Method

for Testing Mercury

Concentration in Water by
Atomic Absorption
Spectrophotometer with
Author Hydride Generation System
Jaye Yang
Application Note
Water

Introduction
This testing method describes a procedure for the
examination and evaluation of Mercury concentration
in water. This method uses Persee 990F Atomic
Absorption Spectrophotometer with Hydride
Generation System. This method is applicable to
surface water, underground water, industry wastewater
and sanitary sewage. This method is not applicable to
the water containing high concentration of organic
compounds. Potassium permanganate – potassium
persulfate digestion method is used. When the sample
volume is 100mL, the detection limit is 0.02𝜇g/L, and
the limit of determination is 0.08 𝜇 g/L; When the
sample volume is 200mL, the detection limit is
0.01𝜇g/L, and the limit of determination is 0.04𝜇g/L
Principle Solution Preparation:
Under heating condition, use potassium 1. Nitric acid solution (1+1): transfer 100mL
permanganate and potassium persulfate concentrated nitric acid into 100mL water,
solutions with sulfuric acid and nitric acid mix well.
media to digest sample; Or use potassium 2. Potassium permanganate solution 𝜌(KMnO4)
bromate – potassium bromide mixed solution = 50g/L: transfer 50g potassium
with sulfuric acid media to digest sample; Or permanganate into 1000mL water, mix well.
use microwave digestion with nitric acid and 3. Potassium persulfate solution 𝜌(K2S2O8) =
hydrochloric acid media to digest sample. After 50g/L: transfer 50g potassium persulfate
digestion, all the mercury ions in sample are into 1000mL water, mix well.
converted to mercuric with +2 oxidation number. 4. Hydroxylamine hydrochloride
Use hydroxylamine hydrochloride to reduce the solution 𝜌(NH2OH∙HCl) = 200g/L: transfer
oxidation agent, then stannous chloride is used 200g hydroxylamine hydrochloride into
to reduce +2 mercuric into metal mercury. 1000 mL water, mix well.
Under room temperature, let mercury gas flow 5. Stannous chloride solution 𝜌(SnCl2) =
into atomic absorption spectrophotometer by air 200g/L: transfer 20g stannous chloride into
or nitrogen gas. At 253.7nm wavelength, the a dried beaker, add 20mL concentrated
mercury concentration can be tested. hydrochloric acid. After dissolving, add
water to 100mL to dilute and mix well.
Reagents and Equipment 6. Potassium dichromate solution 𝜌(K2Cr2O7)
Instrument: = 0.5g/L: transfer 0.5g potassium
1. Persee 990F AAS dichromate into 950mL water, then add
2. Persee Hydride Generation System 50mL concentrated nitric acid, and mix
3. Temperature Adjustable Hot Plate well.
4. Constant Temperature Water Bath 7. Mercury stock solution 𝜌(Hg) = 100 mg/L:
transfer 0.1354g completely dried mercury
Reagent and Preparation: chloride (HgCl2) into prepared potassium
Reagent: dichromate solution, then mix well.
1. Potassium dichromate (K2Cr2O7): guarantee 8. Mercury working solution 𝜌(Hg) = 0.1
reagent; mg/L: transfer 1.00mL prepared mercury
2. Concentrated sulfuric acid: 𝜌(H2SO4) = stock solution into a 1000mL volumetric
1.84 g/mL guaranteed reagent; bottle, then add potassium dichromate
3. Concentrated hydrochloric acid: 𝜌(HCl) = solution to the marker, mix well.
1.19 g/mL guaranteed reagent; 9. Diluent: transfer 0.2g potassium dichromate
4. Concentrated nitric acid: 𝜌(HNO3) = 1.42 into 900mL water; add 27.8mL
g/mL guaranteed reagent; concentration sulfuric acid, then dilute to
5. Potassium permanganate: guaranteed 1000mL marker, mix well.
reagent; 10. Instrument washing liquid: transfer 10g
6. Potassium persulfate: guaranteed reagent; potassium dichromate into 9L water, then
7. Hydroxylamine hydrochloride: guaranteed add 1000mL concentrated nitric acid, mix
reagent; well.
8. Stannous chloride: guaranteed reagent;
9. Completely dried mercury chloride (HgCl2)
Experiment
Sample Preparation: Instrument Set up:
(potassium permanganate-potassium persulfate Lamp Current 1mA
digestion method, other methods are similar) Measuring 253.7nm
Wavelength
1. Shake and mix the sample well before use. Slits 0.2nm
Transfer 100.0mL sample into 250mL KBH4 7.5
volumetric flask. If the sample has a high Carrier Liquid 1% H2SO4
mercury concentration, a smaller volume of Solution Acidity 0.5% HNO3
sample can be used, then diluted into Atomization Room Temperature
100.0mL. Temperature
2. In a sequence, add 2.5mL concentrated
sulfuric acid, 2.5mL prepared nitric acid Standard Curve:
solution and 4mL prepared potassium 1. Transfer 0.00, 0.50, 1.00, 1.50, 2.00, 2.50,
permanganate solution, mix well. If the 3.00 and 5.00mL prepared mercury working
purple color of the final solution does not solution into 8 different 100mL volumetric
maintain for 15min, more potassium flask, then dilute to the marker. The
permanganate solution will need to be added concentration of each final solution is 0.00,
(the maximum volume is 30mL). Finally 0.50, 1.00, 1.50, 2.00, 2.50, 3.00 and
add 4mL prepared potassium persulfate 5.00 𝜇g/L respectively.
solution. 2. Introduce the mercury working solutions
3. Put the flask in a water bath and let the into the hydride generator, in sequence of
solution boil for 1h (make sure it’s concentration from low to high, then record
uncapped.) the values and draw the standard curve.
4. Before testing, add hydroxylamine
hydrochloride solution drop by drop, until Unknown Sample Test:
the purple color is disappeared. (Do not 1. Run the blank by hydride generation system
pour the solution, the volume must be first.
controlled carefully). 2. Run the prepared unknown sample by
5. Blank preparation: use pure water as sample, hydride generation system, then the
repeat the steps 1-4. concentration of mercury is calculated
automatically and shown on the software.

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