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CKIC

Studi o Ultima Analysi


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Changsha Kaiyuan Instruments Co.,


Ltd

Conten
CKIC

Overview

analysis, purpose of element


testing

Testing Procedure
General element
testing
Related standards
Instrument

procedure

Application &

Stud

&Instrum

Element In Coal
CKIC

S:0.3~4.
0%

0.8~5.0
%

45~85
%

0.20~1.5
%

CKIC

Why Test C,H,N


?
To test C,H,N in
is a
parameter to study the Coal Rank,
calculate the Calorific Value, and
estimate Coal Dry Distillation

CKIC

Why TestC,H,N
?
Carbon makes
H2O evaporation
will take away
calorific value.
To calculate the

Net C.V,

H value is

calorific
H2O evaporation

Why Tes C,H,N ?


CKIC

Nitrogen causes air pollution and acid rain.

Why Tes S ?
CKIC

Safe
ty
Producti
Soci
al
Responsib

Eficie
nt
Energy

Sulf
ur

Testin Method
CKIC

C&
H
Liebig
method
Electric
QuantityWeight
Infrared
Absorpti
on
method

N
Semimicro
Kjeldahl
Semimicro
Gasificati
on
Thermal
Conductiv
ity
method

Eschka
method
Calcul
High
at ing
temperature
combustion
metho
method
CoulometricTitrat
d
ion metho
d
Infrared
metho
Absorption
d

Summary

of Element

CKIC

Carbon and hydrogen are detected by


separate infrared detector in the form of
carbon dioxide and water vapor.
Nitrogen is detected by thermal conductivity
detector in the form of N2
Sulfur is detected by infrared detector in the
form of sulfur dioxide.

Principleof InfraredAbsorption
CKIC

Based on the principle of Lambert-Beer

Infrared Cell

Principleof Thermal
CKIC

Thermal
Conductivity
Gas
Molecular formula

Molecular weight

Coefficient of
thermal conductivity

Hydrogen

H2

39

Helium

He

33

Neon

Ne

20

10.4

Oxygen

O2

32

5.7

Nitrogen

N2

28

5.6

Air (dry)

Air

29

5.4

Carbon monoxide

CO

28

5.4

Water vapor

H2O

18

4.0

Argon

Ar

40

3.8

Carbon dioxide

CO2

44

3.3

Sulfur dioxide

SO2

64

1.6

Principl of Therma Conductivity


CKIC

Befor
e
Analys

Reference
Cell

He

He
Measuring
Cell

Stable

Principl of Therma Conductivity


CKIC

Durin
g
Analys

Reference
Cell

N2

He
Measuring
Cell

Balance

CKIC

Sulfur Testing

Standard
CKIC

GB/T
25214

STANDAR
DS
Determination of Total Sulfur in CoalInfrared
Absorpti Metho
on
d

GB/T 214 Determination of Total Sulfur in Coal


Standard Test Methods for Sulfur in the
Analysis Sample of Coal and Coke Using
ASTM
High-Temperature Tube Furnace
D4239
Combustion Method
Solid mineral fuels -- Determination of
ISO 19579
sulfur
by
IR
spectrometr

Standard
CKIC

Techniques for Sulfur Analysis

Esch
ka
Meth

Coulo
mb
M
d
e

I
R
Absorpt

Chemical Method

Physical Method

Physical Method

GB
Approved
ISO

GB
Approved
Apply for
ISO

GB
Approved
ISO
Approved

Standards-General

Procedure

CKIC

Instrument Preparation
Perform the instrument set up according to
the instruction manual:
Temperature setting, leakage checking.

Standards-General Testing
CKIC

Calibration
Calibration should be processed before any
normal determinations.
Verification of the calibration.

Standards-General Testing
CKIC

Determinations
Carry out the determination by weighing out a
test portion of each analysis sample within a
mass range recommended by the manufacturer.

