CN107843585A - The novel detection method of total chrome content in a kind of environmental water sample of anti-various metals ion interference - Google Patents
The novel detection method of total chrome content in a kind of environmental water sample of anti-various metals ion interference Download PDFInfo
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Abstract
The invention discloses a kind of novel detection method of total chrome content in environmental water sample of anti-various metals ion interference, agent prescription is simple, and each reagent dosage can suitably be adjusted according to actual use situation, method is stable, linear and reappearance is preferable, recovery of standard addition meets to require, and is influenceed by other single or a variety of hybrid metal ions smaller.This method is applied in monitoring water quality on line field, there is high practical value, method is simple, workable, and the species of anti-metal ion interference is more, suitable for the demand of monitoring water quality on line industry.
Description
Technical field
The invention belongs to total chromium in analytical chemistry field, more particularly to a kind of environmental water sample of anti-various metals ion interference to contain
The novel detection method of amount.
Background technology
The Method And Principle of total chromium detection is：In acidic dissolution medium, under certain temperature and pressure, in environmental water sample
The chromium of different valence state and form is by persulfate or potassium permanganate oxidation into Cr VI, hexavalent chromium and diphenylsemicarbazide
(DPC) reaction generation aubergine complex, carries out spectrophotometry at wavelength 525nm, dense according to absorbance and Cr VI
Relation fit standard curve between degree, while obtain calculation formula.In test environment water sample during total chrome content, by a system
After row reaction, absorbance is then measured, you can obtain the content of total chromium in environmental water sample.
It is that national standard method (requires that ion interference is less than in national standard currently with diphenylsemicarbazide detection Cr VI
± 15%), can be run into measure in environmental water sample containing in addition to chromium ion other metal ions (such as iron ion, copper ion,
The metal ions such as calcium ion, magnesium ion, zinc ion, lead ion), and part metals ion can also develop the color with diphenylsemicarbazide
Reaction, causes measurement result not to be consistent with the total chrome actually contained in environmental water sample.In most of document all using
The screening agent as interference metal ion such as EDTA, sodium potassium tartrate tetrahydrate, citrate, but this several reagent is only to single or few
Measure several interference metal ions and play masking action, and can also be chemically reacted simultaneously with Cr VI, cause chromogenic reaction not
Sensitive, test result is larger with actual deviation, and the repeatability of measurement is also poor.
The content of the invention
The invention provides a kind of novel detection method of total chrome content in environmental water sample of anti-various metals ion interference,
The interference effect of a variety of common metal ions during water sample detection is aimed to solve the problem that, while the degree of accuracy detected is higher, favorable reproducibility.
To achieve the above object, the technical solution adopted by the present invention is as follows：
The novel detection method of total chrome content in a kind of environmental water sample of anti-various metals ion interference, including following step
Suddenly：
(1) preparation of ρ=100mg/L Cr VIs standard reserving solution：
Potassium bichromate standard reagents of the 0.2829 ± 0.0001g through 120 DEG C of dry 2h accurately is weighed into clean beaker, is added
Enter ultra-pure water to stir to being completely dissolved, be then transferred in 1000ml volumetric flask, clean beaker three times with pure water, cleaning fluid
Pour into above-mentioned volumetric flask, then plus water is settled to scale, shakes up stand-by；
(2) preparation of sexavalence chromium standard solution：
Accurately pipette respectively concentration be 100mg/L Cr VI standard reserving solution 0.2ml, 0.5ml, 1.0ml, 2.0ml,
5.0ml is placed in 1000ml volumetric flasks, and scale is settled to ultra-pure water, and after shaking up up and down, that is, it is 0.02mg/ to respectively obtain concentration
L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L sexavalence chromium standard solution；
(3) preparation of environmental water sample to be measured：
The water sample containing suspension fetched is stood overnight, takes supernatant to measure；
(4) preparation of environmental water sample mark-on solution to be measured：
The accurate concentration that pipettes is added into 1000ml volumetric flask for 100mg/L Cr VI standard reserving solution 1.0ml, so
Constant volume is diluted with the environmental water sample supernatant after standing overnight afterwards, after shaking up up and down, obtains environmental water sample mark-on 0.1mg/L
The mark-on solution of Cr VI；
(5) preparation containing interfering ion environmental water sample：
A, single ionic interference water sample：
A, iron standard liquid, copper standard liquid, the standard calcium that the concentration for accurately pipetting 0.5ml respectively is 1000mg/L are molten
Liquid, magnesium standard solution, aluminum standard solution and Zinc standard solution are into five different 100ml volumetric flask, after standing overnight
