HOME   Cart(0)   Quotation   About-Us Policy PDFs Standard-List
www.ChineseStandard.net Database: 189760 (18 Oct 2025)

HJ 665-2013 English PDF

US$319.00 · In stock
Delivery: <= 3 days. True-PDF full-copy in English will be manually translated and delivered via email.
HJ 665-2013: Water quality. Determination of ammonium nitrogen by continuous flow analysis (CFA) and Salicylic acid spectrophotometry
Status: Valid
Standard IDContents [version]USDSTEP2[PDF] delivered inStandard Title (Description)StatusPDF
HJ 665-2013English319 Add to Cart 3 days [Need to translate] Water quality. Determination of ammonium nitrogen by continuous flow analysis (CFA) and Salicylic acid spectrophotometry Valid HJ 665-2013

Standard similar to HJ 665-2013

HJ 511   HJ 945.3   HJ 943   

Basic data

Standard ID HJ 665-2013 (HJ665-2013)
Description (Translated English) Water quality. Determination of ammonium nitrogen by continuous flow analysis (CFA) and Salicylic acid spectrophotometry
Sector / Industry Environmental Protection Industry Standard
Word Count Estimation 12,195
Quoted Standard HJ 536; HJ/T 91; HJ/T 164
Regulation (derived from) Ministry of Environmental Protection Notice No. 63 of 2013
Issuing agency(ies) Ministry of Ecology and Environment
Summary This standard specifies the determination of ammonia in water continuous flow - salicylic acid spectrophotometry. This standard applies to surface water, groundwater, sewage and industrial measurement WASTEWATER. When using direct colorimetric module dete

HJ 665-2013: Water quality. Determination of ammonium nitrogen by continuous flow analysis (CFA) and Salicylic acid spectrophotometry


---This is a DRAFT version for illustration, not a final translation. Full copy of true-PDF in English version (including equations, symbols, images, flow-chart, tables, and figures etc.) will be manually/carefully translated upon your order.
Water quality.Determination of ammonium nitrogen by continuous flow analysis (CFA) and Salicylic acid spectrophotometry National Environmental Protection Standard of the People's Republic Determination of ammonia nitrogen in water quality Continuous flow-salicylic acid spectrophotometry Water quality-Determination of ammonium nitrogen by Continuous flow analysis (CFA) and Salicylic acid spectrophotometry Published on.2013-10-25 2014-01-01 implementation Ministry of Environmental Protection released

Content

Foreword..II 1 Scope.1 2 Normative references.1 3 principle of the method.1 4 interference and elimination 2 5 Reagents and materials 2 6 Instruments and equipment 4 7 sample 4 8 Analysis steps.4 9 Calculation and representation of results. 5 10 precision and accuracy..5 11 Quality Assurance and Quality Control 6 12 Notes. 7

Foreword

To implement the Environmental Protection Law of the People's Republic of China and the Law of the People's Republic of China on Water Pollution Prevention and Control, to protect the environment, To ensure human health, standardize the determination method of ammonia nitrogen in water, and formulate this standard. This standard specifies a continuous flow-salicylic acid spectrophotometric method for the determination of ammonia nitrogen in water. This standard is the first release. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Suzhou Environmental Monitoring Center Station. This standard is verified by. Jiangyin Environmental Monitoring Station, Taihu Basin Water Environment Monitoring Center, and Jilin City Environmental Protection Monitoring Station, Tianjin Water Environment Monitoring Center, Yellow River Basin Water Environment Monitoring Center and Suzhou Environmental Monitoring Center Station. This standard was approved by the Ministry of Environmental Protection on October 25,.2013. This standard has been implemented since January 1,.2014. This standard is explained by the Ministry of Environmental Protection. Determination of ammonia nitrogen in water - continuous flow - salicylic acid spectrophotometric method

1 Scope of application

This standard specifies a continuous flow-salicylic acid spectrophotometric method for the determination of ammonia nitrogen in water. This standard applies to the determination of ammonia nitrogen in surface water, groundwater, domestic sewage and industrial wastewater. When the direct colorimetric module is used and the detection cell optical path is 30 mm, the detection limit of the method is 0.01 mg/L (in terms of N). The measurement range is from 0.04 mg/L to 1.00 mg/L; when the on-line distillation module is used, the detection method is performed when the optical path of the detection cell is 10 mm. The limit is 0.04 mg/L (in terms of N), and the measurement range is from 0.16 mg/L to 10.0 mg/L.

