HJ 636-2012

Translated English of Chinese Standard: HJ636-2012

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HJ
ENVIRONMENTAL PROTECTION STANDARD

OF THE PEOPLE’S REPUBLIC OF CHINA

HJ 636-2012
Replacing GB 11894-89

Water quality - Determination of total nitrogen -

Alkaline potassium persulfate digestion UV
spectrophotometric method
水质 总氮的测定

碱性过硫酸钾消解紫外分光光度法

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Issued on: February 29, 2012 Implemented on: June 1, 2012

Issued by: Ministry of Environmental Protection

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 HJ 636-2012

ANNOUNCEMENT
Ministry of Environmental Protection of PRC
No. 16, 2012

In order to implement Environmental Protection Law of the People 's Republic of

China, to protect environment, to protect human health, to standardize
environmental monitoring, it hereby approves that five standards - Determination
of soil, ammonia nitrogen, nitrite nitrogen, nitrate nitrogen Extraction of
potassium chloride solution - Spectrophotometric method, as national
environmental protection standards and to be issued.

The names and numbers of standards are as follows:

1. Soil-Determination of ammonium, nitrite and nitrate by extraction with

potassium chloride solution -spectrophotometric methods (HJ 634-2012);

2. Soil - Determination of water-soluble and acid-soluble sulfate - Gravimetric

method (HJ 635-2012);

3. Water quality. Determination of total nitrogen. Alkaline potassium persulfate

digestion UV spectrophotometric method (HJ 636-2012);

4. Water quality- Determination of petroleum oils and animal and vegetable

oils- Infrared spectrophotometry (HJ 637-2012);

5. Ambient air-Determination of phenolic compounds by high performance

liquid chromatography (HJ 638-2012).

The abovementioned standards shall be implemented since June 1, 2012 and

inquired at the website of China Ministry of Environmental Protection
(bz.mep.gov.cn).

Since the date of implementation of the abovementioned standards, the following

two national environmental protection standards shall be abolished. The
standard names and number are as follows:

1. Water quality - Determination of total nitrogen - Alkaline potassium

persulfate digestion - UV spectro photometric method (GB 11894-89)

2. Water quality - Determination of petroleum oil, animal and vegetable oils -

Infrared photometric method (GB/T 16488-1996)

It hereby announces.

February 29, 2012

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 HJ 636-2012

Table of Contents
ANNOUNCEMENT Ministry of Environmental Protection of PRC .................... 2

Foreword .......................................................................................................... 4

1 Application scope ....................................................................................... 6

2 Normative references ................................................................................. 6

3 Terms and definitions ................................................................................. 6

4 Method and principle .................................................................................. 7

5 Interference and elimination ....................................................................... 7

6 Reagents and materials ............................................................................. 7

7 Apparatus ................................................................................................... 8

8 Sample ....................................................................................................... 9

9 Sample ....................................................................................................... 9

10 Results calculation and representation ................................................... 10

11 Precision and accuracy........................................................................... 11

12 Quality assurance and quality control ..................................................... 11

13 Notices ................................................................................................... 12

Annex A (Informative) Method for determination of nitrogen content in sodium

hydroxide and potassium persulfate .............................................................. 13

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 HJ 636-2012

Foreword

This Standard is specified so as to implement Environmental Protection Law of

the People 's Republic of China, Water Pollution Control Act of the People 's
Republic of China, to protect environment, to protect human health, to
standardize the determination method for total nitrogen in water.

This Standard specifies determination of total nitrogen in surface water,

groundwater, industrial wastewater and domestic sewage - Alkaline potassium
persulfate digestion UV spectrophotometric method.

This Standard is the modification of Water quality - Determination of total

nitrogen - Alkaline potassium persulfate digestion - UV spectro photometric
method (GB 11894-89).

This Standard was issued in 1989 for the first time. The original drafting
organization was Shanghai Environmental Monitoring Center. This is the first
revision. The main content of revision is as follows:

- expanded the scope of standard application;

- added nitrogen content requirements of sodium hydroxide and potassium

persulfate and method for determination of nitrogen content;

- added quality assurance and quality control provisions;

- added terms and conditions on precautions.

Since the date of implementation of this Standard, the national environmental

protection standard: Water quality - Determination of total nitrogen - Alkaline
potassium persulfate digestion - UV spectro photometric method (GB 11894-
89) approved and issued by former China State Environmental Protection
Administration on December 25, 1989 shall be abolished.

Annex A of this Standard is informative.

This Standard is organized and made by Department of Science and

Technology Standards, Ministry of Environmental Protection.

Main drafting organization of this Standard: Dalian Environmental Monitoring

Center.

