CN110514499A - A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery - Google Patents
A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery Download PDFInfo
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Abstract
The present invention relates to a kind of pre-treatment optimization methods of promotion solid waste Cr VI detection rate of recovery, belong to the technical field of Cr VI detection, it is the following steps are included: S1: solution is prepared: acquisition sample, sodium carbonate/sodium hydroxide mixed solution is added in sample, magnesium chloride and dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution is added, obtains sample solution；S2: resolution: being sealed sample solution with vinyl chloride film, after stirring 5min under room temperature, clears up 60min at 90 DEG C -95 DEG C；S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of filter membrane, and in batches with 50 DEG C -80 DEG C of hot water, repeatedly washed on a small quantity, collects filtrate in beaker；S4: concentration filtrate: filtrate is concentrated by evaporation at 80 DEG C -95 DEG C to 70-75mL, and pH value is adjusted to 8.8-9.2 or so, 100mL is settled to deionized water, is detected after shaking up by atomic absorption spectrophotometry.The rate of recovery of Cr VI can be improved in the present invention.
Description
Technical field
The present invention relates to the technical fields of Cr VI detection, detect the rate of recovery more particularly, to a kind of promotion solid waste Cr VI
Pre-treatment optimization method.
Background technique
The chromium of two kinds of valence states is stabilized in environment, suitable trivalent chromium can reduce the blood sugar concentration in human plasma, mention
Hyperinsulinism activity, promotes sugar and fat metabolism, promotes stress reaction ability etc., and Cr VI has severe toxicity, has carcinogenesis,
Toxicity is 100 times of trivalent chromium.
Currently, to the detection of chromium content in solid waste mostly according in state environment protecting standard HJ 687-2014
Method carry out.After weighing sample, sample is placed in flask, in flask be added sodium carbonate/sodium hydroxide mixed liquor,
Magnesium chloride and dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution, after being put into stirrer, are sealed with polyethylene film, are stirred under room temperature
It mixes after five minutes, is cleared up 60 minutes at 90 DEG C -95 DEG C.After resolution, it is cooled to room temperature, after suction filtration, then will with concentrated nitric acid
PH is adjusted to 8.8-9.2, after being settled to 100mL with deionized water, then is detected by atomic absorption spectrophotometry.
After prior art among the above has the following deficiencies: resolution, during suction filtration, it is easy to cause
Liquor capacity is more than 100mL, and has to reduce washing times, the final rate of recovery for influencing Cr VI.
Summary of the invention
The purpose of the present invention one is to provide a kind of pre-treatment optimization method of promotion solid waste Cr VI detection rate of recovery, improves
The rate of recovery of Cr VI.
Above-mentioned purpose of the invention has the technical scheme that
A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery, comprising the following steps:
S1: solution is prepared: sodium carbonate/sodium hydroxide mixed solution is added in sample, magnesium chloride and phosphoric acid is added for acquisition sample
Hydrogen dipotassium-potassium dihydrogen phosphate buffer solution, obtains sample solution；
S2: resolution: being sealed sample solution with vinyl chloride film, after stirring 5min under room temperature, is cleared up at 90 DEG C -95 DEG C
60min；
S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of filter membrane, and with 50 DEG C -80 DEG C
Hot water in batches, is repeatedly washed on a small quantity, collects filtrate in beaker；
S4: concentration filtrate: filtrate is concentrated by evaporation at 80 DEG C -95 DEG C to 70-75mL, and pH value is adjusted to the left side 8.8-9.2
The right side is settled to 100mL with deionized water, is detected after shaking up by atomic absorption spectrophotometry.
Dissociate in solution under the alkaline environment that sodium carbonate and sodium hydroxide provide by using above-mentioned technical proposal
Hexavalent chromium is reduced to a possibility that trivalent chromic ion and minimizes；Cr3+Under alkaline environment with hydroxide ion or carbon
Acid ion reaction generates Cr (OH)3With Cr (CO3)3Precipitating；And hexavalent chromium is with dichromate ion Cr2O2 2-The shape of anion
Formula exists, will not be with other anion bindings.
Mg is added into phosphate buffer solution2+It can play the role of inhibiting oxidation, trivalent chromic ion is oxidized to six
A possibility that valence chromium ion, minimizes；It is heated 60 minutes in 90-95 DEG C, can further dissolve Cr VI and stabilizing trivalent
Chromium, to extract the hexavalent chromium in sample.
When suction filtration, Cr (OH)3With Cr (CO3)3Precipitating will be left on filter membrane, and hexavalent chromium is with dichromate ion
Cr2O2 2-The form of anion is present in filtrate；With moisture batch, a small amount of repeatedly washing can reduce the loss of hexavalent chromium
Amount, as far as possible rinses residual liquid on filter membrane, improves the rate of recovery to hexavalent chromium.
