HJ 690-2014Stationary source emission. Determination of benzene soluble particulate matter. Soxhlet extraction gravimetric method (English PDF)

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 °C 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 °C ~ 1000 °C, 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

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, °C.

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; weighing before and after extraction, and operating environment as consistent as possible, to reduce weighing errors.

11.4 Always check the extraction process 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.