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HJ 826-2017: Water quality-Determination of anionic surfactants -- Flow injection analysis(FIA) and methylene blue spectrophotometric method
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Water quality-Determination of anionic surfactants -- Flow injection analysis(FIA) and methylene blue spectrophotometric method
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HJ 826-2017
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Basic data | Standard ID | HJ 826-2017 (HJ826-2017) | | Description (Translated English) | Water quality-Determination of anionic surfactants -- Flow injection analysis(FIA) and methylene blue spectrophotometric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z16 | | Word Count Estimation | 10,154 | | 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 826-2017: Water quality-Determination of anionic surfactants -- Flow injection analysis(FIA) and methylene blue spectrophotometric method
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Water quality-Determination of anionic surfactants
Injection analysis (FIA) and methylene blue spectrophotometric method
National Environmental Protection Standard of the People 's Republic of China
Determination of Water Anionic Surfactants
Flow injection - methylene blue 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 .4
9 Analysis steps
10 results are calculated and expressed
11 Precision and Accuracy
12 Quality assurance and quality control
13 Waste treatment
14 Precautions
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 anionic surfactants in water, the development of this standard.
This standard specifies the flow of anionic surfactants in the determination of surface water, groundwater, domestic sewage and industrial waste
Shot - methylene blue 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 and Changshu City Environmental Monitoring 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.
Determination of Water Anionic Surfactants
Flow injection - methylene blue spectrophotometric method
Warning. Trichloromethane is a toxic substance, the operation should be required to wear protective equipment and in the fume hood, to avoid contact with the skin,
After the detection of waste residue should be properly safe handling.
1 Scope of application
This standard specifies the flow injection-methylene blue spectrophotometric method for the determination of anionic surfactants in water.
This standard is applicable to the determination of anionic surfactants in surface water, groundwater, domestic sewage and industrial waste water.
When the optical path length is 10 mm, the detection limit of this method is 0.04 mg/L (in terms of LAS), the measurement range is 0.13
Mg/L to 2.00 mg/L (in LAS).
2 normative reference documents
The contents of this standard refer to the following documents or their terms. For undated references, the valid version applies to this standard.
Water quality - Anionic surfactants - Methylene blue spectrophotometric method GB 7494
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.
Anionic surfactants anionic surfactants
Refers to the active ingredient of synthetic synthetic detergents, which refers to the most widely used sodium alkylphenylsulfonate (LAS). The
4 principle of the method
4.1 Flow injection analyzer 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
The anionic surfactant in the sample forms a methylene blue active substance (MBAS) with cationic dye methylene blue,
Methyl chloride, and the organic phase was measured at 650 nm. Specific work flow shown in Figure 1.
1. Peristaltic pump; Injection valve; Reaction ring; Phase separation device; Detection cell 10mm, 650nm; R1 Alkaline methylene blue solution
II (6.17); Acid methylene blue solution (6.18) C. Carrier liquid (6.15); Sample; W1. Waste liquid (chloroform); W2. Waste
Liquid (water phase)
Figure 1 Flow chart of flow injection - methylene blue spectrophotometric method for the determination of anionic detergents
5 interference and elimination
The main interferences of this process are organic sulfonates, hydroxyacids, phenols, and inorganic sulfates, sulfites,
Nitrates, cyanates, thiocyanates and the like, and these functional groups containing anionic bonds react with methylene blue to form chloroform
Blue complex, resulting in positive interference, by aqueous solution backwash can not remove the non-surface active substances caused by the interference, can be gas
The extraction of anionic surfactants from the aqueous phase to the organic phase is eliminated by extraction. For details, see GB 7494.
Sulfide in sewage can produce a colorless reduction with methylene blue and consume methylene blue reagent. In this case,
Sample to alkaline, add appropriate amount of hydrogen peroxide, to eliminate interference.
Some cations such as proteins and 4-amino compounds can negatively interfere with the results of this method.
Substances can be removed under appropriate conditions using cation exchange resin. See GB 7494 for details.
6 reagents and materials
Unless otherwise stated, analytical analytical reagents in accordance with national standards are used for the analysis, and the experimental water is freshly prepared
Deionized water or distilled water.
Note. The experimental water in the ultrasonic instrument ultrasonic degassing for 20 min, or in the course of the experiment results in the formation of bubbles. The following reagents are alkali
Methylene blue solution, acidic methylene blue solution, methanol solution equivalent treatment.
6.1 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure.
6.2 Hydrochloric acid. ρ (HCl) = 1.19 g/ml.
6.3 Sodium hydroxide (NaOH). excellent grade pure.
6.4 Sodium tetraborate (Na2B4O7 • 10H2O).
6.5 Trichloromethane (CHCl3). stabilized with pentylene.
Note. Trichloromethane reagents generally have bubbles, in the analysis process is easy to produce periodic bubble peak, affecting the determination of the results. Recommended ultrasound
Wave instrument ultrasonic degassing for 20 min, or with helium degassing 5 min, and then water seal.
