PENENTUAN AMMONIA DI ATMOSFER

Range dan sensitivitas

1. Dengan laju sampling 1-2 L/menit dengan range konsentrsai 20-700 ug/m3 (0.025-1 ppm)
di udara dapat dicapai dengan waktu sampling selama 1 jam.
2. Batas deteksi dari analisis adalah 0.02 ug NH3/ml
Alat
1. VACUUM PUMP. Any vacuum pump that will maintain a vacuum of 60 kPa with an
airflow of 5 L/min
2. FLOW MEASURING DEVICE. A calibrated flow meter or a critical orifice to measure
or control the air flow from 1 to 2 L/min. the flow meter should be calibrated under
condition of use.
3. ABSORBER. a fritted bubbler (3), midget impinge, or other gas scrubber designed for a
flow rate of 1 to 2 L/min with 10 mL or more absorbing solution.
4. PREFILTER HOLDER. An open-face Teflon, lexan or similar filter holder which can
be connected in line before the absorber. Metal or other plastic holder may be used if it is
know that I does no absorb ammonia.
5. PREFILTERS. Organic-free glass fiber filters used for air sampling for suspended
particulate matter are satisfactory. The filters are washed with distilled wter and dried prior
to use.
6. SPECTROPHOTOMETER. Capable of measuring the absorbance at 630 nm
7. GLASSWARE. Low-actinic glassware or vessel must be rinsed with 1.2 N HCL, and
washed at least 6 times with reagent water before immediate use.
Reagents
1. PURITY. All chemicals should meet specifications of ACS Analytical Reagent grade.
2. WATER. Water must meet specifications of ASTM Reagent water Type II, and be
ammonia free.
3. ABSORBING SOLUTION. Dilute 3.0 mL of concentrated H2SO4 (18 M) to 1 L with
water to obtain 0.1 N H2SO4

4. ANALITYCAL REAGENTS
a. Sodium nitroprusside [sodium nitrosylpentacyanoferrate (III)]. Dissolve 2 g
sodium nitroprusside in 100 mL of water. The solution keeps well in the refrigerator
for 2 months.
b. 6.75 M sodium hydroxide. Dissolve 270 g sodium hydroxide in about 1 L of
distilled water. Boil down to 600 mL in order to volatilize the ammonia contained
in the reagent. Cool and fill to 1 L. Store in polyethylene bottle. Caution: this
solution is extremely caustic. Prevent contact with skin or eyes.
c. Sodium Hypochlorite. Dilute 5 to 6 % analytical reagent sodium hypochlorite with
distilled water to give a 0.1 N solution (3.7%). Strength is determined before
dilution by iodimetric titration or colorimetry after appropriate dilution. The
solution keeps well for 2 months in a refrigerator.
d. Phenol solution 45% v/v. melt phenol by immersing a bottle containing the material
in a water bath at 600 C. pour 45 mL (50 g) into a 100 ml warmed cylinder and fill
to mark with methanol. This solution keeps well for 2 months in a refrigerator
e. Buffer. Dissolve 50 g of NA3PO4.12H2O and 74 mL of 6.75 M NaOH in 1 L of
distilled water
f. Working Hypochlorite Solution. Mix 30 mL of 0.1 N sodium hypochlorite and 30
mL of 6.75 M sodium hydroxide and dilute to 100 mL with distilled water. Prepare
fresh daily.
g. Working phenol solution. Mix 20 mL of the 45 % phenol solution with 1 mL of
2% sodium nitroprusside and dilute to 100 mL with distilled water. Prepare fresh
every 4 Hr.
5. AMMONIA STANDARD SOLUTION.
a. Ammonia stock solution. Dissolve 3.18 g of NH4Cl or 3.88 g of (NH4)2SO4 in 1
L of distilled water (1 mL equal to 1 mg NH3). Add a drop of CHCl3 for better
preservation. The solution is stable for 2 months.
b. Ammonia working solution. Dilute 10 mL of the stock solution to 1 L with
absorbing solution I a volumetric flask (1 mL equal to 10 ug NH3). Prepare daily.
6. GLASS CLEANING SOLUTION. Dilute 10 mL of concentrated HCL (12 M) to 100 mL
with distilled water (molarity approximately 12 M).