The verification organizations of this Standard: Tianjin Environmental

Monitoring Center, Liaoning Provincial Environmental Monitoring Experimental
Center, Shenyang Environmental Monitoring Center Station, Anshan
Environmental Monitoring Center Station, Jinzhou Environmental Monitoring
Center Station, Yingkou Environmental Monitoring Center Station.

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 HJ 636-2012

Water quality - Determination of total nitrogen -

Alkaline potassium persulfate digestion UV
spectrophotometric method

1 Application scope

This Standard specifies water quality - determination of total nitrogen - alkaline

potassium persulfate digestion UV spectrophotometric method.

This Standard is applicable to the determination of total nitrogen in surface

water, groundwater, industrial wastewater and domestic sewage.

When the amount of sample is 10 ml, the detection limit of this method shall be
0.05 mg/L; the measuring range shall be 0.20 ~ 7.00 mg/L.

2 Normative references

The following standards contain the provisions which, through reference in this
Standard, constitute the provisions of this Standard. For undated reference
documents, the latest versions apply to this Standard.

HJ/T 91 Technical specifications requirements for monitoring of surface

water and waste water

HJ/T 164 Technical specifications for environmental monitoring

3 Terms and definitions

For the purposes of this document, the following terms and definitions apply.

total nitrogen (TN)

under the conditions specified by this Standard, total nitrogen in dissolved

nitrogen and suspended solids of samples which can be determined, including
nitrogen in nitrite nitrogen, nitrate nitrogen, inorganic ammonium salt, dissolved
ammonia and most of the organic nitrogen compounds

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 HJ 636-2012

Dry it at 105 ~ 110°C for 2h. Cool it to room temperature in dryer.

6.5 Concentrated hydrochloric acid: ρ (HCI) = 1.19 g/ml

6.6 Concentrated sulfuric acid: ρ (H2SO4) = 1.84 g/ml

6.7 Hydrochloric acid solution: 1+9

6.8 Sulfuric acid solution: 1+35

6.9 Sodium hydroxide solution: ρ (NaOH) = 200 g/L

Weigh 20.0 g of sodium hydroxide (6.2) and make it dissolved in a small amount
of water. Dilute to 100 ml.

6.10 Sodium hydroxide solution: ρ (NaOH) = 20 g/L

Weigh 10.0 ml of sodium hydroxide solution (6.9). Use water to dilute to 100 ml.

6.11 Alkaline potassium persulfate solution

Weigh 40.0 g of potassium persulfate (6.3) and make it dissolved in 600 ml of

water (it may heat in 50°C water bath till all is dissolved). Weigh 15.0 g of
sodium hydroxide (6.2) in 300 ml of water. When sodium oxide solution is
cooled to room temperature, mix these two solutions and set volume to 1000
ml. Store in polyethylene bottle, which can be stored for one week.

6.12 Potassium nitrate standard stock solution: ρ (N) = 100 mg/L

Weigh 0.7218 g of potassium nitrate (6.4) and make it dissolved in appropriate

amount of water. Move it to 1000 ml volumetric flask. Use water to dilute it to
gauge mark. Well mix. Add 1 ~ 2 ml of trichloromethane as protector. Store it in
dark place at 0 ~ 10°C. It can be maintained stable for 6 months. It can also
directly purchase the commercially available certified standard solution.

6.13 Potassium nitrate standard use solution: ρ (N) = 10.0 mg/L

Weigh 10.00 ml of potassium nitrate standard stock solution (6.12) to 100 ml

volumetric flask. Use water to dilute it to gauge mark. Well mix. Prepare it when
required.

7 Apparatus

7.1 UV spectrophotometer: with 10 mm quartz cuvette

7.2 High-pressure steam sterilizer: the maximum working pressure shall not
be less than 1.1 ~ 1.4 kg/cm2; the maximum working temperature shall not be
less than 120 ~ 124°C.

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 HJ 636-2012

corresponding Ar value as ordinate to draw calibration curve.

Ab=Ab220 − 2Ab275 ………………………………. (2)

As=As220 − 2As275 ………………………………... (3)

Ar=As − Ab ………………………………………… (4)

Where,
Ab - corrected absorbance of zero concentration (blank) solution;
Ab220 - corrected absorbance of zero concentration (blank) solution at wavelength of 220
nm;
Ab275 - corrected absorbance of zero concentration (blank) solution at wavelength of 275
nm;
As - corrected absorbance of standard solution;
As220 - corrected absorbance of standard solution at wavelength of 220 nm;
As275 - corrected absorbance of standard solution at wavelength of 275 nm;
Ar - difference between corrected absorbance of standard solution and corrected
absorbance of zero concentration (blank) solution.