2 Normative references

The contents of this standard refer to the terms in the following documents. For undated references, the valid version applies to this standard. HJ 536 Water quality - Determination of ammonia nitrogen - Salicylic acid spectrophotometric method HJ/T 91 Surface Water and Wastewater Monitoring Technical Specifications HJ/T 164 Technical Specifications for Groundwater Environmental Monitoring

3 Principle of the method

3.1 Working principle of continuous flow analyzer The sample and the reagent enter the chemical reaction module under the push of the peristaltic pump, and continuously flow in the closed pipeline, and are pressed by the bubble. They are regularly spaced at regular intervals and mixed and reacted in a specific order and proportion. After the color development is completed, they enter the flow detection cell. Photometric detection. 3.2 Principles of chemical reactions In an alkaline medium, the ammonia and ammonium ions in the sample react with the hypochlorite released from the sodium dichloroisocyanurate solution. Chloramine. Chloramine reacts with salicylate to form a blue-green compound in the presence of 40 ° C and potassium nitroferrocyanide. The absorbance was measured at a wavelength of 660 nm. Refer to the workflow diagram, see Figure 1 and Figure 2. 1 peristaltic pump 2 mixing ring 3 mixing reaction ring 4 heating pool (circle) 40 ° C G air 5 Flow detection cell 30mm 660nm 6 De-bubble S sample 0.60ml/min W Waste liquid R1 buffer solution 1 (5.18) 0.60ml/min R2 sodium salicylate solution I (5.20) 0.32ml/min R3 sodium nitroferricyanide solution (5.22) 0.16ml/min R4 sodium dichloroisocyanurate solution I (5.23) 0.32ml/min Figure 1 Flow chart of direct reference colorimetric determination of ammonia nitrogen 1 peristaltic pump 2 mixing (reaction) ring 3.1 heating bath 120 ° C 3.2 distillation unit 4 heating bath 40 ° C 5 flow detection tank 10mm 660nm 6 degassing W waste liquid R1 Distillation Reagent (5.16) 1.60 ml/min R2 Sulfuric Acid Solution I (5.13) 0.42 ml/min S Sample 0.60 ml/min R3 Buffer Solution II (5.19) 0.80 ml/min R4 Sodium Salicylate Solution II (5.21) 0.32 ml/min G1 Air R5 Sodium dichloroisocyanurate solution II (5.24) 0.23 ml/min ReS Secondary injection 0.16 ml/min G2 Nitrogen (5.30) Figure 2 Flow chart of the determination of ammonia nitrogen by colorimetry after distillation

4 interference and elimination

4.1 The residual chlorine in the sample will form a chloramine interference assay, which can be removed by adding an appropriate amount of sodium thiosulfate solution (5.28). 4.2 When the concentration of calcium, manganese and chloride ions in the sample is greater than 150mg/L, 10mg/L and 10000mg/L, respectively, Will cause positive interference to the analysis. Samples can be pre-distilled with HJ 536 or directly with modules with in-line distillation (figure 2) Analysis. When the concentration of magnesium ion and iron ion in the sample is not higher than 300 mg/L, there is no influence on the determination of ammonia nitrogen. 4.3 When the pH of the sample is >10 or pH< 4, the pH should be adjusted to neutral before analysis and then measured. Acid-preserved sample The product easily absorbs ammonia in the air, affecting the measurement results, and should be kept in a closed state. 4.4 Ammonia in the ambient air may drift the baseline and affect the blank value. Connect one at the inlet end of the chemical unit A gas cylinder filled with H2SO4 solution (5.14) and periodically replaced with a scrubbing solution.

