CN110346355A - A kind of method of the total zinc of online automatic detection of anti-various metals ion interference - Google Patents
A kind of method of the total zinc of online automatic detection of anti-various metals ion interference Download PDFInfo
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Abstract
The invention discloses a kind of methods of the total zinc of online automatic detection of anti-various metals ion interference, testing process are as follows: prepare used reagent, first complete the calibration of standard curve, and demonstrate the accuracy of online automatic detection equipment, then single interfering ion solution or mixing interfering ion solution are tested, obtain corresponding absorbance, total Zn content is calculated in the solution containing interfering ion in online automatic detection equipment establishing criteria curve, while also verifying interfering ion whether there is or not influences on testing result.Use this method, on-line automatic equipment it is linear and reproducible, recovery of standard addition is met the requirements, apply this method to pollution sources or surface water quality online auto monitoring field, to the waste water real-time monitoring that blowdown enterprise is discharged, be of great significance, especially for being electroplated, process hides, printing and dyeing, the industries such as metallurgy, even if also being had no significant effect containing other interference metal ions of more and high concentration to test result in the waste water discharged.
Description
Technical field
The present invention relates to a kind of chemical analysis, detection field, in particular to a kind of anti-various metals ion interference it is online
Automatically the method for total zinc is detected.
Background technique
The standard method of zinc detection is: in the acetate buffer solution medium that pH is 4.0~5.5, zinc ion and double sulphur
Hydrazone forms red chelate, which can be completed to measure by chloroform quantified extract with mixed-color method；It needs to make in test
With toxic reagent, and it is easy loss in extraction process, causes test inaccurate；
Another zinc ion detection principle be: the water sample of certain volume, be added buffer solution, by system pH adjust to
Between 8.8~9.0, the zincon dissolved in ethanol forms blue complex with zinc ion under this condition, in wavelength 610nm
Place carries out colorimetric test, and according to the relationship between concentration and absorbance, standard curve is calculated, then unknown molten by measuring
The absorbance of liquid can calculate the zinc ion concentration contained in unknown solution.
The method of the zinc ion of both the above measurement at present can all be led when for containing other metal ion disturbances in water sample
It causes test result large error occur, is not consistent with the content of zinc practical in solution.Generate interference the reason of may be: interfere from
Son can also be chemically reacted with color developing agent, caused chromogenic reaction insensitive or formed similar complex compound, carrying out colorimetric
When measurement, absorbance and actual conditions deviation are larger, and the resultant error being calculated is also larger.Simultaneously because interfering ion concentration
It is unstable, cause measurement repeatability it is also poor.
Summary of the invention
In order to solve above-mentioned deficiency in the prior art, it is dry that the purpose of the present invention is to provide a kind of anti-various metals ions
The method of the total zinc of the online automatic detection disturbed.
The technical solution adopted by the present invention to solve the technical problems are as follows: a kind of anti-various metals ion interference it is online from
The method of the dynamic total zinc of detection, comprising the following steps:
(1) configuration of solution is tested；
Wherein, the test solution includes zinc standard solution and containing interfering ion solution, it is described containing interference from
Sub- solution includes single interfering ion solution, mixing interfering ion solution, mixing interfering ion mark-on solution；
(2) preparation of online automatic detection equipment reagent；
Wherein, the online automatic detection equipment reagent includes oxidant, mixed masking agent, buffer solution and colour developing
Agent；
(3) calibration of online automatic detection equipment:
Use the zinc standard solution that concentration is 2mg/L as the measuring range adjustment solution of online automatic detection equipment,
Line automatic checkout equipment is according to process sequence: being first added in blank solution or measuring range adjustment solution to resolution bottle, adds the oxygen
Agent, be bubbled mixing after, 115~120 DEG C at a temperature of heat, high-temperature closed oxidation resolution 10min after cool down, to temperature
When being down to 42~50 DEG C, mixed masking agent is added into the resolution bottle, after being bubbled mixing, the buffer solution is being added,
After being bubbled mixing again, 1min is stood, then opens the LED light source that wavelength is 610nm, on-line automatic equipment is carried on the back at this time