6.6 Methanol (CH3OH).
6.7 Formaldehyde (CH₂O).
6.8 Sodium dodecylbenzenesulfonate (C18H29NaO3S, LAS).
6.9 Methylene blue (C16H18N3ClS).
6.10 sulfuric acid solution. c (H2SO4) = 0.5 mol/L.
In about 800 ml of water slowly add 26.9 ml of sulfuric acid (6.1), after cooling, diluted with water to 1000 ml, mix.
6.11 sodium tetraborate solution. c = 0.05 mol/L.
Weigh 9.53 g of sodium tetraborate (6.4) in the appropriate amount of water, dissolved and moved to 500 ml volumetric flask, add water to the mark, mix.
6.12 sodium hydroxide solution. c (NaOH) = 0.100 mol/L.
Weigh 2.0 g of sodium hydroxide (6.3) dissolved in the amount of water, dissolved and moved to 500 ml volumetric flask, add water to the mark, mix.
6.13 alkaline boric acid solution.
500 ml of sodium tetraborate stock solution (6.11) and 500 ml of sodium hydroxide solution (6.12) were mixed in volume.
6.14 methylene blue solution. ρ = 0.50 g/L.
Weigh 0.25 g of methylene blue (6.9) into the appropriate amount of water, dissolved and moved to 500 ml volumetric flask, add water to the marking,
After mixing the 0.45 μm nylon filter, the filtrate is stored in a glass bottle with a glass stopper and stored in a dark place for up to 15 days.
6.15 carrier liquid
In the special reagent glass bottle by adding 700 ml of chloroform and.200 ml of water, ultrasound ultrasonic ultrasound about 20 min, static
Stored in a container. Is now available.
6.16 Alkaline methylene blue solution Ⅰ.
Measure the amount of 60 ml of methylene blue solution (6.14) in a 500 ml separatory funnel and add 100 ml of basic boric acid solution (6.13).
Each time with 20 ml of chloroform (6.5) extraction, to chloroform or colorless or methylene blue solution for the very clear purple
(About six times), the bottom of the trichloromethane as far as possible, then use 30 ml of chloroform (6.5) leaching water
Phase, do not shake. After the two phases are completely separated, the chloroform phase is released. The aqueous phase (purified methylene blue) was placed
1000 ml reagent bottle, add.200 ml of alkaline boric acid solution (6.13) and 640 ml of water, the total volume of the test solution is about
1000 ml. Ultrasonic treatment of ultrasonic treatment about 20 min, covered with polyethylene cover, placed in the shade, placed after 24 h to use.
The solution can be stored for 5 days.
6.17 Alkaline methylene blue solution II.
Add 1 ml of 1 M reagent bottle to 100 ml of basic methylene blue solution I (6.16) and 300 ml of water (ultrasonic wave
15 min ~ 30 min degassed water). The solution can be stored for 5 days.
6.18 Acid methylene blue solution.
40 ml of methylene blue solution (6.14) was added to a 500 ml separatory funnel and 20 ml of a basic boric acid solution (6.13)
And 150 ml of water, each with 20 ml of chloroform (6.5) extraction, to chloroform or colorless or methylene blue solution for the non-
Often clear purple (about three times), the bottom of the trichloromethane as far as possible, then use 30 ml of trichloromethane
(6.5) Leaked water phase, do not shake. After the two phases are completely separated, the chloroform phase is released. The aqueous phase (purified
Methylene blue) was placed in a 1000 ml reagent bottle and 10 ml of sulfuric acid solution (6.10) and 780 ml of water were added. At this time the total test solution
The volume is about 1000 ml. Ultrasonic ultrasonic ultrasound about 20 min, covered with polyethylene cover, placed in the shade, placed 24 h
After use. The solution can be stored for 5 days.
6.19 Wash the solution.
Add 400 ml of water to a 1000 ml container, 100 ml of methanol (6.6) and 50 ml of hydrochloric acid (6.2)
Bottle in the storage.
6.20 Sodium Dodecyl Benzenesulfonate Standard stock solution. 100 mg/L (in LAS).
Use a commercially available certified standard solution or weigh 0.100 g sodium dodecylbenzenesulfonate (6.8), accurate to 0.001 g, dissolved
In 50 ml of water, and then moved to 100 ml volumetric flask, add water to the mark, slowly mix. Stored at 5 ℃, can be stored for 2 weeks.
6.21 Sodium dodecylbenzenesulfonate Standard liquid. 10.00 mg/L (in LAS).
Measure the amount of sodium dodecylbenzenesulfonate standard stock (6.20) 10.00 ml to 100 ml volumetric flask, add water to the mark,
Mix slowly. The day of preparation.