Hot water accelerates molecular mobility, and molecular motion is fierce, and washing effect is more preferably.In addition, the temperature of hot water is limited,
So that the temperature of hot water closer to digestion condition, further dissolves hexavalent chromium and stabilizing trivalent chromium ion, trivalent is reduced
A possibility that chromium ion and hexavalent chromium are mutually converted improves accuracy when detection；Secondly, limitation maximum temperature is 80 DEG C
The reason of be, when temperature is more than 80 DEG C, wash bottle can feel like jelly, meanwhile, can relatively scald one's hand when operator picks up wash bottle with hand, no
Convenient for operation.
It is more before the content of filtrate is opposite after collecting filtrate, at this point, the side at 80-95 DEG C by being concentrated by evaporation
Method reduces the volume of filtrate, convenient for being settled to 100mL；Temperature when evaporation and concentration is consistent with digestion condition, can reduce evaporation
A possibility that trivalent chromium and Cr VI are mutually converted when concentration reduces a possibility that Cr VI is evaporated in air；Finally again
The content of hexavalent chromium is detected by atomic absorption spectrophotometry.
The present invention is washed in batches after suction filtration, with hot water, improves the extracted amount of hexavalent chromium, is concentrated by evaporation filter
The volume of liquid, reduces the loss amount of hexavalent chromium, to improve the rate of recovery of hexavalent chromium.
The present invention is further arranged to: in step S3,50 DEG C -80 DEG C of hot water total volume is 60-70mL.
By using above-mentioned technical proposal, the volume of hot water is excessive, is likely to result in hexavalent chromium when being concentrated by evaporation
Loss, volume is too small to be not achieved preferable washing effect, and therefore, it is necessary to control the volume of hot water.
The present invention is further arranged to: being 60-70mL by total volume, the hot water that temperature is 50 DEG C -80 DEG C is extremely in step S3
Divide 8 washings less.
By using above-mentioned technical proposal, washing times are excessive, be easy to cause loss, the very few washing effect of washing times is not
It is good, the number of washing is further limited, can reach best washing effect.
The present invention is further arranged to: in step 3, washing amount in batches are as follows: successively are as follows: 13-15mL, 11-12mL,
11-12mL、7-8mL、7-8mL、4-5mL、4-5mL、3-5mL。
By using above-mentioned technical proposal, point 8 washings, and dosage is washed in reduction trend, can enhance washing effect,
Improve the rate of recovery.
The present invention is further arranged to: in step S4, after evaporation and concentration, then with the deionized water of 4-6mL rinsing wall of cup.
By using above-mentioned technical proposal, after evaporation and concentration, amount of liquid is reduced, and it is molten to be stained with part on wall of cup
Liquid, at this point, rinsing the loss amount that can be reduced when being concentrated by evaporation again with deionized water.
The present invention is further arranged to: in step S3, beaker used is beaker in tall form.
By using above-mentioned technical proposal, the more common beaker height of beaker in tall form is higher, can reduce solution by beaker
A possibility that inside spilling improves the rate of recovery to reduce loss amount.
The present invention is further arranged to: in step S3, it is 0.45 μm of polycarbonate leaching film that filter membrane, which is selected,.
In conclusion advantageous effects of the invention are as follows:
1. the present invention is washed after suction filtration with hot water in batches, the extracted amount of hexavalent chromium is improved, is concentrated by evaporation filtrate
Volume, the loss amount of hexavalent chromium is reduced, to improve the rate of recovery of hexavalent chromium；
2. point 8 washings, and dosage is washed in reduction trend, washing effect can be enhanced, improve the rate of recovery；
3. temperature when being concentrated by evaporation is consistent with digestion condition, trivalent chromium and Cr VI are mutually converted when can reduce evaporation and concentration
Possibility reduces a possibility that Cr VI is evaporated in air, it is ensured that the accuracy of detection.
Specific embodiment
Embodiment 1
A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery, comprising the following steps:
S1: solution is prepared: being accurately weighed solid waste sample 2.50g and is placed in 250mL round-bottomed flask, 50.0mL carbonic acid is added
Sodium/sodium hydroxide mixed solution is added 400mg magnesium chloride and 50.0mL dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution, obtains
Sample solution；
S2: resolution: being put into stirrer, and sealed round-bottomed flask with vinyl chloride film, after stirring 5min under room temperature, opens heating dress
It sets, when temperature reaches 90 DEG C, clears up 60min；
S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of polycarbonate leaching film, and with warm
Degree is 50 DEG C, and hot water point 8 times that volume is 60mL are washed, and collects filtrate in beaker in tall form；The washing amount of washing by several times
Successively are as follows: 13mL, 11mL, 11mL, 7mL, 7mL, 4mL, 4mL, 3mL.
