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HJ 825-2017: Water quality-Determination of volatile phenols - Flow injection analysis(FIA) and 4-AAP spectrophotometric method
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Water quality-Determination of volatile phenols - Flow injection analysis(FIA) and 4-AAP spectrophotometric method
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HJ 825-2017
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Basic data | Standard ID | HJ 825-2017 (HJ825-2017) | | Description (Translated English) | Water quality-Determination of volatile phenols - Flow injection analysis(FIA) and 4-AAP spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 11,143 | | Date of Issue | 4/25/2017 | | Date of Implementation | 6/1/2017 | | Regulation (derived from) | Ministry of Environment Protection Announcement 2017 [16] | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 825-2017: Water quality-Determination of volatile phenols - Flow injection analysis(FIA) and 4-AAP spectrophotometric method
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Water quality-Determination of volatile phenols-Flow
Injection analysis (FIA) and 4-AAP spectrophotometric method
National Environmental Protection Standard of the People 's Republic of China
Determination of Volatile Phenol in Water Quality
Flow injection of 4-amino antipyrine
2017-03-30 released
2017-05-01 Implementation
Ministry of Environmental Protection released
Directory
Preface .ii
1 Scope of application
2 normative reference documents
3 terms and definitions
4 Principle of the method
5 interference and elimination
6 reagents and materials
7 instruments and equipment
8 samples
9 Analysis steps
10 results are calculated and expressed
11 Precision and Accuracy
12 Quality assurance and quality control
13 Waste treatment .7
14 Precautions .7
Foreword
In order to implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on the Prevention and Control of Water Pollution,
Protect the human health, regulate the determination of volatile phenol in water, the development of this standard.
This standard specifies the determination of volatile water in surface water, groundwater, domestic sewage and industrial wastewater by injection of 4-amino
Antipyrine spectrophotometric method.
This standard is the first release.
This standard is organized by the Environmental Monitoring Department of the Ministry of Environmental Protection, the Secretary for Science and Technology Standards.
The main drafting unit of this standard. Jiangsu Province Environmental Monitoring Center.
The standard verification unit. Beijing Environmental Protection Monitoring Center, Wuxi City Environmental Monitoring Center Station, Huai'an City Environmental Monitoring
Central station, Yangzhou City Environmental Monitoring Center Station, Changshu City Environmental Monitoring Station and Jiangsu Province Environmental Monitoring Center.
The environmental protection department of this standard approved on March 30,.2017.
This standard has been implemented since May 1,.2017.
This standard is explained by the Ministry of Environmental Protection.
Determination of Volatile Phenol in Water by Flow Injection - 4 - Aminoantipyrine Spectrophotometric Method
Warning. Phenols are highly toxic substances, the operation should be required to wear protective equipment, to avoid contact with skin, after testing
Residual residue should be properly handled safely.
1 Scope of application
This standard specifies the flow injection of 4-aminoantipyrine spectrophotometric method for the determination of volatile phenols in water.
This standard is applicable to the determination of volatile phenol in surface water, groundwater, domestic sewage and industrial waste water.
When the detection range of 10 mm, the standard method of detection limit of 0.002 mg/L, the determination range of 0.008 mg/L ~ 0.200 mg/L.
2 normative reference documents
The contents of this standard refer to the following documents or their terms. Those who do not specify the date of the reference file, the effective version of the appropriate
For this standard.
Determination of Volatile Phenol in Water Quality 4 - Amino Antipyrine Spectrophotometric Method
Technical specification for surface water and wastewater monitoring
Technical specification for groundwater environmental monitoring
3 terms and definitions
The following terms and definitions apply to this standard.
Volatile phenols
With the steam distillation and can react with 4-aminoantipyrine to produce colored compounds of volatile phenolic compounds, knot
Fruit to phenol.
4 principle of the method
4.1 Flow injection device works
In a closed line, a volume of the sample into the continuous flow of the carrier liquid, the sample and reagents in the chemical reaction mode
The blocks are mixed and reacted in a specific order and proportion, and the reaction is carried out in a non-complete reaction condition into the flow detection cell for photometric inspection
Measurement.
