TRAINING MATERIALS FOR

WASTE WATER TREATMENT LINE

Basic Training for Test

Content
Common Test Standard for Sewage Quality
Measurement of Suspended Solids Weight Method ------------------------------------------------------------------------------------------------3 Measurement of CODcr, by potassium bichromate method (GB11914-89) -----------------------------------------------------------------------------------------------6 Measurement of Biochemical Oxygen Demand for Five Days (BOD5) ----------------------------------------------------------------------------------------------10 Measurement of Ammonia Nitrogen Volumetric Method ----------------------------------------------------------------------------------------------17 Appendix A-------------------------------------------------------------------------------------19 Preparation and Calibration of Sulfuric Acid Standard Titrimetric Solution

Common Test Standard for Sewage Quality

Measurement of Suspended Solids Weight Method
1. Content and scope The present standard stipulates that the suspended solids in domestic sewage shall be measured by weight method. The present standard is applied to the measurement of suspended solids in the sewage that drained into domestic sewer and the sewage in sewage treatment plant. When the volume of the reagent is 100 mL, the minimum concentration measured by the present method is 5 mg/L. 2. Outline of method The non-dissolved solid suspended in the sample shall be stopped by pickling asbestos layer, so as to be measured by weight method.
3.

Reagent and material Analytic pure reagent and distilled water shall be used.

HCl: =1.19 g/mL 3.2 3.3 Pickling asbestos Preparation of asbestos suspension Put the pickling asbestos (15g) into beaker then add water (300 mL) to stir until the coarse asbestos fiber settling to the bottom. Then pour the supernatant to a glass bottle. Repeat the above procedures for 3 times. Store the asbestos suspension in a glass bottle and the left coarse asbestos solution in another one. If there is no pickling asbestos, take non-treated asbestos (15 g) and moistened by water. Then add 20 mL HCl and heat it in the boiled water bath for 12 hours. After being washed by hot water, the pickling asbestos is ready for using. 4. 4.1 4.2 Apparatus 30 mL orifice ceramic crucible Vacuum pump
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4.3 4.4 4.5 5.

Filter flask Drying oven Analytic balance: sensitivity 0.1 mg Sample Typical sample shall be used for suspended solids measurement.

6. 6.1

Procedure Lying of asbestos layer Put the orifice ceramic crucible (30 mL) on the filter flask and pour the coarse asbestos suspension into the crucible. The asbestos suspension shall be filtered to form asbestos layer of 1~2 mm thick. Then pour the fine asbestos suspension into the crucible and wash by water until there is no asbestos fiber contained in the solution. The water stream filtered through the asbestos layer that laid correctly should be discontinued and dense water drops, instead of continuous water line.

6.2

Weighing of empty crucible Dry the crucible with asbestos layer for 1 hour under 105 and then cool for 30 min in the drying oven. Weigh the crucible at once after being taken out from the dryer. Repeat the operations of drying, cooling and weighing until constant weight is obtained. (Namely the weight difference between two weighing is less than or equal to 0.5 mg).

6.3

Reagent Take 100 mL lab sample as the reagent. The volume of the reagent may be increased or reduced according to the approximate content of the suspended solids.

6.4

Filtering After being weighed, put the crucible on the filter flask, and moistened by water. First filter the clear supernatant of the reagent and then pour the left cloudy solution into the crucible. Wash the vessel which contain the reagent by water for several times and also pour into the crucible for filtering.

6.5

Weighing of the total weight of the crucible and suspended solids Operation procedures are the same as item 6.2.

7.