The measurement of scape light intensity measures 30 seconds, automatically records data, the color developing agent is then added into resolution bottle, wait be bubbled mixing
Afterwards, reaction 5min is stood, complex reaction occurs for color developing agent and zinc ion at this time, generates blue complex, being again turned on wavelength is
The LED light source of 610nm, blue complex have absorption at wavelength 610nm, carry out the measurement for absorbing light intensity again, measure 30 seconds,
Automatically record data；Online automatic detection equipment can calculate automatically absorbance according to the absorption light intensity of background light intensity and complex compound；
During online automatic detection equipment Alignment, the absorbance of advanced line blank pure water is tested, then is carried out zinc concentration and be
The test of 2mg/L measuring range adjustment solution absorbance, online automatic detection equipment can successively be recorded twice absorbance respectively, according to lambert
Standard curve can be obtained in Beer law, and standard curve is stored in the control system of online detection instrument；
(4) accuracy of online automatic detection equipment and repeatability verifying；
The accuracy of online automatic detection equipment and repeatability verifying: after the completion of online automatic detection equipment Alignment, according to school
The parameter and sequence of quasi- process are tested, and the use of concentration are respectively the institute of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L
Zinc standard solution is stated to be tested, every group solution follow-on test six times, according to the registration of test result and standard curve, sentence
The accuracy and repeatability of disconnected online automatic detection equipment；
(5) containing total Zn content in interfering ion solution described in testing in online automatic detection equipment, verifying contains
The accuracy of total Zn content test in interfering ion solution；
(6) the online automatic detection equipment is passed through environmental water sample, total zinc in environmental water sample is measured.
Optionally, the configuration method of total zinc standard solution are as follows:
Zinc standard solution 0.1ml, 0.2ml, 0.5ml, 1.0ml, 2.0ml that concentration is 1000 μ g/ml are accurately pipetted respectively
Be placed in 1000ml volumetric flask, be settled to scale with no zinc water, respectively obtained after shaking up concentration be 0.1mg/L, 0.2mg/L,
The zinc standard of 0.5mg/L, 1.0mg/L, 2.0mg/L use solution.
Optionally, the configuration method of the single interfering ion solution are as follows:
The Zinc standard solution that 2.0ml concentration is 1000 μ g/ml is accurately pipetted to be placed in 2000ml volumetric flask, it is fixed with no zinc water
Hold the zinc standard solution for obtaining that concentration is 1.0mg/L after shaking up to scale；
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution are placed in the 100ml volumetric flask of 5 different dryings, the zinc mark for being 1.0mg/L with concentration
Standard is settled to scale using liquid, respectively obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel ion, Cr VI from
The solution that sub, aluminum ions five groups of single interfering ions and zinc concentration are 1mg/L；
The concentration for accurately pipetting 1.0ml respectively is iron standard solution, calcium standard solution, the magnesium standard solution of 1000 μ g/ml
It is placed in the 100ml volumetric flask of 3 different dryings, the zinc standard solution for being 1.0mg/L with concentration is settled to scale, shakes up
Being respectively obtained afterwards containing 10.0mg/L iron ion, calcium ion, three groups of single interfering ions of magnesium ion and zinc concentration is 1mg/L
Solution.
Optionally, the configuration method of the mixing interfering ion solution are as follows:
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution；Accurately pipette 2.0ml concentration be the iron standard solution of 1000 μ g/ml, calcium standard solution,
Magnesium standard solution is placed in the 100ml volumetric flask of the same drying, and the zinc standard solution for being 1.0mg/L with concentration is settled to quarter
Degree is obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminium ion, 10.0mg/L iron from
The solution that son, calcium ion, the mixing interfering ion of magnesium ion and zinc concentration are 1mg/L.
Optionally, the mixing interfering ion mark-on solution preparation method are as follows:
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution；Accurately pipette 2.0ml concentration be the iron standard solution of 1000 μ g/ml, calcium standard solution,
Magnesium standard solution is placed in the 100ml volumetric flask of the same drying；Accurately pipetting 0.10ml concentration again is 1000 μ g/ml zinc standards
Solution is placed in the drying capacity bottle of above-mentioned 100ml, and the zinc standard solution for being then 1.0mg/L with concentration is settled to scale,
Obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminium ion, 10.0mg/L iron ion,
The solution for the mark-on 1.0mg/L that calcium ion, the mixing interfering ion of magnesium ion and zinc concentration are 1mg/L.
