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Standard preparing

Product
AAS / AFS
category
novAA 300, novAA 400, Zeenit 650(P), Zeenit
Instruments 700(P), contrAA 300, contrAA 700, mercur, mercur
duo
Topic Standard preparing

For the quantitative determination of elements are


one or more standards required. It is important to
use a high quality of materials and solutions.

Basics  Waterpurity: distilled water is equivalent to


ultrapure water (dielectric permittivity =
0.055µS/cm or 18.2MΩ*cm)
 Chemicalpurity: depends on the technique „pro
analysis“ (p.A.) or “suprapure”

Flame

Rinsing solution ca. 0.1% HNO3


(for autosampler)  2 mL HNO3 65% (p.A.) are dissolved in 2000
mL distilled water.

Diluent 1.5% HNO3 + 0.1% CsCl/LaCl3


(for autosampler)  20 mL HNO3 65% (p.A.) + 10 mL 10%
CsCl/LaCl3-solution are filled up to 1000 mL
with distilled water.

Calibration Copper:
0/ 0.3/ 0.5/ 0.7/ 1.0/ 2.0 mg/L Cu

Example 2.0 mg/L Cu


 Solution 1: 1g/L Cu
(commercial standard solution)

 Solution 2: 100 mg/L Cu


10 mL solution 1 + 2 mL HNO3 65%
(p.A.) + 1 mL 10% CsCl/LaCl3-
solution are filled up to 100 mL with
distilled water (DF 10).

 Solution 3: 2.0 mg/L Cu (ready to use)


2 mL solution 2 + 2 mL HNO3 65%
(p.A.) + 1 mL 10% CsCl/LaCl3-
solution are filled up to 100 mL with
distilled water (DF 50).

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Flame

0.3 mg/L: 300 µL solution 2


0.5 mg/L: 500 µL solution 2
0.7 mg/L: 700 µL solution 2
1.0 mg/L: 1000µL solution 2

Solution 3 can be stored several


days!

Graphite furnace

Rinsing solution ca. 0.15% HNO3


(for autosampler)  2 mL HNO3 65% (suprapure) are filled up to
1000 mL with distilled water.

Diluent 0.6% HNO3


(for autosampler)  1 mL HNO3 65% (suprapure) are filled up to
100 mL with distilled water.

Calibration Chrom:
0/ 2.0/ 4.0/ 6.0/ 8.0/ 10.0 µg/L Cr

Example 10 µg/L Cr
 Solution 1: 1g/L Cr
(commercial standard solution)

 Solution 2: 10 mg/L Cr
1 mL solution 1 + 1 mL HNO3 65%
(suprapure) are filled up to 100 mL
with distilled water (DF 100).

 Solution 3: 10 µg/L Cr (ready to use)


100 µL solution 2 + 1 mL HNO3
65% (suprapure) are filled up to 100
mL with distilled water (DF 1000).

prepare freshly!

Hydride-
HydrEA

Continuous measurement (HS 60 / 60A)

Acid 3% HCl
 70 mL HCl 37% (fuming) are filled up to 1000
mL with distilled water.

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Continuous measurement (HS 60 / 60A)

Reductant  Solution 1: 3% NaBH4 + 1% NaOH


7.5 g NaBH4 + 2.5 g NaOH (pellets)
are dissolved in 250 mL dist. water
(ultrasonic bath)
Solution 1 can be stored in the
refrigerator 4-6 weeks!
 Solution 2: 0.3% NaBH4 + 0.1% NaOH
(ready to use)
100 mL solution 1 filled up to 1000
mL with dist. water; prepare freshly
(DF 10).

Batch measurement (HS 50 / 55 / 55A)

Acid Not applicable, already contained in standards and


samples.

Reductant
 Solution 1: 3% NaBH4 + 1% NaOH
7.5 g NaBH4 + 2.5 g NaOH (pellets)
are dissolved in 250 mL dist. water
(ultrasonic bath)
Solution 1 can be stored in the
refrigerator 4-6 weeks!
 Solution 2: 1.0% NaBH4 + 0.3% NaOH
(ready to use)
100 mL solution 1 filled up to 300
mL with dist. Water (DF 3).
Solution 2 can be stored in the
refrigerator 1-2 weeks!

Reducing agent for arsenic

Reducing agent 5% Potassium iodide (KI) / 5% Ascorbic acid


 2.5 g Potassium iodide + 2.5 g Ascorbic acid
are dissolved in 50 mL dist. water in a clean
platic tube with screw cap (e.g. Sarstedt or
Falcon or Greiner)
Solution can be stored in the refrigerator
several days, no brown color may occur!

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Hydride (continuous and discontinuous)

Rinsing solution Approx. 0.2 % HCl


(for autosampler) 5 mL HCl 37% (p.A.) filled up to 1000 mL with dist.
water

Diluent 3.0 % HCl


(for autosampler) 70 mL HCl 37% (p.A.) filled up to 1000 mL with dist.
water

Calibration Arsenic:
0/ 2.0/ 4.0/ 6.0/ 8.0/ 10.0 µg/L As

Example 10 µg/L As
 Solution 1: 1g/L As
(commercial standard solution)

 Solution 2: 1 mg/L As
100 µL solution 1 + 7 mL HCl 37%
(p.A.) filled up to 100 mL with dist.
water (DF 1000).
 Solution 3: 10 µg/L As (ready to use)
1 mL solution 2 + 7 mL HCl 37%
(p.A.) + 1 mL Reducing agent. Allow
to stand at ambient temperature for
at least 45 minutes. Filled up to 100
mL with dist. water (DF 100).
Prepare freshly!