Indication of analysis result The concentration of suspended solids (C) shall be shown in mg/L, and calculated by the following formula:

C=

m2 m1 1,0001,000 V

Where: m1----mass of the crucible (g) m2----total mass of the crucible and suspended solids (g) V----volume of the reagent (mL) The result shall be shown as a integer

II Measurement of CODcr, by Potassium Bichromate Method (GB11914-89)

1. 1.1 Description Principle In strong acidic solution, certain amount of potassium bichromate is used to oxidize reducing substances in the water sample. For overdosage of potassium bichromate, phenanthroline ferrioin is used as indicator, and ferrous ammonium sulfate is used for residual titration. And to calculate the oxygen consuming amount of reducing substance in the water sample. 1.2 Acidic potassium bichromate has strong oxidability and can oxidize most organics. When added with silver sulfate as catalyst, straight chain aliphatic compound (fatty compound) can be oxidized completely, but aromatic organics are difficult to be oxidized. Pyridine cant be oxidized. Volatile straight chain aromatic compounds and benzene exist in vapour phase and cannot contact with oxidant solution. Therefore the oxidization of those organics are not obvious. Chloride ion can be oxidized by potassium bichromate and can react with silver sulfate to produce settlement, which will effect the measurement. By adding mercuric sulfate into water sample in refluxing complex is obtained and interfere can be eliminated. Sample with chloride ion content being higher than 2000mg/L shall be diluted quantitatively before measurement, in order to bring chloride ion content down to below 2000mg/L. 1.3 Application of the method Potassium bichromate with 0.25mol/L concentration can be used for measurement of COD value more than 50mg/L; and potassium bichromate solution with 0.025mol/L concentration can be used for measurement of COD value between 5-50mg/L. But the result is not so accurate. 2. Apparatus and reagents

Apparatus Refluxing device: whole glass refluxing device with 250mL conical flask; Heating device: electronic heating plate or rheostatic electric furnace; 50mL acidic titration tube Reagent Potassium bichromate standard solution (1/6K2Cr2O7) 0.2500mol/L: Take 12.258g by
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weighing standard or class A pure potassium bichromate which has been dried for 2 hours at 120, to dissolve it in the water, and move to 1000mL volumetric flask, dilute it to reference mark, and then shake the flask to make the solution uniform. Phenanthroline ferrous indicator: weigh 1.485g ferrioin and 0.695g ferrous sulfate (FeSO47H2O), dissolve it in water and dilute to 100mL. It shall be stored in brown color bottle. Ferrous ammonium sulfate standard solution [(NH4)2FeSO4]26H2O0.1mol/L: weigh 39.5g ferrous ammonium sulfate, dissolve it in water, add 20mL strong sulfuric acid slowly with stirring. Move the solution to 1000mL volumetric flask after cooling. Add water to dilute to mark, and shake the flask to make the solution uniformly. The solution shall be calibration by potassium bichromate before using. Calibration method: Accurately take 10.00mL potassium bichromate standard solution to 500mL conical flask. Add water to dilute to 110mL. Slowly add 30mL strong sulfuric acid, and shake the flask to make the solution uniform. After cooling, add 3 drops of phenanthroline ferrous indicator (about 0.15mL), and titrate with ferrous ammonium sulfate solution. Color of solution turns from yellow to blue-green and to red-brown at last. 0.2500 10.00 C [(NH4)2Fe(S04)2]= V Where, CConcentration of ferrous ammonium sulfate standard solution (mol/l) Vconsuming amount of ferrous ammonium sulfate standard titrate solution (mL) 2.2.4 Sulfuric acid-silver sulfate solution: add 25g silver sulfate to 2500mL strong sulfuric acid, set it at stand-still for 1-2 days. And shake container from time to time to promote dissolving (Add 5g silver sulfate into 500mL strong sulfuric acid if 2500mL container is not available. Mercuric sulfate: crystal or powder.

2.2.5 3.

