CN110261376A - The solution and method that ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode - Google Patents
The solution and method that ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode Download PDFInfo
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Abstract
The solution and method that chromogenic reaction interfere the invention discloses ammonium ion in a kind of removal water sample cyanide content continuous mode, removal water sample cyanide CN‑The solution that ammonium ion interferes chromogenic reaction during assay, by KH2PO4Solution, H3BO3Solution and NH4Cl solution mixing gained, each constituent concentration after mixing are as follows: KH2PO430~40mg/L, H3BO30.10~0.15mg/L, NH4100~150mg/L of Cl.Using CN in isonicotinic acid-pyrazolone colorimetric method for determining water sample‑When content, during obtaining cyanide standard curve, the solution that ammonium ion interferes chromogenic reaction in addition removal water sample cyanide content continuous mode is made with calibration standard curve using CN in the water sample that standard curve determines after correction‑Content is not interfered by ammonium ion, solves the problems, such as that ammonium ion influences measurement result accuracy.
Description
Technical field
The invention belongs to field of chemical detection, are related to a kind of remove using isonicotinic acid-pyrazolone colorimetric method for determining water sample
Middle simple cyanide (CN-) ammonium ion interferes chromogenic reaction during content solution and method.
Background technique
Simple cyanide (CN-) belong to hypertoxic chemical substance, the discharge in " integrated wastewater discharge standard GB 8978-1996 "
Limit value is 0.5mg/L.Simple cyanide content assaying method mainly has silver nitrate titration method, isonicotinic acid-pyrazoles in water sample at present
Quinoline ketone colorimetric method, isonicotinic acid -- barbituric acid spectrophotometry etc..Wherein isonicotinic acid-pyrazolone colorimetric method is most common survey
Determine method, detection mechanism is: in neutral conditions, toluene-sodium-sulfonchloramide is reacted with the cyanide in water sample generates cyanogen chloride, and cyanogen chloride is again
Hydrolysis is acted on isonicotinic acid and generates glutaconaldehyde, finally with pyrazolone-shrinking symphysis au bleu dyestuff, passes through suction at measurement 638nm
Shading value and the content for measuring simple cyanide in water sample.This method is although be suitable for drinking water, surface water, sanitary sewage and work
The measurement of simple cyanide in industry waste water.But we test discovery, ammonium ion present in water sampleIt can seriously do
The chromogenic reaction during isonicotinic acid-pyrazolone colorimetric method is disturbed, absorbance value deviation is caused, seriously affects the standard of measurement result
True property, underestimates the pollution level of simple cyanide in polluted-water.
Summary of the invention
It is anti-to developing the color that the purpose of the present invention is to provide ammonium ions in a kind of removal water sample cyanide content continuous mode
The solution that should be interfered, to solve using ammonium ion during isonicotinic acid-pyrazolone colorimetric method for determining water sample cyanide content
Chromogenic reaction is interfered, the problem of causing absorbance value deviation and influence measurement result accuracy.
Another object of the present invention is to provide ammonium ions in a kind of removal water sample cyanide content continuous mode to aobvious
The method of colour response interference.
The technical scheme adopted by the invention is that ammonium ion is anti-to developing the color in removal water sample cyanide content continuous mode
The solution that should be interfered is by KH2PO4Solution, H3BO3Solution and NH4Cl solution mixes resulting mixed solution, each in mixed solution
The concentration of ingredient are as follows: KH2PO430~40mg/L, H3BO30.10~0.15mg/L, NH4100~150mg/L of Cl.
Further, in the mixed solution each ingredient concentration are as follows: KH2PO4 30mg/L、H3BO3 0.15mg/L、
NH4Cl 150mg/L。
Another technical solution of the present invention is that ammonium ion is to aobvious in removal water sample cyanide content continuous mode
The method of colour response interference is using CN in isonicotinic acid-pyrazolone colorimetric method for determining water sample to be measured-When content, obtaining
During cyanide standard curve, it is dry to chromogenic reaction that ammonium ion in the removal water sample cyanide content continuous mode is added
The solution disturbed, is corrected standard curve, so that using CN in the determining water sample to be measured of standard curve after correction-Content not by
The interference of ammonium ion.