Optionally, the preparation method of the oxidant is to prepare 0.025mol/L ammonium persulfate solution: taking a 500ml
Clean beaker, 300ml is added without zinc water, then accurately weighs that 2.8525g ammonium persulfate is soluble in water, and stirring and dissolving is complete
Afterwards, it is poured into 500ml volumetric flask, is settled to scale, shake up, for use；
The preparation method of the mixed masking agent are as follows: separately take the clean beaker of a 500ml, 300ml is added without zinc water, so
After to accurately weigh 21.814g thiocarbamide soluble in water, after stirring and dissolving is complete, then it is accurate 1.00g sodium thiosulfate is added, stir molten
After solution is complete, then accurate addition aminated compounds 12.258g, after stirring and dissolving is complete, it is poured into 500ml volumetric flask, constant volume
It to scale, shakes up, for use；
The preparation method of the buffer solution is, matches preparing boric acid-potassium chloride-sodium hydroxide buffer solution: pH value is 8.8~
Between 9.0；
The preparation method of the color developing agent are as follows:
A, a 500ml clean beaker separately is taken, measures 200ml dehydrated alcohol with graduated cylinder and be poured into beaker, accurately weighs
The special color developing agent zincon of 0.52g is into dehydrated alcohol, using ultrasonic wave stirring and dissolving；
B, a 500ml clean beaker is separately taken, is added without zinc water 150ml, it is molten to accurately weigh a kind of ammonium class compound 6.50g
In Xie Wu zinc water, stirring and dissolving is complete；
The step b solution prepared is poured into the solution of step a preparation, is poured into 500ml volumetric flask after mixing
In, it is settled to scale with no zinc water, is shaken up, for use.
Optionally, when calibrating the online automatic detection equipment, the blank solution used is no zinc water.
Optionally, single interfering ion or mixing interfering ion is added when detecting, solution to be measured and each reagent are added
Ratio is as follows: 4.3~4.5ml of solution additional amount to be measured, oxidant additional amount: 1.0~1.2ml, and 118~122 DEG C of pyroreaction,
10min, mixed masking agent additional amount: 1.0~1.2ml, buffer solution additional amount: 1.0~1.2ml, color developing agent additional amount: 1.0
~1.2ml.
Optionally, single interfering ion or mixing interfering ion is added when detecting, solution to be measured and each reagent are added
Ratio is as follows: solution additional amount 4.4ml to be measured, oxidant additional amount: 1.1ml, and 120 DEG C of pyroreaction, 10min, mixing masking
Agent additional amount: 1.1ml, buffer solution additional amount: 1.1ml, color developing agent additional amount: 1.1ml.
The present invention by adopting the above technical scheme, compared with prior art, has the advantages that
When the total zinc measurement of the metal ion disturbance containing single or a variety of higher concentrations in environmental water sample, according to this hair
The bright method: first preparing reagent used in online automatic detection equipment, then that online automatic detection equipment Alignment is complete
The solution of metal ion disturbance containing single or a variety of higher concentrations is tested with online automatic equipment, is passed through by Cheng Hou
High temperature airtight digestion is crossed, mixed masking agent is added after cooling, the pH of color development system is adjusted using buffer solution, adds colour developing
Agent carries out chromogenic reaction, and colorimetric measurement absorbance is finally carried out at wavelength 610nm, is calculated in solution by calibration curve
The content of practical total zinc, and judge influence of the interfering ion to test result.This method using ammonium persulfate as oxidant,
The zinc of different shape in solution and valence state is oxidized to divalent zinc, oxidation efficiency is high, and contrastive colours measurement is free from side effects；Together
Shi Caiyong mixed masking agent can eliminate the dry of other metal different kinds of ions in the case where screening agent is not reacted with zinc ion
It disturbs, is not only free from side effects to final colorimetric measurement, but also reproducible.The entire testing process letter of online automatic detection equipment
List, quick, masking effect is good, accuracy is high, reproducible, and mark-on reclaims are met the requirements.By the online automatic detection of this paper
The method of total zinc is applied to pollution sources or surface water quality online auto monitoring field, and the waste water discharged to blowdown enterprise is real
When detect, have a very big significance, especially for being electroplated, process hides, printing and dyeing, the industries such as metallurgy, even if in the waste water discharged
Containing other interference metal ions of more and high concentration, test result is also had no significant effect.