Steps

3.1 Take 20.00mL uniformly mixed water sample (or certain amount of water sample diluted to 20.00ml) into 250mL ground refluxing conical flask. Add 10.00mL potassium bichromate standard solution and some small glass beads or zeolites. Connect ground refluxing condensate tube. Add 30mL sulfuric acidsilver sulfate solution and slowly shake the conical flask to make the solution mixing uniformly. Heat and reflux for 2 hours starting from boiling. Note: 1. For high COD waste water sample, take waste water and reagent with volume 1/10 of above needed amount, and be put into 15150mm hard
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glass test-tube and shake it. Observe the color if it changes to green after heating. If the solution shows green, waste water sample amount shall be reduced to certain amount no green color is found. In this way, water sample volume required for analysis can be determined. During dilution, sample amount shall not be less than 5mL, if the COD is high, the sample shall be diluted repeatedly. 2. If the chloride ion in waste water is more than 30mg/L, 0.4g mercuric sulfate shall be added to refluxing conical flask at first, then add 20.00mL of waste water or certain amount waste water dilute to 20.00mL and shake it. Following steps after are same as above. 3.2 After cooling, 80ml water is used to flush the wall of condensate tube, take off the conical flask. Total volume of solution shall not be less than 140mL, otherwise the end of titration will not be so obvious, because of too strong acidity.

3.3 After re-cooling, add 3 drops of phenanthroline ferrous indicator, and be titrated with ferrous ammonium sulfate standard solution, if color of solution changes from yellow to blue-green and to red-brown, it is the end. Consumption of ferrous ammonium sulfate standard solution shall be recorded. 3.4 At the time of measuring sample, 20.00mL redistilled water is used for blank test in same steps. Record consumption of ferrous ammonium sulfate standard titrate solution. Calculation: (o-L)C81000 CODcr(O2mg/L) V Where, C-concentration (mol/l) of ferrous ammonium sulfate standard solution; V0-consumption of ferrous ammonium sulfate standard solution in titration of blank test; V1- consumption of ferrous ammonium sulfate standard solution in titration of sample; V- volume of sample(ml); 8-oxygen (1/4O2) molar mass (g/mol). Precision and accuracy: Potassium acid phthalate standard solution (COD 150mg/l) is analyzed in 6 test room with unified standard solution. Relative standard difference in test room is 4.3% and relative standard difference is 5.3% between results from each test room. Precautions:
1.

At most 40mg chloride ion can be complexed by 0.4g mercuric sulfate. For 20.00mL water sample, water sample with at most 2000mg/L
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chloride ion concentration can be complexed. If the chloride ion concentration is low, little quantity of mercuric sulfate can be added to keep ratio of mercuric sulfate and chloride at 10:1 (W/W). If little mercuric chloride settlement is found, the measurement result will not be influenced.
2.

Volume of water sample could be between 10.00-50.00mL, but reagent consumption and concentration can be adjusted according to table below.

Table

Water sample quantity and reagent consumption FeSO4(NH4)2SO4 Total volume (mol/L) before titration (mL) 0.050 0.100 0.150 0.200 0.250 70 140 210 280 300

Volume of 0.2500mol/L H2SO4HgSO4 water sample K2Cr2O7 solution Ag2SO4solution g (mL) (mL) (mL) 10.0 20.0 30.0 40.0 50.0 5.0 10.0 15.0 20.0 25.0 15 30 45 60 75 0.2 0.4 0.6 0.8 L.0

3.

For water sample with COD less than 50mg/L, 0.025mol/L potassium bichromate standard solution shall be used instead. 0.01mol/L ferrous ammonium sulfate standard solution is used in titration. After heating and refluxing of water sample, remained potassium bichromate in solution shall be 1/5-4/5 of the added amount. When potassium acid phthalate standard solution is used for reagent quality inspection and operation practice. Its theoritical CODcr is 1.176g. 0.4251g potassium acid phthalate is dissolved in redistilled water. Transfer it to 1000mL volumetric vessel, and use redistilled water to dilute it to the mark, to obtain 500mg/L CODcr standard solution. It shall be prepared just before using. In measuring result of CODcr, three effective digits shall remain. Calibration of ferrous ammonium sulfate standard solution shall be done at each test. Attention shall be paid to the change of concentration when temperature is higher.
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4.
5.

6. 7.

