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HJ 824-2017 English PDF

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HJ 824-2017: Water quality - Determination of sulfide-Flow injection analysis (FIA) and methylene blue spectrophotometric method
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Basic data

Standard ID HJ 824-2017 (HJ824-2017)
Description (Translated English) Water quality - Determination of sulfide-Flow injection analysis (FIA) and methylene blue spectrophotometric method
Sector / Industry Environmental Protection Industry Standard
Classification of Chinese Standard Z16
Word Count Estimation 11,111
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 824-2017: Water quality - Determination of sulfide-Flow injection analysis (FIA) and methylene blue spectrophotometric method


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Water quality-Determination of sulfide-flow injection analysis (FIA) and methylene blue spectrophotometric method National Environmental Protection Standard of the People 's Republic of China Determination of water quality sulfide 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 .2

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, Protection of human health, regulate the determination of sulfide in water methods, the development of this standard. This standard specifies the determination of surface water, groundwater, domestic sewage and industrial waste water sulfide flow injection - methylene blue Spectrophotometry. 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. Nanjing Environmental Monitoring Center Station, Huai'an City Environmental Monitoring Center Station, Yangzhou City Environmental Monitoring Heart station, Changshu City Environmental Monitoring Station, Jiangsu Province, Disease Prevention and Control Center 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. Water quality - Determination of sulfide - Flow injection - methylene blue spectrophotometric method

1 Scope of application

This standard specifies the flow injection-methylene blue spectrophotometric method for the determination of sulfides in water. This standard applies to the determination of sulfides 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 0.004 mg/L (in S2), the determination range is 0.016 Mg/L 2.00 mg/L (in S2).

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 - Determination of sulfide - Methylene blue spectrophotometric method GB/T 16489 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. Sulfide sulfide Refers to the sum of dissolved inorganic sulfides and acid-soluble metal sulfides in water. Including the solubility of H2S, HS-, S2-, and storage In the suspended matter in the soluble sulfide and acid soluble metal sulfide.

4 principle of the method

4.1 Flow injection analyzer works In a closed line, a volume of the sample is injected into the continuous flow of the carrier liquid, the sample and reagent in the chemical reaction module Specific order and ratio of mixing, reaction, in the non-complete reaction conditions, into the flow detection pool for photometric detection. 4.2 Principles of chemical reactions In the acidic medium, the sample through 65 ℃ ± 2 ℃ on-line heating release of hydrogen sulfide gas is absorbed by sodium hydroxide solution. Absorbent liquid Sulfide reacts with p-aminodimethylaniline and ferric chloride to form methylene blue, and absorbance is measured at 660 nm. Specific work The process is shown in Figure 1. 1. Peristaltic pump; Heating pool (65 ℃); Diffusion pool; Injection valve; Reaction ring; Heating pool (30 ℃); Detection pool 10mm, 660nm; R1 Phosphoric acid solution (6.20); Sodium hydroxide solution (6.23); R3. Picoline dimethylaniline solution (6.25); R4 Ferric chloride solution (6.24); C. Carrier solution (sodium hydroxide solution, 6.23); Sample; Waste liquid Figure 1 flow injection - spectrophotometric determination of sulfide reference work flow chart

5 interference

The main disturbances of this method are SO32-, S2O32-, SCN-, NO2-, CN-, Cu2, Pb2, Hg2. The sulfide content was 0.50 mg/L , The maximum permissible levels of interfering substances in the samples were 20 mg/L SO32-, 240 mg/L S2O32-, 400 mg/L SCN-, 65 mg/L NO2-,.200 mg/L NO3-, 400 mg/L I-, 5 mg/L CN-, 2 mg/L Cu2, 25 mg/L Pb2 and 4 mg/L Hg2.