Environmental water sample supernatant be settled to scale, after shaking up up and down, that is, respectively obtain respectively containing 5mg/L iron ions, 5mg/L copper from
Five groups of single interfering ion environmental water samples of son, 5mg/L calcium ions, 5mg/L magnesium ions, 5mg/L aluminium ions and 5mg/L zinc ions
Solution；
B, the concentration for accurately pipetting 0.2ml respectively is 1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid
In the volumetric flask of vanadium standard liquid to four different 100ml, quarter is settled to the environmental water sample supernatant after standing overnight
Degree, after shaking up up and down, that is, respectively obtain respectively containing 2mg/L lead ions, 2mg/L nickel ions, 2mg/L manganese ions and 2mg/L vanadium from
Four groups of single interfering ion environmental water sample solution of son；
C, accurately pipette respectively 50.0 μ L concentration be 1000mg/L mercury standard solution, cadmium standard liquid to two it is different
In 100ml volumetric flask, scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, is respectively obtained
Two groups of single interfering ion environmental water sample solution respectively containing 0.5mg/L mercury ions and 0.5mg/L cadmium ions；
B, hybrid ionic interference water sample：
Iron standard liquid, copper standard liquid, calcium standard solution, the magnesium that 0.5ml concentration is 1000mg/L are accurately pipetted respectively
Standard liquid, aluminum standard solution and Zinc standard solution are into same 100ml volumetric flask；Pipetting 0.2ml concentration respectively again is
1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid and vanadium standard liquid is into above-mentioned 100ml volumetric flasks；Again
It is 1000mg/L mercury standard solution, cadmium standard liquid into above-mentioned volumetric flask to pipette 50.0 μ L concentration respectively；
Then scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, obtained containing 5mg/L
Iron ion, copper ion, calcium ion, magnesium ion, aluminium ion and zinc ion, 2mg/L lead ion, nickel ion, manganese ion, vanadium from
Son, 0.5mg/L mercury ion, the hybrid ionic interference water sample of cadmium ion interference.
(6) preparation of oxidant：
500ml clean beaker is taken, about 300ml ultra-pure waters is added, it is molten then accurately to weigh 17.85g sodium peroxydisulfates
Yu Shuizhong, after stirring and dissolving is complete, it is poured into 500ml volumetric flask, is settled to scale, shake up, it is stand-by；
(7) preparation of dilution heat of sulfuric acid：
500ml clean beaker is taken, adds about 300ml ultra-pure waters, the 70ml concentrated sulfuric acid, side stirring are pipetted with graduated cylinder
While being slowly added into water, after stirring, it is poured into 500ml volumetric flask, is settled to scale, shake up, it is stand-by；
(8) preparation of developer：
A, accurately 9.5g hydroxylamine hydrochlorides are weighed to be dissolved in about 100ml pure water；
B, accurately 2.45g diphenylsemicarbazides are weighed to be dissolved in 250ml ethanol；
Then above-mentioned a and b solution is mixed, be poured into after stirring in 500ml volumetric flasks, and burning is cleaned with pure water
Cup, cleaning fluid are poured into volumetric flask, are finally settled to scale with pure water, shake up, you can obtain developer；
(9) concentration for taking step (2) to prepare respectively is 0.02mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L
Sexavalence chromium standard solution into sealed digestion bottle, then add oxidant carry out high-temperature oxydation, be cooled to 43~46 DEG C again after
Dilution heat of sulfuric acid regulation acidity is added, adds developer, 3~5min of reaction is stood after being well mixed, is entered at wavelength 525nm
Row colorimetric measurement, the relation fit standard curve according to absorbance and concentration；
(10) the various valence states in environmental water sample to be measured and the chromium of form mix with oxidant, the oxygen in high-temperature closed environment
Change resolution into Cr VI；43~46 DEG C are cooled to after the completion of oxidation resolution, dilution heat of sulfuric acid regulation acidity is added, adds colour developing
Agent, 3~5min is stood after being well mixed, colorimetric measurement is carried out at wavelength 525nm, is calculated according to standard curve and formula
The content of total chromium in environmental water sample；
(11) the various valence states in environmental water sample mark-on solution to be measured and the chromium of form mix with oxidant, in high-temperature closed
Oxidation is cleared up into Cr VI in environment；43~46 DEG C are cooled to after the completion of oxidation resolution, adds dilution heat of sulfuric acid regulation acidity, then
Add developer, be well mixed after stand reaction 3~5min, in wavelength 525nm at carry out colorimetric measurement, according to standard curve with
The content of total chromium in environmental water sample is calculated in formula；
(12) containing single interfering ion or various valence states in mixing interfering ion environmental water sample and the chromium of form with
Oxidant is mixed, and resolution is aoxidized in high-temperature closed environment into Cr VI；43~46 DEG C are cooled to after the completion of oxidation resolution, is added
Dilution heat of sulfuric acid adjusts acidity, adds developer, and 3~5min of reaction is stood after being well mixed, is compared at wavelength 525nm
Color measures, and the content of total chromium in environmental water sample is calculated according to standard curve and formula, and judge interfering ion to total chromium
The influence of measurement.