9.2 Determination

Weigh 10.00 ml of sample (8.2) in 25 ml grinding glass colorimetric tube with

plug. Determine according to 9.1 steps.

NOTE 2 When the nitrogen content in the sample exceeds 70 µg, it may reduce the
sampling amount and add water to dilute it to 10.00 ml.

9.3 Blank test

Use 10.00 ml of water to replace sample. Determine according to 9.2 steps.

10 Results calculation and representation

10.1 Results calculation

Calculate sample corrected absorbance and blank test corrected absorbance

difference Ar according to equations (2) ~ (4). The total nitrogen mass
concentration in sample ρ (mg/L) shall be calculated according to equation (5).

Where,
ρ - total nitrogen (in N) mass concentration in sample, in mg/L;
Ar - difference between corrected absorbance of sample and corrected absorbance of
blank test;
a - intercept of calibration curve;

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 HJ 636-2012

total nitrogen content of sample is > 1.00 mg/L, the relative deviation of the
measured results shall be ≤ 5%. The results shall be reported in the average of
two parallel samples.

12.4 Each batch of sample should determine the standard solution of a

calibration curve midpoint concentration. The relative error between its
determination results and this point concentration of calibration curve shall be
≤ 10%; otherwise, it shall redraw the calibration curve.

12.5 At least 10% of the spiked sample should be determined for each batch
of sample. When the number of sample is less than 10, it shall at least
determine a spiked sample. Spike recovery should be between 90% ~ 110%.

13 Notices

13.1 Some nitrogen-containing organic compounds can not be completely

converted to nitrates under the conditions specified in this Standard.

13.2 The determination should be carried out in a laboratory environment free

of ammonia so as to prevent impact of environmental cross-contamination on
the determination results.

13.3 The vessel used in the experiment and the high pressure steam sterilizer
should be free of nitrogen pollution. The glassware used in the experiment
should be soaked in hydrochloric acid solution (6.7) or sulfuric acid solution
(6.8). Rinse with tap water and then rinse with ammonia-free water for several
times. Use immediately after washing. Autoclaves should be cleaned weekly.

13.4 In alkaline potassium persulfate solution preparation process, excessive

temperature shall lead to failure of potassium persulfate decomposition.
Therefore, it must control the water bath temperature below 60°C. And it shall
wait the sodium hydroxide solution cool to room temperature. Then mix it with
potassium persulfate solution. Set volume.

13.5 When using high pressure steam sterilizer, the pressure gauge should
be checked regularly. And it should check the seal of rubber seal so as to avoid
leakage caused by decompression.

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 HJ 636-2012

A.2.7 Hydrazine sulfate solution: ρ (H4N2•H2SO4) = 0.7 g/L

Weigh 0.35 g of hydrazine sulfate and make it dissolved in water. Dilute to 500
ml. Prepare it when required.

A.2.8 Sulfonamide solution: ρ (C6H8N2O2S) = 10 g/L

Weigh 2.0 g of sulfonamide and make it dissolved in 60 ml of concentrated

hydrochloric acid (6.5). Use water to dilute it to 200 ml.

A.2.9 N-1-naphthalene ethylenediamine hydrochloride solution: ρ

(C12H14N2·2HCl) = 1 g/L

Weigh 0.2 g of N-1-naphthalene ethylenediamine hydrochloride and make it

dissolved in water. Dilute it to 200 ml.

A.2.10 Nitrogen standard solution: ρ (N) = 1.00 mg/L

Weigh 10.00 ml of potassium nitrate standard stock solution (6.12) to 1000 ml

volumetric flask. Add water to dilute it to gauge mark. Well mix it. Prepare it
when required.

A.2.11 Sodium hydroxide test solution: ρ (NaOH) = 100 g/L

Weigh 10.0 g of sodium hydroxide to dissolve in 70 ml of water. Set volume to

100 ml after cooling.

A.2.12 Sodium hydroxide test solution

A.2.12.1 Sample solution

Add 25.0 ml of sodium hydroxide test solution (A.2.11) and 40.0 ml of water in
125 ml digestion bottle.

A.2.12.2 Standard solution

In 125 ml digestion bottle, add 25.0 ml of sodium hydroxide test solution (A.2.11),
30.0 ml of water and 10.00 ml of nitrogen standard solution (A.2.10).

A.2.12.3 Blank solution

In 125 ml digestion bottle, add 5.0 ml of sodium hydroxide test solution (A.2.11)
and 60.0 ml of water.

A.2.13 Potassium persulfate test solution: ρ (K2S2O8) = 46 g/L

Weigh 9.2 g of potassium persulfate and make it dissolved in water. Set volume
to 200 ml.

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