Page 1

Soil Fluoride Pretreatment

1) Reagent
Calcium oxide (CaO)
Perchloric acid (HClO 4 )
-Silver perchlorate solution (17.5%): silver perchlorate (AgClO 4 ) solution 17.5g / 100mL
-Nitrophenol indicator (0.5%): Nitrophenol (C 6 H 5 NO 3 ) 0.5g / 100mL
Sodium hydroxide solution (50%): 50 g / 100 ml of sodium hydroxide (NaOH)
-2nd, 3rd purified water
2) Supersonic
500 or 1000 mL beakers, 50 mL measuring cylinder (glass-perchloric acid, plastic-purified water), 50 mL
Falcon, cell, micropipette
3) Pretreatment Process
① Dry the soil for 4 days on a zipper bag and sift with (75/200).
② Take 1g soil sample, put it in the crucible and put 5g calcium oxide.
MB is only 5g of calcium oxide in the crucible and cooled after 6 hours incubation at 550 ℃.
③ Pour the soil sample in the cell and pour 25mL of purified water into the cell while rinsing the inside
of the crucible.
④ Nitrophenol indicator 200㎛ and 50% in 500mL volumetric flask using micro pipette.
Put NaOH 200㎛.
⑤ Put 200 μm of perchloric acid into the cell containing soil sample.
⑥ Add 50 mL of perchloric acid to the cell and mix well before connecting to the distillation unit.
⑦ Properly fix the distillation apparatus and raise the volumetric flask. Then press the Power and Main
button.
All.
⑧ Run the RUN when the temperature reaches 130 ℃.
⑨ Maintain distillation apparatus temperature at 130 ~ 140 ℃.
400 When 400 mL is filled in the volumetric flask, turn off the Main and Power buttons.
(If 400mL is not filled, restart RUN to set it to 400mL and turn it OFF)
500 500ml with 2nd purified water, mix well and fill Falcon.

Page 2
Soil Heavy Metal Pretreatment
1) Background and scope of application
This test method is to measure metals in soil.
The treated sample solution is directly injected into the flame and atomized and analyzed by atomic
absorption spectrophotometry.
This test method is applicable to the analysis of metals such as copper, lead, nickel, zinc and cadmium in
soil.
2) reagents
Nitric acid
- Hydrochloric acid
-0.5M nitric acid: concentrated nitric acid (HNO3) 32mL / 1L
3) Supersonic
Micro pipettes, digester SET, plastic funnel, 50 mL volumetric flask, 4 filter paper, plastic cup 3
Dog, Falcon
4) Pretreatment Process
① Dry the soil for 4 days on a zipper bag and sift (150/100).
② Put about 1.5g of soil sample in the decomposition container.
MB is added 1.5mL of tertiary purified water in the digestion vessel.
③ 10.5mL hydrochloric acid (3500 × 3) → 3.5mL nitric acid (3500 × 1) into pipe
give.
④ After assembly, put 7.5mL (3750 × 2) of 0.5M nitric acid into the hole above it.
⑤ Raise the heater to 80 ℃, and when it reaches 80 ℃, place the decomposition vessel and heat for 2hr.
⑥ After heating, remove the digestion container from the basket and cool it.
Raise the funnel and add 4 eggs.
⑦ Separate the disassembly container separately, shake well and pour it evenly over the sheet.
(At this time, if it leaks, pipette 0.5M nitric acid well on the filter paper, and then put it on the new filter
paper.
Pour into 50mL flask and rinse well.)
⑧ Take 0.5M nitric acid with a pipette (fit to 3000), sprinkle it cleanly in the decomposition container
and pour it into
give.
⑨ Disassemble the rest, not the decomposition container, pour the solution on it and turn it over.
Take it out, clean it and spray it out of the hole.
여과 After some filtration, sprinkle twice around the filter area.
⑪ After filtration, remove the funnel and pipette to 50mL mark with 0.5M nitric acid.
유출 Pour the effluent in the marked flask into the Falcon while mixing well.

Page 3
Soil cyan pretreatment
1) Background
A method of measuring cyanide in soil, adding EDTA in acidity below pH 2
The cyanide and cyanide compound are discharged into hydrogen cyanide and collected in sodium
hydroxide solution.
It is neutralized and collected in the form of CN ions.
2) reagents
-Phenolphthalein-ethyl alcohol solution (0.5%): 0.5g of phenolphthalein (C 20 H 14 O 4 ) to ethyl alcohol
(C 2 H 5 OH)
Dissolve in 50 mL, add purified water to make 100 mL, and remove the solution until the solution turns
red.
Add thridium solution.
Phosphoric Acid
Sodium hydroxide solution (2%): sodium hydroxide (NaOH) 20g / 1L
Ammonium sulfamate solution (10%): 10 g / 100 mL of ammonium sulfamate (NH 4 SO 3 NH 2 )
Ethylenediaminetetraacetic acid sodium acetate solution (EDTA)
10 g of (C 10 H 14 O 8 Na 2 ⦁2H 2 O) is dissolved in purified water and slightly alkaline with 0.4% sodium
hydroxide solution.
Add purified water to make 100 mL.
3) Supersonic
cell, 250 ml beaker, weighing dish, pipette, 250 ml glass measuring cylinder, Falcon
4) pretreatment
① Weigh 10 g of undried sample (weight plate) → MB uses 10 mL of tertiary purified water
② Put 10g of sample + 250mL of purified water into the cell. (Washing the sample container with
purified water)
③ Put 2 ~ 3 drops of phenolphthalein solution into the cell.
(Acid, neutral to colorless / alkaline to red → red turns colorless when acid is added)
④ Add 10 mL of phosphoric acid, 1 mL of ammonium sulfamate solution (10%), and 10 mL of EDTA
into the cell.
⑤ Installed in the pretreatment device → RUN (approximately 6 minutes)
⑥ Put 20 mL of 2% NaOH in the container receiving the distilled sample.
⑦ Mass distillation to 100mL after distillation is completed.

Page 4
Water Heavy Metal Pretreatment
1) Reagent
Nitric acid (atomic)
3rd purified water
2) Supersonic
Plastic funnel, 4 filter papers, micropipette, 50 mL volumetric flask, Falcon
3) Pretreatment Process
① MB in Falcon: tertiary purified water 40mL + nitric acid 5mL
Sample: Add 40 mL of sample + 5 mL of nitric acid.
② Close Falcon stopper with orange cap.
③ 3F device ON → Connect temperature sensor MB and device
Place sample near MB → Run (approximately 45 minutes)
④ Turn off the device → 4 places and mass up with 3rd purified water → Add to Falcon

Page 5
Hexavalent chrome pretreatment
1. Put 2.5g of soil. (MB is tertiary 2.5mL)
2. Add half a tablespoon of magnesium chloride 0.4g + 0.5mL phosphate buffer solution (0.1M).
3. Add 50 mL of decomposition solution. (NaOH 20g + Na2CO3 30g / 1L)
4. Put the magnetic bar, cover the watch plate, and drop a few drops with distilled water.
5. Stir at 90 ° for 1 hour
6. Allow to cool, then filter with GF / C filter paper (easy to falcon)
7. Adjust the filtered sample to pH 7 ~ 8 with 5M nitric acid.
8. Mass filter using 0.45um syringe filter and distilled water to 100mL.