NC Water Analysis PDF

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FlashSmart Analyzer for

saline and acid samples analysis

Dr. Liliana Krotz, OEA Application Manager,


Thermo Fisher Scientific, Milan, Italy
Configurations

Single reactor Double reactors

Manual Injector AI / AS 1310 Liquid Autosampler

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Consumables
• For Single reactor
Reactor: Ceramic tube (18 mm diameter, p/n 468 020 10)
Catalyst: Copper Oxide (p/n 338 217 10)
High Quality Copper (p/n 338 353 12)

• For double reactors


Combustion Reactor: Ceramic tube (18 mm diameter, p/n 468 020 10)
Catalyst: Oxidation catalyst (mix CuO + Pt on allumina, p/n 338 400 00)
Reduction reactor: quartz tube (18 mm diameter, p/n 468 200 70)
High Quality Copper (p/n 338 353 12)

• For both configurations


Nickel sheet (p/n 252 051 10, set of 2, 0.15x130x130 mm)
Big filter (p/n 281 130 64)
Anhydrone (p/n 338 219 00)
Quartz Turnings (p/n 338 223 00)
Quartz Wool (p/n 338 222 00)
IRMS Separation Column (SS, 3 m, 6x5 mm, p/n 260 07931) installed into the oven at 50°C

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Comparison between manual and automatic injection (100 ul)
using a single reactor

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Data comparison between single reactor and double reactors
using the AS 1310 Autosampler (volume injected 100ul)

Lower
N and C
content

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Blank evaluation
Blank analysis was performed with 100 ul of bidistillated water. The area of
Nitrogen and Carbon was evaluated using the single and double reactors.
Method Single reactor Double reactors
Element N C N C
Blank Area (mVolt/sec) 1300 1100 1800 2000
Area of 10 ppm N (mVolt/sec) 2500
Area of 4.2 ppm C (mVolt/sec) 4200 3800
Area of 12 ppm N (mVolt/sec) 4000
Area of 7 ppm C (mVolt/sec) 6000

Overlay of chromatograms
Red chromatogram: Blank – bidistillated water; Black chromatogram solution with the lower content of N and C

Single reactor Double reactors

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Manual injection - 200 ul / Double reactors
Carbon determination

Sample Solution 5 Solution 3.2


ppm C ppm C
3.9 3.1
4.7 3.3
4.0 3.0
4.8 3.0 Overlay of chromatograms
4.9 3.2 Red chromatogram: Blank Area about 2500 mVolt/sec
4.9 3.0 Black chromatogram solution 3.2 ppm C Area about 6000 mVolt/sec
4.0 3.0
4.9 3.1
5.0 3.2
4.9 2.9
Average 4.6 3.1
RSD % 9.668 3.991

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Manual injection - 250 ul / Double reactors
Carbon determination

Sample Solution Solution Solution


3.2 ppm C 2.1 ppm C 1.4 ppm C
3.3 2.2 1.4
3.1 2.3 1.4
3.3 2.0 1.4
3.1 2.1 1.5
3.0 2.0 1.4
2.9 2.2 1.4
Overlay of chromatograms
3.2 2.1 1.4 Red chromatogram: Blank Area about 2000 mVolt/sec
2.8 2.1 1.3 Black chromatogram solution 1.4 ppm C Area about 4300 mVolt/sec
3.0 2.0 1.4
3.1 2.2 1.5
Average 3.1 2.1 1.4
RSD % 5.258 4.872 4.026

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Filling of the Nickel sheet – Lifetime ceramic tube
• Single Reactor method.
• The Nickel sheet is inserted only in the combustion zone.
• Volume injected 100 ul by AS 1310 Liquid Autosampler.

Sample Saline Lake water


Determination TC (ppm) TOC (ppm)
32 4.0
33 4.1
32 4.1
32 4.1
34 3.8
32 3.9
32 4.0
34 4.0
32 3.8
33 3.8
Average 33 4.0
RSD% 2.59 3.19

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Summarize of the lower Carbon results

Sampling Manual Injection AS1310 Liquid Autosampler

Reactor Single tube Double tubes Single tube Double tubes

Volume Injected C (ppm) C (ppm) C (ppm) C (ppm)

100 ul 4 7 4 7

200 ul 3 3 - -

250 ul 1.5* 1.5* - -

* The lowest limit reaches by FlashSmart Analyzer stand-alone

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