6 reagents and materials

Unless otherwise stated, analytical reagents conforming to national standards are used for analysis. The experimental water is freshly prepared for deionized water or Distilled water. In addition to the standard solution, other solutions and experimental water are treated with helium (6.33) or ultrasonic (7.3) degassed. 6.1 hydrochloric acid. ρ (HCl) = 1.19 g/ml, excellent grade pure. 6.2 Phosphoric acid. ρ (H3PO4) = 1.69 g/ml, excellent grade pure. 6.3 sulfuric acid. ρ (H2SO4) = 1.84 g/ml, excellent grade pure. 6.4 Sodium hydroxide (NaOH). excellent grade pure. 6.5 Ferric trichloride [FeCl3 · 6H2O]. 6.6 p-aminodimethylaniline [(CH3) 2NC6H4NH2 · 2HCl]. 6.7 Sodium thiosulfate (Na2S2O3.5H2O). 6.8 Sodium sulfide (Na2S · 9H2O). 6.9 Sodium carbonate (Na2CO3). 6.10 Potassium iodide (KI). 6.11 Zinc acetate (ZnAc2 • 2H2O). 6.12 Sodium acetate (NaAc • 3H2O). 6.13 Iodine (I2). 6.14 Starch (C6H10O5) n. 6.15 potassium dichromate (K2Cr2O7). standard or excellent grade pure. After drying at 105 ℃ for 2h, stand-by. 6.16 ascorbic acid (C6H8O6). 6.17 sulfuric acid solution. 1 5. The volume ratio of sulfuric acid (6.3) to water is 1. 5. 6.18 hydrochloric acid solution. c (HCl) = 3 mol/L. In about 600 ml of water, slowly add 248 ml of hydrochloric acid (6.1), diluted with water to 1000 ml, mix well. 6.19 hydrochloric acid solution. c (HCl) = 0.20 mol/L. About 700 ml of water, slowly add 16.5 ml of hydrochloric acid (6.1), diluted with water to 1000 ml, mix well. 6.20 phosphoric acid solution. 1 10. The volume ratio of phosphoric acid (6.2) to water is 1.10. 6.21 sodium hydroxide solution. c (NaOH) = 15 mol/L. Weigh 60.0 g of sodium hydroxide (6.4) dissolved in the amount of water, dissolved and moved to 100 ml volumetric flask, water volume to the mark, mix. 6.22 sodium hydroxide solution. c (NaOH) = 1 mol/L. Weigh 4.0 g of sodium hydroxide (6.4) in the appropriate amount of water, dissolved and moved to 100 ml volumetric flask, water volume to the mark, mix. 6.23 sodium hydroxide solution. c (NaOH) = 0.025 mol/L. Weigh 1.0 g of sodium hydroxide (6.4) dissolved in the amount of water, dissolved and moved to 1000 ml volumetric flask, water volume to the mark, mix. 6.24 ferric chloride solution Weigh 6.65 g of ferric chloride (6.5) in an appropriate amount of hydrochloric acid solution (6.18), dissolved and transferred to 500 ml volumetric flask, with salt Acid solution (6.18) constant volume to the marking, mixing. 6.25 p-aminodimethylaniline solution Weigh 0.50 g of p-aminodimethylaniline (6.6) in an appropriate amount of hydrochloric acid solution (6.18), dissolved and transferred to 500 ml volumetric flask, With hydrochloric acid solution (6.18) constant volume to the mark, mix. If the color of the solution becomes darker, it should be re-formulated. 6.26 standard solution of potassium dichromate Weigh 2.4515 g potassium dichromate (6.15) dissolved in the amount of water, dissolved and moved to 500 ml volumetric flask, water volume to the mark, mix. 6.27 iodine solution 6.35 g of iodine (6.13) was weighed into a 250 ml beaker and 20 g of potassium iodide (6.10) and an appropriate amount of water were added and dissolved to 500 ml Brown capacity bottle, the water volume to the mark, mix. 6.28 Sodium thiosulfate standard solution Weigh 12.25 g sodium thiosulfate (6.7) in boiling water, add 0.1 g of sodium carbonate (6.9), move to 500 ml Capacity bottle, the water volume to the marking, mixing. The solution was stored in a brown bottle. Before use, use potassium dichromate solution (6.26) calibration. Calibration method. 