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HJ 690-2014: Stationary source emission. Determination of benzene soluble particulate matter. Soxhlet extraction gravimetric method
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Stationary source emission. Determination of benzene soluble particulate matter. Soxhlet extraction gravimetric method
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HJ 690-2014
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Basic data | Standard ID | HJ 690-2014 (HJ690-2014) | | Description (Translated English) | Stationary source emission. Determination of benzene soluble particulate matter. Soxhlet extraction gravimetric method | | Sector / Industry | Environmental Protection Industry Standard | | Classification of Chinese Standard | Z15 | | Word Count Estimation | 10,138 | | Date of Issue | 2/7/2014 | | Date of Implementation | 4/15/2014 | | Quoted Standard | GB 16171 | | Regulation (derived from) | ?Ministry of Environmental Protection Announcement 2014 No. 10 | | Issuing agency(ies) | Ministry of Ecology and Environment | | Summary | This Standard specifies the stationary source emissions of benzene solubles measured Soxhlet - gravimetric method. This Standard applies to the determination of fugitive emissions of benzene soluble particulate matter in oven roof. Determination of other | HJ 690-2014: Stationary source emission. Determination of benzene soluble particulate matter. Soxhlet extraction gravimetric method
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Stationary source emission.Determination of benzene soluble particulate matter.Soxhlet extraction gravimetric method
People's Republic of China National Environmental Protection Standards
Stationary source emission measurement of benzene solubles
Soxhlet Extraction - Gravimetric method
Stationary source emission - Determination of benzene soluble
particulate matter - Soxhlet extraction gravimetric method
(release
draft)
2014-2-7 release
2014-4-15 implementation
Issued by the Ministry of Environmental Protection
Table of Contents
Preface II
1. Scope .1
2 Normative references .1
3 Terms and definitions 1
4 principle of the method .1
5 Reagents and materials 1
6 instruments and equipment 1
Sample 2 7
Analysis Step 8 .2
9 Results Calculation and representation .4
10 precision ..4
11 Quality Assurance and Quality Control 4
12 waste disposal .4
13 Precautions .4
Foreword
To implement the "People's Republic of China Environmental Protection Law" and "People's Republic of China Air Pollution Prevention Law," to protect the environment,
Protection of human health, standardized measurement method fixed source emission of benzene soluble matter, the development of this standard.
This standard specifies the determination of the exhaust gas from stationary sources Soxhlet extraction of benzene-soluble matter - Gravimetric method.
This standard is the first release.
This standard is developed by the Ministry of Environmental Protection Science, Technology organization.
This standard drafting of the main unit. Shanxi Province Environmental Monitoring Center.
The standard verification unit. Taiyuan Environmental Monitoring Center, Environmental Monitoring Station Datong, Linfen City Environmental Monitoring Station, transport
City environmental monitoring, environmental monitoring stations in Jinzhong City, Qingxu County Environmental Monitoring Station
This standard MEP February 7, 2014 for approval.
This standard since April 15, 2014 implementation.
The standard explanation by the Ministry of Environmental Protection.
Stationary source emission measurement of benzene solubles Soxhlet - gravimetric method
Warning. benzene, organic reagents used in the tests is flammable volatile carcinogenic chemicals, operation should be ventilated bar
Good member fume hood. The operator should be required to wear protective equipment requirements to avoid inhalation or contact with skin and clothing,
Guard against fire. Extract must be reasonably safe disposal.
1 Scope
This standard specifies the exhaust gases from stationary sources of benzene soluble matter measured Soxhlet - gravimetric method.
This standard applies to the determination of fugitive particulate matter emissions of benzene-soluble matter in coke oven roof. Other stationary sources of benzene-soluble
The test substance may refer to this standard.
When the sample size is 24m3, the method detection limit of 0.02mg/m3.
2 Normative references
This standard refers to the contents of the following documents or the terms. For undated references, the effective version suitable
For this standard.
GB 16171 coking chemical industry emission standards
3 Terms and definitions
Benzene solubles Benzene-Soluble Particulate Matter
It refers to polycyclic aromatic hydrocarbons and other components of particulate matter that can be extracted with benzene.
