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For conventional separation columns, sample sizes usually vary from a few to
20μl. The capillary column requires the sample amount to be inserted smaller so in
this case the system dividing the sample line is designed in the injector set used to
assign only a fraction of the sample amount injected into the column , the rest is
discharged out.
Injection technique:
Suck the sample solution into the injection pump and adjust the solution to
the line and then pull the plunger out later so that the sample volume is
moved out into the injection pump body (hollow needle head).
After piercing the needle through the silicon rubber gasket of injector to
saddle about 3 to 5 seconds so that the needle is balanced temperature in
injector then new push Pittong.
This helps to avoid a number of hard-to-evaporated structures in the needle
leading to the quantitative tolerances of these structures.
3.1.2.3. Chromatographyc column
3.1.2.3.1. Introduce
In fact there are different forms of split columns to satisfy research purposes. In
general, the column of chromatography needs to satisfy the following
requirements:
Ensure good metabolism between the mobile and static phase by
optimizing the parameters of the Van Deemter equation.
High permeability means a slight pressure drop at a given gas speed.
High load capacity of the column.
Have a wide usage temperature and withstand high temperatures.
3.1.2.3.2. Stuffing column
The column is usually made of stainless steel, nicken, glass with diameters of
about 3 to 6 mm and length range from 1 to 5 m. The stuffing column contains
solid-bearing particles coated with a liquid static phase or a solid particle itself
as a static phase. Uniform particle size will reduce column height and increase
resolution. Small particle size reduces the dissolved balance time thus improving
the efficiency of the column. However, the smaller the particle size, the less free
space between the particles and the pressure to squeeze through the column must
be higher.
The particle size is performed according to the micrometer or mesh, i.e. the mesh
that the particle can pass through or be retained on the sieve. For example
80/100 mesh particles pass through the Sieve 80 mesh (170 μm) but do not go
through the CIN 100 mesh (150 μm).
The requirement of a solid bearing is to not engage in separation and is capable
of holding the static phase (not less than 10%).
Solid carrier:
There are two important things to pay attention to when choosing a bearing
substance: structure and surface properties.
The structure contributes to the effectiveness of the bearing, while the
surface features govern the involvement of the bearing substance on the
outcome of the separation.
These substances are chemical inert substances with all types of samples.
It should have a large surface area so that the liquid phase can undergo a
thin film layer and the surface structure must be appropriate to keep that
thin film layer. However, large surface area is not a guarantee of effective
columns.
Here are some of the most common types of bearing:
Chromosorb A is used in the regulation scale, which is capable of holding
good liquid phase (up to 25%), having a hard-to-break structure and a
fairly inert surface. Are typically produced in sizes 10/20, 20/30 and
30/40 mesh. Used for long columns, low pressure spreads.
Chromosorb G is used to separate polarity compounds. Thanks to its low
surface area, hardness, high density it is used for low-content liquid phase
impregnation cases. Impregnated 5% on Chromosorb G corresponds to
12% impregnation on Chromosorb W.
Chromosorb P is made from the C-22 refractory Brick (P-pink symbol)
and relatively hard. The surface is less absorbent than other Chromosorb
types, which are used for the extraction of hydrocarbons.
Chromosorb W is made from Celite 545, whitish and more fragile than
type G. Relatively non-absorbent surface and used to separate polarized
organic compounds.
Liquid phase percentage:
The amount of liquid needs to be sufficient to wrap the particles by a uniform
thin layer. Excessive liquid phase will stagnate in gaps between particles that
reduce column performance. On CHROMOSRB carrying agent when the liquid
phase ratio is greater than 30% the effect of the column decreases greatly. It was
previously a 15-30% liquid, but now tends to only be 2-10%.
Since the time to save the scale with the liquid phase in the column should allow
analysis as fast as the column has a smaller amount of liquid phase. When liquid
loads are too low will appear the adsorption on the bearing substance. Want to
avoid this need to take inert substances. The evaporation of the prototype must
also be calculated by selecting the liquid phase. Volatile substances like steroit
need to be analyzed in low-load columns (about 3% or lower). Highly volatile
substances such as mild hydrocarbons require a high load column (20-30%) As
the amount of liquid more and more time the substance is in the liquid phase, the
better the distribution.
Stuffing density:
The stuffing density has a pronounced influence on the retention on the static
phase. The static phase is coated on a bearing substance on the basis of the
weight percentage, while the stuffed material is placed in the column on a
volume basis. If the filling density of the bearing substance increases, the total
volume of static phase in the mast increases.
Preparing the static phase and stuffing column:
The carrier is static on a variety of ways, one of which is using a rotating
machine.
Taking an amount of static calculation is readily dissolved into a suitable
solvent in a round bottom, for a solid carrying capacity with the
appropriate amount of calculation. Put the tank in the recording machine.
Spin the tank until the solvent flies out. Heat tank by hydro or infrared
light.