S4: concentration filtrate: it is 70mL that filtrate is evaporated at 80 DEG C and is concentrated into volume, is rushed with the deionized water of 4mL
Walls of beaker is washed, pH value is adjusted to 8.8 or so by concentrated nitric acid, then 100mL is settled to deionized water, obtains prepare liquid,
It is detected after shaking up by atomic absorption spectrophotometry.
Embodiment 2
A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery, comprising the following steps:
S1: solution is prepared: being accurately weighed solid waste sample 2.50g and is placed in 250mL round-bottomed flask, 50.0mL carbonic acid is added
Sodium/sodium hydroxide mixed solution is added 400mg magnesium chloride and 50.0mL dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution, obtains
Sample solution；
S2: resolution: being put into stirrer, and sealed round-bottomed flask with vinyl chloride film, after stirring 5min under room temperature, opens heating dress
It sets, when temperature reaches 92 DEG C, clears up 60min；
S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of polycarbonate leaching film, and with warm
Degree is 70 DEG C, and hot water point 8 times that volume is 65mL are washed, and collects filtrate in beaker in tall form；The washing amount of washing by several times
Successively are as follows: 14mL, 11mL, 11mL, 8mL, 8mL, 5mL, 4mL, 4mL.
S4: concentration filtrate: it is 72mL that filtrate is evaporated at 85 DEG C and is concentrated into volume, is rushed with the deionized water of 5mL
Walls of beaker is washed, pH value is adjusted to 9.0 or so by concentrated nitric acid, then 100mL is settled to deionized water, obtains prepare liquid,
It is detected after shaking up by atomic absorption spectrophotometry.
Embodiment 3
A kind of pre-treatment optimization method promoting the solid waste Cr VI detection rate of recovery, comprising the following steps:
S1: solution is prepared: being accurately weighed solid waste sample 2.50g and is placed in 250mL round-bottomed flask, 50.0mL carbonic acid is added
Sodium/sodium hydroxide mixed solution is added 400mg magnesium chloride and 50.0mL dipotassium hydrogen phosphate-potassium dihydrogen phosphate buffer solution, obtains
Sample solution；
S2: resolution: being put into stirrer, and sealed round-bottomed flask with vinyl chloride film, after stirring 5min under room temperature, opens heating dress
It sets, when temperature reaches 95 DEG C, clears up 60min；
S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of polycarbonate leaching film, and with warm
Degree is 80 DEG C, and hot water point 8 times that volume is 70mL are washed, and collects filtrate in beaker in tall form；The washing amount of washing by several times
Successively are as follows: 15mL, 12mL, 12mL, 8mL, 8mL, 5mL, 5mL, 5mL.
S4: concentration filtrate: it is 75mL that filtrate is evaporated at 95 DEG C and is concentrated into volume, is rushed with the deionized water of 6mL
Walls of beaker is washed, pH value is adjusted to 9.2 or so by concentrated nitric acid, then 100mL is settled to deionized water, obtains prepare liquid,
It is detected after shaking up by atomic absorption spectrophotometry.
Comparative example 1
The difference from example 2 is that being washed in step S3 with the deionized water of room temperature.
Comparative example 2
The difference from example 2 is that being washed 1 time in step S3 with hot water, washing dosage is 14mL.
Comparative example 3
The difference from example 2 is that being washed 3 times in step S3 with hot water, washing dosage is successively are as follows: 13mL, 7mL, 3mL.
Comparative example 4
The preparation of prepare liquid is carried out according to the operating procedure in state environment protecting standard HJ 687-2014.
One, atomic absorption spectrophotometry detecting step:
1, the drafting of standard curve accurately pipette Cr VI standard solution 0.00,0.20,0.80,2.00,4.00,8.00mL in
In 100mL volumetric flask, be settled to graticule with deionized water, shake up, the concentration of Cr VI is respectively 0.00,0.20,0.80,
2.00,4.00,8.00μg/mL.By the absorbance of the sequence sequentially determining standard solution of concentration from low to high.With zero mass concentration
Calibration absorbance is ordinate, with the concentration (μ g/mL) of corresponding chromium for abscissa, draws calibration curve.
2, sample measurement is detected to be measured.
3, blank test is according to preparing blank solution (do not contain hexavalent chromium) the step of prepare liquid, and according to same
Detection method is detected.
Two, testing result
1, precision
Precision: the solid waste sample that content of 6-valence Cr ions is 2.8mg/kg is measured, repeatability limit 0.873mg/
Kg, reproducibility are limited to 1.21mg/kg.
2, recovery of standard addition and relative standard deviation are detected using blank sample (being free of hexavalent chromium), use sample
The method of middle addition standard solution carries out recovery of standard addition experiment according to same detection method, and each concentration does 3 in parallel
Sample, each sample are continuously surveyed 5 times at identical conditions, calculate relative standard deviation, the results are shown in Table 1.