Wherein, the environmental water sample detection to be measured and environmental water sample mark-on solution to be measured detect and added various single dry
When disturbing ion or mixing the environmental water sample detection of interfering ion, water sample and each reagent additional proportion are as follows：Water sample addition：3.2
~3.4ml；Oxidant addition：1.0~1.2ml；Pyroreaction：118~122 DEG C, 9~12min；Dilution heat of sulfuric acid adds
Amount：1.0~1.2ml；Developer addition：1.0~1.2ml.
Wherein, the environmental water sample detection to be measured and environmental water sample mark-on solution to be measured detect and added various single dry
When disturbing ion or mixing the environmental water sample detection of interfering ion, water sample and each reagent additional proportion are as follows：Water sample addition：
3.3ml；Oxidant addition：1.1ml；Pyroreaction：120 DEG C, 10min；Dilution heat of sulfuric acid addition：1.1ml；Developer adds
Enter amount：1.1ml.
Beneficial effects of the present invention：
When the total chromium mark feed of content various metals ion interference in environmental water sample, match somebody with somebody first according to the method described in the present invention
Corresponding reagent is made, then the environmental water sample containing metal ion disturbance is cleared up by high-temperature closed, cooled after the completion of resolution,
Dilute sulfuric acid regulation solution acidity is added, adds developer, reaction is stood after being well mixed, colorimetric is carried out at wavelength 525nm
Measurement, establishing criteria curve and formula calculate the content of total chromium in the environmental water sample containing metal ion disturbance, and judge environment
Whether the interference metal ion contained in water sample has an impact to detection.This method uses sodium peroxydisulfate as oxidant, by environment
The chromium of various valence states and form in water sample is oxidized to Cr VI, and oxidation efficiency is high, and contrastive colours measure no color interference,
Color speed and efficiency are not only increased as screening agent using the hydroxylamine hydrochloride with reducing property simultaneously, while to a variety of
Common metal ion serves masking effect, and the degree of accuracy detected is higher, favorable reproducibility.Whole course of reaction is simple, quick,
The degree of accuracy, repeatability and recovery of standard addition meet to require.This method is applied to water quality online detection instrument field, blowdown is looked forward to
The wastewater recycle that industry is discharged makes great sense, be particularly used to electroplating, process hides, printing and dyeing and chromic salts industry etc., for enterprise
Other metal ion disturbances containing higher concentration influence without obvious in the waste water that industry is discharged.
Brief description of the drawings
The graph of relation of Fig. 1 absorbances and concentration.
Embodiment
The present invention can be explained in more detail by the following examples：
1st, the preparation of standard liquid and environmental water sample and environmental water sample mark-on solution：
(1) preparation of sexavalence chromium standard solution：
Accurately pipette respectively concentration be 100mg/L Cr VI standard reserving solution 0.2ml, 0.5ml, 1.0ml, 2.0ml,
5.0ml is placed in 1000ml volumetric flasks, and scale is settled to ultra-pure water, and after shaking up up and down, that is, it is 0.02mg/ to respectively obtain concentration
L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L sexavalence chromium standard solution.