1 ml of potassium iodide (6.10), 50 ml of water, 15.00 ml of potassium dichromate standard solution (6.26), shake to completely dissolved and add 5 ml of sulfuric acid solution (6.17), immediately mix the dust. After standing for 5 min in the dark, use sulfur Sodium sulfate solution (6.28) titrated to light yellow, add 1 ml of starch solution (6.32), continue to titrate to blue just disappeared to the end Point, record the amount of sodium thiosulfate solution (6.28). At the same time do blank titration test. The concentration of sodium thiosulfate standard solution (6.28) is calculated according to formula (1). Where. c - sodium thiosulfate standard solution concentration, mol/L; 1 V - titration of potassium dichromate standard solution when the amount of sodium thiosulfate solution, ml; 0 V - the amount of sodium thiosulfate solution titrated in the blank solution, ml; 0.1000 - Concentration of potassium dichromate standard solution, mol/L. 6.29 Zinc acetate - sodium acetate solution. Weigh 25 g of zinc acetate (6.11) and 6.26 g of sodium acetate (6.12) in 500 ml of water and mix well. 6.30 sodium sulfide standard stock solution. ρ (S2-) ≈100 mg/L. Weigh 0.375 g of sodium sulfide (6.8) in an appropriate amount of sodium hydroxide solution (6.22) and move to a 500 ml brown volumetric flask. Sodium hydroxide solution (6.23) constant volume to the mark, mix. The solution was stored in a brown volumetric flask and used after calibration. Or purchase evidence standard solution. In a 250 ml iodine flask, add 10 ml of zinc acetate-sodium acetate solution (6.29), 10.00 ml to the standard sodium sulfide standard stock (6.28) and 20.00 ml of iodine solution (6.27), add 20 ml of water, then add 5 ml of sulfuric acid solution (6.17), immediately dense shake. After standing for 5 min in the dark, titration with sodium thiosulfate standard solution (6.28) to pale yellow, add 1 ml of starch solution (6.32) Continue titration to blue just disappeared as the end point, record the amount of sodium thiosulfate standard solution (6.28). At the same time, with 10.00 ml water generation For the sodium sulfide standard solution to do blank test. The concentration of sodium sulfide standard solution is calculated according to formula (2). - sodium sulfide standard solution concentration, mg/L; 0 V - blank titration, the amount of sodium thiosulfate standard solution, ml; 1 V - titration sodium sulfide standard solution, the amount of sodium thiosulfate standard solution, ml; C - sodium thiosulfate standard solution concentration, mol/L; 16.03--1/2 S2- molar mass, g/mol. 6.31 sodium sulfide standard use of liquid. ρ (S2 -) = 10.00 mg/L. With sodium hydroxide solution (6.22) to adjust the water pH = 10 ~ 12, take 150 ml in.200 ml brown volumetric flask, add 1 ~ 2 ml Zinc acetate - sodium acetate solution (6.29), mix well. Measure a certain amount of just calibrated sodium sulfide standard stock solution (6.30) side of the oscillation side drops Into the above brown volumetric flask, and then have been adjusted to pH 10 ~ 12 water diluted to the mark, shake well. The solution was stored in a brown bottle chamber Temperature can be saved for six months. Every time you use, should be fully shaken after access. 6.32 Starch solution. ρ = 10 g/L. Weigh 1 g of soluble starch, with a small amount of water into a paste, slowly add 100 ml of boiling water, after cooling stored in the reagent bottle, With the current distribution. 6.33 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 cell), 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