It is further, described that corrected to standard curve specific step is as follows:
Step S1,6 25mL colorimetric cylinders are taken, the CN of 0,0.2,0.5,1.0,2.0 and 3.0mL is separately added into-Concentration is
Then the standard potassium cyanide solution of 1mg/L is added 0.5mL and removes water sample cyanide (CN-) ammonium ion during assay
To the solution of chromogenic reaction interference, the NaOH solution that mass concentration is 0.1% is added to 10mL；
Step S2, the phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
Step S3,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to mark with distilled water
Line, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, it is bent to draw cyanide standard for the absorbance value of solution after determination step S3 water-bath at 638nm wavelength
Line.
Further, described that CN in water sample to be measured is determined by standard curve after correction-Specific step is as follows for content:
Step S21,0.5~5.0mL water sample to be measured is added in 25mL colorimetric cylinder, it is 0.1% that mass concentration, which is then added,
NaOH solution to 10mL；
Step S22, the phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step 1, after mixing, is rapidly added
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
Step S23,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2, is settled to distilled water
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S24, the absorbance value of solution after 3 water-bath of determination step at 638nm wavelength, and it is bent according to cyanide standard
Line computation goes out CN in water sample-Concentration.
Further, the phosphate buffer solution of the pH=7.0 is to be dissolved in steaming by potassium dihydrogen phosphate and disodium hydrogen phosphate
Gained in distilled water, the concentration of the potassium dihydrogen phosphate are 34g/L, and the concentration of the disodium hydrogen phosphate is 35.5g/L.
Further, the isonicotinic acid-pyrazolone solution is before use by pyrazolone solution and isonicotinic acid solution
Mix resulting mixed solution；The isonicotinic acid solution be 1.5g isonicotinic acid is dissolved in 24mL mass concentration be 2% NaOH it is molten
In liquid, afterwards plus distilled water is settled to the resulting solution of 100mL；The pyrazolone solution is to be dissolved in 0.25g pyrazolone
Solution obtained in 20mL dimethyl formamide solution.
The invention has the advantages that using CN in isonicotinic acid-pyrazolone colorimetric method for determining water sample to be measured-When content,
During obtaining cyanide standard curve, removal water sample cyanide (CN is added-) during assay ammonium ion to aobvious
The solution of colour response interference, the ammonium ion that can be effectively removed in water sampleTo simple cyanide (CN-) measurement it is dry
It disturbs, measurement result is accurate, reliable, and easy to operate, practical, quick, strong operability is solved using isonicotinic acid-pyrazolone
Ammonium ion interferes chromogenic reaction during colorimetric method for determining water sample cyanide content, causes absorbance value deviation and influences to measure
As a result the problem of accuracy.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is the curve graph of the standard curve 1 of water sample concentration of cyanide and absorbance value；
Fig. 2 is the curve graph of the standard curve 2 of water sample concentration of cyanide and absorbance value；
Fig. 3 is corresponding canonical plotting when the solution A of different volumes is added.
Specific embodiment
Following will be combined with the drawings in the embodiments of the present invention, and technical solution in the embodiment of the present invention carries out clear, complete
Site preparation description, it is clear that described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.It is based on
Embodiment in the present invention, it is obtained by those of ordinary skill in the art without making creative efforts every other
Embodiment shall fall within the protection scope of the present invention.
Embodiment 1
Remove ammonium ionTo using the simple cyanide in isonicotinic acid-pyrazolone colorimetric method for determining water sample
(CN-) the content method that display reaction is interfered in the process, specifically follow the steps below:
KCN standard curve 1:
Step S1,6 25mL colorimetric cylinders are taken, the KCN (potassium cyanide) of 0,0.2,0.5,1.0,2.0 and 3.0mL is separately added into
Standard solution, CN in KCN standard solution-Concentration be 1mg/L, then be added mass concentration be 0.1% NaOH solution extremely
10mL；
Step S2, the phosphate buffer solution 5mL of pH=7.0 is added into each colorimetric cylinder, after mixing, is rapidly added 0.2mL
Mass concentration be 1% toluene-sodium-sulfonchloramide solution, toluene-sodium-sulfonchloramide solution is to be dissolved in water by 0.5g toluene-sodium-sulfonchloramide, and be diluted to 50mL, immediately lid plug,
It shakes up, places 3~5min；
Step S3,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2, is settled to distilled water
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and draw as shown in Figure 1
KCN standard curve 1.