5 reagents and materials

Analytically pure reagents in accordance with national standards were used for analysis, unless otherwise stated. Ammonia-free water with a rate greater than 10 MΩ·cm (25 ° C). 5.1 Hydrochloric acid. ρ(HCl) = 1.18g/ml. 5.2 Sulfuric acid. ρ(H2SO4) = 1.84 g/ml. 5.3 Ammonium chloride (NH4Cl). excellent grade, dried at 105 ± 5 ° C °C and stored in a desiccator. 5.4 Sodium hydroxide (NaOH). 5.5 Ethylenediaminetetraacetic acid disodium salt (EDTA-2Na, C10H14N2Na2O8·2H2O). 5.6 Sodium potassium tartrate (C4H4O6KNa·4H2O). 5.7 Trisodium citrate (C6H5O7Na3·2H2O). 5.8 Sodium salicylate (NaC7H5O3). 5.9 Sodium nitrosoferrocyanide dihydrate (Na2[Fe(CN)5NO]·2H2O). 5.10 Sodium dichloroisocyanurate (C3Cl2N3O3Na·2H2O). 5.11 Dodecyl polyglycol ether (Brij35, C58H118O24). 5.12 sodium thiosulfate (Na2S2O3). 5.13 Sulfuric acid solution I.c(H2SO4)=0.16mol/L 7.5 ml of sulfuric acid (5.2) was slowly added to 800 ml of water, and after cooling, it was diluted with water to 1000 ml. Available at the time of use. 5.14 sulfuric acid solution II. c (H2SO4) = 0.5mol/L 27 ml of sulfuric acid (5.2) was slowly added to 800 ml of water, and after cooling, it was diluted with water to 1000 ml. 5.15 sodium hydroxide solution. ρ (NaOH) = 0.2g/ml 200 g of sodium hydroxide (5.4) was weighed and dissolved in an appropriate amount of water, and after cooling, it was diluted with water to 1000 ml. 5.16 Distillation reagent. Weigh 5g EDTA-2Na (5.5) dissolved in 600ml water, add 140g sodium hydroxide (5.4), and dilute to 1000ml with water. Mix well. 5.17 Dodecyl polyglycol ether (Brij35) solution. ω = 30% 30 g of Brij35 (5.11) was weighed and dissolved in 100 ml of water. 5.18 Buffer Solution I. (pH=5.2) Weigh 33g sodium potassium tartrate (5.6) and 24g trisodium citrate (5.7) dissolved in 800ml water, diluted with water to 1000ml, Add 3 ml of Brij35 solution (5.17) and mix. The pH was adjusted to 5.2 ± 0.1 with hydrochloric acid (5.1). The solution is stored in brown In a color bottle, store at 4 °C. Check the pH of the solution every two days. 5.19 Buffer Solution II. (pH=5.2) Weigh 30g of trisodium citrate (5.7) dissolved in 800ml of water, dilute to 1000ml with water, add 1ml Brij35 (5.17), Mix well. The pH was adjusted to 5.2 ± 0.1 with hydrochloric acid (5.1). The solution was stored in a brown bottle and stored at 4 °C. Every second Check the pH of the solution daily. 5.20 Sodium salicylate solution I. Weigh 25g of sodium hydroxide (5.4) dissolved in 800ml of water, add 80g of sodium salicylate (5.8), and dilute to 1000ml with water. Mix well. The solution was stored in a brown bottle and stored at 4 ° C for 1 month. 5.21 Sodium Salicylate Solution II. Weigh 70g of sodium salicylate (5.8) and 1g of sodium nitrosodium ferricyanide (5.9) dissolved in 600ml of water, add while stirring Add 250 ml of sodium hydroxide solution (5.15), dilute to 1000 ml with water, and mix. The solution was stored in a brown bottle at 4 ° C The preservation can be stable for 1 month. 5.22 Sodium nitroferricyanide solution. ω (Na2[Fe(CN)5NO]·2H2O)=0.1% Weigh 1.0 g of sodium nitrosoferrocyanide dihydrate (5.9) dissolved in 800 ml of water, dilute to 1000 ml with water, and mix. The solution The solution was stored in a brown bottle and stored at 4 ° C for 1 month. 5.23 Sodium dichloroisocyanurate solution I. ω (C3Cl2N3O3Na·2H2O)=0.2% Weigh 2.0 g of sodium dichloroisocyanurate (5.10) dissolved in 800 ml of water, dilute to 1000 ml with water, and mix. The solution Store at 4 ° C for 1 month. 5.24 Sodium dichloroisocyanurate solution II. ω (C3Cl2N3O3Na·2H2O)=3.5% 3.419 g of sodium dichloroisocyanurate (5.10) was dissolved in 800 ml of water, diluted with water to 1000 ml, and mixed. The solution The solution was stable at 4 ° C for 1 month. 5.25 Ammonia nitrogen standard stock solution. ρ(N)=1000mg/L Weigh 3.819g of ammonium chloride (5.3) dissolved in water, dissolve it, transfer it to a 1000ml volumetric flask, dilute to volume with water and mix. The The solution was stored in a sealed container at 4 ° C for 6 months. Or buy a commercially available certified standard solution directly. 5.26 Ammonia nitrogen standard use solution I. ρ (N) = 100mg/L Accurately measure 10.00 ml of ammonia nitrogen standard stock solution (5.25), transfer to a 100 ml volumetric flask, dilute to volume with water and mix. The The solution was sealed and stored at 4 ° C for 7 days. 5.27 Ammonia nitrogen standard use solution II. ρ (N) = 10.0 mg/L Accurately measure 10.00 ml of ammonia nitrogen standard solution (5.26), transfer to a 100 ml volumetric flask, dilute to volume with water and mix. Pro Use the match now. 5.28 sodium thiosulfate solution. ρ=3500mg/L 3.5 g of sodium thiosulfate (5.12) was weighed and dissolved in water and diluted to 1000 ml. 5.29 Cleaning solution. A suitable amount of a commercially available sodium hypochlorite (NaClO) solution was weighed and diluted with water to a solution having an effective chlorine content of about 1.3%. 5.30 Nitrogen. purity ≥99% 5.31 Aqueous filter. The pore size is 0.45 μm.