The collection of water samples is carried out in accordance with the relevant provisions of HJ/T 91 and HJ/T 164. Samples were added to the vials by adding sodium hydroxide solution and anti Ascorbic acid, 5 ml of sodium hydroxide solution (6.21) and 4 g of ascorbic acid (6.16) were added to each liter of water so that the pH of the sample was 0.1. kind Products should be analyzed as soon as possible, at room temperature away from light for more than 24 h. Note. The sample preservation method and pretreatment are carried out in accordance with the provisions of GB/T 16489 when using the method module without on-line distillation.

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, to pure water Instead of all reagents, check the integrity of the entire flow path and the smooth flow of the liquid. After baseline stabilization (about 20 min), the system Start pumping 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 In a group of volumetric flask were the appropriate amount of sodium sulfide standard use of the liquid (6.31), with sodium hydroxide solution (6.23) diluted to the standard And the concentration of sulfide (in S2-terms) were 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 Transfer to about 10 ml of the standard series of solution (9.2.1) were placed in the sample cup, from low to high concentrations of sequential sampling analysis To different concentrations of sulfide signal values (peak area). The signal value (peak area) as the ordinate, the corresponding sulfide mass concentration (to S2-meter, mg/L) as the abscissa, draw the calibration curve. 9.3 Determination Measure the signal value (peak area) by measuring about 10 ml of the sample to be measured according to the same measurement conditions as the calibration curve. 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 sulfide concentration in the sample (in S2-, mg/L) is calculated according to equation (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 1.00 mg/L, it will be retained to three decimal places. If the result is greater than or equal to 1.00 mg/L, Bit effective number. 11 precision and accuracy 11.1 precision 6 samples of the sulfide mass concentration of 0.20 mg/L, 1.00 mg/L, 1.80 mg/L of the unified samples were measured, The relative standard deviation of the laboratory was 1.9% ~ 3.4%, 1.0% ~ 5.0%, 0.3% ~ 5.0%; the relative standard deviation between the laboratory was 1.0% 1.0%, 0.5%, the repeatability limit was 0.013 mg/L, 0.045 mg/L, 0.048 mg/L, the reproducibility limit was 0.013 mg/L, 0.050 mg/L, 0.050 mg/L. 11.2 Accuracy (0.713 ± 0.026) mg/L, (0.713 ± 0.062) mg/L, respectively, in six laboratories, The relative error was -6.5% -5.4%, - 1.9% -1.3%, and the relative error was (-4.9 ± 4.6)%, respectively, (-1.6 ± 0.6)%. The concentration of sulfide in the six laboratories was 0.001 mg/L ~ 0.003 mg/L, 0.068 mg/L ~ 1.59 mg/L, 0.143 Mg/L ~ 1.29 mg/L of surface water, industrial wastewater and other actual samples were measured by spiked assays, spiked recovery were 91.4% 105%, 87.1% ~ 97.4%, 88.8% ~ 98.6%. The final recoveries were (99.1 ± 10.0)%, (93.3 ± 9.1)%, (93.4 ± 8.0)%. 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 reasons for re-points Until the qualified sample can be measured. 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 of the 10 samples was calibrated with an intermediate concentration calibration solution with a calibration curve, and the results were compared with the last The relative deviation of the 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 reasons for re-points Until the qualified sample can be measured. 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, twice The relative deviation of the parallel measurement results 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 a spiked sample, spiked The recovery rate should be between 70% and 120%. If necessary, each batch of samples at least a certified reference material or laboratory self-prepared quality control samples, certified reference material determination The results should be given in the uncertain range, the laboratory self-prepared quality control test results should be controlled at 90% to 110%. laboratory Self-prepared quality control should pay attention to the state with 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 p-aminodimethylaniline reagent should be stored in the dryer as far as possible after opening. If the solid powder color becomes dark yellow, stop using. 14.2 If a burr peak appears continuously during the analysis, replace the degassing tube; if a bimodal or shoulder-shaped peak appears, replace the membrane of the diffusion cell. 14.3 Specimens with significant particles or precipitates are sonicated by sonication.

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