CN108535348A - The assay method of adsorbable organic halogen in a kind of water - Google Patents
The assay method of adsorbable organic halogen in a kind of water Download PDFInfo
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- CN108535348A CN108535348A CN201810212413.4A CN201810212413A CN108535348A CN 108535348 A CN108535348 A CN 108535348A CN 201810212413 A CN201810212413 A CN 201810212413A CN 108535348 A CN108535348 A CN 108535348A
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Abstract
Include that the pretreatment of column absorption and oscillation absorption is carried out to water sample, utilizes progress microcoulomb measurement after combustion and pyrolysis stove oxidizing fire the invention discloses a kind of assay method of adsorbable organic halogen in water;Wherein, electrolyte and part operation parameter is optimized in the present invention, improves the stability of electrolyte, reduces calibration steps, to improve sensitivity, accuracy and the stability of micro-coulometric determination, improves work efficiency.
Description
Technical field
The present invention relates to field of chemical detection, the assay method of adsorbable organic halogen in especially a kind of water.
Background technology
AOX (Adsorbable Organic Halogen) indicates that adsorbable organic halogen, adsorbable organic halogen are printing
The fields such as dye, weaving, fire retardant and dry cleaning agent are widely used.AOX has stronger lipophile, is not easy in natural water body
Degradation is easy deposition in cell tissue fat sites, and can by blood in each organ distribution of whole body, cause it is permanent and
Complicated harm.Furthermore, it is also possible to act synergistically with heavy metal, the bioactivity of heavy metal is improved, to be produced to body
The harm of raw bigger.Therefore, it although important function has occurred in the performance for improving part specific products in AOX, also threatens
Daily water consumption safety has been arrived, extensive attention is caused.
In water adsorbable organic halogen be paper-making industrial waste water and technique for the treatment of textile dyeing waste water exploitation, technique adjustment and
One of main Con trolling index of water quality emission compliance, external generally using adsorbable organic halogen in water as evaluating water quality (packet
Include drinking water, sanitary sewage, industrial wastewater etc.) composite target of poisonous organic pollution, and then it is in the starting stage in China.
The method of detection AOX has at present《Water quality -- measurement of adsorbable organic halogen (AOX) -- small-hole drilling》(GB/T 15959-
1995) and《Water quality -- measurement of adsorbable organic halogen (AOX) -- chromatography of ions》(HJ/T 83-2001).It is limited to detect
Condition and maturity, small-hole drilling are still the main method for measuring adsorbable organic halogen in water at this stage.However it is existing
National standard small-hole drilling comes with some shortcomings, and the electrolyte stability and sensitivity used due to it is not high, thus actually detected
When need that calibration is repeated to Coulomb meter, greatly extend detection the working time, reduce efficiency, simultaneously for some compared with
The water sample of low concentration is possible to can not achieve and accurately detect.Therefore, it is necessary to existing method is improved, it is micro- to improve
The accuracy and stability of adsorbable organic halogen in acrylonitrile by Coulometry water adapt to the discharge standard constantly updated.
Invention content
The technical problem to be solved by the present invention is to:In view of the above problems, providing can inhale in a kind of improved water
The assay method of attached organic halogen improves the accuracy and stability of micro-coulometric determination, reduces operating procedure, improves work effect
Rate.
