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Typical Pretreatment for As by HVG-1

Sample 50mL

add HClO4; 1 mLHNO3; 2mL


Heat up, Decompose organic substitute

Treat with white fume of HClO4 and evaporate HNO3

Let it cool, add 6mol/L-HCl


Dissolve salts

Add 20W/V%-KI solution; 2.5mL

Fill up to 50mL

Let it stand for 30 minuets, As5+ As3+


Measure by HVG-1

Pre-Treatment Method for Hydride Vapor Generation Method


(Based on JIS [Japan Industrial Standard] K 0101 for plant waste water)

Put the sample* into 25ml volumetric flask

Add 2.5mL concn. (12mol/L) HCl and 1.25mL 20%-KI solution

Fill the flak with pure water

Let it stand for 30 minuets at room temperature


Final concentrations; HCl; 1.0 1.2 mol/L, KI; 1%
Same reagents and concentrations should be contained in standard solutions.

Put the sample* into 25ml volumetric flask

Add 20mL (6mol/L) HCl and heat it at 90100 for 10 minuets

After cooling fill the flak with pure water


Final concentrations; HCl; ca. 5 mol/L
Same reagents and concentrations should be contained in standard solutions

Put the sample* into 25ml volumetric flask

Add 5mL (12mol/L) HCl and 3mL (0.1mol/L) thiourea solution

Fill the flak with pure water


0.1mol/L thiourea solutionDissolve 0.76g Thiourea into 100mL water
Final concentrations; HCl; ca. 2.4 mol/L, Thiourea; 0.012mol/mL
Same reagents and concentrations should be contained in standard solutions

Sophisticated preparation of
real life samples

Typical pretreatment methods


Wet ashing
HCl, HNO3
HNO3 + HCLO4

Dry ashing
H2SO4 + Heat by electric furnace (500-600)
Alkali fusion

Typical pretreatment for water samples 1/2


1 . Add 1-5 mL HNO3 (or HCl) to 100mL sample.
2 . Heat up to boil for about 10 minutes.
3 . After cooling, transfer the sample into 100mL
volumetric-flask and fill it up with pure water.

Typical pretreatment for water samples 2/2


1 . Add 1-5 mL HNO3 (or HCl) to 100mL sample.
2 . Heat up to boil and keep heating until the sample
volume decrease to about 15 mL.
3 . After cooling, transfer the sample into 100mL
volumetric-flask and fill it up with pure water.

In case of Citrus leaves 1/5


Put dried sample (about 0.1g) into the beaker and weigh it (0.1144g).
Add 10mL HNO3(1+1) and 2mL perchloric acid.
Decompose it on the sand-bath(about 200.
Add 10mL HNO3(1+1) gradually to decompose the organic compounds
completely.

Treat with white fume


Let it cool, then add 10mL HCl(1+1)
Dissolve the salts on the sand bath (about 100)
Let it cool.
Transfer the treated sample into the 25mL-volumetric flask.
Fill it up with pure water: Sample Solution A.

In case of Citrus leaves 2/5


For Na
Transfer 5mL of the sample solution A into the 25mL-volmetric flask .
Add 5mL Cs(0.5w/v%) solution.
Fill it up with water to 25mL.

For K ;
Transfer 2mL of the sample solution A into the 100mL-volmetric
flask .

Transfer 5mL of the above solution into the 25mL-volmetric flask .


Add 5mL Cs(0.5w/v%) solution.
Fill it up with water to 25mL.

In case of Citrus leaves 3/5


Result

Na
K

Concentration
in measured
solution

Concentration
in
citrus leaves

Certified Value

0.1543 ppm

169 ppm

160 20 ppm

0.3418 ppm

1.87 %

1.87 0.06%

In case of Citrus leaves 4/5


For Mg
Transfer 2mL of the sample solution A into the 100mL-volmetric flask .

Transfer 5mL of the above solution into the 25mL-volmetric flask .


Add 0.5mL La(5w/v%) solution.
Fill it up with water to 25mL.

For Ca
Transfer 1mL of the sample solution A into the 100mL-volmetric flask .
Add 2mL La(5w/v%) solution.
Fill it up with water to 100mL.

In case of Citrus leaves 5/5


RESULT
Concentration
in measured
solution

Concentration
in
citrus leaves

Certified Value

Mg

0.1015 ppm

0.555 %

0.58 0.03 %

Ca

1.424 ppm

3.11 %

3.15 0.10%

Preparation for Hydride Vapor


Generation Method 1/3
Put dried sample into the beaker and weigh it (1.000g).
Add 10mL HNO3(1+1) and 2mL perchloric acid.
Decompose it on the sand-bath(about 200.
Add 10mL HNO3(1+1) gradually to decompose the organic
compounds completely.

Treat with white fume


Let it cool, then add 20mL HCl(1+1)
Dissolve the salts on the sand bath (about 100)
Let it cool.
Transfer the treated sample into the 100mL-volumetric flask.
Fill it up with pure water: Sample Solution A.

Preparation for Hydride Vapor


Generation Method 2/3
Transfer 5mL of the sample solution A into the 50mLvolmetric flask .
Add 10mL HCl(1+1) and KI(10w/v%) solution
Fill it up with water to 50mL.
Let it stand for 30minuites before measurement.

Preparation for Hydride Vapor


Generation Method 3/3
RESULTS
Samples
Citrus
Leaves
Rice Flour
Pond
Sediment

Concentration Concentration Certified Values


in solution
in solid
samples
3.10 ppb

3.10 ppm

3.1 0.3ppm

2.97 ppb

0.297 ppm

0.29 ppm

2.10 ppb

10.5 ppm

12 2 ppm

Example of pretreatment of citrus leaves1/8


Take
sample and
weigh

Example of pretreatment of citrus leaves 2/8


Add 5mLHNO3 and
put on the
sand-bath.
Start heating

Example of pretreatment of citrus leaves 3/8


As the decomposition
of the organic
compounds proceeds,
brown color nitrous
acid fume is generated.

Example of pretreatment of citrus leaves 4/8


Keep heating until the brown fume degrease.

Example of pretreatment of citrus leaves 5/8


After cooling, add 5mLHNO3 and 2mL-HCLO4
and heat again.
White fume (perchloric
acid) is generated.

Example of pretreatment of citrus leaves 6/8


Keep heating until
almost dryness.

Example of pretreatment of citrus leaves 7/8


Add 20mL-HCl(1+1)
to dissolve the salts

Example of pretreatment of citrus leaves 8/8


Keep heating about
10-20minutes to
dissolve the salts
completely
After cooling, transfer
the solution into the
volumetric flask.

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Alkali fusion method 1/3


for elements; Si, Al
for samples; ceramics, minerals, bricks
1 Put the sample into the
Pt crucible.
2 Add the flux (Na2CO3 ,
LiBO2, Na2B4O7, etc. 510 folds of sample weight)

Alkali fusion method 2/3


Put the Pt crucible into
the ceramic crucible
for protecting.
Set the crucible into
the electrical
furnace(temp.;7001000 for 0.5-1.0hr.)

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Alkali fusion method 3/3


After cooling add the
diluted HCl to disolve
the salt
Transfer the solution
into the volmetricflask made of plastic.

High pressure Teflon vessel

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