4 principle of the method
Under the dynamic action of the pump, a volume of air or gas through the constant weight of glass fiber filters, the particles
Material is retained on the filter. The filters were sampled weighed into a Soxhlet extractor using benzene as solvent extraction, after extraction
Membrane through volatilization after drying to constant weight, according to the previous extraction, and the difference between the weight of the membrane after sampling volume, calculate the benzene solubles
concentration.
5 Reagents and materials
5.1 benzene, AR.
5.2 slow quantitative filter diameter of 90mm, for the analysis of process backdrop protect the sample filters.
5.3 ultra-fine glass fiber filters, diameter 90mm, 0.3μm membrane holdout efficiency of standard particle is not less than 99%. Membrane so that
Before use, do not overlap flat in a muffle furnace burning about 400 ℃ 1h, cooled to 7.3 and 8.1 deal with constant weight (W0) on a smooth
In a clean paper bag and stored in a box back. Filter before sampling can not be bent and folded.
6 instruments and equipment
6.1-volume sampler (with no cover, no hierarchical sampling head). Range 90 ~ 120L/min, flow error ≤5%.
6.2 equilibrium chamber. built-in color gel glass drier placed balance room.
6.3 Analytical balance. verification scale 0.01mg.
6.4 Soxhlet extractor. for extracting a sample on the filter particles soluble in benzene, volume 100ml.
6.5 muffle furnace. Temperature range 250 ℃ ~ 1000 ℃, with a temperature value is displayed.
6.6 temperature water bath. single row, the temperature can be regulated.
6.7 blast oven.
6.8 Membrane storage bags and storage boxes.
7 Sample
7.1 Sample Collection
7.1.1 Sample collection shall be in accordance with the relevant provisions of GB 16171 5.3.3 at the time of normal production status, continuous sampling 4h
In a filter on.
Point 7.1.2 of the sample arrangement, collection frequency should be consistent
GB 16171 of the relevant provisions of 5.3.3. Point a schematic arrangement
Shown in Figure 1, the sample inlet should be 1.5m from the base surface
Above relative height.
7.1.3 before the beginning of the sampling, the filters with tweezers from a paper bag
Remove the "matte side" up sampling head mounted on the recording sampling
Point number, date, time.
7.1.4 Start sampler, the flow rate adjusted 100L/min,
5min after sampling starts, before sampling the middle, end of sampling
5min, each record atmospheric pressure and a flow rate, temperature and
Meteorological parameters.
7.1.5 Traffic frequently observed during sampling, due to the concentration of pollutants
Resulting in high sample flow rate falls more than 5%, in 4 hours
When sampling within the segment, each segment recording sampling time and volume,
Consolidate average concentration.
7.1.6 Sampling finished, close the sampler, sampling record
Room tweezers carefully remove the membrane, so that the stack twice in the dust on face, back into the original bag and stored in a box and returned to the laboratory analysis.
7.1.7 field blank. The filters were prepared to transport 5.3 sample site, the filters were installed in random sampling head, do not smoke
Take air or gas, immediately remove from the sampling head into the original bag, the same processing as the sample filters.
7.2 Sample Storage
Filter after sampling if not promptly returned to the laboratory or timely analysis shall be wrapped with aluminum foil, and stored back into the original bag
In box, sealed conditions at 4 ℃ cold storage, complete extraction within 14d.
7.3 Preparation of the sample
The filters and standard filters after sampling, field blank membrane, laboratory blank filters (from 5.3 spare filter randomly selected
Take) together into balance balance indoor 24h become a sample for analysis.
Analysis Step 8
After sample weighing 8.1
Samples were removed from the balance placed on weighing scales chamber, recording the weight W1 and balance room temperature and humidity. Balance room temperature
Should be maintained at between 18 ~ 35 ℃, relative humidity should be less than 50%. Under the same conditions of equilibrium, balance again one hour after weighing,
1 oven roof schematic arrangement of sampling points
Detecting apertures
Coal loading hole
Sampling point
Dust removal device
Movement route
Oven roof
Sampling point
The weight difference between the two should be less than 0.25mg.
8.2 Extraction of samples
(1) filters after weighing in accordance with the method shown in Figure 2 folded carefully into a clean, dry Soxhlet extractor extraction tube
(Do not block the filter and return pipe below the siphon). To avoid the extraction of particles leak into the extracting agent, and particulate matter and Crafts
To take more effective contact agents, should be placed in the membrane by the method shown in FIG slow quantitative filter paper is folded, placed in a Soxhlet extractor with
The extraction cartridge extraction. To avoid breakage when extracting the central membrane or filter paper, each folded, Do not crease
Near centralized point of creases pressure.