(2) preparation of environmental water sample to be measured：
The water sample containing suspension fetched is stood overnight, takes supernatant to measure.
(3) preparation of environmental water sample mark-on solution to be measured：
The accurate concentration that pipettes is added into 1000ml volumetric flask for 100mg/L Cr VI standard reserving solution liquid 1.0ml,
Then constant volume is diluted with the environmental water sample supernatant after standing overnight, after shaking up up and down, obtains environmental water sample mark-on
The mark-on solution of 0.1mg/L Cr VIs.
(4) preparation containing interfering ion environmental water sample：
A, single interfering ion environmental water sample：
A, iron standard liquid, copper standard liquid, the standard calcium that the concentration for accurately pipetting 0.5ml respectively is 1000mg/L are molten
Liquid, magnesium standard solution, aluminum standard solution and Zinc standard solution are into five different 100ml volumetric flask, after standing overnight
Environmental water sample supernatant be settled to scale, after shaking up up and down, that is, respectively obtain respectively containing 5mg/L iron ions, 5mg/L copper from
Five groups of single interfering ion environmental water samples of son, 5mg/L calcium ions, 5mg/L magnesium ions, 5mg/L aluminium ions and 5mg/L zinc ions
Solution.
B, the concentration for accurately pipetting 0.2ml respectively is 1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid
In the volumetric flask of vanadium standard liquid to four different 100ml, quarter is settled to the environmental water sample supernatant after standing overnight
Degree, after shaking up up and down, that is, respectively obtain respectively containing 2mg/L lead ions, 2mg/L nickel ions, 2mg/L manganese ions and 2mg/L vanadium from
Four groups of single interfering ion environmental water sample solution of son.
C, accurately pipette respectively 50.0 μ L concentration be 1000mg/L mercury standard solution, cadmium standard liquid to two it is different
In 100ml volumetric flask, scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, is respectively obtained
Two groups of single interfering ion environmental water sample solution respectively containing 0.5mg/L mercury ions and 0.5mg/L cadmium ions.
B, hybrid ionic interference water sample：
Iron standard liquid, copper standard liquid, calcium standard solution, the magnesium that 0.5ml concentration is 1000mg/L are accurately pipetted respectively
Standard liquid, aluminum standard solution and Zinc standard solution are into same 100ml volumetric flask；Pipetting 0.2ml concentration respectively again is
1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid and vanadium standard liquid is into above-mentioned 100ml volumetric flasks；Again
It is 1000mg/L mercury standard solution, cadmium standard liquid into above-mentioned volumetric flask to pipette 50.0 μ L concentration respectively；
Then scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, obtained containing 5mg/L
Iron ion, copper ion, calcium ion, magnesium ion, aluminium ion and zinc ion, 2mg/L lead ion, nickel ion, manganese ion, vanadium from
Son, 0.5mg/L mercury ion, the hybrid ionic interference water sample of cadmium ion interference.
2nd, the preparation of reagent：
(1) preparation of oxidant：
The clean beaker of a 500ml is taken, about 300ml ultra-pure waters is added, then accurately weighs 17.85g sodium peroxydisulfates and be dissolved in
In water, after stirring and dissolving is complete, it is poured into 500ml volumetric flask, is settled to scale, shake up, it is stand-by.
(2) preparation of dilution heat of sulfuric acid：
The clean beaker of a 500ml is taken, adds about 300ml ultra-pure waters, the 70.0ml concentrated sulfuric acid, side stirring are pipetted with graduated cylinder
While being slowly added into water, after stirring, it is poured into 500ml volumetric flask, is settled to scale, shake up, it is stand-by.
(3) preparation of developer：
A, accurately 9.5g hydroxylamine hydrochlorides are weighed to be dissolved in about 100ml pure water；
B, accurately 2.45g diphenylsemicarbazides are weighed to be dissolved in 250ml ethanol；
Then above-mentioned a and b solution is mixed, be poured into after stirring in 500ml volumetric flasks, and burning is cleaned with pure water
Cup, cleaning fluid are poured into volumetric flask, are finally settled to scale with pure water, shake up, you can obtain developer.
