HJ 537-2009 English PDF

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HJ 537-2009: Water quality. Determination of ammonia nitrogen. Distillation-neutralization titration
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GB 5085.7   HJ 536   GB 5085.1   HJ 535   HJ 533   

Basic data

Standard ID: HJ 537-2009 (HJ537-2009)
Description (Translated English): Water quality. Determination of ammonia nitrogen. Distillation-neutralization titration
Sector / Industry: Environmental Protection Industry Standard
Classification of Chinese Standard: Z16
Classification of International Standard: 13.060
Word Count Estimation: 8,841
Date of Issue: 2009-12-31
Date of Implementation: 2010-04-01
Older Standard (superseded by this standard): GB 7478-1987
Quoted Standard: GB/T 16157; HJ/T 55; HJ/T 373; GB/T 6682
Regulation (derived from): Department of Environmental Protection Notice No. 77 of 2009
Issuing agency(ies): Ministry of Ecology and Environment
Summary: This standard specifies the determination of ammonia distillation neutralization titration method. This standard applies to domestic sewage and industrial wastewater ammonia determination. When the sample volume is 250ml, the method detection limit of 0. 05mg/L (expressed in N dollars).

HJ 537-2009: Water quality. Determination of ammonia nitrogen. Distillation-neutralization titration

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Water quality.Determination of ammonia nitrogen.Distillation-neutralization titration National Environmental Protection Standard of the People's Republic Replace GB 7478-87 Determination of ammonia nitrogen in water quality Distillation-neutralization titration Water quality-Determination of ammonia nitrogen -Distillation-neutralization titration Published on December 12,.2009 2010-04-01 Implementation Ministry of Environmental Protection released Ministry of Environmental Protection announcement No. 77 of.2009 In order to implement the "Environmental Protection Law of the People's Republic of China", protect the environment, and protect human health, we now approve "Ammonia of ambient air and exhaust gas. The five standards, such as the determination of Nessler's reagent spectrophotometry, are national environmental protection standards and are released. The standard name and number are as follows. I. Determination of Ammonia Reagent Spectrophotometry for Ambient Air and Exhaust Gas Ammonia (HJ 533-2009); 2. Determination of Ammonia in Ambient Air - Sodium Hypochlorite - Salicylic Acid Spectrophotometry (HJ 534-2009); 3. Determination of Ammonia Nitrogen in Water Quality by Nessler Reagent Spectrophotometry (HJ 535-2009); 4. Determination of Ammonia Nitrogen in Water Quality by Salicylic Acid Spectrophotometry (HJ 536-2009); The above standards have been implemented since April 1,.2010 and published by the China Environmental Science Press. The standard content can be found on the website of the Ministry of Environmental Protection. From the date of implementation of the above standards, the following five national environmental protection standards approved and issued by the former National Environmental Protection Agency shall be abolished. The name and number are as follows. I. Determination of Air Quality Ammonia by Nessler Reagent Colorimetric Method (GB/T 14668-93); 2. Determination of Ammonia for Air Quality - Sodium Hypochlorite - Salicylic Acid Spectrophotometry (GB/T 14679-93); Third, "the determination of ammonium water quality Nessler reagent colorimetric method" (GB 7479-87); 4. Determination of Ammonium in Water Quality by Salicylic Acid Spectrophotometry (GB 7481-87); V. Determination of Distillation and Titration of Ammonium Water (GB 7478-87). Special announcement. December 31,.2009

Content

Foreword..iv 1 Scope..1 2 Method principle..1 3 interference and elimination.1 4 Reagents and materials.1 5 instruments and equipment. 2 6 samples. 2 7 Analysis steps..3 8 result calculation..3 9 Accuracy and precision..3 10 Quality Assurance and Quality Control.3

Foreword

To protect the environment and protect the human body 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 Water Pollution Prevention and Control To develop and standardize the monitoring methods for ammonia nitrogen in water. This standard specifies the distillation-neutralization titration method for the determination of ammonia nitrogen in water. This standard is a revision of the "Determination of Distillation and Titration of Ammonium Water" (GB 7478-87). This standard was first published in 1987. The original standard drafting unit was the Jiangsu Provincial Environmental Monitoring Station. This is the first revision. The main contents of this revision are as follows. -- Revised the name of the standard, modified from "Determination of Water Ammonium by Distillation and Titration" to "Determination of Ammonia Nitrogen in Water Quality" - Neutralization titration. -- In the scope of application, the sensitivity is eliminated; the method detection limit is clarified. -- Added calibration method for hydrochloric acid standard solution. -- Modified the preparation method of the mixed indicator. -- A table of conversion factors for the mass concentration of various forms of nitrogen has been eliminated. -- Added quality assurance and quality control provisions. As of the date of implementation of this standard, the former National Environmental Protection Agency approved and issued the “Distillation of Ammonium Water” approved by the National Environmental Protection Agency on March 14, 1987. And the titration method (GB 7478-87) is abolished. This standard was formulated by the Science and Technology Standards Department of the Ministry of Environmental Protection. This standard is mainly drafted by. Shenyang Environmental Monitoring Center Station. This standard was approved by the Ministry of Environmental Protection on December 31,.2009. This standard has been implemented since April 1,.2010. This standard is explained by the Ministry of Environmental Protection. Iv Water quality - Determination of ammonia nitrogen - Distillation - Neutralization titration

