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Analysis of Ammonical & Organic Nitrogen | Wastewater Quality Testing | Lecture Series Part 1| Lec 2 — Transcript

by SWA Environmental Consultants & Engineers · 2,867 words · 440 segments · language en · Watch on YouTube

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0:00Hello friends welcome to another video
0:02of SWA environment consultants and
0:04Engineers this is water and waste water
0:07quality resting lecture series part one
0:10and this is video number five in this
0:13video we are going to learn about the
0:15measurement of ammonical nitrogen and
0:17organic nitrogen as per method of alpha
0:1923rd Edition method number 4,500 uh
0:23which is given for ammonical nitrogen as
0:25well as for organic nitrogen so now
0:28let's start the video so in this video
0:31we will uh see the introduction of
0:33ammonical nitrogen and organic nitrogen
0:36then we'll uh understand the principle
0:38of measurement for both then we will see
0:40which equipments will require to perform
0:42the procedure and then uh we will
0:44understand the procedure of analysis in
0:46two parts in first part we will see the
0:49analysis of ammonical nitrogen and in
0:52second part we will see the analysis of
0:53organic nitrogen then we will move to
0:56the calculation and lastly we will
0:58discuss about measurement on uncertainty
1:01so let's start with brief introduction
1:03of Ammon nitrogen and organic
1:06nitrogen so uh in the nature there are
1:09many types of nitrogen available there
1:13ammonical nitrogen and organic nitrogen
1:15are one of them and generally they
1:17occurs
1:18naturally uh ammonical nitrogen is
1:20generally present in ammonia form and
1:23organic trogen uh is present in nature
1:26various form forms like Ura protein
1:29amino acids amides amines
1:32Etc uh excessive amount of ammonical
1:35nitrogen or organic nitrogen in water
1:37bodies can cause utr fication Okay so
1:41this utopic can harm the uh water
1:45quality as well as the biodiversity of
1:48the water body permissible limit for
1:52ammonical nitrogen is 50 migam per liter
1:55and for organic nitrogen it is uh 50 g
1:58per liter separately combinedly the
2:00organic nitrogen and uh ammonical
2:03nitrogen are referred as total gal
2:06nitrogen because uh the ammonal nitrogen
2:09and uh the organic nitrogen are measured
2:12by the gal method okay so this gar due
2:16to this gal distillation method they are
2:18measured so it is known as it is
2:20referred as total gal nitrogen and the
2:24permissible limit of total gal nitrogen
2:27is 100 mg per liter as per cpcb
2:31standards so this was the introduction
2:35now now let's understand the principle
2:36of measurement for the process now we
2:39will understand the principle of
2:40measurement of measuring ammonal
2:42nitrogen as well as uh measuring the
2:45organic nitrogen by the method of Gile
2:47distillation process it starts with the
2:50ammonical nitrogen so basically
2:51ammonical nitrogen can be determined by
2:54the titration against standardized h2so4
2:57so for titrating this ammonal nitrogen
2:59uh we have to distillate it first so uh
3:02we have to make the pH 9.5 with the help
3:05of no and fix the pH with the help of
3:08buffer solution so at pH 9.5 ammonia
3:12present in the sample will get
3:14distillated uh due to the alkaline
3:17medium that we have provided to it uh at
3:199.5 pH the hydrolysis of organic
3:23nitrogen and cites will get decreased
3:25only ammonia will get liberated so this
3:28liberated ammonia uh will get collected
3:30in indicating boric acid at the end of
3:33distillation assembly it will get
3:35condensed and after the ammonia is
3:37collected it will get tiated against
3:39h204 and we can calculate the amount of
3:42ammonia present into the sample for
3:45organic nitrogen whatever residue is
3:48remaining after performing the procedure
3:50of ammonical nitrogen will get digested
3:53with the help of digestion reagent the
3:56digestion reagent containing h2so4 c04
3:59and K 2 s04 so after the digestion is
4:02completed the organic nitrogen which is
4:05present into the residue will get
4:08converted into ammonical nitrogen or
4:10ammonium after the organic nitrogen
4:13converts into ammonical nitrogen uh the
4:16alkaline medium is provided to the
4:18sample with the help of sodium hydroxide
4:20and sodium tho sufate reagent so this
4:24sodium hydroxide and sodium tho sufate
4:26reagent provides the high alkaline
4:28medium so due to this High alkaline
4:30medium the ammonia will again get uh
4:33distillate and will absorb into the