CKIC

Sulfur Testing
--Coulomb Titration Method

Standard
CKIC

About Coulomb Titration Method


Sample covered with the aid of Catalyst combusts
in air flow, sulfur is absorbed by KI Solution in the
form of SO2then titrated by the Iodine which
produced by electrolyze the KI Solution. Then
calculate the electric quantity consumed during
electrolysis to calculate total sulfur in sample.

Standard
CKIC

About Coulomb Titration Method

Maintenance
CKIC

Dust cleaning
Surface cleaning
Internal cleaning: filters, electrolytic cell

Leakage checking
O-ring, combustion/reagent tube

Reagent
KI solution, silica gel

Crucible replacement

Application
CKIC

Notes for Sulfur testing:


1. The analyzer can determine solid and liquid
substances;
2. The sample mass can be reduced or increased
according to the pre-determined value of the
sample;
3. It is essential that a representative and uniform
sample be analyzed.

Application
CKIC

About Coulomb Titration Method

Material
Heavy Oil
Plant, Feed,
Grain, and
Coal, Coke,
and
Fertilizers

Pretreatment
0.1 gram, add quartz
sand
to sampl
cove entir
r
e
e
0.1 gram, uniform
powder
0.05 gram, uniform
powder
0.05-0.1 gram, uniform
powde
r

CKIC

Sulfur Testing
--Infrared Absorption Method

Standard
CKIC

About Infrared Absorption Method


Sample combusts at a specified temperature in a
stream of oxygen, Moisture and particulates are
removed from the gas by filters, sulfur is detected
by the IR cell in the form of SO2.

Standard
CKIC

About Infrared Absorption Method

Maintenance
CKIC

Dust cleaning
Surface cleaning
Internal cleaning: reagent tube, filters, IR cell chamber

Leakage checking
Gas supply, o-ring, combustion/reagent tube

Reagent
Magnesium perchlorate

Crucible replacement

Application
CKIC

Notes for Sulfur testing:


1. The analyzer can determine any solid substance
which can be burned;
2. The sample mass can be reduced or increased
according to the pre-determined value of the
sample;
3. It is essential that a representative and uniform
sample be analyzed.
4. Draft calibration is also needed before each
patch of analysis.

Application
CKIC

Material
Cement,
Limestone, Lime,
andPlant,
Similar-Type
Feed,
Grain, and
Flo and
Coal, Coke,
Graphite
Ore
s
Fertilizers

Plant tissue

Pretreatment
0.3 gram, uniform powder
0.35 gram, uniform powder
0.3 gram, uniform powder
0.1 gram, uniform powder
0.05-0.1 gram, uniform
powder
Weigh 0.25 gram sample
which should be of uniform
consistency
and dried at 85 for two
hours
prior to analysis.

Instrumen
CKIC

Medium Model
IR Absorption

Economic Model
Coulomb Method

5EIRS3000
5EIRSII

5ES3200

Advanced Model
IR Absorption

CKIC

CHN Testing

Standard
CKIC

ISO
29541
ASTM
D5373

GB
?

STANDAR
DS
Solid mineral
fuels Determination
of total
carbon, hydrogen and nitrogen
Standard Test Methods for
Instrumental Determination of
Carbon, Hydrogen, and Nitrogen
in Laboratory Samples of Coal
Determination of total carbon,
hydrogen and nitrogen content in
coal by Instrumental method

Standards-General Testing
CKIC

Instrument Set-Up
Verify the specifications according to the
instrument operating manual.
Verify the condition and quantities of all
chemicals.
Leakage checking.

Standards-General Testing
CKIC

Blank Analyses
Perform blank analyses to establish carbon,
hydrogen and nitrogen levels in the
combustion and carrier gases.

Standards-General Testing
CKIC

Conditioning
Select a proper coal to check the stability of
the instrument, whether a corrective action
needed before proceeding with calibration.

Standards-General Testing
CKIC

Calibration
Calibration should be processed before any
normal determinations.
Verification of the calibration.

Standards-General Testing
CKIC

Determinations
Carry out the determination by weighing out a
test portion of each analysis sample within a
mass range recommended by the manufacturer.

