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HJ 823-2017: Water quality-Determination of cyanide - Flow injection analysis(FIA) and spectrophotometric method
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Water quality-Determination of cyanide - Flow injection analysis(FIA) and spectrophotometric method
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HJ 823-2017
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Basic data | Standard ID | HJ 823-2017 (HJ823-2017) | | Description (Translated English) | Water quality-Determination of cyanide - Flow injection analysis(FIA) and spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 12,133 | | Date of Issue | 3/30/2017 | | Date of Implementation | 5/1/2017 | | Regulation (derived from) | Ministry of Environment Protection Announcement 2017 [16] | | Issuing agency(ies) | Ministry of Ecology and Environment | HJ 823-2017: Water quality-Determination of cyanide - Flow injection analysis(FIA) and spectrophotometric method
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Water quality-Determination of cyanide - Flow injection analysis (FIA) and spectrophotometric method
National Environmental Protection Standard of the People 's Republic of China
Determination of cyanide in water
Flow injection - spectrophotometric method
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
14 Precautions .8
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,
Protection of human health, regulate the determination of cyanide in water method, the development of this standard.
This standard specifies the flow injection-spectrophotometric method for the determination of cyanide in surface water, groundwater, domestic sewage and industrial waste water.
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 Xuzhou City Environmental Monitoring Center Station.
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.
Water quality - Determination of cyanide - Flow injection - spectrophotometric method
Warning. cyanide and pyridine are highly toxic substances, the operation should be required to wear protective equipment, to avoid contact with the skin
And clothes, after the detection of residue residue should be properly safe handling.
1 Scope of application
This standard specifies the flow injection-spectrophotometric method for the determination of cyanide in water.
This standard is applicable to the determination of cyanide in surface water, groundwater, domestic sewage and industrial waste water.
When the optical path length was 10 mm, the detection limit of cyanide in water was 0.001 mg/L by isonicotinic acid-barbituric acid method.
And the detection limit of cyanide in water was 0.002 mg/L, and the detection limit was 0.002 mg/L,
The assay range is 0.008 mg/L 0.50 mg/L.
2 normative reference documents
The contents of this standard refer to the following or their terms. For undated references, the valid version applies to this standard.
Determination of water quality cyanide and its 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.
Total cyanide total cyanide
In the presence of phosphoric acid and EDTA in the presence of phosphoric acid and EDTA, the cyanide of cyanide is heated and distilled to form cyanide, including all simple
Cyanide (mostly alkali metal and alkaline earth metal cyanide, ammonium cyanide) and the vast majority of complex cyanide (zinc cyanide complex
Iron cyanide complex, nickel cyanide complex, copper cyanide complex, etc.), excluding cobalt cyanide complex.
3.2 easy to release cyanide easily liberatable cyanide
In the presence of zinc nitrate in the presence of zinc nitrate in the presence of zinc nitrate, the cyanide of cyanide is heated and distilled to form cyanide, including all simple cyanide
(Mostly cyanide of alkali and alkaline earth metals) and zinc cyanide complexes, excluding ferricyanide complexes, ferrocyanide complexes, copper
Cyanide complex, nickel cyanide complex, cobalt cyanide complex.
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 are subjected to photometric detection under a non-complete reaction condition into the flow detection cell.
4.2 Principles of chemical reactions
4.2.1 isonicotinic acid-barbituric acid method
Under acidic conditions, the samples were hydrolyzed by high temperature and high pressure at 140 ℃ and UV digestion. The released hydrogen cyanide gas was oxidized by hydrogen
Sodium solution absorption. The cyanide in the absorbing solution reacts with chloramine T to form cyanogen chloride, which is then hydrolyzed with isonicotinic acid to produce
And then with barbituric acid to produce blue-violet compounds, measured at 600 nm wavelength absorbance. Specific workflow
See Figure 1.
4.2.2 pyridine-barbituric acid method
Under acidic conditions, the samples were hydrolyzed by high temperature and high pressure at 140 ℃ and UV digestion. The released hydrogen cyanide gas was oxidized by hydrogen
Sodium solution absorption. Under neutral conditions, the cyanide in the absorbing solution reacts with chloramine T to form cyanogen chloride, which reacts with pyridine
The formation of glutaraldehyde, and finally with barbituric acid to produce condensed reddish purple compounds, measured at 570 nm wavelength absorbance. With
Body work flow shown in Figure 1.