The technical solution adopted by the present invention is as follows:
1) water sample pre-processes:
Column adsorbs:It takes 100ml water samples to be measured to pour into activated carbon pressure filter, sodium nitrate storing solution 2-5ml is added and is pressed
Filter after press filtration is complete, is added sodium nitrate leacheate 25mL and carries out press filtration elution;
Oscillation absorption:It takes 100ml water samples to pour into conical flask, 5ml sodium nitrate storing solutions is added, check pH value less than 2, then
40-50mg activated carbons are added, conical flask is placed on thermostatic control oscillator vibration support plate, vibrates 1h or more, water sample after oscillation is adopted
Press filtration is carried out with activated carbon pressure filter, with 25ml sodium nitrate cleaning solutions score time washing and filter pressing;
2) sample measures:Pretreated water sample is placed in 900-1000 DEG C of combustion and pyrolysis stove, oxygen combustion is passed through
Pyrolysis generates hydrogen halides, absorbs hydrogen halides using electrolyte, the concentration of hydrogen halides is measured with microcoulombmeter;Electrolyte is using following
It is prepared by method:
It measures in 100-200ml acetic acid to 1000ml volumetric flasks, adds 500ml water, add 4ml nitric acid, with water constant volume, obtain
To solution a;4g gelatin is weighed, is added to while stirring in 400ml water, is expanded 3 hours in 80 DEG C of water, then at 50 DEG C -60
DEG C or so dissolving, obtain clear solution b1;It dissolves in 1.0g thymols and 0.3g thymol blues to 300-500ml methanol, obtains
To solution b2;It is stirred continuously at 50-60 DEG C or so and solution b1 is added in solution b2, be filled into 1000ml volumetric flasks
In, with water constant volume, form solution b;It pipettes in 8ml solution b to 100ml volumetric flasks, is supplemented to scale with solution b and shakes up, obtain
Electrolyte;
3) blank determination:Water sample is replaced to carry out sample pretreatment and determination step using 100ml experimental waters.
When preparing electrolyte, the amount of acetic acid and methanol can be increased according to the amount of organic halogen contained by water sample to be measured
Subtract.Under conditions of meeting detection demand, the dosage of acetic acid and methanol is reduced as far as possible.Because acetic acid and methanol have volatilization
Property and corrosivity can mitigate the harm to human body and the pollution of environment after decrement, also reduce testing cost.
Preprocess method includes that column absorption is adsorbed with oscillation, and oscillation absorption need to be used when Suspended Substance in Water Sample content is more
After measure, when suspension content is less then directly carry out column absorption.
Using individual acetic acid solution be electrolyte in existing small-hole drilling, before each measure, need to its into
Row is replaced, and is calibrated with 10 μ L chlorides standard solutions, then injects the hydrochloric acid solution of 1-10 μ L into titration cell successively, is surveyed
The amount of migration of charge in the case of fixed.After electrolyte using the present invention, the addition of gelatin enables to the electrolysis of script
Liquid forms stable disperse system solution, improves the stability of electrolyte, and Coulomb meter current potential is stablized in continuous mode, it is ensured that
It measures for a long time.Thymol and thymol blue in electrolyte mainly play indicator, can during storage and use
To judge whether electrolyte fails according to thymol and thymol blue color change, judge without being switched on measurement.
The failure of electrolyte is just can determine whether for pink when color is shoaled by aubergine.So as to avoid the waste of electrolyte, subtract simultaneously
The number that electrolyte is frequently replaced is lacked, has increased usage time, but also the result of detection is more accurate.
Preferably, the temperature of combustion and pyrolysis stove is 950 DEG C.
Further, it when testing more containing volatile halogenated in water sample, needs before foregoing pre-treatment step
Increase stripping step, stripping is carried out to the volatile halogenated in water sample using oxygen, carries out pyrolysis oven burning, small-hole drilling is surveyed
Surely can stripping organic halogen content.
Further, the activated carbon pressure filter has Filled with Quartz tubule, and water sample is placed in Filled with Quartz tubule when test
Interior, Filled with Quartz tubule is mounted under activated carbon pressure filter in square groove, and tubule needs to prevent water sample from overflowing equipped with rubber washer up and down.
Further, when being filtered using activated carbon pressure filter, the control water sample rate of filtration is 25-35 per minute
Drop.
Further, sodium nitrate storing solution of the present invention is 17g/L, and preparation method is:Weigh the sodium nitrate of 17g
It is soluble in water, 1.4mL concentrated nitric acids are added, move into constant volume in 1000mL volumetric flasks.
Further, sodium nitrate cleaning solution of the present invention is 0.85g/L, and preparation method is:Take 50mL sodium nitrate
Storing solution moves into 1000mL volumetric flasks, is diluted with water to scale.
