Tool for Trace N,S,Cl with

Sulphur analysis compliant to

Euro6 Specs Fuel, UOP987,
UOP988 International method

NSX-2100 series
29 November 2017
th
,
Skytech Systems, Thane , India
Mitsubishi Chemical Analytech Co., LTD.
 Euro6 Specs Fuel
Almost All the Sulphur Analyser in the market based on EDXRF technique will
go obsolete due to non complaince of methods for <10 ppm. UVF can easily meet
the need of Euro6 specs Fuel and more Accurately and Precisely backed with an
international method and offer the following advantages
 No matrix effect – only 1 calibration line using Iso-octane or toulene can be used for measurement of
all samples (ie. Petrol, Diesel, Base oil, Lube etc..)

 No films or samples cups consumables after every analysis. Very very low running cost

 50 ul or less CRM enough for calibration

 Unattended analysis for 50 samples

 No Helium or Vacuum required

 User friendly – no sample preparation or frequent / Multiple calibration line

 No need to the risk of rays exposure or disposal of Xray tubes etc..

 Has international Method Compliance from ppb level to ppm level

 Background
 Almost All the Sulphur Analyser in the market based on UV Fluorescence technique
can analyse < 500 ppb of Sulphur in liquids but the challenge is to measure these
levels Accurately and Precisely backed with an international method.

Why International method compliance ????

When all the parties (ie. Customer, TPI, Vendor, Licensor
etc..) are in acceptance with the results, then it is fine
But
Incase of objection or challenge, it has been seen the easy
way out for the non complying party is just to question
1) Is this analysis complaint to any International
method???
2) How can we accept results of <500 ppb as
ASTM D7183 is valid only from 500 ppb
onwards?
 Solution for liquid is Standard
method,UOP987-11
 Ultra-Trace Sulfur in Liquid Hydrocarbons by Oxidative
Combustion with Ultraviolet Fluorescence Detection

Scope : 10 - 1500 ng/g

 NSX-2100V with liquid sampler ASC-250L

 Option: trap & release unit TRU-210

 Shall maintain at 15 C for both sample tray and syringe

for high volatile sample.

 Option: sample temp. controller STC-

210L .
 Solution for Gas/LPG is Standard
method,UOP988-11
 Low Trace Sulfur in LPG and Gaseous
Hydrocarbons by Oxidative Combustion with
Ultraviolet Fluorescence Detection
Scope: 10 – 1400 ng/g

 LPG shall be expanded to gas before analysis.

NSX-2100V with Gas injector GI-220

Option: trap and release unit TRU-210
 Option1: Trap & Release
VF-210 injection
Enrichment and separation
TRU-210
Trap/release tube Enrichment of Sulfur
SD-210
furnace

Gas

Trap
column
filling heater
Separation of NOx
： SO2
： NO
Trap and Release Unit is consist of a trap column ｘ

and a temperature controller. Gas

By changing temperature of trap column, SO 2 is
Adsorbed (low temp) and desorbed (high temp).
By this method, SO2 is concentrated and separated from other
elements (CO2 and NOx gas).
Feature 1 : Trap & Release
 True Nitrogen and Sulfur separation.

NOx

SO2

Combustion&Trap Release&Sampling
Feature 2: Trap & Release
 Obtain higher signal/noise ratio
50ppb 200ul
with Trap& Release unit
50ppb 200ul
without Trap& Release unit
 Effect of TRU
Peak profile by changing amount of sample
Non –trap Sulfur peak BIG peak by trap
95
50ng/ml 25,50,100,150,200ul
50ng/ml 25,50,100,150,200ul 50ng/ml 50,100,200ul
43
43

37
30
37

Peak will be spread to time Peak profile will not spread to

axis by amount. Not so easy time axis by amount. Thus
to detect small peak even easier to detect because of
higher amount. getting higher peak .
 Trap & Release
 Ultra trace Sulfur to 5 ppb (liquid)

gas

： SO2
Separation
： NO ｘ

Gas

Concentration
Application (Ultra Trace Sulfur)
Conc.
Sample Injection (ml ） Repeat RSD （％）
（ V/V)