Detailed description of the invention
Fig. 1 is the canonical plotting between blank and measuring range adjustment solution of the invention.
Specific embodiment
The application is described in further detail with reference to the accompanying drawings and examples.It is understood that this place is retouched
The specific embodiment stated is used only for explaining related invention, rather than the restriction to the invention.It also should be noted that in order to
Convenient for description, part relevant to invention is illustrated only in attached drawing.
It should be noted that in the absence of conflict, the features in the embodiments and the embodiments of the present application can phase
Mutually combination.The application is described in detail below with reference to the accompanying drawings and in conjunction with the embodiments.
The invention discloses a kind of method of the total zinc of online automatic detection of anti-various metals ion interference, specific steps
Are as follows:
S1, zinc standard solution and the preparation containing interfering ion solution and containing interfering ion mark-on solution:
(1) preparation of zinc standard solution:
Accurately pipetting the Zinc standard solution that concentration is 1000 μ g/ml respectively, (national non-ferrous metal and electronic material analysis are surveyed
Examination center, similarly hereinafter) 0.1ml, 0.2ml, 0.5ml, 1.0ml, 2.0ml are placed in 1000ml volumetric flask, are settled to quarter with no zinc water
Degree respectively obtains the zinc standard that concentration is 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L, 2.0mg/L and uses after shaking up
Solution.
(2) preparation containing interfering ion solution:
A, single interfering ion solution:
The Zinc standard solution that 2.0ml concentration is 1000 μ g/ml is accurately pipetted to be placed in 2000ml volumetric flask, it is fixed with no zinc water
Hold the zinc standard solution for obtaining that concentration is 1.0mg/L after shaking up to scale；
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution (national non-ferrous metal and electronic material Institute of Analysis) are placed in 5 different dryings
In 100ml volumetric flask, the zinc standard solution for being 1.0mg/L with concentration is settled to scale, respectively obtained after shaking up containing
5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminum ions five groups of single interfering ions and zinc concentration are
The solution of 1.0mg/L；
The concentration for accurately pipetting 1.0ml respectively is iron standard solution, calcium standard solution, the magnesium standard solution of 1000 μ g/ml
(national non-ferrous metal and electronic material Institute of Analysis) is placed in the 100ml volumetric flask of 3 different dryings, is with concentration
The zinc standard solution of 1.0mg/L is settled to scale, respectively obtains after shaking up containing 10.0mg/L iron ion, calcium ion, magnesium
The three groups of single interfering ions and zinc concentration of ion are the solution of 1.0mg/L；
B, interfering ion solution is mixed:
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution；Accurately pipette 2.0ml concentration be the iron standard solution of 1000 μ g/ml, calcium standard solution,
Magnesium standard solution (national non-ferrous metal and electronic material Institute of Analysis) is placed in the 100ml volumetric flask of the same drying,
The zinc standard solution for being 1.0mg/L with concentration is settled to scale, obtained after shaking up containing 5.0mg/L copper ion, lead ion,
Nickel ion, hexavalent chromium, aluminium ion, 10.0mg/L iron ion, calcium ion, the mixing interfering ion of magnesium ion and zinc concentration are
The solution of 1.0mg/L；
C, mixing interfering ion mark-on solution is prepared:
Accurately pipette respectively 0.5ml concentration be the copper standard solution of 1000 μ g/ml, lead standard solution, nickel standard solution,
Chromium standard solution and aluminum standard solution；Accurately pipette 2.0ml concentration be the iron standard solution of 1000 μ g/ml, calcium standard solution,
Magnesium standard solution (national non-ferrous metal and electronic material Institute of Analysis) is placed in the 100ml volumetric flask of the same drying；
Accurately pipetting 0.10ml concentration again is that 1000 μ g/ml Zinc standard solutions are placed in the drying capacity bottle of above-mentioned 100ml, then with dense
Degree be 1.0mg/L zinc standard solution be settled to scale, obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel from
Son, hexavalent chromium, aluminium ion, 10.0mg/L iron ion, calcium ion, the mixing interfering ion of magnesium ion and zinc concentration are
The solution of the mark-on 1.0mg/L of 1.0mg/L；
The preparation of S2, online automatic detection equipment reagent:
(1) preparation of oxidant:
It prepares the ammonium persulfate solution of 0.025mol/L: taking the clean beaker of a 500ml, about 300ml is added without zinc water,
Then it is soluble in water to accurately weigh 2.8525g ammonium persulfate, after stirring and dissolving is complete, is poured into 500ml volumetric flask, is settled to
Scale shakes up, for use.