6 Instruments and equipment

6.1 Continuous flow analyzer. by autosampler, chemical reaction unit (ie chemical reaction module, multi-channel peristaltic pump, Manifold, pump tube, mixed reaction ring, heating coil, etc.), detection unit (flow detection cell optical path 10mm and 30mm,), Data processing unit and other components. 6.2 Distillation unit with flow meter (optional). 6.3 Balance. Accuracy is 0.0001g. 6.4 pH meter. Accuracy is ±0.02. 6.5 Centrifuge. Maximum speed 4000r/min. 6.6 Common instruments and equipment used in general laboratories.

7 samples

7.1 Sample collection and preservation Samples should be collected in polyethylene or glass bottles and analyzed as soon as possible. If necessary, add sulfuric acid (5.2) to pH< 2, 2°C~5°C Store in the air for 7 days, and adjust the pH to neutral before acidifying the sample. 7.2 Preparation of samples When the sample is clear, without interference of color, turbidity, organic matter, etc., it can be directly sampled and analyzed. When the sample is turbid and analyzed by direct colorimetric module, the sample should be filtered or centrifuged with a filter (5.31). Take the filtrate or supernatant for analysis. The treatment effect must be checked by the standard for recycling. When the sample contains high concentrations of metal ions, is colored or contains some organic matter that is difficult to eliminate (high molecular weight In the case of the compound, the method module with on-line distillation should be used for the analysis. If the direct colorimetric module is used for analysis, it must Pre-distillation is required. See HJ 536 for the method of operation.