1. Peristaltic pump; Heating pool (140 ℃); UV digestion device; Diffusion pool; Injection valve; Reaction ring; Heating tank (60 ℃)
8. Detection cell 10mm, 600nm or 570nm; R1 Phosphoric acid solution (6.17); Sodium hydroxide solution (6.19); R3. Phosphate buffer
Liquid (6.24); R4 Chloramine-T solution (6.25 or 6.26); R5. Pyridine-barbituric acid solution (6.27) or isonicotinic acid-barbituric acid solution (6.28)
C. Carrier solution (sodium hydroxide solution, 6.19); Sample; Waste liquid
Figure 1 flow injection - spectrophotometric determination of cyanide reference work flow chart
5 interference and elimination
The presence of active chlorine and other oxidizing substances in the sample interference determination, can be added before the distillation of sodium sulfite (Na2SO3) solution
In addition to interference; the presence of nitrite ion interference in the sample, can be used before the distillation of sulfamic acid (NH2SO3H) to eliminate interference;
Sulfide interference is present in the sample, and carbonate (CdCO3) or lead carbonate (PbCO3) solid powder can be added before distillation
Eliminate interference; Thiocyanate produces less than 1% of positive interference.
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 (6.35) or ultrasonic (7.3) degassed.
Unless otherwise stated, analytical analytical reagents conforming to national standards are used in the analysis, and the test water is a newly prepared deionized
Water or distilled water. Experimental reagents and water are required to use helium or ultrasonic degassing, the specific method. the use of 140KPa helium
Over the helium air tube 1min degassing, or the use of ultrasonic oscillation 15min ~ 30min degassing.
6.1 Phosphoric acid. ρ (H3PO4) = 1.69 g/ml.
6.2 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.3 Sodium hydroxide (NaOH). excellent grade pure.
6.4 Potassium hydroxide (KOH). excellent grade pure.
6.5 Sodium chloride (NaCl). Reference level.
Dry at 600 ℃ for 1h, cooler in the dryer, stand-by.
6.6 Silver nitrate (AgNO3).
6.7 Potassium cyanide (KCN).
6.8 tartaric acid (C4H6O6).
6.9 Zinc nitrate [Zn (NO3) 2 · 6H2O].
6.10 anhydrous potassium dihydrogen phosphate (KH2PO4).
6.11 Chloramine-T [C7H7ClNNaO2S · 3H2O].
6.12 pyridine (C5H5N).
6.13 try silver spirit (p-dimethylaminobenzylidene rhodanine).
6.14 Potassium chromate (K2CrO4).
6.15 barbituric acid (C4H4N2O3).
6.16 isonicotinic acid (C6H5 NO2).
6.17 Phosphoric acid solution. c (H3PO4) = 0.67 mol/L.
In about 700 ml of water, add 45 ml of phosphoric acid (6.1) slowly, dilute to 1000 ml with water and mix well.
6.18 Sodium hydroxide solution. ρ = 20 g/L.
Weigh 2.0 g of sodium hydroxide (6.3) dissolved in the amount of water, dissolved and added volume to 100 ml. The solution was transferred to plastic
Save the container.
6.19 Sodium hydroxide solution. c = 0.025 mol/L.
Weigh 1.0 g sodium hydroxide (6.3) dissolved in the amount of water, dissolved and moved to 1000 ml volumetric flask, add water to the marking,
Mix well. The solution was transferred to a plastic container for storage.
6.20 tartaric acid solution. ρ = 150 g/L.
Weigh 150 g of tartaric acid (6.8) in the appropriate amount of water, diluted with water to 1000 ml, mix well.
6.21 zinc nitrate solution. ρ = 100 g/L.
Weigh 100 g of zinc nitrate (6.9) in the appropriate amount of water, diluted with water to 1000 ml, mix.
6.22 Sodium hydroxide solution. ρ = 10 g/L.
Weigh 10 g of sodium hydroxide (6.3) in the appropriate amount of water, diluted with water to 1000 ml, mix.
6.23 sodium hydroxide solution. ρ = 40 g/L.
Weigh 40 g of sodium hydroxide (6.3) in the appropriate amount of water, diluted with water to 1000 ml, mix.
Note. 6.20 ~ 6.23 for the determination of easy release of cyanide pretreatment operation used.
6.24 Phosphate buffer. pH = 4.24.
Weigh 95.0 g of anhydrous potassium dihydrogen phosphate (6.10) dissolved in 800 ml of water (magnetic stirring about 2 h can be completely dissolved),
Dissolved after the addition of water to 1L. If the formation of precipitation, can be filtered or abandoned without. The solution can be stored for 1 month.
6.25 Chloramine-T solution I. ρ = 6 g/L.
Weigh 3.0 g of chloramine-T (6.11) in 500 ml of water and mix well. Pro when the current allocation.
Note. Chloramine-T easily oxidized, after opening should be stored in the dryer as much as possible. This reagent Kaifeng six months later, after verification and then use.
6.26 Chloramine-T solution II. ρ = 2 g/L.
Weigh 1.0 g of chloramine-T (6.11) in 500 ml of water and mix well. Pro when the current allocation.