4.2 Principles of chemical reactions
Under acidic conditions, the sample was released from the column by 160 ° C ± 2 ° C. The distorted phenolic compounds are weak
Alkaline medium, in the presence of potassium ferricyanide, and 4-amino antipyrine reaction to produce orange-yellow antipyrine dyes, in
Absorbance was measured at 500 nm wavelength. Specific work flow shown in Figure 1.
1. Peristaltic pump; Heating pool (160 ℃); Phase separation device; Condenser; Injection valve; Reaction ring; Detection pool 10mm,
100 nm; Phosphoric acid solution (6.18); Potassium ferricyanide buffer (6.21); R3.4-aminoantipyrine solution (6.20); Contained
Liquid (experimental water); Ice water (0-4 ℃); Sample; Waste liquid
Figure 1 flow injection-4-amino antipyrine spectrophotometric determination of volatile phenol reference work flow chart
5 interference and elimination
The main disturbances of this method are oxidants, oils, sulfides, organic or inorganic reducing substances and anilines.
5.1 Elimination of oxidizing agents such as free chlorine
The sample drops on the starch-potassium iodide test paper and appears blue, indicating the presence of an oxidizing agent, which can be added to excess iron sulfate to remove it.
5.2 Elimination of sulfide
When the sample has a black precipitate, it is desirable to take a drop of sample on the lead acetate test paper, if the test paper turns black, indicating sulfur
The presence of chemicals. At this point the sample continued to add phosphoric acid acidification, set the ventilation cabinet to stir aeration until the formation of hydrogen sulfide completely Yi
Out
5.3 elimination of organic or inorganic reducing substances such as formaldehyde and sulfite
Can be divided into appropriate sample in the separatory funnel, add sulfuric acid solution to make acidic, were added 50 ml, 30 ml, 30 ml
Ether to extract phenol, combined ether layer in another separatory funnel, by adding 4 ml, 3 ml, 3 ml of sodium hydroxide solution into
Line back extraction, so that phenols into sodium hydroxide solution. Combined with alkali extract, into the beaker, set the water bath to heat, in addition to
To remove the residual ether, and then use the experimental water to dilute the alkali extract to the original volume of water samples.
At the same time should be experimental water for blank test.
5.4 Elimination of oil
After the sample was left to separate the oil slick, follow the steps in 5.3.
5.5 Elimination of aniline
Aniline can be detected with 4-aminoantipyrine color reaction to interfere with the determination of phenol, generally in the acidic (pH < 0.5)
, Which can be separated by pre-distillation.
6 reagents and materials
Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The experimental water is freshly prepared
Ionized water or distilled water. In addition to the standard solution, other solutions and experimental water are treated with helium (6.28) or ultrasonic (7.3) degassed.
6.1 Phenol-free water. Prepared according to the method specified in HJ 503.
6.2 Purified phenol (C6H5OH). Prepared according to the procedure specified in HJ 503.
6.3 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
6.4 Phosphoric acid. ρ (H3PO4) = 1.69 g/ml, excellent grade pure.
6.5 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.6 Sodium hydroxide (NaOH).
6.7 boric acid (H3BO3).
6.8 Potassium ferricyanide [K3Fe (CN) 6].
6.9 Potassium chloride (KCl).
6.10 Potassium Bromate (KBrO3).
6.11 Potassium Bromide (KBr).
6.12 Potassium iodate (KIO3).
6.13 Sodium thiosulfate (Na2S2O3).
6.14 Sodium carbonate (Na2CO3).
6.15 Potassium iodide (KI).
6.16 4-aminoantipyrine (C11H13N3O).
6.17 sulfuric acid solution. 1 5.
The volume ratio of sulfuric acid (6.3) to water is 1. 5.
6.18 Phosphoric acid solution. 1 10.
The volume ratio of phosphoric acid (6.4) to water is 1.10.
6.19 Sodium hydroxide solution. c (NaOH) = 1 mol/L.
Weigh 20 g of sodium hydroxide (6.6) in the appropriate amount of water, dissolved and moved to 500 ml volumetric flask, the water volume to the standard
Line, mix well.
