Two. background technology: copper is very big to aquatic organism toxicity, and its toxicity is relevant with its form in water, and the toxicity of free state copper ion is than big many of the toxicity of complex state copper ion.Copper ion is 0.6mg/L to the critical harm concentration of paddy rice in the irrigation water.Because the existence of copper ion causes crop products to be polluted.The main pollution source of copper is in the waste water of dischargings such as industry such as plating, smelting, five metals and petrochemical complex, chemical industry.
At present, traditional copper content test method has atomic absorption spectrophotometry, cupral extraction spectrophotometric method etc.The basic step of cupral extraction spectrophotometric method is:
1. colour developing extraction
Draw an amount of sample in the 125mL separating funnel, add water to 50mL, add the 10mLEDTA-ammonium citrate, 5mL ammonium chloride-Ammonia shakes up.
Add 0.2% cupral solution 5mL, shake up, left standstill 5 minutes.
Add the 10mL phenixin, firmly duration of oscillation is no less than 2 minutes, leaves standstill, and waits for layering.
2. measure
Inhale the moisture content that removes the funnel neck with filter paper, fill in one little absorbent cotton, discard the phenixin phase 1~2mL of initial outflow, then phenixin is put into mutually the cuvette of 20mm drying, as reference, measure absorbance in 440nm wavelength place with phenixin.Replace sample with 50mL water, carry out blank test simultaneously by above-mentioned steps, deduct the absorbance of blank sample with the absorbance of sample after, find the content of copper from typical curve.
3. the drafting of typical curve
In 8 separating funnels, add 0mL, 0.20mL, 0.50mL, 1.00mL, 2.00mL, 3.00mL, 5.00mL respectively, 6.00mL copper standard is used liquid, adds water to 50mL, be made into one group of standard serial solution, developing the color by the aforesaid operations step then extracts and measures.After the absorbance that records made blank correction, again with corresponding copper content drawing standard curve.
The problem that the cupral extraction spectrophotometric method exists:
(1) employed copper standard solution and phenixin etc. can cause secondary pollution.
(2) operating process such as drafting of extraction and typical curve are tediously long, complexity, and labour intensity is big.
(3) need to use the Instrument measuring absorbance also with formula calculating concentration value, high to the operator quality requirement, the testing cost height.
(4) extraction and colorimetric operating process are wanted rapidly, in order to avoid resultant of reaction decomposes under light.
(5) in the test process, disturbing factor is many, deals with improperly and causes test error easily.
Three. the utility model content:
The purpose of this utility model is: at disadvantages of background technology, make a kind of easy to carry, copper colorimetric test tube of using simple and fast.
Technical solutions of the utility model are:
A kind of copper 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 copper 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: 2~10.
Described copper colorimetric test tube, the copper determination solution in the glass tube is an example with the unit volume, contain 0.05% ferrosin compound 1~30 unit volume, pH damping fluid 1~20 unit volume, mixed preparing forms, measure the raising or the reduction of each components and concentration in the liquid, its volume is corresponding to be dwindled or increases.
Described copper colorimetric test tube, 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: 5~7.
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 need during operation to fracture in the water sample to be measured capillary tube segment of test tube makes in the water sample automatic ration tail pipe to be measured and measures liquid generation metachromasia, with the contrast of standard color range, just can draw copper content more accurately in 5~10 minutes behind the colour stable.Need not be when each test preparing standard solution, reagent, can simplify the detection step greatly, save minute, reduce workload, reduce labor intensity.
2. 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 standard, and encapsulation forms the contrast color range, carries out the scene and detects, and need not to prepare other any reagent, and testing result accurately and reliably.The standard colour code can be made by standard color range pipe of the present 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 traditional cupral extraction spectrophotometric method, the utility model has reduced measuring process, has accelerated finding speed.