III Measurement of Biochemical Oxygen Demand for Five Days (BOD5)

Various organics in large amount are contained in domestic sewage and industrial waste water. If a water body is polluted, these organics in water will consume a great deal of dissolved oxygen for decomposition. Balance of oxygen quantity in water is thus be destroyed, and the water quantity deteriorated. Composition of organics in water is complex, and it is difficult to measure each content. Oxygen consumption amount of organics under certain condition is always used to indirect indicate quantity of organics in water. Biochemical oxygen demand (BOD) is one of the important indexes for this. Typical measuring method of biochemical oxygen demand (BOD) is dilution and inoculation method. The water sample used for BOD measurement, shall be collected in bottle fully filled and tightly sealed. It shall be kept at 0~4, and be analyzed with 6 hours. In case of transfer to far distance, storage time shall never excess 24 hours. Description 1. Method and principle Biochemical oxygen demand (BOD) refers to under specified conditions, the amount of dissolved oxygen required for microbes to decompose oxidizable substances in water, especially organics. Whole process of this biochemical oxidization takes very long time. For example, at 20, it needs more than 100 days. Normally, in China and abroad, it is specified as to culture for 5 days at 201. Then separately measure the dissolved oxygen amount before and after culture of sample. The difference between the two numbers is BOD5 value, expressed in mg/L of oxygen. Due to large amount of organics, some ground water and most industrial waste water need to be culture and measured after dilution to decrease the concentration and ensure enough dissolved oxygen. Dilution shall be made so as to keep consumption of dissolved oxygen being more than 2mg/L in culture, and remained dissolved oxygen, more than 1mg/L. To ensure there is enough dissolved oxygen in water sample after dilution, the diluted water always needs to be aerated by air (or oxygen), so as to make the dissolved oxygen in diluted water close to saturation. Certain amount of inorganic nutrient salt and buffer materials (phosphate, calcium, magnesium and molysite, etc.) shall be added to the diluted water to meet the microbe growth requirement. For industrial waste water without or with little microbe, inoculation shall be done during measurement of BOD5, for the purpose of introducing microbes that can decompose organics in water. If the waste water contains organics which are
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difficult to be degraded by microbes in normal domestic sewage at normal speed or toxic substances acclimated microbes shall be introduced to water sample for inoculation. This method is applicable for measurement of samples with BOD5 being more than or equals to 2mg/L, not exceed 6000mg/L. If BOD5 of water sample is more than 6000mg/L, there will be some differences because of dilution. Apparatus
a.

Thermostatic constant culture box (201) 5-20L narrow-mouthed bottle 1000-2000mL volumetric cylinder Glass stirring rod, length of the rod shall be 200mm higher than the volumetric cylinder. A rubber pad with some small holes and the diameter is less than volumetric cylinder bottom will be fixed at bottom end of the paddle. Dissolved oxygen cylinder, 250mL~300mL, with ground glass stopper and belled opening for water sealing. Siphon tube, used for separate and receive water sample and adding dilution water.

b. c.
d.

e.

f.

Reagent 1. Phosphate buffer solution Dissolve 8.5g monopotassium phosphate (KH2PO4), 21.75g dipotassium hydrogen silicate (K2HPO4), 33.4g disodium hydrogen phosphate heptahydrate Na2HPO4 and 1.7g sal ammoniac (NH4CL), dilute to 1000mL. pH value of the solution shall be 7.2. 2. Sal amarum solution Dissolve 22.5g bitter salt (MgSO47H2O) in water, and dilute to 1000mL. 3. Calcium chloride solution Dissolve 27.5g anhydrous calcium chloride in water, and dilute to 1000mL. 4. Ferric chloride solution Dissolve 0.25g ferric chloride hexahydrate (FeCl36H2O) in water, and dilute to 1000mL. 5. Hydrochloric acid solution (0.5mol/L) Dissolve 40mL (P=1.18g/mL) hydrochloric acid in water, and dilute to
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1000mL. 6. Sodium hydroxide solution (0.5mol/L) Dissolve 20g sodium hydroxide in water, and dilute to 1000mL.
7.

