美国环保署 EPA Method 15A-炼油厂硫回收装置总减少硫排放量的测定 2017

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Method 15A 8/3/2017

While we have taken steps to ensure the accuracy of this Internet version of the document, it is not the

official version. To see a complete version including any recent edits, visit:

https://www.ecfr.gov/cgi-bin/ECFR?page=browse and search under Title 40, Protection of

Environment.

Method 15A - Determination of Total Reduced Sulfur Emissions From Sulfur Recovery Plants in

Petroleum Refineries

Note: This method does not include all of the specifications (e.g., equipment and supplies) and procedures

(e.g., sampling and analytical) essential to its performance. Some material is incorporated by reference

from other methods in this part. Therefore, to obtain reliable results, persons using this method should

have a thorough knowledge of at least the following additional test methods: Method 1, Method 6,

Method 15, and Method 16A.

1.0 Scope and Application

1.1 Analytes.

Analyte

CAS No.

Sensitivity

Reduced sulfur compounds

None assigned

Not determined.

1.2 Applicability. This method is applicable for the determination of emissions of reduced sulfur

compounds from sulfur recovery plants where the emissions are in a reducing atmosphere, such as in

Stretford units.

1.3 Data Quality Objectives. Adherence to the requirements of this method will enhance the quality of

the data obtained from air pollutant sampling methods.

2.0 Summary of Method

2.1 An integrated gas sample is extracted from the stack, and combustion air is added to the oxygen (O2)-

deficient gas at a known rate. The reduced sulfur compounds [including carbon disulfide (CS2), carbonyl

sulfide (COS), and hydrogen sulfide (H2S)] are thermally oxidized to sulfur dioxide (SO2), which is then

collected in hydrogen peroxide as sulfate ion and analyzed according to the Method 6 barium-thorin

titration procedure.

3.0 Definitions[Reserved]

4.0 Interferences

4.1 Reduced sulfur compounds, other than CS2, COS, and H2S, that are present in the emissions will also

be oxidized to SO2, causing a positive bias relative to emission standards that limit only the three

compounds listed above. For example, thiophene has been identified in emissions from a Stretford unit

and produced a positive bias of 30 percent in the Method 15A result. However, these biases may not

affect the outcome of the test at units where emissions are low relative to the standard.

Method 15A 8/3/2017

4.2 Calcium and aluminum have been shown to interfere in the Method 6 titration procedure. Since these

metals have been identified in particulate matter emissions from Stretford units, a Teflon filter is required

to minimize this interference.

4.3 Dilution of the hydrogen peroxide (H2O2) absorbing solution can potentially reduce collection

efficiency, causing a negative bias. When used to sample emissions containing 7 percent moisture or less,

the midget impingers have sufficient volume to contain the condensate collected during sampling.

Dilution of the H2O2 does not affect the collection of SO2. At higher moisture contents, the potassium

citrate-citric acid buffer system used with Method 16A should be used to collect the condensate.

5.0 Safety

5.1 Disclaimer. This method may involve hazardous materials, operations, and equipment. This test

method may not address all of the safety problems associated with its use. It is the responsibility of the

user of this test method to establish appropriate safety and health practices and determine the applicability

of regulatory limitations prior to performing this test method.

5.2 Corrosive reagents. The following reagents are hazardous. Personal protective equipment and safe

procedures are useful in preventing chemical splashes. If contact occurs, immediately flush with copious

amounts of water for at least 15 minutes. Remove clothing under shower and decontaminate. Treat

residual chemical burns as thermal burns.

5.2.1 Hydrogen Peroxide (H2O2). Irritating to eyes, skin, nose, and lungs.

5.2.2 Sodium Hydroxide (NaOH). Causes severe damage to eyes and skin. Inhalation causes irritation to

nose, throat, and lungs. Reacts exothermically with limited amounts of water.

5.2.3 Sulfuric Acid (H2SO4). Rapidly destructive to body tissue. Will cause third degree burns. Eye

damage may result in blindness. Inhalation may be fatal from spasm of the larynx, usually within 30

minutes. May cause lung tissue damage with edema. 3 mg/m3 will cause lung damage in uninitiated. 1

mg/m3 for 8 hours will cause lung damage or, in higher concentrations, death. Provide ventilation to limit

inhalation. Reacts violently with metals and organics.

6.0 Equipment and Supplies

6.1 Sample Collection. The sampling train used in performing this method is shown in Figure 15A–1,

and component parts are discussed below. Modifications to this sampling train are acceptable provided

that the system performance check is met.