Sample measurement 1:
0.5~5.0mL of water sample to be measured is added in step 1 in 25mL colorimetric cylinder, and the amount of water sample to be measured is according to CN in water sample-
Concentration depending on, in water sample to be measuredConcentration be set as 50.0mg/L, in usual sanitary sewageConcentration be 20
~30mg/L, in industrial wastewaterConcentration be higher than 50.0mg/L when, can be diluted in water sampleConcentration be
50.0mg/L is handled, the NaOH solution that addition mass concentration is 0.1% to 10mL；
Step 2, the phosphate buffer solution 5mL that pH=7.0 is added into the colorimetric cylinder of step 1, after mixing, are rapidly added
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2 for step 3, is settled to 25mL with distilled water,
In 25~35 DEG C of water-bath 40min after shaking up；
Step 4, after 3 water-bath of determination step at 638nm wavelength solution absorbance value, and according to KCN standard curve 1
(Fig. 1) calculates simple cyanide (CN in water sample-) concentration, measurement result is shown in Table 1:
The sample concentration result data of 1 establishing criteria curve 1 of table measurement
| Water sample compound concentration (mg CN/L) | 1.0 | 2.0 | 3.0 |
| Water sample measured concentration (mg CN/L) (SD) | 0.78(0.02) | 1.64(0.03) | 2.38(0.02) |
Embodiment 2
KCN standard curve 2 (correction):
Step S1,6 25mL colorimetric cylinders are taken, the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL is separately added into,
CN in KCN standard solution-Concentration be 1mg/L, then be added 0.5mL solution A, solution A is by KH2PO4Solution, H3BO3Solution and
NH4Three kinds of solution of Cl solution mix, and the concentration of three kinds of components is respectively 30mg/L KH in solution A after mixing2PO4、
0.15mg/L H3BO3With 150mg/L NH4Cl adds the NaOH solution that mass concentration is 0.1% to 10mL；
Step S2, the phosphate buffer solution of pH=7.0 is added into each colorimetric cylinder, after mixing, is rapidly added 0.2mL mass
The toluene-sodium-sulfonchloramide that concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
Step S3,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to mark with distilled water
Line, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and draw as shown in Figure 2
KCN standard curve 2.
Sample measurement 2:
0.5~5.0mL of water sample to be measured is added (according to CN in water sample in step 1 in 25mL colorimetric cylinder-Concentration depending on, to
It surveys in water sampleConcentration be 50.0mg/L), the NaOH solution that mass concentration is 0.1% is added to 10mL；
Step 2, the phosphate buffer solution that pH=7.0 is added into each colorimetric cylinder, after mixing, are rapidly added 0.2mL mass
The toluene-sodium-sulfonchloramide 0.2 that concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2 for step 3, is settled to 25mL with distilled water,
In 25~35 DEG C of water-bath 40min after shaking up；
Step 4, after 3 water-bath of determination step at 638nm wavelength solution absorbance value, and according to KNC standard curve 2 count
Calculate simple cyanide (CN in water sample-) concentration, measurement result is shown in Table 2.
The sample concentration result data of 2 establishing criteria curve 2 of table measurement
| Water sample compound concentration (mg CN/L) | 1.0 | 2.0 | 3.0 |
| Water sample measured concentration (mg CN/L) (SD) | 1.03(0.02) | 2.18(0.05) | 3.18(0.02) |
Embodiment 3
The selection of KCN standard curve:
Step S1,6 25mL colorimetric cylinders are taken, the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL is separately added into,
CN in KCN standard solution-Content be 1mg/L, add the solution A of 0.2,0.5 and 1.0mL respectively, then again plus 0.1%
NaOH solution is to 10mL；
Step S2, the phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step 1, after mixing, is rapidly added
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
Step S3,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2, is settled to distilled water
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution, obtains different standard curves after 3 water-bath of determination step at 638nm wavelength,
And simple cyanide (CN in water sample is calculated according to different standard curves respectively-) concentration, as shown in figure 3, addition 0.2mL
The standard curve fit equation of solution A is y1, standard curve (correction) fit equation of addition 0.5mL solution A is y2, it is added
The standard curve fit equation of 1.0mL solution A is y3。
Simple cyanide (the CN measured in water sample to be measured is calculated with various criterion curve-) concentration, as a result such as 3 institute of table
Show:
Simple cyanide (the CN in water sample to be measured that 3 various criterion curve of table calculates-) concentration
| Water sample compound concentration (mg CN/L) | 1.0 | 2.0 | 3.0 |
| Standard curve y1It calculates water sample measured concentration (mg CN/L) (SD) | 0.83(0.02) | 1.75(0.04) | 2.54(0.02) |
| Standard curve y2It calculates water sample measured concentration (mg CN/L) (SD) | 1.03(0.02) | 2.18(0.05) | 3.18(0.02) |
| Standard curve y3It calculates water sample measured concentration (mg CN/L) (SD) | 1.23(0.03) | 2.60(0.05) | 3.77(0.03) |
The phosphate buffer solution of pH=7.0 is that 100mL steaming is dissolved in by 3.40g potassium dihydrogen phosphate and 3.55g disodium hydrogen phosphate
Gained in distilled water.
