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HJ 535-2009Water Quality - Determination of Ammonia Nitrogen - Nessler Reagent Spectrophotometry (English PDF)

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Issued by

Ministry of Environmental Protection Ministry of Environmental Protection of the PRC Announcement

Level / Type

National · Mandatory

Issue date

December 31, 2009

Implementation date

April 1, 2010

Scope

HJ 535-2009 (Water Quality - Determination of Ammonia Nitrogen - Nessler Reagent Spectrophotometry) is available as an English-translated PDF.

HJ 535-2009 — This Standard specifies Nessler's reagent spectrophotometry to determine the ammonia nitrogen in water. This Standard is applicable to determine the ammonia nitrogen in surface water, underground water, domestic sewage, and industrial waste water.

When the volume of water sample is 50ml, and 20mm cuvette is used; the detection limit for this method is 0.025mg/L, the lower determination limit is 0.10mg/L, and the upper determination limit is 2.0mg/L (calculated as per N).

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Document preview — HJ 535-2009

National Standard of the People's Republic of China

Issued by: Ministry of Environmental Protection Ministry of Environmental Protection of the PRC Announcement

Contents

  • Foreword...5
  • 1 Scope...7
  • 2 Method Principles...7
  • 3 Interference and Elimination...7
  • 4 Reagents and Materials...8
  • 5 Apparatus and Equipment...10
  • 6 Samples...10
  • 7 Analysis Procedures...11
  • 8 Result Calculation...12
  • 9 Accuracy and Precision...13
  • 10 Quality Assurance & Quality Control...13

Foreword

This Standard was prepared for the purposes of implementing Environmental

Protection Law of the People's Republic of China, and Water Pollution Prevention and

Control Law of the People's Republic of China, protecting environment, safeguarding

human health, as well as regulating the detection method of ammonia nitrogen in

water.

This Standard specified Nessler's Reagent Spectrophotometry to measure the

ammonia nitrogen in water.

This Standard revised Water Quality - Determination of Ammonium - Nessler's

Reagent Colorimetric Method (GB 7479-87).

This Standard was first-time published in 1987; the drafting organization of the original

standard was Jiangsu Environmental Monitoring Central Station; this is the first-time

revision. The major revised contents are as follows.

--- Standard name was changed FROM Water Quality - Determination of

Ammonium - Nessler's Reagent Colorimetric Method TO Water Quality -

Determination of Ammonia Nitrogen – Nessler's Reagent Spectrophotometry.

--- Add the cuvette's optical path length (10-20mm); reduce the detection limit of

the method; expand the applicable scope of the method. Clearly define the

upper and lower detection limit of the method.

--- Delete the visual colorimetry.

--- Regulate and adjust the structure and format of the standard text.

--- Add the precautions to the key steps such as main reagent preparation and the

sample pretreatment.

--- Combine the calculation formula of the results.

Since the implementation date of this Standard, the Water Quality - Determination of

Ammonium - Nessler's Reagent Colorimetric Method (GB 7479087) that was

approved & published by the original State Environmental Protection Agency on

March 14, 1987 shall be abolished.

This Standard was organized-formulated by Science, Technology and Standard

Division of Ministry of Environmental Protection, Department.

Chief drafting organization of this Standard. Shenyang Environmental Monitoring

Center.

This Standard was approved by Ministry of Environmental Protection on December 31,

Water Quality – Determination of Ammonia Nitrogen –

Nessler's Reagent Spectrophotometry

Warning. Mercuric chloride (HgCl2) and mercuric iodide (HgI2) are highly toxic

substances; avoid the dermal and oral exposure.

1 Scope

This Standard specifies Nessler's reagent spectrophotometry to determine the

ammonia nitrogen in water.

This Standard is applicable to determine the ammonia nitrogen in surface water,

underground water, domestic sewage, and industrial waste water.