Prosedur
1. SAMPLE COLLECTION. Place 10 ml of absorbing solution in each bubbler for samples
and field banks. Cap bubblers for transport. Assemble (in order) prefilter and holder,
flowmeter, bubbler and pump. Sample at the rate of 1 to 2 L/min for a sufficient time to
obtain an adequate sample, usually 1 h. Record sampling time and flow rate. After sample
collection, recap the bubblers.
a. Prefilters. If prefilters are not used the method will determine both gaseous
ammonia and ammonium contained particulates. At high humidity, acid gas will
promote reaction on the filter causing loss of ammonia gas from the sample. In the
absence of acid gases, ammonia collected momentarily on the filter during high
humidity. Will be stripped off during sampling with little loss. The filter must be
prevented from being wetted by rain.
2. ANALYSIS. if bubbler is marked at the 25.0 mL level, the color may be developed in the
flask. If not, transfer contents to a 25 mL glass stoppered graduated cylinder, bein sure to
blow out residual sample from the frits if they are used. Maintain all solution and sample
at 250 C. Add 2 mL buffer, Add 5 mL of the working phenol solution, mix, fill to about 22
mL, then add 2.5 mL of the working hypochlorite solution and rapidly mix. Dilute to 25
mL, mix and store in the dark at 250 C for 30 min to develop color. Measure the absorbance
of solution against a reagent blank at 630 nm, using 1 cm cells.
3. FIELD BANKS. At least one bubbler of collection solution is carried into the field and
treated in the same fashion as the actual samples except that no air is drawn into the bubbler.
It is treated in analysis as if it was a sample. The value of the field blank(s) is compared
with a reagent blank to determine wheter sampling glassware is introducing appreciable
contamination.
Calibration and standardization
1. PREPARATION OF STANDARDS. Pipet 0.5, 1.0, and 1.5 mL of the working standard
solution into 25-mL glass stoppered graduated cylinders. These correspond to 5,10,15 ug
of ammonia/25 mL of solution. Fill to the 10 mL mark with absorbing solution. A reagent

blank with 10 mL of absorbing solution is also prepared. Add reagents to each cylinder as
in the procedur for analysis. read the absorbance of each standard against the reagent blank
2. STANDARD CURVE. Plot the absorbance as the ordinate versus the concentration as the
abscissa on linear graph paper. Alternatively, determine the slope by the method of least
squares
Calculations
g/m3 NH3 = W/Vo
dimana

W = g NH3 in 25 mL from standard curve

Vo = volume of air sampled in m3 at 250 C and 101.3 kPa

Vo= (F/1000) t (Ps/101.3) 298/(273 + Ts)

Dimana,

F = flow rate (L/min)

T = elapsed sampling time in min.
Ps = atmospheric pressure in kPa at sampling point
Ts = temperature, C at sampling point.

PENENTUAN HIDROGEN SULFIDA DI ATMOSFER

Alat
1. ABSORBER. Midget bubbler fitter with coarse-porosity frit.
2. AIR PUMP with a flow meter and gas meter having a minimum capacity of drawing 2
L/min of air through a midget bubbler.
3. SPECTROPHOTOMETER. Capable of operation at 670 nm.
4. AIR VOLUME MEASUREMENT
Reagents
1. Solution should be refrigerated when not in use.
2. AMINE-SULFURIC ACID STOCK SOLUTION. Add 50 ml concentrasion H2SO4 to
30 mL water and cool. Dissolve 12 g of N, N-dymethyl-p-phenylenediamine
dihydrochloride in the sulfuric acid solution.
3. SULFURIC ACID, 50%. Add 500 mL concentration H2SO4 slowly to 400 mL water and
allow to cool. Quantitatively transfer to a 1-L volumetric flask and make up to the mark.
4. AMINE TEST SOLUTION. Dilute 25 mL of the amine-sulfuric acid stock solution to 1
L with 50% of H2SO4.
5. FERRIC CHLORIDE SOLUTION, 3.7 M. Dissolve 100 g of FeCL3.6H2O in 30 mL
water and 9 mL of concentration HCL. The volume of the solution will be approximately
100 mL.
6. AMMONIUM PHOSPHATE, 40 % w/v. Dissolve 400 g of diammonium phosphate in
water and make up to 1 L in a volumetric flask.
7. ABSORBING SOLUTION. Dissolve 4.3 gr of 3 CdSO4.8H2O and 1.8 g NaOH to
separate 250 mL portions of water. Add the two solutions to each other, add 10 g of
arabinogalactan and dilute to 1 L. shake the resultant suspension vigorously before
removing aliquot. Prepare fresh every 3 days. Previous versions of this method prescribe a
smaller amount of NaOH in the absorber solution. The pH of the absorber solution
recommended here is ~10 and yields superior result.