Ethylene 100 3 26ppb 9.5

Methane 100 7 46ppb 9.6

Desulfurized
100 3 30ppb 10.8
Natural gas

Hydrogen gas 50 5 112ppb 1.7

NSX-2100V (SD)+GI-220+TRU-200
 Reference, NSX-2100V+TRU+GI220
customer Sample purpose

Electric mfg. Desulfurized fuel gas Monitoring catalyst

CO2 QC for CO2 gas for beverage

Gas mfg.
Natural gas Monitoring desulfurization

Chemical mfg. Gas in plant QC

Refinery Fuel gas Quality after desulfurization

 Auto repeat analysis
 Sulfur in hydrogen gas (n=5 ）
injection 50ml
average 112.3ppb
RSD 1.8 ％
140.00

120.00
Sulfur conc （ｐｐｂ V/V）

100.00

80.00

60.00

40.00

20.00

0.00
 Gas injector GI-220
 Auto syringe injection
 Up to 200mL
 Variable injection amount
 High level safety for
flammable sample handling
 TRU-210
ASC-250L GI-220
liquid gas/pump •TRU unit is for Vertical, UVFL sulfur.
•Auto sample injector
•ASC-250L (liquid)
•GI-220 (gas)

SD-210 VF-210
Detectors Furnace
Ultra trace with Trap & Release
system injector LOQ injection  High amount injection/low
concentration is realized
0.05
NSX-2100V
GI-220 ug/L
200ml by NSX-2100V+TRU-
+TRU-200
200+GI-220
 Option 2: STC-210L

Sample temperature Controller

 Cooling ON, Before After
Conc. aver RSD Conc. aver RSD
age age
(ppm) (ppm)

2.59 7.59
4.71 7.62
3.56 7.42
3.43 7.53
3.67 7.52
3.59 21.05 % 7.54 1.02 %
tray=20 C,syringe = 15 C
 STC-210L
Peltier cooling for both tray and syringe
Condensation considered
 Cooling and/or Heating
 Cool:
 High volatile sample

Tray: 15 C
Syringe: 15C

 Heat:
 Viscous sample
 Tray: 60 C
 Syringe 60 C
 Feature
Modular system – customized configuration

CRI-210V ASC-250L GI-210 GI-220 GI-250 ABC-210

liquid liquid gas gas/pump gas/LPG solids

MCD-210 / ND-210 / SD-210

Vertical Horizontal
Detectors IC
Furnace
For Horizontal
 NSX-2100 Series Line-up
PC Printer ASC-240S ASC-250L

ABC-210

GI-210

GI-230

GI-220

MCD-210 / ND-210 / SD-210 / GA-210 VF-210 or HF-210 GI-240

Detectors Furnace Samplers

 One 4 all
 MCD Coulometric Chlorine & Sulfur
 SD UVFL- Sulfur
 ND CLD- Nitrogen
 GA (prep station) followed IC. (S, Br, Cl, F, I)

 Sample Injectors, options

 Liquid/Solid/Gas/LPG sampler
Specific option for element
 TRU for SD/MCD(S), Water sampler for ND.
Principle, combustion - detection
MFC ： MASS FLOW

Pyrolysis Tube
CONTROLLER

Filter

Mixer
Exhaust

Tube Dryer

Furnace
Electric
OZONE
SCRUBBER
N Cell
OZONIZER
S cell
(exhaust)
 Chlorine
Ag Working electrodes Constant rate injection
Ag Detection electrode
Reference electrode

Sample Controller unit

Titration cell unit injection port

Valve
Mass flow controller

Heater furnace

Combustion tube

Stirrer Dehydration Tube heater

 Key Features of NSX-2100
1. BETTER LDL NITROGEN: 30 ppb
(UOP981)
2. BETTER LDL Chloride : 70 ppb (ASTM
D7457)
3. BETTER LOQ Sulphur : 10 ppb (UOP
987 Part B)
4. BETTER LOQ Sulphur : 100 ppb (UOP
987 Part A)
5. FASTER! shorter time for Sulfur
6. STABLE UVFL Sulfur cell
7. SIMPLE, 2 measurement range, N/S.
 Nitrogen
Injection Volume = 90 ul
n=5
STD Mass RSD Low Range ・ Pyridine/Toluene STD
(ug/ml)
Area 7000
(ng) %
6000
0.00 0 24.3 3.29
5000
0.01 0.9 26.7 5.19 2
r = 0.9998
4000
0.05 4.5 43.4 4.65
0.1 9 71.7 1.71 Area 3000