When the volume of water sample is 50ml, and 20mm cuvette is used; the detection

limit for this method is 0.025mg/L, the lower determination limit is 0.10mg/L, and the

upper determination limit is 2.0mg/L (calculated as per N).

2 Method Principles

Ammonia nitrogen, existed in the free state of ammonia and ammonium ions, reacts

with Nessler's reagent, and generates light reddish brown complex compound; the

absorbance of such complex compound is proportional to the ammonia nitrogen

contents, then determine the absorbance at the wavelength of 420nm.

3 Interference and Elimination

When water sample contains suspended solids, residual chlorine, metal ions such as

calcium-magnesium, sulfides and organic substances, then they may generate

interference and needs proper treatment, so as to eliminate the influence on the

determination.

If there is residual chlorine in the sample, add proper amount of sodium thiosulfate

solution to remove; use potassium iodide-starch test paper to test whether the

residual chlorine was eliminated completely. When colorization, add proper amount of

potassium sodium tartrate solution, which can eliminate the interference from metal

ions such as calcium-magnesium. If the sample is thick or colorful, it can be treated

with pre-distillation or flocculation methods.

Weigh 20g of hydrochloric acid; dissolve into water; dilute to 1L.

4.12 Bromthymol blue indicator, rho=0.5g/L.

Weigh 0.05g of bbromthymol blue; dissolve into 50ml of water; add 10ml of anhydrous

ethanol; then use water to dilute to 100ml.

4.13 Potassium iodide-starch test paper

Weigh 1.5g of soluble starch into a beaker; use small amount of water to make it into

paste state; add 200ml of boiling water; stir-mix evenly, and cool down. Add 0.50g of

potassium iodide (KI) and 0.50 g of sodium carbonate (Na2CO3); use water to dilute to

250ml. After immersion of the filter paper, take it out and get dry; then seal-store in the

brown bottle.

4.14 Ammonia nitrogen standard solution

4.14.1 Standard stock solution of ammonia nitrogen, rhoN=1000µg/ml.

Weigh 3.8190g of ammonium chloride (NH4Cl, guaranteed reagent, dry for 2h at

100~105°C); dissolve into water; move to 1000ml flask; dilute to the marked-scale; it

can be stored for 1 month at 2~5°C.

4.14.2 Ammonia nitrogen standard working solution, rhoN=10µg/ml.

Absorb 5.00ml of ammonia nitrogen standard stock solution (4.14.1) into a 500ml

flask; dilute to the marked-scale. It shall be prepared before use.

5 Apparatus and Equipment

5.1 Visible-light spectrophotometer. with 20mm cuvette.

5.2 Ammonia nitrogen distillation device. consists of 500ml Kjeldahl flask, nitrogen

ball, straight condenser and catheter; the end of condenser can be directly connected

with certain length of dropper, so that the outlet tip is immersed under the absorption

liquid surface. 500ml distillation flask can also be used.

6 Samples

6.1 Sample collection and preservation

Collect water sample into the polyethylene or glass bottle; analyze as soon as

possible. If it needs preserving, add sulfuric acid so as to ; make the acidify the water

sample till pH< 2; it can be stored for 7d at 2~5°C.

9 Accuracy and Precision

For the standard solution of which the ammonia nitrogen concentration is

1.21mg/L, the repeatability limit is 0.028mg/L, the reproducibility limit is 0.075mg/L,

and the recovery rate is 94%~104%.

For the standard solution of which the ammonia nitrogen concentration is

1.47mg/L, the repeatability limit is 0.024mg/L, the reproducibility limit is 0.066mg/L,

and the recovery rate is 95%~105%.

10 Quality Assurance & Quality Control

10.1 The absorbance of reagent blank shall not exceed 0.030 (10mm cuvette).

10.2 Preparation of Nessler's reagent

In order to guarantee the good color developing ability of the Nessler's reagent,

during the preparing period, it must control the adding amount of HgCl2, till...

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This preview omits tables, figures, formulas and parts of the technical clauses. The complete document — 13 pages — is available in the English PDF.

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