6.27 pyridine-barbituric acid solution.
Weigh 7.5 g of barbituric acid (6.15) in a 500 ml beaker, add 50 ml of water, add 37.5 ml
Pyridine (6.12), followed by 7.5 ml of hydrochloric acid (6.2) and 412 ml of water until barbituric acid was completely dissolved. Store in brown
Bottle, with the time is now with. Stored in the refrigerator can be stable for a week.
Note. barbituric acid reagent opened a year after the proposed, no longer recommended.
6.28 isonicotinic acid - barbituric acid solution.
Add 12 g of sodium hydroxide (6.3) to 700 ml of water and add 12 g of barbituric acid (6.15) and 12 g
Isonicotinic acid (6.16), dissolved in water after the volume to 1000 ml. When used with the time.
6.29 sodium chloride standard solution. c = 0.0100 mol/L.
Weigh 0.2922 g sodium chloride (6.5) dissolved in the amount of water, dissolved and moved to 500 ml volumetric flask, add water to the volume
Marking, mixing.
6.30 Silver nitrate standard solution. c = 0.0100 mol/L.
Weigh 0.850 g silver nitrate (6.6) dissolved in water, dissolved after adding water to 500 ml. The solution was stored in a brown bottle
, Before use with sodium chloride standard solution (6.29) calibration.
Calibration method. measure 10.00 ml sodium chloride standard solution (6.29) in 150 ml Erlenmeyer flask, add 50 ml of water.
Add 3 to 5 drops of potassium chromate indicator (6.34) to the conical flask and add the nitric acid to be calibrated from the burette
Silver standard solution (6.30) until the solution changed from yellow to shallow brick, the amount of silver nitrate standard solution (V1) was recorded.
At the same time, with 10.00 ml of water instead of sodium chloride standard solution to do blank test.
The concentration of silver nitrate standard solution is calculated according to formula (1).
1 10.00
VV
(1)
Where. c - concentration of silver nitrate standard solution, mol/L;
1 c - sodium chloride standard solution concentration mol/L;
1 V - titration of sodium chloride standard solution, the amount of silver nitrate standard solution, ml;
0 V - blank titration, the amount of silver nitrate standard solution, ml.
6.31 cyanide standard stock solution. 1000 mg/L (in CN-).
Weigh 1.0 g of potassium hydroxide (6.4) dissolved in about 400 ml of water, then add 1.252 g potassium cyanide (6.7), completely
Dissolved after the addition of water to 500 ml, mix. The solution must be calibrated weekly. Or purchase a certified reference material.
Preserved cyanide standard stock solution Calibration method. measure 10.00 ml cyanide standard stock solution (6.31) in a conical flask
, Add 50 ml of water and 1 ml of sodium hydroxide solution (6.18), add 0.2 ml test silver Ling indicator solution (6.33), with nitric acid
Silver standard solution (6.30) titration, the solution from yellow to orange until the red, record the amount of silver nitrate standard solution (V1).
At the same time, with 10 ml of water instead of cyanide standard stock solution as a blank test, record the amount of silver nitrate standard solution (V0).
The concentration of cyanide standard stock solution is calculated according to formula (2).
1 0 106
52 04
C VV.
(2)
Where. - concentration of cyanide standard stock solution, mg/L;
C - silver nitrate standard solution concentration, mol/L;
0 V - titration of blank solution, silver nitrate standard solution dosage, ml;
1 V - titration of potassium cyanide standard stock solution, silver nitrate standard solution dosage, ml;
52.04 - molar mass of cyanide ion (2CN-), g/mol;
10.00 - the volume of potassium cyanide standard stock solution, ml.
6.32 cyanide standard use of the liquid. 500μg/L (in CN-dollars).
The appropriate amount of cyanide standard stock solution (6.31) was prepared by dilution with sodium hydroxide solution (6.19).
6.33 try silver Ling indicator liquid.
Weigh 0.02 g of tryin (6.13) in 100 ml of acetone. The solution is stored in a brown bottle and stored in a dark place
Save for 1 month.
6.34 potassium chromate indicator solution.
Weigh 10.0g of potassium chromate (6.14) in a small amount of water, add a few drops of silver nitrate solution (6.30) to produce orange-red
After settling, leave overnight, filter, dilute to 100 ml with water.
6.35 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 flow
Detection pool, the optical path is generally 10 mm, through the pipeline diameter of about 1.5 mm), peristaltic pump, data processing system.
7.2 Analysis of the balance. accuracy of 0.1 mg.
7.3 Ultrasonic instrument. frequency 40kHz.
7.4 General laboratory equipment and equipment commonly used.
8 samples
The collection of water samples is carried out in accordance with the relevant provisions of HJ/T 91 and HJ/T 164. Samples should be collected in a closed plastic vial
in. After the sample collection, should immediately add sodium hydroxide (6.3) fixed, usually every liter of water plus 0.5g solid sodium hydroxide.