Sodium sulfite solution (1/2Na2SO3=0.025mol/L) Dissolve 1.575g sodium sulfite in water, and dilute to 1000mL. This solution is unstable, so need to be prepared everyday.

8.

Dextrose-glutaminic acid standard solution Keep the dextrose (C6H12O6) and glutaminic acid (HOOC-CH2-CH2-CHNH2COOH) drying at 103 for 1 hour. Weigh 150mg each and dissolve in water, then transfer to 1000mL volumetric cylinder, dilute to the mark and mix uniformly. This solution shall be prepared just before using.

9.

Dilution water Certain amount of water is filled in 5-20L glass bottle, and the water temperature will be kept at about 20. Oil free air compressor or membrance pump are used. The introduced air first passes through activated carbon adsorption tube and water washing tube, then into dilution water for 2-8 hours is carried out aeration, to make the dissolved oxygen in dilution water close to saturation. Pure oxygen also can be introduced after aeration. Two layers of gauzes after washing and air to drying will be covered on the cylinder opening. The cylinder will be kept in 20 culture box for several hours to make the water dissolved oxygen content reach 8mg/L. Before using, add calcium chloride, ferric chloride solution, sal amarum solution and phosphoric acid buffer solution 1mL separately in each liter of water and mix uniformly. PH value of the dilution water is 7.2 and BOD5 shall be less than 0.2mg/L.

10.

Inoculation liquid Applicable inoculation liquid can be obtained by any one of the following methods.

10.1 10.2

City sewage: Normally take domestic sewage to be settled in room temperature for 24 hours, and take the supernatant liquid for use. Leachate from surface on soil. Take 100g soil from garden or where plant grows. Add 1L water in it, mix and set stand-still for 10 minutes. The supernatant liquid is taken for use. River or lake water containing city sewage. Water outlet from sewage treatment plant. If the analysis water contains substances difficult to degradate, take sample at
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10.3 10.4 10.5

3-8km downstream from the outlet as acclimated inoculation liquid of waste water. If no such water sauce, waste water after being neutralized or diluted can be used for continuous aeration. Every day add small quantity of this waste water and leachate from surface on soil or domestic sewage to make microbe which adaptable to this waste water could propagate in large amount. When there are lots of floc generated in water or suddenly change in COD decreasing value, that means the applicable microbe have been propagated, and the water can be used as inoculation liquid. Normally acclimation takes 3-8 days. 11. Inoculation diluted water Add proper amount of inoculation liquid into diluted water, mix uniformly. Amount of inoculation liquid added for each liter of diluted water for domestic sewage 1-10mL; for leachate from surface on soil 20-30mL; for river or lake water 10-100mL. pH value of inoculation diluted water shall be 7.2. BOD5 value shall between 0.3-1.0mg/L. Inoculation diluted water shall be used immediately after being prepared. Steps 1. Pre-treatment of water sample