Dari bahan-bahan penelitian diatas maka dapat dibuat larutan induk asam sulfide, larutan amine
sulfuric, larutan amin test, larutan ferric klorida, ammonium phosphate, dan larutan penyerap
sesuai langkah kerja yang terdapat di dalam standard method.
Larutan penyerap hydrogen sulfide yang digunakan di dalam penelitian ini adalah campuran dari
3 CdSO4.H2O, NaOH, dan aquades (Lodge, 1989). Menurut Jacobs (1985), penambahan
arabinogalactan dapat meminimalirsir photo-dekomposisi dari penguapan cadmium sulfat. Hal ini
selaras dengan hasil uji coba terhadap sampling hydrogen sulfide yang menggunakan penambahan
arabinogalactan mampu menyerap hydrogen sulfide sebanyai 201.59% lebih banyak dibandingkan
dengan larutan yang tidak menggunakan arabinogalactan.
Metode pengambilan sampel H2S
Peralatan terdiri dari midget impinger, pompa vacuum, dan flowmeter dirangkai sedemikian rupa
sebelum dilakukan pengambilan sampel.
Metode pengambilan sampel dilakukan dengan langkah kerja sesuai standard method dari lodge
(1989), yaitu
1.

Siapkan larutan penyerap

2.

10 ml larutan penyerap dipipet ke dalam midget impinge

3.

Midget impinge dihubungan (via absorption tube) dengan pump sampling menggunakan

short flexible tubing

4.

Kecepatan aliran diatur, pada 0.5 L/menit suhu dan tekanan dicatat

5.

Dilakukan pencuplikan selama 2 jam

6.

Analisis dengan spektrofotometer

Pengolahan data
Spektofotometer
Penggunaan spektofotometer di dalam penelitian ini bertujuan untuk pembacaan nilai absorbansi.
Setelah dilakukan sampling dan pemberian reagen pada sampel, maka dilakukan pembacaan
serapan (absorbansi) dengan menggunakan spektrofotometer. Namun, sebelum spektrofotometer
digunakan untuk membaca nilai absorbansi, terlebih dahulu dilakukan pembuatan kurva kalibrasi
dengan uraian sebagai berikut.
Kurva kalibarasi dibuat pada saat sebelum dilakukannya pembacaan sampel menggunakan
spektrofotometer dapat dicapai. Larutan standar sulfide diperlukan untuk membuat kurva kalibrasi
untuk hydrogen sulfide ini. Larutan standar dibuat dengan cara melarutkan Na2S.9H20 dengan air.
Kurva kalibrasi ini berguna pada saat perhitungan untuk menentukan besarnya H2S dalam sampel.
Kuantitas H2S diperoleh dengan menggunakan hasil persamaan dari kurva kalibrasi yaitu berupa
volume H2S di udara.
Preparasi sampel terlebih dahulu dilakukan sebelum pembacaan nilai absorban pada larutan
absorban menggunakan spektrofotometer dengan metode Lodge (1989)
1. 1.5 ml larutan amin dimasukkan ke dalam midget bubbler melalui lubang inlet udara dan
campurkan
2. Ditambahkan 1 tetes larutan feri klorida dan campurkan
3. Sampel dipindahkan ke labu ukur 25 ml
4. Ditambahkan 1 tetes larutan ammonium fosfat. Jika warna kuning belum hilang, lanjutkan
tetesan sampai warna kuning tersebut menghilang
5. Dilarutkan dengan air suling sampai tanda tera, dibiarkan selama 30 menit
6. Masukan sampel ke dalam kuvet 2 cm (20 mm) secukupnya.
7. Ukur masing-masing nilai absorbansi larutan dengan menggunakan spektrofotometer pada
panjang gelombang 670 nm
8. Hitung konsentrasi sampel menggunakan kurva kalibrasi.
Setelah dianalisis dengan menggunakan spektrofotometer dilakukan, kemudian akan diperoleh
hasil berupa nilai absorbansi. Kemudian, nilai absorbansi ini dimasukkan ke dalam persamaan

yang telah diperoleh pada saat kalibrasi spektrofotometer. Hasil akhir dari persamaan tersebut
merupakan nilai actual H2S dalam larutan penyerap yang merupakan sampel uji (mg/l). kemudian
dilakukan perhitungan dengan langkah sebagai berikut.

25
1000

Keterangan:
C adalah konsentrasi hydrogen sulfide dalam fasa cair (mg/l)
A adalah jumlah hydrogen sulfide dari sampel uji (mg/l)
25 adalah volume sampel uji yang diencerkan dalam labu ukur 25 ml
1000 adalah faktor pengali untuk konversi satuan ke dalam liter
Vs adalah volume contoh gas uji dalam kondisi normal, yaitu pada suhu 25 C, 1 atm

Pada persamaan diatas terdapat volume contoh uji gas yang diperoleh dari hasil koreksi pada
kondisi normal dengan persamaan berikut:

=

Ps = tekanan udara kondisi standard

Vs= volume udara kondisi standard
Ts= suhu udara kondisi standard
P= tekanan udara pada saat sampling
V= volume udara pada saat sampling, 60 liter (dari perhitungan 120 menit x 0.5 L/menit)
T adalah suhu udara pada saat sampling