1.5g isonicotinic acid is dissolved in the NaOH solution that 24mL mass concentration is 2%, afterwards plus distilled water is settled to 100mL,
Obtain isonicotinic acid solution；And 0.25g pyrazolone is dissolved in 20mL dimethyl formamide solution and obtains pyrazolone solution, face
The isonicotinic acid solution of above-mentioned pyrazolone solution and 100mL are mixed with preceding, acquired solution is that isonicotinic acid-pyrazolone is molten
Liquid.
Embodiment 4
Individually add the potassium dihydrogen phosphate of various concentration:
Step S1 takes 6 25mL colorimetric cylinders, is separately added into the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL,
CN in KCN standard solution-Content be 1mg/L, the KH of 0.5mL different quality concentration is added into each colorimetric cylinder respectively2PO4
Then solution adds the NaOH solution that mass concentration is 0.1% to 10mL；
The phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step 1, after mixing, is rapidly added by step S2
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3-5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step 2, is settled to distilled water by step S3
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and according to addition various concentration
KH2PO4Standard curve obtained by solution, calculates separately simple cyanide (CN in water sample-) concentration, the results are shown in Table 4.Add
Add 20mg/L KH2PO4The standard curve of solution: y=1.8969x, R2=0.995；Add 30mg/L KH2PO4The standard of solution
Curve: y=1.7465x, R2=0.9976；Add 50mg/L KH2PO4The standard curve of solution: y=1.8378x, R2=
0.9959。
Table 4 individually adds KH2PO4CN in the water sample to be measured that standard curve obtained by solution calculates-Concentration
Embodiment 5
Individually add the boric acid solution of various concentration:
Step S1 takes 6 25mL colorimetric cylinders, is separately added into the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL,
CN in KCN standard solution-Content be 1mg/L, reenter the H of 0.5mL various concentration into each nasal obstruction pipe respectively3BO3Solution, then
Add the NaOH solution that mass concentration is 0.1% to 10mL；
The phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added by step S2
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to distilled water by step S3
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and according to addition various concentration
H3BO3Standard curve obtained by solution, calculates separately simple cyanide (CN in water sample-) concentration, the results are shown in Table 5.Addition
0.07mg/L H3BO3The standard curve of solution: y=1.8248x (R2=0.9981) 0.15mg/L H, is added3BO3The mark of solution
Directrix curve: y=1.781x, R2=0.9981；Add 0.30mg/L H3BO3The standard curve of solution: y=1.7486x, R2=
0.9896。
Table 5 individually adds H3BO3CN in the water sample to be measured that standard curve obtained by solution calculates-Concentration
Embodiment 6
Individually add the ammonium chloride solution of various concentration:
Step S1 takes 6 25mL colorimetric cylinders, is separately added into the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL,
CN in KCN standard solution-Content be 1mg/L, the NH of 0.5mL various concentration is added into each colorimetric cylinder respectively4Cl solution,
Then the NaOH solution that mass concentration is 0.1% is added to 10mL；
The phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added by step S2
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to distilled water by step S3
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and according to addition various concentration
NH4Standard curve obtained by Cl solution, calculates separately simple cyanide (CN in water sample-) concentration, the results are shown in Table 6.Addition
75mg/L NH4The standard curve of Cl solution: y=1.7927x, R2=0.9979；Add 150mg/L NH4The standard of Cl solution is bent
Line: y=1.4686x, R2=0.9944；Add 300mg/L NH4The standard curve of Cl solution: y=1.3706x, R2=
0.9929。
Table 6 individually adds NH4CN in the water sample to be measured that standard curve obtained by Cl solution calculates-Concentration
Embodiment 7
Add the solution A of different formulations:
Step S1 takes 6 25mL colorimetric cylinders, is separately added into the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL,
CN in KCN standard solution-Concentration be 1mg/L, then respectively into each colorimetric cylinder be added 0.5mL different formulations solution A (formula
1: KH in mixing acquired solution A2PO4 30mg/L、H3BO30.15mg/L, formula 2: KH in mixing acquired solution A2PO4 30mg/
L、NH4Cl 150mg/L, formula 3: H in mixing acquired solution A3BO3 0.15mg/L、NH4Cl 150mg/L, formula 4: mixing institute
Obtain KH in solution A2PO4 30mg/L、H3BO3 0.15mg/L、NH4Cl 150mg/L), then adding mass concentration is 0.1%
NaOH solution to 10mL；
The phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added by step S2
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to distilled water by step S3
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and according to addition different formulations
Mixed solution obtained by standard curve calculate separately simple cyanide (CN in water sample-) concentration, the results are shown in Table 7.Addition
It is formulated the standard curve of 1 solution: y=1.7741x (R2=0.999), the standard curve of 2 solution of addition formula: y=1.7964x
(R2=0.9932), the standard curve of 3 solution of addition formula: y=1.7868x (R2=0.9946), the mark of 4 solution of addition formula
Directrix curve: y=1.5344x (R2=0.9954).