6.20 4-Amino Antipyrine solution. ρ = 0.64 g/L.
Weigh 0.32 g of 4-aminoantipyrine (6.16) in an appropriate amount of water, diluted with water to 500 ml and mixed. Purification side
Method, save time see HJ 503. When the sample size is small, it may be appropriate.
6.21 potassium ferricyanide buffer. pH = 10.3.
Weigh 2.0 g of potassium ferricyanide (6.8), 3.1 g of boric acid (6.7) and 3.75 g of potassium chloride (6.9) in an appropriate amount of water,
Dissolved and moved to 1000 ml volumetric flask, add 47 ml sodium hydroxide solution (6.19), water volume to the mark, mix.
Store in a refrigerator for one week; see HJ 503. When the sample size is small, it can be configured in small proportion.
6.22 potassium bromate - potassium bromide solution. c = 0.100 mol/L.
Weigh 2.784 g of potassium bromate (6.10) in the appropriate amount of water, then add 10 g of potassium bromide (6.11), dissolved and moved to 1000
Ml capacity bottle, the water volume to the marking, mixing.
6.23 potassium iodate standard solution. c = 0.0250 mol/L.
Weigh 0.8917 g Potassium iodate (6.12) dried in advance at 180 ° C in an appropriate amount of water, dissolved and moved to 1000 ml
Capacity bottle, the water volume to the marking, mixing.
6.24 sodium thiosulfate standard solution. c≈0.0125 mol/L.
Weigh 3.1 g of sodium thiosulfate (6.13) in boiling water, add 0.2 g of sodium carbonate (6.14), after dissolving
Moved to 1000 ml volumetric flask, water volume to the mark, mix. The solution was stored in a brown bottle. Before use with potassium iodate
Standard solution (6.23) calibration.
Calibration method. 250 ml iodine bottle by adding 20.00 ml potassium iodate standard solution (6.23), 80 ml of experimental water,
1 g potassium iodide (6.15), plus 5 ml sulfuric acid solution (6.17), stopper, gently shake. Set the dark place for 5 min, with sulfur
Sodium sulphate standard solution (6.24) titrated to light yellow, add 1 ml of starch solution (6.27), continue to titrate to blue fade
To date, record the amount of sodium thiosulfate standard solution.
The concentration of sodium thiosulfate standard solution is calculated according to formula (1).
Where. c - sodium thiosulfate solution concentration, mol/L;
1 V - titration of potassium iodate standard solution when the amount of sodium thiosulfate solution, ml;
2 V - Removal of potassium iodate standard solution volume, ml;
0.0250 - potassium iodate standard solution concentration, mol/L.
6.25 Phenol Standard stock solution. ≈ 500 mg/L.
Weigh 0.500 g refined phenol (6.2) dissolved in the amount of water, moved to 1000 ml volumetric flask, the volume of water to the standard line,
Mix well. Proposed before use. The refrigerator can be kept for a month. Or purchase a certified standard solution.
Set the standard solution of phenol calibration method. measure 10.00 ml of phenol stock solution (6.25) in 250 ml iodine bottle,
Diluted with water to 100 ml, add 10.0 ml of potassium bromate - potassium bromide solution (6.22), immediately add 5 ml of hydrochloric acid (6.5), cover
Good cork, gently shake, place the dark 10 min. Add 1 g potassium iodide (6.15), sealed, and then gently shake, place
Dark 5 min. Was titrated to pale yellow with sodium thiosulfate standard solution (6.24), 1 ml of starch solution (6.27) was added,
Continued titration to blue just faded, record the amount. At the same time to phenol-free phenol instead of phenol stock solution to do blank test, record sulfur thio
Sodium salt standard solution dosage.
The concentration of the phenol stock solution is calculated according to formula (2).
