HJ 683-2014 PDF in English
HJ 683-2014 (HJ683-2014) PDF English
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Ambient air. Determination of aldehyde and ketone compounds. High performance liquid chromatography
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Standards related to (historical): HJ 683-2014
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HJ 683-2014: PDF in English HJ 683-2014
HJ
NATIONAL ENVIRONMENTAL PROTECTION
STANDARD OF THE PEOPLE’S REPUBLIC OF CHINA
Ambient air – Determination of aldehyde and ketone
compounds – High performance liquid chromatography
ISSUED ON. JANUARY 13, 2014
IMPLEMENTED ON. APRIL 1, 2014
Issued by. Ministry of Environmental Protection
Table of Contents
Foreword ... 3
1 Application Scope ... 4
2 Normative References ... 4
3 Method principle ... 4
4 Interference and elimination ... 5
5 Reagents and materials ... 5
6 Instruments and equipment ... 6
7 Samples ... 6
8 Analytical procedures ... 7
9 Calculation and expression of results ... 9
10 Precision and accuracy ... 9
11 Quality assurance and quality control ... 10
12 Waste treatment ... 11
Annex A (Normative) Method detection limits and determination low-limits
... 12
Annex B (Informative) Method precision and accuracy ... 13
Ambient air – Determination of aldehyde and ketone
compounds – High performance liquid chromatography
Warning. Some chemicals used in this Method are harmful to human health, so
protective devices shall be worn as required during operation to avoid contact
with the skin and clothes. All chemicals shall be fully sealed and independently
stored in a cool, shady place to prevent leakage and pollution.
1 Application Scope
This Standard specifies high performance liquid chromatography for the determination
of aldehyde and ketone compounds in ambient air.
This Standard applies to the determination of thirteen aldehyde and ketone
compounds in ambient air, including formaldehyde, acetaldehyde, acrolein, acetone,
propionaldehyde, crotonaldehyde, methacrolein, 2-butanone, butyraldehyde,
benzaldehyde, valeraldehyde, m-tolualdehyde and n-hexaldehyde. Other aldehyde
and ketone compounds can also be used in the analysis of this Standard provided that
they pass the suitability validation.
When the sampling volume is 0.05 m3, the detection limit of this Method is 0.28 μg/m3
~ 1.69 μg/m3 and the low-limit of determination is 1.12 μg/m3 ~ 6.76 μg/m3. For details
see Annex A.
2 Normative References
This Standard cites the following documents or clauses therein. For undated reference
documents, their valid editions apply to this Standard.
HJ/T 55, Technical guidelines for fugitive emission monitoring of air pollutants
HJ/T 194, Manual methods for ambient air quality monitoring
3 Method principle
Use sampling tubes packed with coating 2,4-Dinitrophenylhydrazine (DNPH) to collect
a certain volume of air sample. The aldehyde and ketone compounds in sample react
with DNPH coated on silica gel in accordance with Equation (1) through the catalytic
action of strong acid, generating stable, coloured hydrazine derivatives. After the
elution of acetonitrile, use the ultraviolet (360 nm) or diode array detector of high
performance liquid chromatographer for detection. Use the retention time for
Use sealing caps to seal both ends of sampling tubes; use tin foil or aluminum foil to
wrap sampling tubes up for storage and transportation at low temperature (< 4°C). If
analysis can’t be carried out in time, samples shall be stored for not more than 30 days
at low temperature (< 4°C).
7.3 Preparation of samples
Add acetonitrile to elute sampling tubes; let acetonitrile to flow past sampling tubes
naturally with the flow direction opposite to the direction of air flow. Collect the eluent
in a 5 mL volumetric flask before adding acetonitrile to scale; use injection syringe (5.7)
to absorb the eluent; filter through syringe filter (5.8); and transfer to a 2 mL brown
bottle for determination. If the eluent can’t be analyzed in time after filtration, it can be
stored for 30 days at 4°C.
7.4 Preparation of blank samples
7.4.1 Whole-course blanks
Each sampling shall include at least one whole-course blank. bring a sampling tube to
site with its both ends open; continue for a sampling cycle without collecting sample in
it; seal it in the same way as that of sampling tubes with samples; and bring it to
laboratory. Prepare blank samples in accordance with the same procedures of 7.3.
7.4.2 Blank sampling tubes
Take the same batch of sampling tubes in laboratory to prepare blank samples in
accordance with the same procedures of 7.3.
8 Analytical procedures
8.1 Reference chromatographic conditions
Mobile phase. acetonitrile/water. Gradient elution. maintain 60% acetonitrile for 20 min;
increase acetonitrile from 60% linearly to 100% within 20 ~ 30 min; then reduce
acetonitrile to 60% within 30 ~ 32 min; and maintain for 8 min.
Test wavelength. 360 nm.
Flow rate. 1.0 mL/min.
Sample size. 20 μL.
8.2 Calibration
8.2.1 Preparation of standard series
Measure respectively 100 μL, 200 μL, 500 μL, 1 000 μL and 2 000 μL of standard
working solution (5.4) to pour into a 10 mL volumetric flask; use acetonitrile to add to
For the details of the results of precision and accuracy see Annex B.
11 Quality assurance and quality control
11.1 Blank sampling tubes
At least 10% of each batch of sampling tubes shall be taken for blank value testing and
the blank value shall meet the following requirements.
Formaldehyde less than 0.15 μg/tube;
Acetaldehyde less than 0.10 μg/tube;
Acetone less than 0.30 μg/tube;
Other matters less than 0.10 μg/tube.
11.2 Whole-course blanks
Each batch of samples shall include at least one whole-course blank and the
determination result shall be lower than the method detection limit.
11.3 Parallel double sample
Each batch of samples shall include 10% of parallel double sample; when the sample
quantity is less than 10, at least one parallel double sample shall be determined; and
the relative deviation of the results of two parallel determinations shall be less than or
equal to 25%.
11.4 Sampling flow
Observe from time to time whether the flow of sampler is stable during the sampling
period. If the flow at the end of sampling is more than 15% different from the flow at
the beginning of sampling, the samples shall be abandoned, and sampling shall be
done once again.
11.5 Control of breakthrough capacity
The upper limit of aldoketone content in samples taken (in terms of formaldehyde) shall
be less than 75% of the DNPH content of sampling tubes. The breakthrough capacity
of aldoketones can be calculated in accordance with Equation (3).
where,
......
Source: Above contents are excerpted from the PDF -- translated/reviewed by: www.chinesestandard.net / Wayne Zheng et al.
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