Table 7 adds CN in the water sample to be measured that standard curve obtained by different formulations solution A calculates-Concentration
It is not difficult to find out from the result of embodiment 4~7, adds and be formulated in step S1: in formula 4 i.e. mixing acquired solution A
KH2PO4 30mg/L、H3BO3 0.15mg/L、NH4When Cl 150mg/L, simple cyanide (CN in water sample-) measured concentration with
Compound concentration is closest, removal ammonium ion to show in water sample cyanide content continuous mode react interference effect it is best,
And when using the solution A of various other formulas, survey simple cyanide (CN in water sample-) concentration it is obviously relatively low.
Embodiment 8
Step S1 takes 6 25mL colorimetric cylinders, is separately added into the KCN standard solution of 0,0.2,0.5,1.0,2.0 and 3.0mL,
CN in KCN standard solution-Concentration be 1mg/L, then respectively into each colorimetric cylinder be added 0.5mL different formulations mixed solution
(formula 1: KH in mixing acquired solution A2PO4 35mg/L、H3BO3 0.15mg/L、NH4Cl 150mg/L, formula 2: mixing gained
KH in solution A2PO4 40mg/L、H3BO3 0.15mg/L、NH4Cl 150mg/L, formula 3: KH in mixing acquired solution A2PO4
30mg/L、H3BO3 0.10mg/L、NH4Cl 150mg/L, formula 4: KH in mixing acquired solution A2PO4 30mg/L、H3BO3
0.12mg/L、NH4Cl 150mg/L, formula 5: KH in mixing acquired solution A2PO4 30mg/L、H3BO3 0.15mg/L、NH4Cl
100mg/L, formula 6: KH in mixing acquired solution A2PO4 30mg/L、H3BO3 0.15mg/L、NH4Cl 130mg/L), then again
The NaOH solution that mass concentration is 0.1% is added to 10mL；
The phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added by step S2
The toluene-sodium-sulfonchloramide that 0.2mL mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to distilled water by step S3
25mL, in 25~35 DEG C of water-bath 40min after shaking up；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength, and according to addition different formulations
Mixed solution obtained by standard curve calculate separately simple cyanide (CN in water sample-) concentration, the results are shown in Table 8.Addition
It is formulated the standard curve of 1 solution: y=1.4397x (R2=0.9961), the standard curve of 2 solution of addition formula: y=1.4487x
(R2=0.9936), the standard curve of 3 solution of addition formula: y=1.4657x (R2=0.9995), the mark of 4 solution of addition formula
Directrix curve: y=1.4634x (R2=0.9944), the standard curve of 5 solution of addition formula: y=1.4503x (R2=0.9905),
The standard curve of addition 6 solution of formula: y=1.4578x (R2=0.9987).