3rd, the drafting of standard curve：
The sexavalence chromium standard solution that concentration is 0.02mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L is taken respectively
3.3ml, 1.1ml oxidant is added, be heated to 120 DEG C, confined reaction 10min, be then cooled to 45 DEG C；Add dilute sulfuric acid
1.1ml, after being well mixed, developer 1.1ml is added, stand 5min after remixing uniformly, then the colorimetric at wavelength 525nm
Measurement, the absorbance corresponding to various concentrations is obtained, standard curve, such as table is calculated in the relation according to concentration and absorbance
1 and Fig. 1.
4th, the measurement of environmental water sample solution：
Environmental water sample solution 3.3ml is taken, adds 1.1ml oxidant, is heated to 120 DEG C, confined reaction 10min, then
It is cooled to 45 DEG C；Dilute sulfuric acid 1.1ml is added, after being well mixed, adds developer 1.1ml, 5min is stood after remixing uniformly,
Then the colorimetric measurement at wavelength 525nm, obtains absorbance, and total chromium of establishing criteria curve and formula computing environment water sample contains
Amount, testing result are shown in Table 2.
5th, the measurement of environmental water sample mark-on solution：
Environmental water sample mark-on solution 3.3ml is taken, 1.1ml oxidant is added, is heated to 120 DEG C, confined reaction 10min,
Then 45 DEG C are cooled to；Dilute sulfuric acid 1.1ml is added, after being well mixed, adds developer 1.1ml, is stood after remixing uniformly
5min, the then colorimetric measurement at wavelength 525nm obtain absorbance, establishing criteria curve and formula computing environment water sample it is total
Chromium content, and recovery of standard addition is calculated, testing result is shown in Table 2.
6th, the measurement of environmental water sample repeatability：
Environmental water sample solution 3.3ml is taken, adds 1.1ml oxidant, is heated to 120 DEG C, confined reaction 10min, then
It is cooled to 45 DEG C；Dilute sulfuric acid 1.1ml is added, after being well mixed, adds developer 1.1ml, 5min is stood after remixing uniformly,
Then the colorimetric measurement at wavelength 525nm, obtains absorbance, and total chromium of establishing criteria curve and formula computing environment water sample contains
Amount, and repeatability is calculated, testing result is shown in Table 3.
7th, the measurement of single interfering ion environmental water sample：
The environmental water sample solution 3.3ml containing the interference of 5mg/L iron is taken, adds 1.1ml oxidant, is heated to 120 DEG C, it is close
Reaction 10min is closed, is then cooled to 45 DEG C；Dilute sulfuric acid 1.1ml is added, after being well mixed, adds developer 1.1ml, then mix
5min is stood after closing uniformly, then the colorimetric measurement at wavelength 525nm, obtain absorbance, establishing criteria curve and formula calculate
The total chrome content of environmental water sample, and judge the influence of interfering ion；Other copper, calcium, magnesium, aluminium, zinc, lead, nickel, manganese, vanadium, mercury and cadmium
The environmental water sample of interference is similarly detected according to the method described above, and the total chrome content in computing environment water sample and judgement are disturbed
The influence of ion, testing result are shown in Table 4.
8th, the measurement of interfering ion environmental water sample is mixed：
The environmental water sample solution 3.3ml containing hybrid ionic interference is taken, 1.1ml oxidant is added, is heated to 120 DEG C,
Confined reaction 10min, then it is cooled to 45 DEG C；Dilute sulfuric acid 1.1ml is added, after bubbling is well mixed, adds developer
1.1ml, 5min is stood after remixing uniformly, then the colorimetric measurement at wavelength 525nm, obtains absorbance, establishing criteria curve
With the total chrome content of formula computing environment water sample, and judge to mix the influence of interfering ion, testing result is shown in Table 5.
The hexavalent chromium concentration of table 1 and absorbance relation
The environmental water sample of table 2 and environmental water sample mark-on solution testing table
The environmental water sample reperformance test table of table 3
The single interfering ion environmental water sample test table of table 4
Note：In environmental water sample provide total chrome content be 0.140mg/L calculate ion interference influence (requirements of the national standard from
The index request of son interference is less than ± 15%).
Table 5 mixes interfering ion environmental water sample test table
Note：It is the influence that 0.140mg/L calculates ion interference that total chrome content is provided in environmental water sample.