1 Scope of application

This standard specifies the distillation-neutralization titration method for the determination of ammonia nitrogen in water. This standard applies to the determination of ammonia nitrogen in domestic sewage and industrial wastewater. When the sample volume is 250 ml, the detection limit of the method is 0.05 mg/L (both in N).

2 Principle of the method

The pH of the water sample is adjusted to 6.0 to 7.4, and light magnesium oxide is added to make it slightly alkaline, and the ammonia released by distillation is absorbed by the boric acid solution. Take A Base red-methylene blue is an indicator, and the ammonia nitrogen (in N) in the distillate is titrated with a hydrochloric acid standard solution.

3 interference and elimination

Substances that can be distilled under the conditions specified in this standard and which are capable of reacting with an acid interfere with the measurement. For example, urea, volatile amines and Chloramine in chlorinated samples, etc.

4 reagents and materials

Unless otherwise stated, the reagents used in the analysis were analyzed analytical reagents in accordance with national standards, and the experimental water was prepared according to 4.1. water. 4.1 No ammonia water, prepared in one of the following ways in an ammonia-free environment (see 10.1 for inspection without ammonia). 4.1.1 Ion exchange method The distilled water was passed through a strong acid cation exchange resin (hydrogen type) column, and the effluent was collected in a glass bottle with a ground plug. Outflow per liter Add 10 g of the same resin to facilitate storage. 4.1.2 Distillation method Add 0.1 ml of sulfuric acid (4.2) to 1 000 ml of distilled water, distill it in a full glass distiller, and discard the first 50 ml of distillate. Approximately 800 ml of distillate was then collected in a glass vial with a ground plug. 10 g of strong acid cation exchange resin per liter of distillate (hydrogen type). 4.1.3 Water Purifier Method Prepared directly using a commercially available water purifier. 4.2 Sulfuric acid, ρ(H2SO4) = 1.84 g/ml. 4.3 Hydrochloric acid, ρ = 1.19 g/ml. 4.4 absolute ethanol, ρ =0.79 g/ml. 4.5 Anhydrous sodium carbonate (Na2CO3), a reference reagent. 4.6 Light Magnesium Oxide (MgO), free of carbonates. Heat at 500 ° C to remove the carbonate. 4.7 sodium hydroxide solution, c (NaOH) = 1 mol/L. Weigh 20 g of sodium hydroxide (NaOH) dissolved in about.200 ml of water, cool to room temperature, and dilute to 500 ml. 4.8 Sulfuric acid solution, c(1/2H2SO4) = 1 mol/L. Measure 2.8 ml of sulfuric acid (4.2) and slowly add 100 ml of water. 4.9 Boric acid (H3BO3) absorption solution, ρ = 20 g/L. Weigh 20 g of boric acid dissolved in water and dilute to 1 000 ml. 4.10 methyl red indicator solution, ρ = 0.5 g/L. Weigh 50 mg of methyl red in 100 ml of ethanol (4.4). 4.11 bromothymol blue indicator, ρ =1 g/L. Weigh 0.10 g of bromothymol blue in 50 ml of water, add 20 ml of ethanol (4.4), and dilute to 100 ml with water. 4.12 Mixed indicator Weigh.200 mg of methyl red in 100 ml of ethanol (4.4); otherwise weigh 100 mg of methylene blue in 100 ml of ethanol (4.4). Take two portions of methyl red solution and one portion of methylene blue solution for use. This solution is stable for 1 month. 4.13 sodium carbonate standard solution, c (1/2Na2CO3) = 0.020 0 mol/L. Weigh anhydrous sodium carbonate (4.5) 0.530 0 g dried at 180 ° C for 2 h, dissolve in freshly boiled cold water, and transfer to 500 ml volumetric flask. Medium, diluted to the mark. 4.14 Hydrochloric acid standard titration solution, c (HCl) = 0.02 mol/L. Measure 1.7 ml of hydrochloric acid (4.3) in a 1 000 ml volumetric flask and dilute to the mark with water. Calibration method. Pipette 25.00 ml sodium carbonate standard solution (4.13) in a 150 ml Erlenmeyer flask, add 25 ml water, add 1 drop of methyl red The indicator liquid (4.10) was titrated to a reddish color with a hydrochloric acid standard solution (4.14). Record the volume consumed. Calculate hydrochloric acid solution using formula (1) Concentration of liquid (4.14). 1(HCl) c Vc ×= (1) Where. c--hydrochloric acid standard titration solution (4.14) concentration, mol/L; C1--sodium carbonate standard solution (4.13) concentration, mol/L; Volume of V1--sodium carbonate standard solution (4.13), ml; V2--volume of hydrochloric acid standard titration solution (4.14), ml. 4.15 glass beads 4.16 Antifoaming agents, such as paraffin fragments.