4:36indicating boric acid after it is
4:39condensed into the indicating boric acid
4:42it again we can titrate it with the help
4:45of h24 and we can calculate the amount
4:47of organic nitrogen present into the
4:49sample this was brief understanding of
4:53the principle for both ammonical and
4:55organic nitrogen in step by step
4:57procedure we will understand more about
4:59about it so now let's see which type of
5:02equipments will be required to perform
5:04this procedure so in reents we will
5:07require six normal no uh which will use
5:10to adjust the pH of the sample then
5:12bored buffer solution which will help us
5:15to fix the pH of the solution then uh
5:18indicating boric acid this will work as
5:20absorbant sulfuric acid 0.02 normal
5:24which will work as titrant in this
5:26process then the digestion reagent to
5:29digest the residue of ammonical nitrogen
5:31and it will eventually uh convert the
5:34organic nitrogen into ammonical form
5:36which we will uh understand in the
5:39procedure again and lastly will require
5:42sodium hydroxide and sodium thiosulfate
5:44reagent which will provide highly
5:47alkaline medium for distillation process
5:49the procedure of preparing all these
5:51reagents are given in an exture you can
5:53refer to the anex and you can uh know
5:56the exact procedure of preparing all
5:58these in agents so in instruments and
6:00glassw will require uh gal
6:04assembly hitting mental conical
6:08flask measuring cylinder to measure the
6:10sample prepared uh for adding the sample
6:13and reagents and the buit for titration
6:17so these are basically the instruments
6:19and glassw we will require to perform
6:21this process so now let's see the
6:23step-by-step procedure for measuring the
6:26ammonical nitrogen as we have discussed
6:28in content slide that we will going to
6:31see these procedures in two parts in
6:33first part we will understand the
6:34procedure of analysis for ammonical
6:36nitrogen and in second part we will
6:39understand the procedure of analysis of
6:40organic nitrogen so let's uh start with
6:43part one measurement of ammonical
6:47nitrogen so now uh let's start the
6:50procedure of measuring ammonal nitrogen
6:53we will uh measure first the ammonical
6:55nitrogen then after we will uh measure
6:58organic nitrogen in into the S so let's
7:01start this so ideal simple that in this
7:04process is 250 so you can see the table
7:07on your screen if you suspect the higher
7:10amount of ammonical hydrogen is present
7:12into uh your sample you can dilute as
7:15per your requirement as per given table
7:18okay so here we are taking the sample of
7:20STP Outlet so between 5 to 10 uh the
7:24total amount of nitrogen may be present
7:26into the sample so let's measure it
7:28first so we are taking uh hold 250 ml of
7:31sample into uh measuring cylinder so
7:35after measuring the sample add 20 ml of
7:39borate buffer solution into this sample
7:49okay so add this bed buer solution into
7:53the
7:55sample after that adjust pH at 9 .5 with
8:00the help of 6 normal NaOH so here we are
8:04having six normal NaOH so let's add
8:07approximate uh one drop of
8:14NaOH add the 250 ml of sample into
8:18this distillation Blas after adding the
8:22sample add few glass bits into
8:26it to avoid any excessive boiling while
8:28the distillation
8:30process after adding glass bits into the
8:34distillation class measure 50 mL of
8:38boric acid indicating boric acid into
8:41the chical
8:43class so here we are having indicating
8:45boric acid here measure 50 mL of
8:51it add the boric acid into Coral
8:55FL now the reagents are ready to get
8:59distillate so let's set up the distill
9:03assem so after uh we have taken the
9:06sample Let's uh set up the assembly
9:08first so here we are having this boric
9:11acid 50 mL of indicating boric acid make
9:14sure the tip of condenser is dipped into
9:18the boric acid so basically what happens
9:21during distillation is uh we have made
9:24the condition of the solution alkaline
9:27we have settled up the pH at 9.5 so when
9:31the solution will get heated by the
9:33heating mental the nitrogen which is in
9:36form of ammonic it will get liberated it
9:39will get condensed into this boric acid
9:42to trap that ammonical nitrogen into the
9:45boric acid this boric acid will work as
9:48absorbent so to that ammonal
9:51nitrogen into this boric acid make sure
9:53the tip of the condenser is dipped into
9:55the boric acid if the tip is not dipped
9:58into the foric acid the ammonal nitrogen
10:00will get escaped and you will have error