Claims (3)
- A kind of 1. novel detection method of total chrome content in environmental water sample of anti-various metals ion interference, it is characterised in that bag Include following steps：（1）The preparation of ρ=100mg/L Cr VI standard reserving solutions：Potassium bichromate standard reagents of the 0.2829 ± 0.0001g through 120 DEG C of dry 2h accurately is weighed into clean beaker, is added super Pure water is stirred to being completely dissolved, and is then transferred in 1000ml volumetric flask, cleans beaker three times with pure water, cleaning fluid also pours into In above-mentioned volumetric flask, then plus water is settled to scale, shakes up stand-by；（2）The preparation of sexavalence chromium standard solution：Cr VI standard reserving solution 0.2ml, 0.5ml, 1.0ml, 2.0ml, 5.0ml that concentration is 100mg/L are accurately pipetted respectively Be placed in 1000ml volumetric flasks, scale be settled to ultra-pure water, after shaking up up and down, that is, respectively obtain concentration for 0.02mg/L, 0.05mg/L, 0.1mg/L, 0.2mg/L, 0.5mg/L sexavalence chromium standard solution；（3）The preparation of environmental water sample to be measured：The water sample containing suspension fetched is stood overnight, takes supernatant to measure；（4）The preparation of environmental water sample mark-on solution to be measured：The accurate concentration that pipettes is added into 1000ml volumetric flask for 100mg/L Cr VI standard reserving solution 1.0ml, Ran Houyong Environmental water sample supernatant after standing overnight is diluted constant volume, after shaking up up and down, obtains environmental water sample mark-on 0.1mg/L sexavalences The mark-on solution of chromium；（5）Preparation containing interfering ion environmental water sample：A, single ionic interference water sample：A, the concentration for accurately pipetting 0.5ml respectively is 1000mg/L iron standard liquid, copper standard liquid, calcium standard solution, magnesium Standard liquid, aluminum standard solution and Zinc standard solution are into five different 100ml volumetric flask, with the environment after standing overnight Water sample supernatant is settled to scale, after shaking up up and down, that is, respectively obtains respectively containing 5mg/L iron ions, 5mg/L copper ions, 5mg/L Calcium ion, 5mg/L magnesium ions, five groups of single interfering ion environmental water sample solution of 5mg/L aluminium ions and 5mg/L zinc ions；B, the concentration for accurately pipetting 0.2ml respectively is 1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid and vanadium Standard liquid is settled to scale into four different 100ml volumetric flask, with the environmental water sample supernatant after standing overnight, on Under shake up after, that is, respectively obtain four respectively containing 2mg/L lead ions, 2mg/L nickel ions, 2mg/L manganese ions and 2mg/L vanadium ions The single interfering ion environmental water sample solution of group；C, accurately pipette respectively 50.0 μ L concentration be 1000mg/L mercury standard solution, cadmium standard liquid to two it is different In 100ml volumetric flask, scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, is respectively obtained Two groups of single interfering ion environmental water sample solution respectively containing 0.5mg/L mercury ions and 0.5mg/L cadmium ions；B, hybrid ionic interference water sample：The iron standard liquid, copper standard liquid, calcium standard solution, magnesium standard that 0.5ml concentration is 1000mg/L are accurately pipetted respectively Solution, aluminum standard solution and Zinc standard solution are into same 100ml volumetric flask；Pipetting 0.2ml concentration respectively again is 1000mg/L lead standard liquid, nickel standard liquid, manganese standard liquid and vanadium standard liquid is into above-mentioned 100ml volumetric flasks；Again It is 1000mg/L mercury standard solution, cadmium standard liquid into above-mentioned volumetric flask to pipette 50.0 μ L concentration respectively；Then scale is settled to the environmental water sample supernatant after standing overnight, after shaking up up and down, that is, obtains the iron containing 5mg/L Ion, copper ion, calcium ion, magnesium ion, aluminium ion and zinc ion, 2mg/L lead ion, nickel ion, manganese ion, vanadium ion, 0.5mg/L mercury ion, the hybrid ionic interference water sample of cadmium ion interference；（6）The preparation of oxidant：500ml clean beaker is taken, about 300ml ultra-pure waters is added, then accurately weighs 17.85g sodium peroxydisulfates and be dissolved in water In, after stirring and dissolving is complete, it is poured into 500ml volumetric