimetric determination tube therefor |
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| CN103411962B (en) * | 2013-05-15 | 2015-12-02 | 中国科学院烟台海岸带研究所 | A kind of cobalt ions colorimetric determination kit and detection method thereof |
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Non-Patent Citations (4)
| Title |
|---|
| 1-亚硝基-2-萘酚固相萃取光度法测定痕量钴（II）的研究. 董学畅，贾智若，刘志华，缪明明，翁哲慧.云南民族大学学报（自然科学版），第14卷第4期. 2005 |
| 1-亚硝基-2-萘酚固相萃取光度法测定痕量钴（II）的研究. 董学畅，贾智若，刘志华，缪明明，翁哲慧.云南民族大学学报（自然科学版），第14卷第4期. 2005 * |
| 酸性镀金液中微量钴的光度测定. 丘星初，丘山，何伟明，刘春娣.电镀与精饰，第22卷第2期. 2000 |
| 酸性镀金液中微量钴的光度测定. 丘星初，丘山，何伟明，刘春娣.电镀与精饰，第22卷第2期. 2000 * |
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Assignee: ZHENGZHOU WATER TESTING TECHNOLOGY CO., LTD. Assignor: Bai Li Contract record no.: 2012410000012 Denomination of invention: Cobalt determination solution and colorimetric determination tube therefor Granted publication date: 20090708 License type: Exclusive License Open date: 20060503 Record date: 20120306 |
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