10:02in the results now let's set up the
10:10assembly after setting up the assembly
10:13make sure you switch on the continuous
10:17water flow because when uh the heating
10:21mental will heat the solution the
10:24solution will get evaporated and uh this
10:27assembly will get heated so uh by this
10:30continuous flow of water the evaporated
10:33the air portion of the sample will get
10:36condens into liquid and we will get the
10:39condens it into this boric acid okay so
10:42let's uh switch on the heating mental
10:44set the temperature at 100° centigrade
10:47and let the distillation happens collect
10:50approximately 150 to 200 mL of condens
10:53set if ammonal nitrogen is present into
10:56the sample this purple color of boric
10:58acid will get converted into pale green
11:01color after that we will measure the
11:04ammonical nitrogen by titrating it with
11:16h24 uh here we have collected the
11:18distillate uh after the distillation of
11:21ammonical nitrogen you can see we have
11:23collected
11:24approximately 200 mL of distillate now
11:27we will titrate it with
11:290.02 normal standardized
11:32h2so4 uh the standardization process of
11:35h2so4 is given in anx you can refer to
11:38that and you can get accurate normality
11:40of h2so4 we have filled the buet with
11:440.02 normal standardized h204 now we
11:47will tight it and note the reading and
11:49after that we will move to the
11:51calculation part so let's titrate this
11:54ammonical nitrogen
11:57distillate
12:01so as you can see the purple color is
12:03visible end point of tightra is the
12:05purple color the ammonia which is
12:08present into the sample will get
12:10neutralized by the h204 and the color of
12:13boric acid will appear again so whenever
12:16the boric acid color appears stop the
12:18titration and note the reading here we
12:20can see the reading is 3.4 ml now uh we
12:24will note the reading now we will see
12:26the measurement of organic nitrogen uh
12:28so I want to make here a point if you
12:31require the both ammonal nitrogen and
12:34organic nitrogen then you have to
12:36perform the measurement of organic
12:38nitrogen immediately after distillation
12:41of ammonal nitrogen okay but in case you
12:44only require the organic nitrogen so for
12:47that you have to perform the
12:50distillation process of ammonical
12:52nitrogen and remove the ammonia from the
12:54sample but you do not have to collect
12:56the condens it so after the ammonal
12:59nitrogen or ammonia is removed for the
13:01from the sample you can move to the
13:04digestion of the organic nitrogen now
13:07let's see how we can do
13:10that so now let's start the measurement
13:13of organic nitrogen present into the
13:16sample this is the remaining residue of
13:19ammonical nitrogen distillation process
13:21this residue is containing uh organic
13:24nitrogens into it add this digestion
13:28reagent
13:29this digestion reagent is made up of
13:31potassium sulfate copper sulfate and
13:34sulfuric acid in presence of all these
13:36three uh the organic nitrogen which is
13:39present into the sample will get
13:42converted into ammonium form so uh the
13:46converted ammonium form uh will get
13:48again uh measured by the same
13:50distillation process that you will see
13:53uh after the digestion process so first
13:56add 50 mL of digestion reagent into it
13:59it
14:04slowly and let the sample get digested
14:09till 25 to 50 mL of the solution is
14:12remaining into distillation FL after
14:15that we will move
14:21further so now after the digestion is
14:23completed uh take out the distillation
14:26flask make sure you wear gloves because
14:29the distillation flask is high in
14:31temperature or else lend the
14:32distillation flask cool down at room
14:34temperature so we are taking this
14:37distillation flask firstly add 300 mL of
14:41distill water
14:43into add the distill water
14:53slowly so now when distill water is
14:56added add 50 m mL of sodium hydroxide
15:00sodium thyr sulfate solution tilt the
15:05flask so you can see the color is
15:10changing shake it
15:13slowly and add the whole 50 mL of sodium
15:17hydroxide sodium thyr sulfate
15:20solution now uh this residue which is
15:24digested uh the this contains uh the
15:27converted ammonical nitrogen into it the
15:30organic nitrogen is converted into
15:32ammonical nitrogen and again we have
15:34made this solution alkaline by adding
15:38the sodium hydroxide and sodium thyr
15:40sulfate solution so again the solution
15:43the sample is in alkaline condition so
15:45when we will distillate this the
15:48ammonium form of nitrogen will get
