HJ/T 40-1999 English PDF (HJT40-1999)

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HJ/T 40-1999: Stationary source emission. Determination of benzo(a) pyrene. High performance liquid chromatography
HJ/T 40-1999
HJ
STANDARD OF THE ENVIRONMENTAL
PROTECTION AUTHORITY
Stationary Source Emission – Determination of Benzo
(a) Pyrene – High Performance Liquid
Chromatography
ISSUED ON: AUGUST 18, 1999
IMPLEMENTED ON: JANUARY 01, 2000
Issued by: National Environmental Protection Authority
Table of Contents
1 Scope ... 3
2 Method Principle ... 3
3 Normative References ... 3
4 Reagents and Materials ... 3
5 Apparatus ... 5
6 Collection and Storage of Sample ... 5
7 Pre-Processing of Sample ... 6
8 Operation Procedures of chromatographic Analysis ... 7
9 Presentation of Results ... 11
10 Precision and Accuracy ... 12
11 Description ... 12
Additional Information ... 13
Stationary Source Emission
– Determination of Benzo (a) Pyrene
– High Performance Liquid Chromatography
1 Scope
1.1 This Standard is applicable to the determination of benzo (a) pyrene discharged
from a stationary pollution source in an intentional emission manner.
1.2 When the gas production volume is 1.0m3, the constant volume of the sample is
1.0mL, and chromatographic injection volume is 10µL, the limit of detection for the
benzo (a) pyrene shall be 2ng/m3, and the concentration range for quantitative
determination shall be 7.6ng/m3~4.0µg/m3.
2 Method Principle
Collect samples by non-glue glass fiber filter cartridge or glass fiber filter membrane;
extract benzo (a) pyrene by cyclohexane; and pass the extract through a Florisil
chromatography column; then use a mixed solvent of dichloromethane and acetone to
elute the benzo (a) pyrene absorbed on the column; after concentration, then
measured on a high performance liquid chromatograph that is equipped with a
fluorescence detector.
3 Normative References
The following standards contain provisions which, through reference in this Standard,
constitute provisions of this Standard.
GB 16157-1996 The Determination of Particulates and Sampling Methods of
Gaseous Pollutants Emitted from Exhaust Gas of Stationary Source
4 Reagents and Materials
Unless otherwise specified, analytical reagents and pure water prepared in
accordance with 4.1, both of which comply with the national standard, are used in the
analysis.
4.1 Pure water
Use deionized water (or distilled water) to add potassium permanganate; and re-distill
by an all-glass distiller under alkaline conditions. During the whole distillation process,
the purple-red color shall always be maintained; otherwise, potassium permanganate
shall be added. The obtained pure water shall have no significant interference peak
after the blank test of this method.
4.2 Methanol
Use an all-glass distiller to add alkali for re-distilling; collect the distillate; filter it through
0.45µm microporous filter membrane and use it. There shall be no significant
interference peak after the blank test of this method.
4.3 Methylene chloride
Use an all-glass distiller to add alkali for re-distilling; there shall be no significant
interference peak after the blank test of this method.
4.4 Acetone
Undertake the treatment with the same procedures as 4.3.
4.5 Cyclohexane
Undertake the treatment with the same procedures as 4.3.
4.6 Florisil: 60~100mesh, it is used for chromatographic analysis.
Heat for 2h at 400°C; after cooling, use water (4.1) to adjust evenly till the water content
is 11%; seal to store into the reagent bottle with grinding mouth.
4.7 Benzo (a) pyrene standard stock solution
Accurately take 20.0 mg of solid benzo (a) pyrene standard substance; dissolve it in
60mL of cyclohexane (4.5); transfer to a 100 mL volumetric flask; and dilute to the mark
with cyclohexane (4.5). Or use benzo (a) pyrene standard solution and dilute it with
cyclohexane (4.5) or methylene chloride (4.3) to the concentration of 200μg/mL.
The above stock solution shall be stored in a refrigerator at 3~5°C.
4.8 Benzo (a) pyrene standard use solution
Pipette 1.00mL of standard stock solution (4.7) into a 100mL volumetric flask; and
dilute to the mark with cyclohexane (4.5) or methylene chloride (4.3). As the sensitivity
of the used instrument or the concentration of the analyzed sample is different, the
concentration of the standard use solution shall be changed as needed.
Select the sampling method according to 8.2 in GB 16157-1996 (the selected sampling
method shall be consistent with the configuration of the sampling instrument); install
the glass fiber filter cartridge or filter membrane on the sampler; and take sampling
according to certain items (depending on the sampling method) in 8.3~8.6; and the
gas production volume is about 1.0m3.
6.3 Sample storage
The collected samples must be protected from light, or they may be wrapped in black
paper and stored in a 3~5°C freezer. Pre-processing shall be carried out within 24
hours as soon as possible after sampling; and the processed samples shall finish the
analysis within 1 month.
7 Pre-Processing of Sample
7.1 Extraction of benzo (a) pyrene in the sample: carefully put the non-glue filter
cartridge or ultrafine glass fiber filter membrane (after folding the dust side inward) of
the sampled product into the extraction cylinder (be careful not to block the siphon
return pipe) of the Soxhlet extractor (5.3). Add 80mL of cyclohexane (4.5); place it in a
water bath (5.9) at a temperature above 95°C; continue to reflux for extraction for 6h;
and cool for later use.
7.2 Purification of the extract: The obtained extract (7.1) is purified (and enriched) by
a Florisil chromatography column.
7.2.1 Filling of the chromatography column: first fill a small amount of glass wool (5.7)
into the lower end of the glass chromatography column (5.4) to support the filler. Add
2~3mL of cyclohexane (4.5) to wet the column. Weigh about 5g of Ferolisil (4.6) in a
small beaker; make a homogenate with cyclohexane (4.5); fill the above column by
wet filling method; and release excessive cyclohexane in the column to above the
interface of the filler.
7.2.2 Purification of the extract: add the sample extract (7.1) from the top of the
chromatography column (7.2.1); and use 20~40mL cyclohexane (4.5) to clean the
Soxhlet extractor used in the Subclause (7.1) for three times; then it is added to the
upper end of the column at the same time; and the entire solution passes through the
column at a flow rate of < 4mL/min; and the cyclohexane passing through the column
is recovered. Then use 20mL of a mixed solution of methylene chloride (4.3) and
acetone (4.4) (CH2Cl2 : CH3COCH3 = 4 : 1) to elute the benzo(a) pyrene adsorbed on
the column. The eluent was collected in 25mL K-D concentrating bottle (5.5) to be
concentrated. (If the content of benzo (a) pyrene in the sample is high, it does not need
to be concentrated, and the liquid chromatograph can be used for analysis after making
constant volume).
7.3 Concentration of the sample: connect the K-D concentrating bottle containing the
8.2.6.2 Paper speed: 0.3 or 0.5 cm/min.
8.3 Calibration
8.3.1 Quantification by external standard method
8.3.2 Standard sample
8.3.2.1 For the preparation of standard samples, see Subclause 4.8.
8.3.2.2 Use frequency: use standard samples (4.8) to perform periodic re-calibration.
Depending on the stability of the chromatograph, determine the length of the re-
calibration cycle. Generally, it is measured 1 or 2 times every working day, or calibrate
once after measuring every 5 samples.
8.3.2.3 Conditions for using standard sample...