8 Analysis steps

8.1 Commissioning of the instrument Install the analysis system, set the operating parameters, and debug the instrument according to the instrument manual. After starting the machine, first replace the reagent with water, check Check the tightness of the flow path and the smoothness of the liquid flow. After the baseline is stable (about 15min), the system starts to test After the baseline is stabilized again, proceed to 8.2~8.4. If using an analytical module with distillation, adjust according to the instructions of the instrument The flow rate of the meter distillation unit flow meter. 8.2 Calibration 8.2.1 Preparation of the standard series Calibration curve I. Measure the appropriate amount of ammonia nitrogen standard solution (5.27), dilute to 100ml with water, prepare 6 The standard series of concentration points, ammonia nitrogen concentration. 0.00 mg/L, 0.05 mg/L, 0.25 mg/L, 0.50 mg/L, 0.80 Mg/L and 1.00 mg/L. Calibration curve II. separately take appropriate amount of ammonia nitrogen standard solution (5.26), dilute to 100ml with water, prepare 6 The standard series of concentration points, ammonia nitrogen concentration. 0.00 mg/L, 0.20 mg/L, 1.00 mg/L, 3.00 mg/L, 6.00 Mg/L and 10.0 mg/L. 8.2.2 Drawing of the calibration curve Take appropriate amount of standard series solution (8.2.1), put it in the sample cup, and proceed from the low concentration to the high concentration by the injector according to the procedure. Sampling and measurement. Taking the measured signal value (peak height) as the ordinate, the corresponding ammonia nitrogen mass concentration (in N, mg/L) is On the abscissa, draw a calibration curve. 8.3 Determination The appropriate amount of the sample (7.2) was measured and measured according to the same conditions as those for drawing the calibration curve. Note. If the ammonia nitrogen content of the sample exceeds the detection range of the calibration curve, an appropriate amount of the sample should be diluted and measured on the machine. 8.4 Blank test Replace the sample with experimental water and perform a blank test in accordance with step 8.3.

9 Calculation and representation of results

9.1 Calculation of results The mass concentration of ammonia nitrogen in the sample (in N, mg/L) is calculated according to formula (1). Yaf ρ −= × (1) In the formula. Ρ--the mass concentration of ammonia nitrogen in the sample, mg/L; y -- determine the signal value (peak height); a -- the intercept of the calibration curve equation; b -- the slope of the calibration curve equation; f -- dilution factor. 9.2 Results representation When the measurement result is less than 1.00 mg/L, the result is retained to two decimal places; when it is greater than or equal to 1.00 mg/L, the result Keep three significant digits. 10 Precision and accuracy 10.1 Precision Six laboratories used a direct colorimetric method for uniform samples of ammonia nitrogen concentrations of 0.10 mg/L, 0.50 mg/L, and 0.90 mg/L, respectively. The products were measured, and the relative standard deviations in the laboratory were. 1.8%~9.2%, 0.6%~2.8%, 0.4%~2.6%; The relative standard deviations between the examination rooms were. 5.0%, 3.5%, and 2.2%; the repeatability limits were. 0.01 mg/L, 0.02 mg/L, respectively. 0.03 mg/L; reproducibility limits were. 0.02 mg/L, 0.05 mg/L, 0.06 mg/L. Six laboratories used a post-distillation colorimetric method to unify ammonia nitrogen concentrations of 1.00 mg/L, 5.00 mg/L, and 9.00 mg/L, respectively. The samples were measured and the relative standard deviations in the laboratory were. 0.5%~2.8%, 0.2%~2.4%, 0.1%~1.1%; The relative standard deviations between laboratories were. 2.7%, 2.3%, and 2.3%; the repeatability limits were. 0.05 mg/L, 0.17 mg/L, respectively. 0.18 mg/L; reproducibility limits were. 0.09 mg/L, 0.35 mg/L, 0.60 mg/L. 10.2 Accuracy Six laboratories used direct colorimetry to determine ammonia nitrogen concentrations of 0.54 mg/L ± 0.03 mg/L and 0.67 mg/L ± 0.03 mg/L, respectively. The certified standard substances were determined, and the relative errors were. 0.9%~4.3%, 0.3%~3.2%; the relative error final value They were. 2.8% ± 2.6%, 1.9% ± 2.6%. Six laboratories used direct colorimetry for ammonia nitrogen concentration Three actual samples of 0.04mg/L~0.22mg/L, 0.22 mg/L ~0.40 mg/L, and 0.44 mg/L ~0.84 mg/L were added. Standard recovery test, the standard recovery rate is. 96.0% ~ 102%, 93.6% ~ 104%, 94.6% ~ 106%; spiked recovery The final values were. 99.8% ± 5.2%, 99.6% ± 8.2%, and 100% ± 8.4%. Six laboratories used a post-distillation colorimetric method for ammonia nitrogen concentrations of 1.33 mg/L ± 0.03 mg/L and 2.74 mg/L ± 0.12, respectively. The reference standard of mg/L was determined, and the relative errors were. 0.0%~3.8%, 0.0%~3.6%; the relative error was the most The final values were. 1.9% ± 4.4%, 1.9% ± 2.8%. Six laboratories used a post-distillation colorimetric method for ammonia nitrogen concentrations of 0.22 mg/L to 2.36 mg/L and 1.71 mg/L to 5.32 mg/L. The three actual samples of 2.24 mg/L~8.05 mg/L were spiked and the recoveries were 95.0%~106%. 