15:50liberated and again it will collected in
15:53boric acid the same way it was in
15:55ammonical nitrogen so set up the
15:58assembly
15:59again measure the 50 mL of indicating
16:02boric acid and set up the assembly same
16:04way we have uh set up it in ammonical
16:07nitrogen practical
16:12so again make sure the tip of the
16:14condenser is uh dipped into the boric
16:17acid after setting the assembly uh make
16:21sure again you uh switch on the
16:23continuous flow of water and switch on
16:26the rating mental at 100 cting rate and
16:29collect approximate 150 to 200 mL of
16:32distillate and then we will move further
16:34for titration we are having the
16:36distillate collected after the
16:38distillation of organic nitrogen here
16:40approximate 200 mL of distillate we have
16:42collected again this distillate is
16:45containing the ammonical nitrogen and we
16:48will tiate it again with 0.02 normal
16:50standardized h2so4 the h2so4 will
16:53neutralize the ammonical nitrogen
16:56present into this distillate and color
16:58will again change back to the color of
17:00boric a which is purple color so
17:03whenever purple color appears stop the
17:05tit and note the reading so let's
17:07tighten this
17:15sample so you can see the purple color
17:18is appeared and the this is the Endo of
17:22titration so the reading is
17:254.1 ml note the reading and let's move
17:29to the calculation part so now let's see
17:31the calculation of ammonical nitrogen as
17:34well as organic nitrogen for ammonal
17:36nitrogen the formula of calculation is
17:40uh me into n into 14 into 1,000 divided
17:45by volume of sample in ml so here b
17:48stands for the M reading which we got uh
17:51while the titration n stands for the
17:53standardized normality of
17:56h2so4 so uh this standardized normality
17:59of s24 which we have taken is 0.02
18:03normal 14 is the molecular weight of
18:06nitrogen gam per mole and 1,000 is the
18:10conversion factor of gam to milligram so
18:14this is the terms now if we apply the uh
18:19values to this formula so the answer
18:22comes uh as 3.4 * by 0.02 which is the
18:26normality into 4 14 into 1,000 / 250
18:31which we have taken the sample so the
18:33answer will be 3.8 migam per liter for
18:37ammonical nitrogen same formula applies
18:40for the organic nitrogen also but here
18:44The Bu reading will be different so for
18:47organic nitrogen we got the bu reading
18:504.1 so the answer will be 4.59 mg per
18:55liter so this was the calculation of
18:57ammonical nitrogen an organic nitrogen
19:00so for total geld nitrogen as we have
19:04discussed in initial slide that
19:07ammonical nitrogen and organic nitrogen
19:09combinedly referred as a total gine
19:12nitrogen because both are measured by
19:15the method of gal distillation okay so
19:17if you require total gal nitrogen then
19:21uh you have to Su the ammonal nitrogen
19:24and organic nitrogen so answer will be
19:278. 39 so 3.8 + 4.59 will come as uh 8.39
19:33mgram per liter so this was about the
19:37calculation of both ammonical nitrogen
19:40and organic nitrogen now let's move to
19:42the measurement uncertainty so uh now
19:45let's uh see the measurement uncertainty
19:48uh data for ammonical nitrogen first so
19:52the 200 microgram per liter ammonical
19:55nitrogen the standard solution which
19:57contains uh fluide nitrate and other
20:01interferences to was uh analyzed by uh
20:0521 participating Laboratories and the
20:07standard deviation for that was 69.8
20:10same goes with the uh 800 microgram per
20:13liter ammonical nitrogen uh 20
20:16Laboratories was analyzed the sample and
20:19the standard deviation was
20:2128.6% for 1500 microgram per liter
20:24ammonal nitrogen standard 21
20:27Laboratories analyze the sample and the
20:29standard deviation was
20:3321.6% uh for S swlf uh 9.1 MGR per lit
20:39of standard solution was analyzed and
20:41the standard deviation deriv was
20:4510.54% so this was about the measurement
20:48uncertainty of OB monical nitrogen so
20:51yes uh this was it about the ammonical
20:53nitrogen and organic nitrogen
20:55measurements so I hope you understand
20:58everything uh if you have any doubts or
21:00any questions you can comment down and
21:02if you have any suggestions uh for us to
21:05improve our qualities of video um again
21:08in the suggestions are welcome we will
21:11soon make another video for another
21:13parameter till then take care of
21:15yourself take care the environment
21:18around you and yes please subscribe
21:20bye-bye

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