0.5 45 292.2 0.41 2000

1 90 582.6 1.07 1000

5 450 3101.8 1.41 0

10 900 6347.7 0.63 0 200 400 600 800

mass(ng)
 FAST Analysis
 Improve productivity, reduce utility.
 5 min  3 min

 TS-100V about 5  NSX-2100V about

min. 3min.
DBDS / Toluene 20 ug/ml 20ul injection
 Measurement Stability
 Excellent measurement stability has been realized
with the new temperature controlled detector cell.
UVFL Sulfur 10μg/ml 10μl RSD 0.78%

20
18
Concentration (ug/ml)

16
14
12
10
8
6
4
2
0
0 5 10 15 20 25 30
Number of Measurements
Vertical Furnace

Open/Close furnace.
Higher Volume > 200 uL can be
injected
Samples is injected at 1ul /sec and
forms a drop and falls at the same point
again and again.
Very high precision
Better controlled combustion
Connection to gas line is done via ball
joint and clip.
Incomplaince with International method
 Coulometry MCD-210
 Only Vertical System compliant to ASTM D7457 (ie.
LDL of 70 ppb)
 High sensitive measurement on Cl (S)
 Cl- 0.05ppm, S- 0.10ppm
 Stable cell, Efficient dehydration, No acid mist.
 One cell for all over range.
 No need to have sets of cell for each range.
 Larger volume dehydration for automation (20ml,
vertical ） .
Software NSX-2100

Full-automation
from “Heater on”
to “Gas shut
down”.
Simultaneous N & S
 Recent trends from Indian Petroleum Industry
…. NSX 2100 with TRU (UOP987 Part B)
 UOP Gudgaon

 Borl

Ril Dahej

Essar Jamnagar

RIL Jamnagar – 3 units

We though that only Private Refineries and Petroleum institutes can go for this ….

We were proved wrong

 Recent trends from Indian Petroleum Industry
…. NSX 2100 with TRU (UOP987 Part B)
 HPCL Vizag

 BPCL Mahul

 HPCL Mahul (recently placed order)

CPCL Chennai – an IOCL Refinery (recently placed order)

 NRL Numaligarh – an BPCL Group Refinery (recently placed order)

why did all of them prefer NSX 2100V with TRU ?

When any one of the involved party (ie. Licensor, Refinery QC, Certification Agency/
Third Party Testing Lab or Customer) is not happy with the result of < 500 ppb – the first
question raised is which methods does the instrument comply for these < 500 ppb
reading. The only solution is NSX 2100 V with TRU which is complaint from 10 ppb
onwards.
Products for Petroleum/Chemicals
 Combustion prep
station AQF-2100H

 Convertible KF
moisture KF-31

Potentiometric Titrator
GT-200
 Training for
Petroleum/PetroChemicals
 Elemental Analysis – OEA
 Trace N/S/Cl Analysis

 Note – above training can be done onsite

too…….
 Operation and hands on the above
technologies & instrument
 Conclusion

 Vertical Furnace – clean combustion – as sample is combusted drop by drop – no sooth

formation (ie. Carbon Deposition) – also same temperature for the comlpete sample – better
Precision

 Vertical Furnace – higher volume injection > 200 ul – better lower detection limit

 NSX 2100 V with TRU – 2 ppb LOD and has method compliance (UOP 987 part B) from 10
ppb onwards – only instrument in market for method compliance for < 500 ppb

 NSX 2100 V N – 30 ppb with method compliance (ie. UOP 981) – only instrument in market
for method compliance for < 100 ppb

Easy Maintenance with Open/Close Furnace

 NSX 2100 V Cl – 50 ppb and has method complaince (ASTM D7457) from 70 ppb –
Only vertical instrument in market for method compliance for < 1000 ppb

India’s customers preference - NSX 2100 V with TRU for N, S, Cl analysis – only instrument
with lowest detection limit with International Method compliance

Incase of interest for Carbon analysis, opt for ASTM D5291 complaint instrument. Separate
instrument for C determination will ensure your all important trace level NSCl analysis (ie. ppb
levels) is not contaminated
Training and application infrastructure of Skytech in addition to the expertise of >20 years
Any Questions
please ???
Thank you