1.1 If the pH value of water sample goes beyond the range of 6.5-7.5, hydrochloric acid or sodium hydroxide week solution will be used for adjusting the pH value to about 7. But the consumption shall not exceed 0.5% of water sample volume. If acidity or alkalinity is very high, alkaline or acid liquid with high concentration can be used for neutralization. 1.2 If there are toxic substances such as copper, lead, zinc, cadmium, chrome, arsenic and cyanogens, etc. in water sample, diluted water of microbe inoculation liquid after acclimation could be used for dilution, or increase the dilution factors to decrease the toxic concentration,. 1.3 For water sample contains little amount of free chloride, the free chloride will normally disappear after being set standstill for 1-2h. For water sample with free chloride cant be removed in short time, reagent can be added for removing. The adding amount is to be determined according to method below. Take neutralized water sample 100mL, add 1+1 acetic acid 10mL and 10% (m/v) potassium iodide 1mL. Mix them to uniformly. Starch is used as indicator, and sodium sulfite is used to titrate the free iodide. According to the sodium sulfite volume consumed, calculate out amount of sodium sulfite to be added to the water sample. Water sample taken from low temperature water area or eutrophic lake, supersaturated dissolved oxygen maybe contained in it. In this case, increase the temperature of water sample quickly to about 20. Shake the bottle not fully filled and open the plug time to time to expel out supersaturated
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dissolved oxygen. Water sample taken from high temperature water area or waste water outlet, it shall be cooled quickly to about 20, and shake the bottle uniform adequately mixing, to set and bring to make the oxygen pressure close to balance. 2. Measurement for water sample without dilution For ground water with high dissolved oxygen content and less organics content no dilution is required. Uniformly mixed water sample at about 20 will be transferred into two dissolved oxygen cylinders by siphon method. No air bubble shall be found in the transfer. Make other two dissolved oxygen cylinder full of water sample will overflow by the same method. Cover with plug. No air bubble shall remain in the cylinder. Soon one of the two cylinders is used for measurement of dissolved oxygen, the other one is to be cultured after water sealed in culture box at 201 for 5 days. In culture process, water for sealed shall be added. After 5 days and nights calculated from putting into culture box, remove sealed water and measure the remained dissolved oxygen. 3. Measurement for water sample with dilution

Determination of dilution factors: according to experience, calculation method below can be used for reference in dilution. For ground water, dilution factor can be calculated by multiplying of measured permanganate index with certain coefficient. For details, refer to table 7-2. Table 7-2 dilution factor calculated by multiplying product measured permanganate index with certain coefficient. Permanganate index (mg/L) <5 5.10 10.20 >20 Coefficient 0.2, 0.3 0.4, 0.6 0.5, 0.7, 1.0

For industrial waste water, normally three dilution ratio shall be calculated according to COD value measured from potassium bichromate method. When using dilution water, Three dilution factors can be calculated by multiplying COD value multiply with coefficient 0.075, 0.15 and 0.225 respectively. When using inoculation water, to multiply with coefficient 0.075m 0.15 and 0.25. Dilution operation: normal dilution method According to selected dilution ratio, bring part of diluted water (or
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inoculation diluted water) to 1000mL volumetric cylinder, by siphon method along wall of cylinder. Add uniformly mixed water sample of required amount, and introduce diluted water (or inoculation diluted water) to 800mL. Use glass rod with rubber sheet to carefully stir it up and down. During stirring, do not expose rubber sheet out of water to avoid air bubble. Follow same steps of measurement for water sample without diluted, to fill in bottle, measure intraday dissolved oxygen and dissolved oxygen after 5 days culture. Take other two dissolved oxygen cylinder, fully fill with diluted water (or inoculation diluted water) by siphon method for blank test. Measure dissolved oxygen before and after 5 days. Calculation 1. Directly cultured water sample without dilution BOD5 (mg/L)=C1-C2 Where, C1dissolved oxygen concentration of water sample before culture (mg/L); C2remaining dissolved oxygen concentration of water sample after 5 days culture (mg/l). 2. Cultured water sample after dilution C1-C2-B1-B2f1 BOD5mg/L= f2 Where, B1dissolved oxygen (mg/L) of diluted water (or inoculation diluted water) before culture; B2dissolved oxygen (mg/L) of diluted water (or inoculation diluted water) after culture; f1ratio of diluted water (or inoculation diluted water) in culture liquid; f2ratio of water sample in culture liquid; Note: calculation of f1 and f2 For example, diluted ratio of culture liquid is 3%, meaning 3 shares of water sample, 97 shares of diluted water, f1=0.97, f2=0.03. Precautions:
1.

In order to check quanlity of diluted water and inoculation liquid and workmanship of analyst, 20mL dextrose-glutaminic acid standard solution and dilute it to 1000mL by using inoculation diluted water. Follow steps for BOD5 measurement. Measured BOD5 value shall be between 180-230mg/L, otherwise there maybe some problems on quality of inoculation liquid and
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diluted water or operation skills. 2. If the dilution factor of water sample exceed 100 items, it shall be diluted primarily in volumetric cylinder with water, and then take get proper quantity for final dilution and culture.