2.0 µg/L: 200 µL solution 2


4.0 µg/L: 400 µL solution 2
6.0 µg/L: 600 µL solution 2
8.0 µg/L: 800 µL solution 2

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HydrEA (continuous and discontinuous)

Rinsing solution ca. 0.2 % HCl


(for autosampler)  5 mL HCl 37% (p.A.) are filled up to 1000
mL with dist. water

Diluent 3.0 % HCl


(for autosampler)  70 mL HCl 37% (p.A.) are filled up to 1000
mL with dist. water.

Calibration Arsenic:
0/ 0.2/ 0.4/ 0.6/ 0.8/ 1.0 µg/L As

Example 1 µg/L As
 Solution 1: 1g/L As
(commercial standard solution)

 Solution 2: 10 mg/L As
1 mL solution 1 + 7 mL HCl 37%
(p.A.) are filled up to 100 mL with
dist. water (DF 100).

 Solution 3: 100 µg/L As


1 mL solution 2 + 7 mL HCl 37%
(p.A.) are filled up to 100 mL with
dist. water (DF 100).
Solution can be stored several
days!

 Solution 4: 1 µg/L As (ready to use)


1 mL solution 3 + 7 mL HCl 37%
(p.A.) +1 mL Reducing agent.
Allow to stand at ambient
temperature for at least 45
minutes. Filled up to 100 mL with
dist. water (DF 100).
Prepare freshly!

0.2 µg/L: 200 µL Solution 3


0.4 µg/L: 400 µL Solution 3
0.6 µg/L: 600 µL Solution 3
0.8 µg/L: 800 µL Solution 3

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mercur

Rinsing solution 2 % HCl


(for autosampler)  50 mL HCl 37% (ultra pure) filled up to 1000
mL with dist. water.

Diluent 2.0 % HCl


(for autosampler)  50 mL HCl 37% (ultra pure) filled up to 1000
mL with dist. water.

Reducing agent 2.0 % SnCl2 in 2 % HCl


 10 g SnCl2 *2H2O + 50 mL HCl 37% (ultra
pure) filled up to 500 mL with dist. water.
To remove any traces of mercury, bubble
the solution with argon, nitrogen or air e.g.
at a flow rate of 2 L per minute for 15 min.
Solution can be stored 3 days!

Hydroxylammonium 12 % NH2OH*HCl
chloride  12 g NH2OH*HCl filled up to 100 mL with
dist. water.

Potassium bromide/ In a fluoropolymer or glass bottle dissolve 1.08 g


Potassium bromate of KBr in 100 mL HCl. Use a clean magnetic stir
bar, stir for appr. 20 min. Slowly add 1.52 g of
KBrO3 to the acid while stirring. The colour of the
solution should change to orange or yellow.

Warning!
This process generates copious quantities of free
halogens, which are released from the bottle

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mercur – Atomic fluorescence

Calibration Mercury:
0/ 30/ 100 ng/L Hg

Example 100 ng/L Hg


 Solution 1: 1g/L Hg
(commercial standard solution)

 Solution 2: 1 mg/L Hg
100 µL solution 1 + 1 mL
KBr/KBrO3-solution are filled up
to 100 mL with dist. water (DF
1000).

 Solution 3: 10 µg/L Hg
1 mL solution 2 + 1 mL
KBr/KBrO3-solution are filled up
to 100 mL with dist. Water
(DF 100).
Prepare freshly!

 Solution 4: 100 ng/L Hg (ready to use)


1 mL solution 3 + 1 mL
KBr/KBrO3-solution + 50 µL
hydroxylammonium chloride
solution are filled up to 100 mL
with dist. water (DF 100).
Prepare freshly!

30 ng/L: 300 µL solution 3

Warning!
Volumetric flasks and bottles made of quarz,
borosilicate glass or fluoropolymer (PFA).

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mercur – Atomic absorption

Calibration Mercury:
0/ 100/ 500 ng/L Hg

Example 100 ng/L Hg


 Solution 1: 1g/L Hg
(commercial standard solution)

 Solution 2: 1 mg/L Hg
100 µL solution 1 + 1 mL
KBr/KBrO3-solution are filled up
to 100 mL with dist. water (DF
1000).

 Solution 3: 10 µg/L Hg
1 mL solution 2 + 1 mL
KBr/KBrO3-solution are filled up
to 100 mL with dist. Water
(DF 100).
Prepare freshly!

 Solution 4: 100 ng/L Hg (ready to use)


1 mL solution 3 + 1 mL
KBr/KBrO3-solution + 50 µL
hydroxylammonium chloride
solution are filled up to 100 mL
with dist. water (DF 100).
Prepare freshly!

500 ng/L: 5000 µL solution 3

Warning!
Volumetric flasks and bottles made of quarz,
borosilicate glass or fluoropolymer (PFA).

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