The testing result of table 1 embodiment 1-3 and comparative example 1-4
| Project | Average recovery of standard addition (%) | Relative standard deviation (%) |
| Embodiment 1 | 83.9 | 1.23 |
| Embodiment 2 | 84.5 | 1.18 |
| Embodiment 3 | 84.1 | 1.25 |
| Comparative example 1 | 70.2 | 1.19 |
| Comparative example 2 | 71.2 | 1.21 |
| Comparative example 3 | 76.7 | 1.30 |
| Comparative example 4 | 62.3 | 1.31 |
As seen from Table 1, the rate of recovery of embodiment 1-3 can reach 80% or more, and the rate of recovery of comparative example 1-4 is lower.It is right
It is washed in ratio 1 with cold water, the rate of recovery is lower than embodiment 2, illustrates the washing effect of hot water more preferably；Hot water wash is used in comparative example 2
It washs once, the rate of recovery is slightly above comparative example 1 lower than embodiment 2, illustrates that the effect of hot water washs multiple effect phase with cold water
Difference is very few, but the effect that washed once can not show a candle to washing repeatedly；It is washed 3 times in comparative example 3 with hot water, the rate of recovery is higher than comparative example
3 but still be lower than embodiment 2, illustrate that the more washing effects of washing times are better.
Comparative example 4 is seen again, and comparative example 4 is using the method in state environment protecting standard HJ 687-2014, with embodiment 2
Difference be free from washing and be concentrated by evaporation the step of, be directly settled to deionized water after polycarbonate leaching film filters
100mL can be detected.The rate of recovery of embodiment 1-3 is much higher than comparative example 4.
In conclusion the present invention is washed in batches after suction filtration, with hot water, the extracted amount of hexavalent chromium is improved,
It is concentrated by evaporation the volume of filtrate, the loss amount of hexavalent chromium is reduced, to improve the rate of recovery of hexavalent chromium.
The embodiment of present embodiment is presently preferred embodiments of the present invention, not limits protection of the invention according to this
Range, therefore: the equivalence changes that all structures under this invention, shape, principle are done, should all be covered by protection scope of the present invention it
It is interior.
Claims (7)
1. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery, it is characterised in that: the following steps are included:
S1: solution is prepared: sodium carbonate/sodium hydroxide mixed solution is added in sample, magnesium chloride and phosphoric acid is added for acquisition sample
Hydrogen dipotassium-potassium dihydrogen phosphate buffer solution, obtains sample solution；
S2: resolution: being sealed sample solution with vinyl chloride film, after stirring 5min under room temperature, clears up 60min at 90-95 DEG C；
S3: washing: the sample solution after resolution is cooled to room temperature, then is filtered with 0.45 μm of filter membrane, and with 50 DEG C -80 DEG C
Hot water in batches, is repeatedly washed on a small quantity, collects filtrate in beaker；
S4: concentration filtrate: filtrate is concentrated by evaporation at 80 DEG C -95 DEG C to 70-75mL, and pH value is adjusted to the left side 8.8-9.2
The right side is settled to 100mL with deionized water, is detected after shaking up by atomic absorption spectrophotometry.
2. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 1, feature
Be: in step S3,50 DEG C -80 DEG C of hot water total volume is 60-70mL.
3. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 2, feature
It is: is 60-70mL by total volume in step S3, temperature is that 50 DEG C -80 DEG C of hot water at least divides 8 washings.
4. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 3, feature
It is: in step 3, washing amount in batches are as follows: successively are as follows: 13-15mL, 11-12mL, 11-12mL, 7-8mL, 7-8mL, 4-
5mL、4-5mL、3-5mL。
5. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 1, feature
It is: in step S4, after evaporation and concentration, then with the deionized water of 4-6mL rinses wall of cup.
6. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 1, feature
Be: in step S3, beaker used is beaker in tall form.
7. a kind of pre-treatment optimization method for promoting the solid waste Cr VI detection rate of recovery according to claim 1, feature
Be: in step S3, it is 0.45 μm of polycarbonate leaching film that filter membrane, which is selected,.
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| CN110967239A (en) * | 2020-01-02 | 2020-04-07 | 国家地质实验测试中心 | Method for dissolving and oxidizing metallic chromium |
| CN113533311A (en) * | 2020-04-16 | 2021-10-22 | 内蒙古第三地质矿产勘查开发有限责任公司 | Method for measuring content of hexavalent chromium in soil or solid waste |
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| CN106770205A (en) * | 2017-01-03 | 2017-05-31 | 淮南市产品质量监督检验所 | The method of content of 6-valence Cr ions in ICP OES methods analysis coal ash |
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Application publication date: 20191129 |