Where. - the concentration of phenol standard stock solution, mg/ml;
0 V - Standard volume of sodium thiosulfate consumed in blank test, ml;
1 V - the amount of sodium thiosulfate standard solution consumed when titrating the phenol stock solution, ml;
V - Phenol stock volume, ml;
C - sodium thiosulfate standard solution concentration, mol/L;
15.68 - 1/6 molar mass of C6H5OH, g/mol.
6.26 Phenol Standard Use. 10.00 mg/L.
Remove the appropriate amount of phenol standard stock solution (6.25), step by step dilution obtained.
6.27 Starch solution.
Weigh 1 g of soluble starch, with a small amount of water into a paste, add boiling water to 100 ml, after cooling, set the refrigerator to save.
6.28 Helium. purity ≥99.99%.
7 instruments and equipment
7.1 Flow injection device. including autosampler, chemical reaction module (pretreatment channel, injection pump, reaction channel and circulation
Detection pool) peristaltic pump, data processing system.
7.2 Analysis of the balance. accuracy of 0.1 mg.
7.3 Ultrasonic instrument. Frequency 40 kHz.
7.4 General laboratory equipment and equipment commonly used.
8 samples
Samples were collected according to the relevant regulations of HJ/T 91 and HJ/T 164. Application of glass vials to collect water samples.
After the sample was collected, the solution was adjusted to pH 2 with phosphoric acid (6.4). Or with 0.01 g ~ 0.02 g of ascorbic acid to remove residual chlorine, with hydrogen
Sodium oxide (6.6) was fixed so that the sample had a pH ≥ 12. Typically, 0.5 g of solid sodium hydroxide (6.6) is added to each liter of water,
When the water acidity is high, the appropriate increase in solid sodium hydroxide (6.6) dosage. Samples were stored at 4 ° C for 24 h
Internal determination.
Note. The pretreatment operation is carried out as specified in HJ 503 when analyzed using a method module without on-line distillation.
9 Analysis steps
9.1 Commissioning and calibration of instruments
Install the analysis system, commissioning the instrument and setting the operating parameters according to the instrument manual. According to the order of the instrument after the boot,
Use the test water instead of all reagents to check the integrity of the entire flow path and the smooth flow of liquid. After the baseline is stable
(About 20 min), the system began to pump reagents, to be stable again after the baseline, according to 9.2 ~ 9.4 operation.
9.2 Calibration
9.2.1 Preparation of standard series
(6.26) in a set of volumetric flask, diluted with water to the mark and mix, the system
The concentration of volatile phenol (in terms of phenol) was 0.000 mg/L, 0.010 mg/L,
0.025 mg/L, 0.050 mg/L, 0.100 mg/L, 0.200 mg/L.
9.2.2 Drawing of calibration curves
The amount of standard solution (9.2.1) was placed in the sample cup, and the sample was taken from low concentration to high concentration
And the signal values (peak area) of different concentrations of volatile phenol were obtained. To the signal value (peak area) as the ordinate, the corresponding
The concentration of volatile phenol (in terms of phenol, mg/L) as the abscissa, draw the calibration curve.
9.3 Determination
According to the same measurement conditions with the drawing calibration curve, measure the amount of the sample to be measured and record the signal value (peak area).
If the concentration is higher than the highest point of the standard curve, dilute the sample.
9.4 blank test
Replace the sample with 10 ml of water and perform the same procedure as the sample analysis to record the signal value (peak area).
10 results are calculated and expressed
10.1 Result calculation
The concentration of volatile phenol in the sample (in terms of phenol, mg/L) was calculated according to equation (3)
Where. - mass concentration of volatile phenol in the sample, mg/L;
Y - measured signal value (peak area);
A - intercept of the calibration curve method;
B - the slope of the calibration curve method;
F - dilution factor.
10.2 results are shown
When the determination result is less than 1.00 mg/L, after the decimal point is retained, the result is greater than or equal to 1.00 mg/L.
Leaving three valid digits.
11 precision and accuracy
11.1 precision
Six laboratories conducted a unified sample of volatile phenol concentrations of 0.020 mg/L, 0.100 mg/L, 0.180 mg/L
The relative standard deviations in the laboratory were 2.7% ~ 5.5%, 0.9% ~ 1.7%, 0.6% ~ 1.1%, respectively.