5 Instruments and equipment

5.1 Ammonia Nitrogen Distillation Unit. consists of 500 ml Kay flask, nitrogen ball, straight condenser and conduit. The end of the condenser can be connected for a suitable period. The length of the dropper is such that the tip of the outlet is immersed under the surface of the absorbing liquid. A distillation flask can also be used. 5.2 Acid burette. 50 ml.

6 samples

6.1 Sample storage Water samples should be collected in polyethylene or glass bottles and analyzed as soon as possible. If you need to save, you should add sulfuric acid to acidify the water to pH< 2, 2~5. It can be stored for 7 days at °C. 6.2 Sample pre-distillation Transfer 50 ml of boric acid absorbing solution (4.9) into the receiving bottle to ensure that the condensing tube outlet is below the level of the boric acid solution. Divide 250 ml of water Sample (such as high ammonia nitrogen content, can take less water sample, add water to 250 ml) into the flask, add 2 drops of bromothymol blue indicator (4.11), If necessary, adjust the pH to 6.0 with a sodium hydroxide solution (4.7) or sulfuric acid solution (4.8) (the indicator is yellow) ~ 7.4 (the indicator is blue) Color), add 0.25 g of light magnesium oxide (4.6) and several glass beads, if necessary, add anti-foaming agent (4.16), immediately connect nitrogen ball and condenser The distillation was heated to a distillate rate of about 10 ml/min, and the distillation was stopped when the distillate reached.200 ml.

7 Analysis steps

7.1 Sample Analysis Transfer all distillate to the Erlenmeyer flask, add 2 drops of mixed indicator (4.12), and titrate with hydrochloric acid standard titration solution (4.14). The end point of the distillate from green to lavender is recorded, and the volume Vs of the standard hydrochloric acid titration solution consumed is recorded. 7.2 Blank test Replace the water sample with 250 ml of water, pre-distillate according to 6.2, titrate according to 7.1, and record the body of the standard hydrochloric acid titration solution consumed. Product Vb.

8 Calculation of results

The concentration of ammonia nitrogen in the water sample is calculated by equation (2). Sb N 14.01 1000 VV c ρ −= × × × (2) Where. ρN--the concentration of ammonia nitrogen in the water sample (in N), mg/L; V--the volume of the sample, ml; Vs--the volume of hydrochloric acid standard titration solution consumed by the titration sample, ml; Vb--the volume of hydrochloric acid standard titration solution consumed by titration blank, ml; C--concentration of hydrochloric acid standard solution for titration, mol/L; 14.01--Atom atomic weight, g/moL.

9 Accuracy and precision

Table 1 Accuracy and precision of standard and actual samples Sample ammonia nitrogen content/(mg/L) Repeatability limit r/(mg/L) Reproducibility limit R/(mg/L) relative error /% Standard 1 2.76 0.106 0.146 0.73 Standard 2 23.8 0.641 1.39 −0.42 Surface water 6.60 0.109 0.515 - Domestic sewage 21.4 0.694 3.09 - Note. Five laboratories participated in the validation, and each laboratory repeated the number of measurements for each sample six times. 10 Quality Assurance and Quality Control 10.1 Inspection without ammonia. 250 ml of water should be titrated with hydrochloric acid standard solution (4.14). The volume of the standard solution for consumption of hydrochloric acid should not be greater than 0.04 ml. 10.2 Distillator cleaning. Add 350 ml of water to the distillation flask, add several glass beads (4.15), install the instrument, and distill to at least collect. After 100 ml of water, the distillate and the residual liquid in the bottle were discarded. 10.3 Pre-distillation. At the beginning of the distillation, the ammonia gas is evaporated faster, and the heating cannot be too fast, otherwise the water sample will be bumped and the distillate temperature will rise. High, ammonia absorption is incomplete, and the distillate rate should be kept at about 10 ml/min. If residual chlorine is present in the water sample, a few more crystalline sulfur should be added. Sodium sulfate (Na2S2O3 or Na2S2O3·5H2O) was removed. 10.4 When calibrating the standard titration solution of hydrochloric acid, at least 3 times of parallel titration, the maximum allowable deviation of parallel titration is not more than 0.05 ml. ......

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