(2) preparation of mixed masking agent:
The clean beaker of a 500ml is taken, about 300ml is added without zinc water, then accurately weighs 21.814g thiocarbamide and is dissolved in water
In, after stirring and dissolving is complete, then accurately weighs 1.00g sodium thiosulfate and be dissolved in above-mentioned solution, after stirring and dissolving is complete, then it is quasi-
It really weighs a kind of aminated compounds 12.258g to be dissolved in above-mentioned solution, after stirring and dissolving is complete, be poured into 500ml volumetric flask,
It is settled to scale, is shaken up, for use.
(3) preparation of buffer solution:
With preparing boric acid-potassium chloride-sodium hydroxide buffer solution: pH value is between 8.8~9.0；
(4) preparation of color developing agent:
A, a 500ml clean beaker is taken, 200ml dehydrated alcohol is measured with graduated cylinder and is poured into beaker, accurately weigh
The special color developing agent zincon of 0.52g is into dehydrated alcohol, ultrasonic wave stirring and dissolving；
B, it separately takes a 500ml beaker, is added without zinc water about 150ml, accurately weigh a kind of ammonium class compound 6.50g and be dissolved in
Without in zinc water, stirring and dissolving is complete；
B solution is poured into a solution, is poured into 500ml volumetric flask after mixing, is settled to quarter with no zinc water
Degree, shakes up, for use.
S3, online automatic detection equipment Alignment and accuracy and repeatability verifying:
Use the zinc standard solution that concentration is 2mg/L as online automatic detection equipment measuring range adjustment solution, it is on-line automatic
Equipment is according to process sequence: being first added in 4.4ml blank solution (no zinc water) or measuring range adjustment solution to resolution bottle, adds oxidation
Agent after being bubbled mixing, heats 118~122 DEG C, such as 120 DEG C, cools down after high-temperature closed oxidation resolution 10min, be down to temperature
At 45 DEG C, mixed masking agent 1.1ml is added, after being bubbled mixing, adds 1.1ml buffer solution, is bubbled mixing again, stands
After 1min, the LED light source that wavelength is 610nm is opened, online automatic detection equipment carries out the measurement of background light intensity, measurement 30 at this time
Second, data are automatically recorded, then add 1.1ml color developing agent into resolution bottle, after being bubbled mixing, stand reaction 5min, at this time
Complex reaction occurs for color developing agent and zinc ion, generates blue complex, is again turned on the LED light source that wavelength is 610nm, blue network
Close object has absorption at wavelength 610nm, carries out the measurement for absorbing light intensity again, measures 30 seconds, automatically record data；It is on-line automatic
Detection device can calculate automatically absorbance according to the absorption light intensity of background light intensity and complex compound.
During online automatic detection equipment Alignment, the absorbance of advanced line blank pure water is tested, then is carried out zinc concentration and be
The test of 2mg/L measuring range adjustment solution absorbance is recorded twice absorbance respectively, and standard song can be obtained according to langbobier law
Line (absorbance and standard curve are shown in Table 1 and attached drawing 1 respectively)；
S4, the accuracy of online automatic detection equipment and repeatability verifying: after the completion of online automatic detection equipment Alignment, do not change
Variable element and process sequence are the zinc standard solution of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L using concentration respectively
Tested, every group solution follow-on test six times, detailed test the results are shown in Table 2；
The test of S5, single interfering ion solution:
The zinc solution containing single interfering ion is put to online automatic detection equipment respectively, connects pipeline, is joined
It is consistent when number setting and process sequence are with calibration, it is carried out continuously test, three times, detailed test the results are shown in Table 3 to every group of solution testing；
S6, the test for mixing interfering ion solution:
Zinc solution containing mixing interfering ion is put to online automatic detection equipment, connects pipeline, parameter is set
It is consistent when setting with process sequence with calibration, it is carried out continuously test three times, detailed test the results are shown in Table 4；
S7, the test for mixing interfering ion mark-on solution:
The mark-on solution of zinc solution containing mixing interfering ion is put to online automatic detection equipment, pipe is connected
Consistent when road, parameter setting and process sequence are with calibration, three times, detailed test the results are shown in Table 5 to follow-on test.