The standard deviation was 4.7%, 1.8%, 0.9%; the repeatability limit was 0.003 mg/L, 0.003 mg/L, 0.004 mg/L;
The limit was 0.003 mg/L, 0.006 mg/L, 0.006 mg/L.
11.2 Accuracy
The concentration of volatile phenol was (41.4 ± 3.0) μg/L, (49.8 ± 4.5) μg/L, (0.203 ± 0.012)
Mg/L, the relative error was -6.0% -1.3%, 8.1% ~ 4.6%, 2.0% ~
-2.7%; the relative error was (-3.7 ± 6.7)%, (-1.7 ± 18.0)%, (- 0.9 ± 5.0)%.
The concentration of volatile phenol in the laboratory was 0 mg/L ~ 0.003 mg/L, 0.017 mg/L ~ 0.187 mg/L, 0.044
Mg/L ~ 0.102 mg/L surface water and waste water were measured by spiked assimilation, the recoveries were 92.3% ~ 106%
(99.5 ± 11.4)%, (96.6 ± 16.4)%, respectively, and the recoveries were (99.5%
(96.1 ± 9.0)%.
12 quality assurance and quality control
12.1 blank test
Each laboratory should be at least two laboratory blanks, the blank value shall not exceed the method detection limit. Otherwise it should identify the cause,
Re-analysis until qualified after the determination of the sample.
12.2 Calibration validity check
Each batch of samples must be drawn with a calibration curve, and the correlation coefficient of the calibration curve is γ ≥ 0.995.
Each test of 10 samples need to use a calibration curve of the intermediate concentration calibration solution for calibration verification, the determination of the results and
The relative deviation of the nearest calibration curve should be ≤ ± 10%, otherwise the calibration curve should be redrawn.
12.3 Full program blank
At least one full program blank is set for each batch, and the blank value must not exceed the lower limit of the method. Otherwise it should identify the cause,
Re-analysis until qualified after the determination of the sample.
12.4 precision control
Each batch of samples should be measured at least 10% of the parallel sample, the number of samples less than 10, should be measured at least a parallel double
The relative deviation of the two parallel measurements should be ≤ ± 20%.
12.5 Accuracy control
Each batch of samples should be measured at least 10% of the spiked sample, the number of samples less than 10, should be measured at least one plus standard
Product, spike recovery rate should be between 70% to 120%.
If necessary, each batch of samples at least a certified reference material or laboratory self-prepared quality control samples, certified standards
Quality test results should be given in the uncertainty of the range, the laboratory self-prepared quality control test results should be controlled at 90% ~
110%. Laboratory self-prepared quality control should pay attention to the state and the standard material comparison.
13 Waste treatment
Analysis of the waste generated during the process should be centralized recovery, qualified to deal with the disposal of qualified professional waste.
14 Precautions
14.1 4-amino-antipyrine reagents to be purified when the purity is low, purification methods see HJ 503.4-amino antipyrine reagent Kaifeng
Should be stored in the dryer.
14.2 The condenser supply water should be kept at about 4 ° C. Condenser condensate replacement requirements see the instrument manual.
14.3 If there is a sparkling peak of continuous bubbles during the analysis, it is confirmed that there are small bubbles in the non-flowing pool,
For a bimodal or shoulder-shaped peak, the membrane of the phase separator should be replaced.
14.4 To extend the service life of the separation membrane, only after the heater temperature reaches the set temperature, the reagent or phenol-free water
Through a phase separator. After the analysis, with phenol-free water rinse 0.5h, in addition to all the pipes outside the condenser are pumped into the air, dry
Dry separation membrane 0.5h to 1h side to stop and shut down.
14.5 potassium ferricyanide solution of the injection tube do not touch the bottom of the bottle, so as not to absorb impurities in the solution.
14.6 condensate tube easy bacteria, add the right amount of 1% sodium hypochlorite solution to prevent bacteria, such as recycling, should be replaced weekly.
14.7 Specimens with significant particles are sonicated by sonication.
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