Take the straight pipe with the desired length and diameter, a glass-
headed button, the other one fitting a tube, filled with a bearing that was
soaked in the liquid. Shake the column with the shake or lightly smash the
column until there is no decrease in the volume of the substance, the
column is fully loaded. The rest of the head button is glass and rolled
again to suit the heat stabilizer of the GC machine.
Practice the column:
The column needs to put at least 2 hours at 25 oC on the maximum temperature
that the column will use but cannot be too upper limit of the evaporation
temperature of the liquid phase. A small bearing airflow (5-10 ml/ph) is given
through a column. The output of the open column does not connect to the
detector to avoid.
3.1.2.3.3. Capillary column
The majority of the analysis of the gas chromatography using the capillary
columns is between 15 and 100 m long and the diameter is very small from 0.10
to 0.53 mm. These columns are made from melted pure oxide glass that has a
much higher level of cross-linking than the glass usually should be durable and
withstand a high temperature to 350oC. The high tension of the glass tube allows
the fabrication of thin and malleable columns.
The open capillary columns have thin-coated film layers on the pipe to provide
higher resolution, shorter analysis time and higher sensitivity than the stuffing
column but they have lower capacity for samples. The narrowed capillary
column provides a higher resolution than the capillary expansion column but
they require higher pressure to operate and have capacities for smaller samples.
The film grade thin liquid phase thickness ranges from 0.1 to 5 μm on the inner
surface as illustrated in Figure 2.5. If lowering the thickness of this movie layer
will increase the resolution, reduce the saving time and reduce the amount of
space for the sample. Another type is that the capillary columns have solid
particles that are coated with a liquid static layer mounted on the inner surface of
the column. Because the surface area of this type increases, this column can
handle samples larger than the thin Film overlay column on the column. This
type of column is an intermediate between the film-coatedcapillary column and
the stuffing column.
3.1.2.4. Detector
Very strict detector requirements: all components present in the 0.1 μl form must
be detected at 1% for should be quickly detected 0.002 μl (with a volume of 10-6g)
sample. The detector now measures smaller quantities to the ranks. Currently in the
GC method one uses the following types of detector:
Thermal conductivity Detector (TCD): The operation of the detector based on
the thermal balance of a heated conductor. When the substance needed to be
analyzed, the conductivity of the gas mixture will be low, the cord will heat up,
appearing an electrical signal. Thermal conductivity Detector suitable for many
substances to analyze.
Flame ionization Detector (FID): When burning organic compounds in the
flame, they will produce ions. Electrodes near the flame will detect the
presence of ions by the occurrence of a small electric current that runs through
the circuit. Lines can be measured even if the certificate is approximately 10-
12A. This is the most used detector, detected up to 10-9g.
Electron capture Detector (electron-ECD Detector): Thanks to a radioactive
source such as 3 H or 63Ni, the gas bearing ionization creates a "certain line" in
the Detector circuit. When an electron absorbent analyzer is absorbed it will
reduce this strain, especially when the compound contains high-voltage
elements. The line will decrease, generating the recording signal to. Detector is
especially sensitive to halogen-containing compounds. Electron absorption
Detector is very favorable for environmental analysis. High sensitivity, reaches
10-12g.
3.1.2.5. GC information
Conventional chromatography represents on two X and Y axes, in which the
detector signal is indicated on the y-axis and the time indicated on the x-axis.
When a component of the sample is steamed and detected thanks to the detector,
the signal will be recorded. The recording time at the signal is KD's function and
hence it provides the same sample information as the semi-common wave in the
extreme spectrum, and will identify a component in the sample. Quantitative
information from the decoction is drawn from the spot signal detector is the
function of time. Area below at scale with the amount of analyzed substance. This
amount can be displayed in molar units or mass units, but proportional constants
will vary:
SA = Area below pic - R A
In there R is an area on a gas A is represented by one or the area on a gram of gas
A represents a gram of.
Figure 3: Gas chromatographic graph
References
[1] http://hoathucpham.saodo.edu.vn/tin-tuc/sac-ky-khi-phuong-phap-phan-tich-hien-dai-
ung-dung-dinh-luong-dang-vet-cac-doc-to-thuc-pham-110.html
[2] Bùi Xuân Vững, Cơ sở phân tích sắc ký
[3] https://en.wikipedia.org/wiki/Gas_chromatography
[4] Hoàn Minh Châu, Cơ sở hóa học phân tích, nhà xuất bản khoa học và kỹ thuật, Hà
Nội, 2002
[5] Vũ Thị Thúy Hằng, Xác định đa dư lượng hóa chất bảo vệ thực vật trong một số loại
thực phẩm có nguồn gốc từ chè bằng phương pháp sắc ký khí GC – MS, 2016
[6] Lê Thu Thảo, Nghiên cứu xây dựng quy trình phân tích chất ma túy tổng hợp
methamphetamine(MA) và methylennedioxy menthamphetamine(MDMA) trong tóc bằng
sắc ký khí khối phổ, 2015