In conclusion by adopting the above-described technical solution, the beneficial effects of the invention are as follows:
1, by changing electrolyte quota condition, electrolyte stability is improved, without being calibrated repeatedly to Coulomb meter, is contracted
Short detection time improves working efficiency;
2, it can judge whether electrolyte fails by indicator, avoid the waste of electrolyte;
3, the optimization of compounding practice parameter and electrolyte improves small-hole drilling measurement sensitivity.
Specific implementation mode
Following narration is in conjunction with specific embodiments further described the present invention, but that the present invention is not restricted to these is real
Apply example.
Embodiment 1 carries out method precision analysis using parachlorophenol standard specimen
Parachlorophenol storing solution is prepared:0.725g parachlorophenols are weighed, are settled in 1000ml volumetric flasks with water dissolution.It moves
It takes in 5ml solution to 1000ml volumetric flasks, with water constant volume, content of organic chloride is 1.0mg/L in solution at this time.
Parachlorophenol is prepared using liquid:It is 50 that parachlorophenol storing solution is diluted to content of organic chloride respectively using distilled water
μ g/L and 200 μ g/L.
First, content of organic chloride is selected to carry out the survey of adsorbable organic halogen in water using liquid for the parachlorophenol of 50 μ g/L
Determine method, comprises the steps of:
1) water sample pre-processes:
Column adsorbs:Take 100ml parachlorophenols to be poured into activated carbon pressure filter using liquid, be added sodium nitrate storing solution 2ml into
Row press filtration after press filtration is complete, is added sodium nitrate leacheate 25mL and carries out press filtration elution;
2) sample measures:Pretreated water sample is placed in 950 DEG C of combustion and pyrolysis stove, the oxygen of 700ml/min is passed through
Gas combustion and pyrolysis generates hydrogen halides, absorbs hydrogen halides using electrolyte, the concentration of hydrogen halides is measured with microcoulombmeter;Electrolyte is adopted
It prepares using the following method:
It measures in 100ml acetic acid to 1000ml volumetric flasks, adds 500ml water, add 4ml nitric acid, with water constant volume, obtain molten
Liquid a;4g gelatin is weighed, is added to while stirring in 400ml water, is expanded 3 hours in 80 DEG C of water, then on 50 DEG C of -60 DEG C of left sides
Right dissolving obtains clear solution b1;It dissolves in 1.0g thymols and 0.3g thymol blues to 300ml methanol, obtains solution b2;
It is stirred continuously at 50-60 DEG C or so and solution b1 is added in solution b2, be filled into 1000ml volumetric flasks, it is fixed with water
Hold, forms solution b;It pipettes in 8ml solution b to 100ml volumetric flasks, is supplemented to scale with solution b and shakes up, obtain electrolyte.
3) blank determination:Water sample is replaced to carry out sample pretreatment and determination step using 100ml experimental waters.
Above-mentioned 6 groups of parallel tests are carried out altogether.
It uses 100ml content of organic chloride to repeat the above steps using liquid for the parachlorophenol of 200 μ g/L, obtains following experiment
As a result:
The measurement result of 1 parachlorophenol standard specimen of table
Parallel sample is numbered | Concentration 1 (50 μ g/L) | Concentration 2 (200 μ g/L) |
1 | 48.9 | 178 |
2 | 46.1 | 184 |
3 | 44.7 | 187 |
4 | 45.4 | 176 |
5 | 42.4 | 186 |
6 | 40.8 | 216 |
Average value (μ g/L, with cl-Meter) | 44.7 | 188 |
Standard deviation S (μ g/L, with cl-Meter) | 2.85 | 14.5 |
Relative standard deviation RSD (%) | 6.37 | 7.71 |
Measured parachlorophenol precision in this method:Its precision is measured in 6.37-7.71 to the sample of various concentration
Left and right, measurement result meet the requirements, and meet detection work requirements at present.