95.9%~107%, 96.8%~103%; the final recoveries of the spiked recovery were. 102%±9.2%, 99.6%±8.4%, 100% ± 4.8%. 11 Quality Assurance and Quality Control 11.1 Blank test At least 2 blank samples shall be measured for each batch of samples, and the blank value shall not exceed the method detection limit. Otherwise, the cause should be identified, The sample can only be determined after the new analysis has passed. 11.2 Calibration validity check A calibration curve must be drawn for each batch of samples. The correlation coefficient of the calibration curve is γ ≥ 0.995. For each sample analyzed, a calibration curve intermediate concentration solution is used for calibration verification. The deviation should be ≤ 5%, otherwise the calibration curve should be redrawn. 11.3 Precision Control At least 10% of the parallel samples should be determined for each batch of samples. When the number of samples is less than 10, at least one parallel sample should be determined. When the ammonia nitrogen concentration of the sample is 0.02mg/L~0.10mg/L, the allowable relative deviation of the parallel sample should be ≤20%; when the ammonia nitrogen concentration For the range of 0.10 mg/L ~ 1.0 mg/L, the relative deviation of the parallel sample should be ≤ 15%; when the ammonia nitrogen concentration is > 1.0 mg/L, parallel The allowable relative deviation should be ≤10%. 11.4 Accuracy Control At least 10% of the spiked sample shall be determined for each batch of samples. When the number of samples is less than 10, at least one spiked sample shall be determined. The spiked recovery rate should be between 80 and 120%. If necessary, each batch of samples shall have at least one known quality control sample, and the test results shall be in the uncertainty given by it. Inside. 12 Precautions 12.1 Reagent and ambient temperature influence analysis results, reagents stored in the refrigerator should be placed at room temperature before analysis, during the analysis Room temperature fluctuations do not exceed ± 5 ° C. 12.2 In order to reduce the baseline noise, the reagent should be kept clear, and if necessary, the reagent should be filtered; after the analysis, the flow should be timely The filter in the test cell is removed and placed in a desiccator to protect it from dust and moisture. 12.3 Pay attention to the cleanliness of the flow path. After the analysis is completed every day, all the flow paths should be cleaned with pure water for 30 minutes. Weekly cleaning solution (5.29) Rinse for 30 min, then rinse with pure water for 15 min. 12.4 When the concentration of the sample analyzed in the same batch fluctuates greatly, a blank can be inserted between the sample and the sample as the sample is analyzed to reduce The effect of high concentration samples on low concentration samples. 12.5 Different types of flow analyzers can refer to this standard to select the appropriate instrument conditions.

Tips & Frequently Asked Questions:

Question 1: How long will the true-PDF of HJ 665-2013_English be delivered?

Answer: Upon your order, we will start to translate HJ 665-2013_English as soon as possible, and keep you informed of the progress. The lead time is typically 1 ~ 3 working days. The lengthier the document the longer the lead time.

Question 2: Can I share the purchased PDF of HJ 665-2013_English with my colleagues?

Answer: Yes. The purchased PDF of HJ 665-2013_English will be deemed to be sold to your employer/organization who actually pays for it, including your colleagues and your employer's intranet.

Question 3: Does the price include tax/VAT?

Answer: Yes. Our tax invoice, downloaded/delivered in 9 seconds, includes all tax/VAT and complies with 100+ countries' tax regulations (tax exempted in 100+ countries) -- See Avoidance of Double Taxation Agreements (DTAs): List of DTAs signed between Singapore and 100+ countries

Question 4: Do you accept my currency other than USD?

Answer: Yes. If you need your currency to be printed on the invoice, please write an email to [email protected]. In 2 working-hours, we will create a special link for you to pay in any currencies. Otherwise, follow the normal steps: Add to Cart -- Checkout -- Select your currency to pay.