Folded filter paper method shown in Figure 2. First semi-folded filter paper and then folded into a quarter circle, expand FIG. 2- (a).
Then fold in 1 to 4 out of 4 folding 5,3 6,1 7,3 to 6 fold out of 5 out of 8 fold, as shown in Figure 2- (b); and 3 to 6 fold out of 5 9,1 fold
Out of 10, as 2- (c), and then 10, 10 and 1 and 5,5 and 7,9 and 3 each folded back, as shown in Figure 2- (d). The paper hit
Open in the direction of 1 and 3 of a small stack of folded inward surface, and finally made as shown 2- (e) of the folded filter paper.
(2) the upper and lower part of the extraction tube connected with the condenser and receiving flask, placed in a constant temperature water bath, turn on cooling water,
Added 60mL benzene at 95 ℃ water bath (not seen in the water requirement is appropriate to accept the bottle), heated to reflux, full flow from the first opening
Start time, extraction 4h (FIG. 3).
(3) stopping heating, cooling, remove the membrane and slow quantitative filter paper, the filters were placed on clean filter paper, natural evaporation
1h after blast into the oven, and then benzene at 85 ℃ volatile 2h, into the balance chamber.
8.3 Extraction Weigh
Membrane after extraction equilibrium under the same conditions as before the balance chamber and extraction 24h, removed placed on the weighing scales, weighing to meet
Constant weight requirements, record the weight W2 and balance room temperature and humidity.
Figure 2 folded filter paper method
9 Results Calculation and representation
Benzene soluble concentration is calculated as follows.
C (mg/m3) = 106 × (W1-W2)/V0.
Where.
C-- benzene soluble concentration, mg/m3;
After W1-- sampling filter weight, g;
After W2-- extraction membrane weight, g;
V0 - standard conditions (101.325kPa,
Sampling volume 273K) under, L;
Vt - sample volume, L;
P - sampling of atmospheric pressure, Pa;
t - the average temperature during sampling, ℃.
After calculating the results of decimal places and methods
The detection limit of alignment.
10 Precision
Seven laboratories solubles content of benzene in 42 0.00036g ~ 0.01019g actual samples were compared to measured real
Mortem indoor relative standard deviation of 0.46% to 13%; of benzene solubles content in 0.00126g ~ 0.01286g actual sample of 24
Products were compared to the measured laboratory relative standard deviation of 3.3% to 20%.
11 Quality Assurance and Quality Control
11.1 Each filter shall be carefully examined before use in the presence of a pinhole light, fractured, uneven, particulate matter or other defects.
11.2 Sampling should keep accurate and constant sample flow. Sampler before each use need to be calibrated flow, flow diagram
Calibration error value should be less than 5%.
11.3 should be used before and after sampling the same weighing scales membrane; membrane weighing before and after extraction, and operating environment as consistent as possible,
To reduce weighing errors.
11.4 Always check the extraction process reflux, reflux of not less than 8 times per hour.
11.5 each batch of samples at least 1 site and 1 blank blank measurement laboratory, blank samples before and after the on-site laboratory blank
He said difference before and after the extraction of value shall be within ± 0.5mg range.
12 waste disposal
Waste produced after filtration extract centralized collection, commissioned by qualified unit for disposal.
13 Notes
After taking filters 13.1 Sampling should pay particular attention to whether the membrane debris left in the sample folder, shall remain in the sample folder inside the membrane to take cuttings
Out, together with the collection.
P × 273
101.325 × (273 t) V0 = Vt ×
Figure 3 Soxhlet extraction means extracts a benzene soluble matter
Benzene solubles
Matter and benzene
filter paper
Condensate
Condenser
Extraction tube
Receiving flask
siphon
13.2 sample filter is weighed in the manner shown in Figure 2. After folding, folded in the same manner as the slow quantitative filter paper,
With long tweezers to grab the entire external filter paper into (or remove) Soxhlet extraction tube to prevent membrane damage, particulate matter and leakage
Causing analytical error.
13.3 hundred thousandth before weighing in the balance for at least 60 minutes of warm-up time to obtain a stable working condition, to ensure that said
The amount of accuracy of the results.
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