Standards-General Testin

Procedure

CKIC

Determinations

Preparing foil
cup

Weighing
sample

Making foil
capsule

Loading
sample

InstrumentCKIC

Analysis Process
Each sample analysis is divided into
three

Purg
e

Clean sample
Clean gas blending tank
Clean gas path tube
Read blank voltage

stages
.

Combusti
on

Sample fully
combusts
Remove gas
impurities and dust
particle.

Analys
is

CO2 and H2O are detected


through Infrared cell.
N2 is analyzed in TCD.

Instrument18

99.995%
O2

Sample

C Result

reagents

H Result

H2O IR Cell

CO2 IR Cell

Thermal
Conductivity Cell

CO2
H2O
SOx
NOx

Purify
N2

CO2
H2O
NOx
O2

CO2
H2O
NOx
O2

CO2 Reduced
H2O
N2

N Result

InstrumentCKIC

Gas Blendin Tan


g
k

Control
Circuit

Infrare cell
d

Double layer
sample
automatic

loade
r

InstrumentCKIC

MODEL
Analysis
time(min.)
Auto-Sampler
Analysis Range

5E-CNH 2200
Approx. 5-6
35 Samples, stackable to 70
samples

C:0.005%~100%50ppm;H:0.02%~50%200ppm;N:0.0
08~50%80ppm

Sample Mass
(mg)

80-100recommended

Analysis
Method

C&H:
by IR Absorption Method N:Thermal
detection
method
Carrier Gas: Helium gas, purity 99.995%,
(0.250.01)Mpa
Combustion Gas: Oxygen,for measuring C&H:
purity99.50%;
for measuring nitrogen, the purity of higher
99.995%
0.250.01Mpa, power gas: Compressed air or

Gas
Required
Furnace
Type

C0.5%;H0.15%;N0.08%

Maintenance
CKIC

Dust cleaning
Surface cleaning
Internal cleaning: reagent tube, filters, ballast tank, IR cell
chamber

Leakage checking
Gas supply, o-ring, combustion/reduction tube

Reagent
Magnesium perchlorate, CO2 absorb reagent, high purity
copper, N-catalyst

Crucible replacement

Application
CKIC

Power plants
Coal mines
Commercial Labs
Steel Plant
Organic Chemicals
Milling
Applications
(Feeds, Oilseeds)
Agriculture
Plant Food
industry
Fertilizer Plant

Application
CKIC

Meat, Food product


Biomass
Hydro-carbons,
Flour, grain,
agriculture
Fertilizer
Leaves and tobacco
Plastics

Need do pre

Application
CKIC

Notes for CHN testing:


1. Its suit for solid substance which can be burned;
2. The sample mass can be reduced or increased
according to the pre-determined value of the
sample;
3. Blank and draft calibration are also.
4. It is essential that a representative and uniform
sample be analyzed.

Application
CKIC

Nitrogen in Meat and Similar Food Stuff


Weigh 0.08gram sample into the tin foil cup, seal
immediately after the sample has been prepared.

C,H,N in Hydrocarbons, Flour and Plant


tissue
Follow the analysis procedure with coal.

Application
CKIC

Nitrogen in fertilizer
Weigh 0.05 gram uniform powder into tin foil cup,
calibration should be processed with EDTA before
any analysis.

C, N in leaves and tobacco


Weigh 0.25 gram uniform powder into bigger size
of tin foil cup, 24-hole carousel instead of the
normal 35-hole carousel of the instrument.

Application
CKIC

Nitrogen in Plastics
Weigh 0.15-0.25 gram uniform powder into bigger
size of tin foil cup, 24-hole carousel instead of the
normal 35-hole carousel of the instrument.

C,H in Biomass
Weigh 0.15 gram uniform powder into bigger size
of tin foil cup, 24-hole carousel instead of the
normal 35-hole carousel of the instrument.

Case Stud
27

Ultra low element content sample


1

Characteristic

Solution

Note

Case
28

N content
<300ppm

Case
29

Increase
weight

80mg

800mg

Case
30

Increase analyzed gas

5ml

10ml

Case Stud
31

Keep air out

Questio

CKIC

Than You

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