4. to measure the chromogenic reaction of liquid and determinand copper 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 meets the requirement of water analysis error precision accurately and reliably, and detection limit meets national potable water requirement 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 cupral extraction spectrophotometric method data comparison sheet:
Five. embodiment
Embodiment one: make the series standard colour code that detects copper content in advance, form color range.For example make 13 the color range pipes of standard colour code that detect copper content in the water quality, copper content is respectively 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, 3.0mg/L, the standard colour code of 4.0mg/L.At first get 0.05% phenanthroline 56mL, NaNO
3-NaOH damping fluid 18mL is mixed and made into mensuration liquid.Making copper content then respectively is 0.0mg/L, 0.1mg/L, 0.2mg/L, 0.3mg/L, 0.4mg/L, 0.5mg/L, 0.6mg/L, 0.8mg/L, 1.0mg/L, 1.5mg/L, 2.0mg/L, 3.0mg/L, 4.0mg/L 13 kinds of normal concentration copper liquors, will measure liquid and various normal concentration copper liquor and pour into reaction solution in 13 charomatrons respectively, and constant color in 1: 8 ratio, 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 copper liquor volume when measuring the corresponding formulation standard of the ratio color range pipe of liquid volume and the volume of leaving a blank in the pipe.Measure formula of liquid not simultaneously, the corresponding standard colour code of making, the color range of formation is also different.Only use the compound method of method description standard colour code for example at this.
Measure the pipe implementation method: referring to Fig. 1,1 is the uniform cross section glass tube with vacuum among the figure, and 2 is capillary tube segment, and 3 is copper determination solution.H
1For measuring liquid height, H
2For the uniform cross section glass tube with vacuum is left a blank highly.The mensuration liquid of the corresponding preparation standard colour code of present embodiment, promptly measuring liquid and aqueous solution volume ratio to be measured is 1: 8.6.5 millimeters of uniform cross section vacuum glass external diameter of pipe, 11.9 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.1 centimetres, the height H of leaving a blank
2Be 8.8 centimetres, capillary tube segment length is 2.0 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 2~5 minutes colour stables, the pairing copper concentration of colour code that is near the mark most numerical value is the copper content that records, if measure pipe color rank between two standard colour codes, then gets its mean value.
Copper colorimetric test tube of the present invention is measured formula of liquid: represent with unit volume, contain 0.05% phenanthroline 28 unit volumes, NaNO
3-NaOH 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 7.3 millimeters in the present embodiment, 8.4 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 2.3 centimetres, the height H of leaving a blank
2Be 4.6 centimetres, capillary tube segment length is 1.5 centimetres.Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% phenanthroline 10 unit volumes, NaNO
3-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 7.3 millimeters in the present embodiment, 12.7 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 10 centimetres, capillary tube segment length is 1.7 centimetres.
Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% phenanthroline 15 unit volumes, NaNO
3-NaOH damping fluid 6 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 6.9 millimeters in the present embodiment, 8.8 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 6 centimetres, capillary tube segment length is 1.6 centimetres.
Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% dark ferrosin 1 unit volume, KCl-HCl damping fluid 13 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, 12.2 centimetres of overall heights, the height H of mensuration liquid in the glass tube
1Be 1.3 centimetres, the height H of leaving a blank
2Be 9.1 centimetres, capillary tube segment length is 1.8 centimetres.
Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% dark ferrosin 20 unit volumes, KCl-HCl 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 7.1 millimeters in the present embodiment, 10.4 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 2.0 centimetres.
Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% 2,9-dimethyl-4,7-dihydroxy-1,10-ferrosin 10 unit volumes, NaOH damping fluid 20 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 6.9 millimeters in the present embodiment, and 10.2 centimetres of overall heights are in the glass tube
Measure the height H of liquid
1Be 1.1 centimetres, the height H of leaving a blank
2Be 7.7 centimetres, capillary tube segment length is 1.5 centimetres.
Copper colorimetric test tube in the present embodiment, the copper determination solution prescription is: represent with unit volume, contain 0.05% 2,9-dimethyl-4,7-dihydroxy-1,10-ferrosin 15 unit volumes, NaOH damping fluid 1 unit volume.