The detection limit of 2 detection method of embodiment is analyzed
According to the Overall Steps of 1 sample analysis of embodiment, replication n (n=7) secondary blank test calculates 7 parallel surveys
Fixed standard deviation calculates this method minimum detectability by formula (1)
MDL=t (n-1,0.99) × S
In formula:
MDL --- method detection limit;
The parallel determination number of n --- sample;
T --- degree of freedom n-1, t when confidence level is 99% are distributed (unilateral side);
S --- the standard deviation of n times parallel determination.
When parallel determination number is 8, t values are 3.143.
The detection limit of 2 assay method of table is analyzed
As can be seen from Table 2, the minimum detectability in this method is 8.14 μ g/L, with cl-Meter, measurement result conform to
It asks, meets detection demand.
Certain the sewage treatment plant inflow sample analysis of embodiment 3
The assay method of adsorbable organic halogen, comprises the steps of in a kind of water:
1) water sample pre-processes:
Oscillation absorption:It takes 100ml water samples to pour into conical flask, 5ml sodium nitrate storing solutions is added, check pH value less than 2, then
50mg activated carbons are added, conical flask is placed on thermostatic control oscillator vibration support plate, vibrate 1h or more, by water sample after oscillation using work
Property charcoal pressure filter carry out press filtration, with 25ml sodium nitrate cleaning solutions score time washing and filter pressing;
2) sample measures:Pretreated water sample is placed in 950 DEG C of combustion and pyrolysis stove, the oxygen of 700ml/min is passed through
Gas combustion and pyrolysis generates hydrogen halides, absorbs hydrogen halides using electrolyte, the concentration of hydrogen halides is measured with microcoulombmeter;
Electrolyte is prepared using following methods:
It measures in 100ml acetic acid to 1000ml volumetric flasks, adds 500ml water, add 4ml nitric acid, with water constant volume, obtain molten
Liquid a;4g gelatin is weighed, is added to while stirring in 400ml water, is expanded 3 hours in 80 DEG C of water, then on 50 DEG C of -60 DEG C of left sides
Right dissolving obtains clear solution b1;It dissolves in 1.0g thymols and 0.3g thymol blues to 300ml methanol, obtains solution b2;
It is stirred continuously at 50-60 DEG C or so and solution b1 is added in solution b2, be filled into 1000ml volumetric flasks, it is fixed with water
Hold, forms solution b;It pipettes in 8ml solution b to 100ml volumetric flasks, is supplemented to scale with solution b and shakes up, obtain electrolyte.
3) blank determination:Water sample is replaced to carry out sample pretreatment and determination step using 100ml experimental waters.
Six groups of parallel tests are carried out altogether, obtain following result:
3 water determination result of table
Water sample is numbered | Measurement result (μ g/L) |
TW170724014 | 37.8 |
TW170724014 | 41.4 |
TW170724014 | 38.3 |
TW170724014 | 37.3 |
TW170724014 | 37.5 |
TW170724014 | 33.0 |
Average value (μ g/L, with cl-Meter) | 37.6 |
Standard deviation S (μ g/L, with cl-Meter) | 2.69 |
Relative standard deviation RSD (%) | 7.15 |
It is 7.15 to measure its precision to sewage treatment plant's water sample analysis, and measurement result meets the requirements, and stability is good, is met
Detection work requirements at present.
The invention is not limited in specific implementation modes above-mentioned.The present invention, which expands to, any in the present specification to be disclosed
New feature or any new combination, and disclose any new method or process the step of or any new combination.