6.22 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 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. A good sample was added with formaldehyde (6.7)
So that formaldehyde volume concentration of 1%, 4 ℃ to save, can save a week.
Note. Anionic surfactants are easily adsorbed on suspended solids or deposits. Samples should be well mixed and samples with significant particles are applied.
The sonicator was sintered after ultrasonic injection.
9 Analysis steps
9.1 Commissioning and calibration of flow analyzers
Install the analysis system, commissioning the instrument and setting the operating parameters according to the instrument manual. After the instrument is switched on, the flow path system is carried out
Of the pre-regulation, pay attention to avoid the water phase into the flow cell. Until the water phase, organic phase separation system pre-adjusted, the flow system
Fine tune to get the best analysis conditions. After the baseline is stable (about 5 min), according to 9.2 ~ 9.4 operation.
9.2 Calibration
9.2.1 Preparation of standard series
In a group of volumetric flask were measured appropriate amount of sodium dodecyl benzene sulfonate standard liquid (6.21), diluted with water to the standard
And the standard series of 6 concentration points were prepared. The mass concentration of the anionic surfactant (in terms of LAS)
As follows. 0.00 mg/L, 0.10 mg/L, 0.20 mg/L, 0.50 mg/L, 1.00 mg/L, 2.00 mg/L.
9.2.2 Drawing of calibration curves
Measure the amount of about 10 ml of the standard series solution (9.2.1) were placed in the sample cup, from low to high concentrations of sampling points
(Peak area) of different concentrations of anionic surfactants. To the signal value (peak area) as the ordinate,
Corresponding to the anionic surfactant concentration (LAS, mg/L) as the abscissa, the calibration curve was drawn.
9.3 Determination
According to the same measurement conditions as the calibration curve, measure about 10 ml of the sample to be measured, record the signal value (peak
area). If the concentration is higher than the highest point of the standard curve, the sample should be properly diluted.
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 anionic surfactant in the sample (in LAS, mg/L) was calculated according to equation (1)
Where. - mass concentration of anionic surfactant 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 mg/L, the two 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
The concentration of anionic surfactant (LAS) in the six laboratories was 0.20 mg/L, 1.00 mg/L, 1.80 mg/L
The relative standard deviations in the laboratory were 2.2% ~ 6.9%, 1.2% ~ 6.1%, 0.6% ~ 6.7% respectively.
The relative standard deviations were 9.0%, 9.5% and 3.2%, respectively. The repeatability limits were 0.02 mg/L, 0.11 mg/L,
0.17 mg/L, and the reproducibility limits were 0.26 mg/L, 1.31 mg/L and 2.27 mg/L, respectively.
10.2 Accuracy
The concentration of anionic surfactant (LAS) in the five laboratories was (0.772 ± 0.064) mg/L, (0.300 ± 0.020)
Mg/L, (0.544 ± 0.040) mg/L, the relative error was -3.0% ~ 1.0%
(-0.7 ± 3.3)%, (- 2.1 ± 6.1)%, respectively, and the relative error was (-0.7 ± 3.3)%,
(0.01 ± 0.3)%.
6 laboratories, respectively, on the anionic surfactant concentration of 0.008 mg/L ~ 0.457 mg/L of the actual sample into
The recoveries were 93.0% ~ 103%, 97.0% ~ 110% and 88.5% ~ 112%, respectively.
The recoveries were (97.9 ± 7.2)%, (103 ± 9.8)% and (97.2 ± 16.4)%, 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 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 ≤ 25%.
12.5 Accuracy control
Each batch of samples should be measured at least 10% of the spiked samples, the number of samples less than 10, should be measured at least one plus standard
Product, spike recovery rate should be between 80% 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 process of trichloromethane waste generated, should be concentrated recovery, qualified to deal with the disposal of qualified professional waste.
14 Precautions
14.1 The glassware used in this method should be cleaned with cleaning solution (6.19) and deionized water, and should not be washed with synthetic detergent.
14.2 After the end of the test, observe whether the methylene blue waste bottle contains chloroform, if the lower layer of a small amount of chloroform, then
Indicating that the separation effect of the separation membrane decreased, should check the membrane separator or replace the separation membrane.
14.3 should pay attention to the maintenance of piping systems, regular cleaning lines, with the amount of 1% sodium hypochlorite cleaning; before each test should be
Check the pump tubing for wear and replace the damaged tubing in time. Should always check the trace valve, if the accumulation of particles in the trace
In the valve, it should be cleaned.
14.4 If the flow cell is in contact with the water, noise is significantly increased or the baseline is significantly increased, resulting in no signal being detected,
The water phase should be prevented from entering the flow cell.
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