When the water acidity is high, should add more solid sodium hydroxide, so that the sample pH between 12 to 12.5. Collect samples as soon as possible
set. Otherwise, the sample should be stored below 4 ° C and measured within 24 h after sampling.
Determination of total cyanide and easy release of cyanide, using the method without the use of online distillation method for analysis, the pretreatment operation
Respectively, in accordance with the provisions of HJ 484.
Note. samples with obvious particles were sonicated by sonication.
9 Analysis steps
9.1 Commissioning of the instrument
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,
Replace all reagents with pure water, check the integrity of the entire flow path and the smooth flow of liquid. After the baseline is stable (about
30 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
(1) isonicotinic acid - barbituric acid method
In a group of volumetric flask were measured in appropriate amount of cyanide standard use of liquid (6.32), with sodium hydroxide solution (6.19) dilute
And the concentration of cyanide (in CN-terms) were 0.00 μg/L, and the concentration of cyanide was in the range of 0.00 μg/L,
2.00 μg/L, 5.00 μg/L, 10.0 μg/L, 50.0 μg/L, 100 μg/L.
(2) pyridine-barbituric acid method
(6.32) in a set of volumetric flask, with sodium hydroxide solution (6.19), the amount of cyanide solution,
Diluted to the mark and mix, the preparation of six concentrations of the standard series, cyanide mass concentration (in CN-meter) were. 0.00
Μg/L, 5.00 μg/L, 50.0 μg/L, 125 μg/L, 250 μg/L, 500 μg/L.
9.2.2 Drawing of calibration curves
The amount of standard solution (9.2.1) was placed in the sample cup, and the samples were sampled from low concentration to high concentration.
The signal values (peak area) of cyanide at different concentrations were obtained. To the signal value (peak area) as the ordinate, the corresponding cyanide material
The concentration curve (in CN-meter, g/L) is the abscissa, and the calibration curve is drawn.
9.3 Determination
According to the same measurement conditions with the drawing calibration curve, measure the amount of sample to be measured, record the signal value (peak
product). 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 cyanide in the sample (in CN-meter, mg/L) is calculated according to formula (3).
10-03
f
Ya (3)
Where. - mass concentration of sulfide in 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 mg/L, the three digits after the decimal point are retained. When the result is greater than or equal to 1 mg/L, three
effective number.
11 precision and accuracy
11.1 precision
Isonicotinic acid-barbituric acid method. the concentration of cyanide in laboratory was 0.010 mg/L, 0.050 mg/L, 0.090 mg/L
The relative standard deviations in the laboratory were 1.9% ~ 3.9%, 2.0% ~ 2.8%, 2.5% ~
2.8%.
Pyridine-barbituric acid method. 6 laboratories, respectively, the concentration of cyanide 0.050 mg/L, 0.100 mg/L, 0.450
Mg/L of the unified samples were measured, the relative standard deviation of the laboratory were 1.8% 6.1%, 0.3% 5.0%
0.12% 3.2%. The relative standard deviations were 5.3%, 1.7% and 2.7%, respectively. The repeatability limits were 0.005 mg/L,
0.017 mg/L and 0.021 mg/L, respectively. The reproducibility limits were 0.009 mg/L, 0.019 mg/L and 0.040 mg/L, respectively.
11.2 Accuracy
Isonicotinic acid-barbituric acid method. the laboratory for the concentration of cyanide (0.126 ± 0.011) mg/L of the certified reference material
The relative error was 0.6% 6.0%, and the reference substance with concentration of (65.6 ± 5.8) μg/L was measured.
The relative error is 3.8% 7.8%. Laboratory of surface water and industrial wastewater and other actual samples of the standard analysis of the determination of its
The recoveries were 70.8% ~ 94.1%.
Pyridine-barbituric acid method. the concentration of cyanide in the laboratory was (65.6 ± 5.8) μg/L, (0.504 ± 0.039) mg/L,
(0.126 ± 0.011) mg/L, the relative error was 0.2% 5.2%, respectively,
(2.0 ± 5.6)%, (1.6 ± 7.9)%, (3.1 ± 11.4)%, respectively. The relative error of the final error was (2.0 ± 5.6)%, (1.6 ± 7.9)% and (3.1 ± 11.4)%, respectively.
Six laboratories were tested for surface water and industrial wastewater by spiking, and the recoveries were in the range of 79.0%
107%. The recoveries were (98.6 ± 10.8)%, (94.0 ± 17.2)% and (94.0 ± 14.4)%, respectively.
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...
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