Claims (6)
1. the assay method of adsorbable organic halogen in a kind of water, which is characterized in that comprise the steps of:
1) water sample pre-processes:
Column adsorbs:It takes 100ml water samples to be measured to pour into activated carbon pressure filter, sodium nitrate storing solution 2-5ml is added and carries out press filtration, pressure
After having filtered, sodium nitrate leacheate 25mL is added and carries out press filtration elution;
Oscillation absorption:It takes 100ml water samples to pour into conical flask, 5ml sodium nitrate storing solutions is added, check pH value and be less than 2, add
Conical flask is placed on thermostatic control oscillator vibration support plate by 40-50mg activated carbons, vibrates 1h or more, by water sample after oscillation using work
Property charcoal pressure filter carry out press filtration, with 25ml sodium nitrate cleaning solutions score time washing and filter pressing;
2) sample measures:Pretreated water sample is placed in 900 DEG C -1000 DEG C of combustion and pyrolysis stove, oxygen combustion heat is passed through
Solution generates hydrogen halides, absorbs hydrogen halides using electrolyte, the concentration of hydrogen halides is measured with microcoulombmeter;
Electrolyte is prepared using following methods:
It measures in 100-200ml acetic acid to 1000ml volumetric flasks, adds 500ml water, add 4ml nitric acid, with water constant volume, obtain molten
Liquid a;4g gelatin is weighed, is added to while stirring in 400ml water, is expanded 3 hours in 80 DEG C of water, then on 50 DEG C of -60 DEG C of left sides
Right dissolving obtains clear solution b1;It dissolves in 1.0g thymols and 0.3g thymol blues to 300-500ml methanol, obtains molten
Liquid b2;It is stirred continuously at 50-60 DEG C or so and solution b1 is added in solution b2, be filled into 1000ml volumetric flasks,
With water constant volume, solution b is formed;It pipettes in 8ml solution b to 100ml volumetric flasks, is supplemented to scale with solution b and shakes up, be electrolysed
Liquid;
3) blank determination:Water sample is replaced to carry out sample pretreatment and determination step using 100ml experimental waters.
2. the assay method of adsorbable organic halogen in a kind of water according to claim 1, it is characterised in that:The burning
The temperature of pyrolysis oven is 950 DEG C.
3. the assay method of adsorbable organic halogen in a kind of water according to claim 2, it is characterised in that:The activity
Charcoal pressure filter has Filled with Quartz tubule, and when test in water sample merging Filled with Quartz tubule, Filled with Quartz tubule is mounted on activity
Under charcoal pressure filter in square groove, tubule needs to prevent water sample from overflowing equipped with rubber washer up and down.
4. the assay method of adsorbable organic halogen in a kind of water according to claim 3, it is characterised in that:Using work
Property charcoal pressure filter when being filtered, the control water sample rate of filtration is 25-35 drops per minute.
5. the assay method of adsorbable organic halogen in a kind of water according to claim 1, it is characterised in that:The nitric acid
The preparation method of sodium storing solution be weigh 17g sodium nitrate it is soluble in water, be added 1.4mL concentrated nitric acids, move into 1000mL volumetric flasks
Middle constant volume.
6. the assay method of adsorbable organic halogen in a kind of water according to claim 5, it is characterised in that:The nitric acid
The preparation method of sodium cleaning solution is to take 50mL sodium nitrate storing solutions, moves into 1000mL volumetric flasks, is diluted with water to scale.
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CN112505204A (en) * | 2020-12-16 | 2021-03-16 | 中煤浙江检测技术有限公司 | Organic halogen extracting solution and method for detecting adsorbable organic halogen in soil |
CN113376307A (en) * | 2021-06-23 | 2021-09-10 | 国家纺织服装产品质量监督检验中心(浙江桐乡) | Method for measuring AOX content in textile by adopting oscillation extraction and ion chromatography |
CN113848244A (en) * | 2021-09-17 | 2021-12-28 | 浙江环境监测工程有限公司 | Microcoulomb method for measuring adsorbable organic halogen in seawater |
CN115343401A (en) * | 2022-07-11 | 2022-11-15 | 浙江格临检测股份有限公司 | Method for measuring adsorbable organic halogen AOX in soil and sediment |
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN112505204A (en) * | 2020-12-16 | 2021-03-16 | 中煤浙江检测技术有限公司 | Organic halogen extracting solution and method for detecting adsorbable organic halogen in soil |
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