Table 8 adds CN in the water sample to be measured that standard curve obtained by solution A calculates-Concentration
It can be seen that after the solution A that step S1 adds 6 kinds of different formulations from the measurement result of embodiment 8, it is simple in water sample
Single cyanide (CN-) measured concentration and compound concentration relatively, removal ammonium ion water sample cyanide content was measured
Show that reaction interference effect is also ideal in journey.That is KH in mixed liquor A2PO4Concentration range be 30~40mg/L, H3BO3's
Concentration range is 0.10~0.15mg/L, NH4The concentration range of Cl is 100~150mg/L.But the optimal of mixed solution A is matched
Fang Shi: KH2PO4 30mg/L、H3BO3 0.15mg/L、NH4Cl 150mg/L is formulated the simple cyaniding in measurement water sample using this
Object (CN-) measured concentration and compound concentration it is closest.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (7)
1. the solution that ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode, which is characterized in that be
By KH2PO4Solution, H3BO3Solution and NH4Cl solution mixes resulting mixed solution, the concentration of each ingredient in mixed solution are as follows:
KH2PO430~40mg/L, H3BO30.10~0.15mg/L, NH4100~150mg/L of Cl.
2. ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode according to claim 1
Solution, which is characterized in that the concentration of each ingredient in the mixed solution are as follows: KH2PO4 30mg/L、H3BO3 0.15mg/L、NH4Cl
150mg/L。
3. the method that ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode, which is characterized in that adopt
With CN in isonicotinic acid-pyrazolone colorimetric method for determining water sample to be measured-When content, during obtaining cyanide standard curve, add
Enter the solution that ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode as claimed in claim 1 or 2, it is right
Standard curve is corrected, so that using CN in the determining water sample to be measured of standard curve after correction-Content is not by ammonium ion
Interference.
4. ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode according to claim 3
Method, which is characterized in that described corrected to standard curve specific step is as follows:
Step S1,6 25mL colorimetric cylinders are taken, the CN of 0,0.2,0.5,1.0,2.0 and 3.0mL is separately added into-Concentration is 1mg/L's
Then it is dry to chromogenic reaction that ammonium ion in 0.5mL removal water sample cyanide content continuous mode is added in standard potassium cyanide solution
The solution disturbed adds the NaOH solution that mass concentration is 0.1% to 10mL；
Step S2, the phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S1, after mixing, is rapidly added 0.2mL matter
The toluene-sodium-sulfonchloramide that concentration is 1% is measured, lid is filled in, shaken up immediately, places 3~5min；
Step S3,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S2, is settled to graticule with distilled water, shakes
In 25~35 DEG C of water-bath 40min after even；
Step S4, the absorbance value of solution after determination step S3 water-bath at 638nm wavelength draws cyanide standard curve.
5. ammonium ion interferes chromogenic reaction in removal water sample cyanide content continuous mode according to claim 3
Method, which is characterized in that described that CN in water sample to be measured is determined using standard curve after correction-Specific step is as follows for content:
Step S21,0.5~5.0mL water sample to be measured is added in 25mL colorimetric cylinder, it is 0.1% that mass concentration, which is then added,
NaOH solution is to 10mL；
Step S22, the phosphate buffer solution of pH=7.0 is added into the colorimetric cylinder of step S21, after mixing, is rapidly added 0.2mL
The toluene-sodium-sulfonchloramide that mass concentration is 1%, lid is filled in, is shaken up immediately, places 3~5min；
Step S23,5mL isonicotinic acid-pyrazolone solution is added into the colorimetric cylinder of step S22, is settled to 25mL with distilled water,
In 25~35 DEG C of water-bath 40min after shaking up；
Step S24, the absorbance value of solution after determination step S23 water-bath at 638nm wavelength, and according to cyanide standard curve
Calculate CN in water sample-Concentration.
6. ammonium ion is dry to chromogenic reaction in removal water sample cyanide content continuous mode according to claim 4 or 5
The method disturbed, which is characterized in that the phosphate buffer solution of the pH=7.0 is dissolved in by potassium dihydrogen phosphate and disodium hydrogen phosphate
Gained in distilled water, the concentration of the potassium dihydrogen phosphate are 34g/L, and the concentration of the disodium hydrogen phosphate is 35.5g/L.
7. ammonium ion is dry to chromogenic reaction in removal water sample cyanide content continuous mode according to claim 4 or 5
The method disturbed, which is characterized in that the isonicotinic acid-pyrazolone solution is before use that pyrazolone solution and isonicotinic acid is molten
Liquid mixes resulting mixed solution；
The isonicotinic acid solution is in the NaOH solution that 1.5g isonicotinic acid is dissolved in 24mL mass concentration and is 2%, afterwards plus distilled water
It is settled to the resulting solution of 100mL；
The pyrazolone solution is that 0.25g pyrazolone is dissolved in solution obtained in 20mL dimethyl formamide solution.
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