flask, is settled to scale, shakes up, it is stand-by；（7）The preparation of dilution heat of sulfuric acid：500ml clean beaker is taken, about 300ml ultra-pure waters is added, the 70ml concentrated sulfuric acid is pipetted with graduated cylinder, is delayed while stirring Slowly add into water, after stirring, be poured into 500ml volumetric flask, be settled to scale, shake up, it is stand-by；（8）The preparation of developer：A, accurately 9.5g hydroxylamine hydrochlorides are weighed to be dissolved in about 100ml pure water；B, accurately 2.45g diphenylsemicarbazides are weighed to be dissolved in 250ml ethanol；Then above-mentioned a and b solution is mixed, be poured into after stirring in 500ml volumetric flasks, and beaker is cleaned with pure water, clearly Washing lotion is poured into volumetric flask, is finally settled to scale with pure water, is shaken up, you can obtains developer；（9）Step is taken respectively（2）The concentration of preparation is 0.02 mg/L, 0.05 mg/L, 0.1 mg/L, 0.2 mg/L, 0.5 mg/ L sexavalence chromium standard solution into sealed digestion bottle, then add oxidant carry out high-temperature oxydation, be cooled to 43 ~ 46 DEG C again after Dilution heat of sulfuric acid regulation acidity is added, adds developer, 3 ~ 5min of reaction is stood after being well mixed, is entered at wavelength 525nm Row colorimetric measurement, the relation fit standard curve according to absorbance and concentration；（10）The chromium of various valence states and form in environmental water sample to be measured mixes with oxidant, aoxidizes and disappears in high-temperature closed environment Solution is into Cr VI；43 ~ 46 DEG C are cooled to after the completion of oxidation resolution, dilution heat of sulfuric acid regulation acidity is added, adds developer, mix 3 ~ 5min is stood after closing uniformly, colorimetric measurement is carried out at wavelength 525nm, ambient water is calculated according to standard curve and formula The content of total chromium in sample；（11）The chromium of various valence states and form in environmental water sample mark-on solution to be measured mixes with oxidant, in high-temperature closed environment Middle oxidation is cleared up into Cr VI；43 ~ 46 DEG C are cooled to after the completion of oxidation resolution, dilution heat of sulfuric acid regulation acidity is added, adds Developer, 3 ~ 5min of reaction is stood after being well mixed, colorimetric measurement is carried out at wavelength 525nm, according to standard curve and formula The content of total chromium in environmental water sample is calculated；（12）Contain the various valence states in single interfering ion or mixing interfering ion environmental water sample and chromium and the oxidation of form Agent is mixed, and resolution is aoxidized in high-temperature closed environment into Cr VI；43 ~ 46 DEG C are cooled to after the completion of oxidation resolution, adds dilute sulphur Acid solution adjusts acidity, adds developer, and 3 ~ 5min of reaction is stood after being well mixed, colorimetric survey is carried out at wavelength 525nm Amount, the content of total chromium in environmental water sample is calculated according to standard curve and formula, and judge interfering ion to total chromium measurement Influence.
- 2. the new inspection of total chrome content in a kind of environmental water sample of anti-various metals ion interference according to claims 1 Survey method, it is characterised in that environmental water sample detection to be measured and environmental water sample mark-on solution to be measured are detected and added various single During the environmental water sample detection of interfering ion or mixing interfering ion, water sample and each reagent additional proportion are as follows：Water sample addition： 3.2~3.4ml；Oxidant addition：1.0~1.2ml；Pyroreaction：118 ~ 122 DEG C, 9 ~ 12min；Dilution heat of sulfuric acid addition： 1.0~1.2ml；Developer addition：1.0~1.2ml.
- 3. the new inspection of total chrome content in a kind of environmental water sample of anti-various metals ion interference according to claims 2 Survey method, it is characterised in that the environmental water sample detection to be measured and environmental water sample mark-on solution to be measured are detected and added various During the environmental water sample detection of single interfering ion or mixing interfering ion, water sample and each reagent additional proportion are as follows：Water sample adds Amount：3.3ml；Oxidant addition：1.1ml；Pyroreaction：120 DEG C, 10min；Dilution heat of sulfuric acid addition：1.1ml；Colour developing Agent addition：1.1ml.
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