S8, after the test in step S5~S7 is qualified, then be passed through ambient water and carry out online automatic detection.
Table 1: total zinc concentration and absorbance relationship
Table 2: the accuracy of online automatic detection equipment and repeatability verifying
Table 3: single interfering ion test result (Guangdong Province's provincial standard error requirements≤± 20%)
Table 4: mixing interfering ion test result
Table 5: mixing interfering ion mark-on test result
Above description is only the preferred embodiment of the application and the explanation to institute's application technology principle.Those skilled in the art
Member is it should be appreciated that invention scope involved in the application, however it is not limited to technology made of the specific combination of above-mentioned technical characteristic
Scheme, while should also cover in the case where not departing from the inventive concept, it is carried out by above-mentioned technical characteristic or its equivalent feature
Any combination and the other technical solutions formed.Such as features described above has similar function with (but being not limited to) disclosed herein
Can technical characteristic replaced mutually and the technical solution that is formed.
Except for the technical features described in the specification, remaining technical characteristic is the known technology of those skilled in the art, is prominent
Innovative characteristics of the invention out, details are not described herein for remaining technical characteristic.
Claims (9)
1. a kind of method of the total zinc of online automatic detection of anti-various metals ion interference, which comprises the following steps:
(1) configuration of solution is tested；
Wherein, the test solution includes zinc standard solution and contains interfering ion solution, described molten containing interfering ion
Liquid includes single interfering ion solution, mixing interfering ion solution, mixing interfering ion mark-on solution；
(2) preparation of online automatic detection equipment reagent；
Wherein, the online automatic detection equipment reagent includes oxidant, mixed masking agent, buffer solution and color developing agent；
(3) calibration of online automatic detection equipment:
Use the zinc standard solution that concentration is 2mg/L as the measuring range adjustment solution of online automatic detection equipment, online certainly
Dynamic detection device is according to process sequence: it is first added in blank solution or measuring range adjustment solution to resolution bottle, adds the oxidant,
Be bubbled mixing after, 115~120 DEG C at a temperature of heat, high-temperature closed oxidation resolution 10min after cool down, be down to temperature
At 42~50 DEG C, mixed masking agent is added into the resolution bottle, after being bubbled mixing, the buffer solution is being added, to again
After secondary bubbling mixing, 1min is stood, then opens the LED light source that wavelength is 610nm, on-line automatic equipment carries out bias light at this time
Strong measurement measures 30 seconds, automatically records data, then adds the color developing agent into resolution bottle, quiet after being bubbled mixing
Reaction 5min is set, complex reaction occurs for color developing agent and zinc ion at this time, generates blue complex, and being again turned on wavelength is 610nm
LED light source, blue complex has absorption at wavelength 610nm, carries out the measurement for absorbing light intensity again, measures 30 seconds, automatically
Record data；Online automatic detection equipment can calculate automatically absorbance according to the absorption light intensity of background light intensity and complex compound；
During online automatic detection equipment Alignment, the absorbance of advanced line blank pure water is tested, then carrying out zinc concentration is 2mg/L
The test of measuring range adjustment solution absorbance, online automatic detection equipment can successively be recorded twice absorbance respectively, according to lambert Bill
Standard curve can be obtained in law, and standard curve is stored in the control system of online detection instrument；
(4) accuracy of online automatic detection equipment and repeatability verifying；
The accuracy of online automatic detection equipment and repeatability verifying: it after the completion of online automatic detection equipment Alignment, is flowed according to calibration
The parameter and sequence of journey are tested, and are respectively the zinc of 0.1mg/L, 0.2mg/L, 0.5mg/L, 1.0mg/L using concentration
Standard solution is tested, every group solution follow-on test six times, according to the registration of test result and standard curve, judge
The accuracy and repeatability of line automatic checkout equipment；
(5) containing total Zn content in interfering ion solution described in testing in online automatic detection equipment, verifying contains interference
The accuracy of total Zn content test in solion；
(6) the online automatic detection equipment is passed through environmental water sample, total zinc in environmental water sample is measured.
2. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In the configuration method of total zinc standard solution are as follows:
Zinc standard solution 0.1ml, 0.2ml, 0.5ml, 1.0ml, 2.0ml that concentration is 1000 μ g/ml is accurately pipetted respectively to be placed in
In 1000ml volumetric flask, be settled to scale with no zinc water, respectively obtained after shaking up concentration be 0.1mg/L, 0.2mg/L,
The zinc standard of 0.5mg/L, 1.0mg/L, 2.0mg/L use solution.
3. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In the configuration method of the single interfering ion solution are as follows:
It accurately pipettes the Zinc standard solution that 2.0ml concentration is 1000 μ g/ml to be placed in 2000ml volumetric flask, be settled to no zinc water
Scale obtains the zinc standard solution that concentration is 1.0mg/L after shaking up；
The concentration for accurately pipetting 0.5ml respectively is copper standard solution, lead standard solution, nickel standard solution, the chromium mark of 1000 μ g/ml
Quasi- solution and aluminum standard solution are placed in the 100ml volumetric flask of 5 different dryings, and the zinc standard for being 1.0mg/L with concentration makes
It is settled to scale with liquid, is respectively obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminium
The five groups of single interfering ions and zinc concentration of ion are the solution of 1mg/L；
Iron standard solution, calcium standard solution, the magnesium standard solution that the concentration for accurately pipetting 1.0ml respectively is 1000 μ g/ml are placed in 3
In the 100ml volumetric flask of a different drying, the zinc standard solution for being 1.0mg/L with concentration is settled to scale, after shaking up i.e.
Respectively obtaining containing 10.0mg/L iron ion, calcium ion, three groups of single interfering ions of magnesium ion and zinc concentration is the molten of 1mg/L
Liquid.
4. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In the configuration method of the mixing interfering ion solution are as follows:
The concentration for accurately pipetting 0.5ml respectively is copper standard solution, lead standard solution, nickel standard solution, the chromium mark of 1000 μ g/ml
Quasi- solution and aluminum standard solution；The concentration for accurately pipetting 2.0ml is iron standard solution, calcium standard solution, the magnesium mark of 1000 μ g/ml
Quasi- solution is placed in the 100ml volumetric flask of the same drying, and the zinc standard solution for being 1.0mg/L with concentration is settled to scale,
It is obtained after shaking up containing 5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminium ion, 10.0mg/L iron ion,
The solution that calcium ion, the mixing interfering ion of magnesium ion and zinc concentration are 1mg/L.
5. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In the mixing interfering ion mark-on solution preparation method are as follows:
The concentration for accurately pipetting 0.5ml respectively is copper standard solution, lead standard solution, nickel standard solution, the chromium mark of 1000 μ g/ml
Quasi- solution and aluminum standard solution；The concentration for accurately pipetting 2.0ml is iron standard solution, calcium standard solution, the magnesium mark of 1000 μ g/ml
Quasi- solution is placed in the 100ml volumetric flask of the same drying；Accurately pipetting 0.10ml concentration again is 1000 μ g/ml Zinc standard solutions
It is placed in the drying capacity bottle of above-mentioned 100ml, the zinc standard solution for being then 1.0mg/L with concentration is settled to scale, shakes up
Afterwards i.e. obtain containing 5.0mg/L copper ion, lead ion, nickel ion, hexavalent chromium, aluminium ion, 10.0mg/L iron ion, calcium from
The solution for the mark-on 1.0mg/L that son, the mixing interfering ion of magnesium ion and zinc concentration are 1mg/L.
6. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In the preparation method of the oxidant is to prepare 0.025mol/L ammonium persulfate solution: taking the clean beaker of a 500ml, add
Enter 300ml without zinc water, it is soluble in water then to accurately weigh 2.8525g ammonium persulfate, after stirring and dissolving is complete, is poured into 500ml
In volumetric flask, it is settled to scale, is shaken up, for use；
The preparation method of the mixed masking agent are as follows: separately take the clean beaker of a 500ml, addition 300ml is then quasi- without zinc water
It is soluble in water really to weigh 21.814g thiocarbamide, after stirring and dissolving is complete, then accurate addition 1.00g sodium thiosulfate, stirring and dissolving are complete
Quan Hou, then accurate addition aminated compounds 12.258g, after stirring and dissolving is complete, are poured into 500ml volumetric flask, are settled to quarter
Degree, shakes up, for use；
The preparation method of the buffer solution is to match preparing boric acid-potassium chloride-sodium hydroxide buffer solution: pH value is 8.8~9.0
Between；
The preparation method of the color developing agent are as follows:
A, a 500ml clean beaker separately is taken, measures 200ml dehydrated alcohol with graduated cylinder and be poured into beaker, accurately weighs 0.52g
Special color developing agent zincon is into dehydrated alcohol, using ultrasonic wave stirring and dissolving；
B, it separately takes a 500ml clean beaker, is added without zinc water 150ml, accurately weigh a kind of ammonium class compound 6.50g and be dissolved in
Without in zinc water, stirring and dissolving is complete；
The step b solution prepared is poured into the solution of step a preparation, is poured into 500ml volumetric flask after mixing, used
No zinc water is settled to scale, shakes up, for use.
7. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In when calibrating the online automatic detection equipment, the blank solution used is no zinc water.
8. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 1, feature exist
In, be added single interfering ion or mixing interfering ion when detecting, solution to be measured and each reagent additional proportion are as follows: to be measured
Solution 4.3~4.5ml of additional amount, oxidant additional amount: 1.0~1.2ml, 118~122 DEG C of pyroreaction, 10min, mixing is covered
Agent additional amount: 1.0~1.2ml is covered, buffer solution additional amount: 1.0~1.2ml, color developing agent additional amount: 1.0~1.2ml.
9. the method for the total zinc of online automatic detection of anti-various metals ion interference according to claim 8, feature exist
In, be added single interfering ion or mixing interfering ion when detecting, solution to be measured and each reagent additional proportion are as follows: to be measured
Solution additional amount 4.4ml, oxidant additional amount: 1.1ml, 120 DEG C of pyroreaction, 10min, mixed masking agent additional amount:
1.1ml, buffer solution additional amount: 1.1ml, color developing agent additional amount: 1.1ml.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111208076A (en) * | 2020-01-19 | 2020-05-29 | 安徽英凯环境技术有限公司 | Detection method for on-line determination of total chromium in water |
| WO2024046369A1 (en) * | 2022-08-31 | 2024-03-07 | 上海博取仪器有限公司 | Anti-interference water quality analysis instrument test method |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107843585A (en) * | 2017-11-22 | 2018-03-27 | 安徽皖仪科技股份有限公司 | The novel detection method of total chrome content in a kind of environmental water sample of anti-various metals ion interference |
-
2019
- 2019-06-28 CN CN201910582766.8A patent/CN110346355A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107843585A (en) * | 2017-11-22 | 2018-03-27 | 安徽皖仪科技股份有限公司 | The novel detection method of total chrome content in a kind of environmental water sample of anti-various metals ion interference |
Non-Patent Citations (3)
| Title |
|---|
| 孙延一: "《仪器分析》", 28 February 2012, 华中科技大学出版社 * |
| 李友君等: "锌试剂分光光度法测定发锌", 《中华预防医学杂志》 * |
| 陈斌: "《第十二次环境监测学术交流会论文集》", 31 July 2015, 中国环境出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111208076A (en) * | 2020-01-19 | 2020-05-29 | 安徽英凯环境技术有限公司 | Detection method for on-line determination of total chromium in water |
| WO2024046369A1 (en) * | 2022-08-31 | 2024-03-07 | 上海博取仪器有限公司 | Anti-interference water quality analysis instrument test method |
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Application publication date: 20191018 |