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 Measurement of Ammonia Nitrogen Volumetric Method

1. Content and applying scope The present standard stipulates that the ammonia nitrogen content in domestic sewage shall be measured by volumetric method The present standard is applied to the measurement of ammonia nitrogen content both in the sewage that drained into the domestic sewer and the sewage in sewage treatment plant. The measurement limit of ammonia nitrogen of the present method is 0.2mg/L. 2. Method The sample shall be distilled after being regulated by phosphate buffer liquid. The ammonia released from distillation shall be absorbed by boric acid solution first and then titrated by standard sulfuric acid solution by using the methyl red & methylene blue mixed solution as indicator. 3. Reagent Analytic pure reagent and distilled water without ammonia shall be used. 3.1 Sulfuric acid standard titrimetric solution C (1/2H2SO4)=0.1 mol/L Calibrate diluted strong sulfuric acid standard titrimetric solution with sodium carbonate. (Refer to appendix A) 3.2 Mixed indicator Dissolve 0.1 g methyl red and 0.05 g methylene blue in 100 mL alcohol. 3.3 4. 4.1 Sodium carbonate Procedure Blank test Take 250 mL water instead of sample and then operate as items 4.3~4.4 below. 4.2 Reagent If the ammonia nitrogen content in the sample is know, the volume of the reagent shall be selected according to the following table:

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Table 1 Concentration of ammonia nitrogen (mg/L ) 10 10~20 20~50 50~100 4.3 Distillation Take certain amount of reagent and pour into a 500 mL matrass. Then add water to 300 mL. Put some glass beads into the matrass and add 10 mL of phosphate buffer liquid. Add 50 mL of boric acid solution into the absorption bottle and add 2 drops of mixed indicator (item 3.3). Put the guide tube down below the surface of absorption liquid. Distill by heating and stop when the distillate reaches 200 mL. 4.4 Titration Use the sulfuric acid standard titrimetric solution to titrate the absorption liquid, until the color of the solution just turns purple from green. Compare the lightness of the purple with blank titration. 5. Indication of analysis result Calculate the content of ammonia nitrogen by the following formula: CN= V1 - V2 C14.011000 V0 Volume of reagent (mL) 250 100 50 25

Where: V0-----------volume of the reagent (mL) V1----------volume of sulfuric acid standard titrimetric solution consumed for titrating the reagent (mL) V2---------- volume of sulfuric acid standard titrimetric solution consumed for blank titration (mL) C------------standard concentration of sulfuric acid (mol/L) 14.01-------molar mass of nitrogen atom (g/mol)

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Appendix A
Preparation and Calibration of Sulfuric Acid Standard Titrimetric Solution (Supplement) Concentration: (1/2H2SO4)=0.1 mol/L Preparation: add 2.8 mL strong sulfuric acid into 1 L of water Calibration: take 0.1 g (0.002g) of anhydrous sodium carbonate, and dry for 1 hour under 180 . Then dissolve it by 50 mL water in conical flask. Shake the flask thoroughly and then add 3 to 4 drops of methyl orange indicator. Add sulfuric acid solution which is to be calibrated into a burette of 25 mL, and then titrate the sodium carbonate solution in the conical flask, until the color of the solution in the conical flask turns orange from yellow. Remember the reading. Blank test shall be carried out with 50 mL water. The concentration of calibrated sulfuric acid shall be calculated as following: C= m 1000 53 (V 1 V 0 )

Where: m-----weight of anhydrous sodium carbonate (g) V1----volume of sulfuric acid consumed for titrating anhydrous sodium carbonate (mL) V0----volume of sulfuric acid consumed for blank titration (mL) 53-----mass of 1 mol anhydrous sodium carbonate (g/mol)

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