6.1.1 Probe. 6.4-mm (1/4-in.) OD Teflon tubing sequentially wrapped with heat-resistant fiber strips, a

rubberized heating tape (with a plug at one end), and heat-resistant adhesive tape. A flexible

thermocouple or some other suitable temperature-measuring device shall be placed between the Teflon

tubing and the fiber strips so that the temperature can be monitored. The probe should be sheathed in

stainless steel to provide in-stack rigidity. A series of bored-out stainless steel fittings placed at the front

of the sheath will prevent flue gas from entering between the probe and sheath. The sampling probe is

depicted in Figure 15A–2.

6.1.2 Particulate Filter. A 50-mm Teflon filter holder and a 1- to 2-mm porosity Teflon filter (available

through Savillex Corporation, 5325 Highway 101, Minnetonka, Minnesota 55345). The filter holder must

be maintained in a hot box at a temperature high enough to prevent condensation.

Method 15A 8/3/2017

6.1.3 Combustion Air Delivery System. As shown in the schematic diagram in Figure 15A–3. The rate

meter should be selected to measure an air flow rate of 0.5 liter/min (0.02 ft3/min).

6.1.4 Combustion Tube. Quartz glass tubing with an expanded combustion chamber 2.54 cm (1 in.) in

diameter and at least 30.5 cm (12 in.) long. The tube ends should have an outside diameter of 0.6 cm

(1/4in.) and be at least 15.3 cm (6 in.) long. This length is necessary to maintain the quartz-glass

connector near ambient temperature and thereby avoid leaks. Alternatively, the outlet may be constructed

with a 90 degree glass elbow and socket that would fit directly onto the inlet of the first peroxide

impinger.

6.1.5 Furnace. Of sufficient size to enclose the combustion tube. The furnace must have a temperature

regulator capable of maintaining the temperature at 1100 ±50°C (2,012 ±90°F). The furnace operating

temperature must be checked with a thermocouple to ensure accuracy. Lindberg furnaces have been found

to be satisfactory.

6.1.6 Peroxide Impingers, Stopcock Grease, Temperature Sensor, Drying Tube, Valve, Pump, and

Barometer. Same as in Method 6, Sections 6.1.1.2, 6.1.1.4, 6.1.1.5, 6.1.1.6, 6.1.1.7, 6.1.1.8, and 6.1.2,

respectively, except that the midget bubbler of Method 6, Section 6.1.1.2 is not required.

6.1.7 Vacuum Gauge and Rate Meter. At least 760 mm Hg (30 in. Hg) gauge and rotameter, or

equivalent, capable of measuring flow rate to ±5 percent of the selected flow rate and calibrated as in

Section 10.2.

6.1.8 Volume Meter. Dry gas meter capable of measuring the sample volume under the particular

sampling conditions with an accuracy of 2 percent.

6.1.9 U-tube manometer. To measure the pressure at the exit of the combustion gas dry gas meter.

6.2 Sample Recovery and Analysis. Same as Method 6, Sections 6.2 and 6.3, except a 10-ml buret with

0.05-ml graduations is required for titrant volumes of less than 10.0 ml, and the spectrophotometer is not

needed.

7.0 Reagents and Standards

Note: Unless otherwise indicated, all reagents must conform to the specifications established by the

Committee on Analytical Reagents of the American Chemical Society. When such specifications are not

available, the best available grade shall be used.

7.1 Sample Collection. The following reagents and standards are required for sample analysis:

7.1.1 Water. Same as Method 6, Section 7.1.1.

7.1.2 Hydrogen Peroxide (H2O2), 3 Percent by Volume. Same as Method 6, Section 7.1.3 (40 ml is

needed per sample).

7.1.3 Recovery Check Gas. Carbonyl sulfide in nitrogen [100 parts per million by volume (ppmv) or

greater, if necessary] in an aluminum cylinder. Concentration certified by the manufacturer with an

accuracy of ±2 percent or better, or verified by gas chromatography where the instrument is calibrated

with a COS permeation tube.

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标签： #测定

摘要：

美国环保署 EPA Method 15A 2017 是针对炼油厂硫回收装置总减少硫排放量测定的标准方法，适用于硫回收装置硫排放控制效果评估、总硫减排量测定、监测与合规性验证。该规范涵盖采样、分析、计算及质量控制要求，可帮助炼油企业准确掌握硫回收效率，满足 EPA 排放法规和环保监管要求。通过正确实施 EPA Method 15A，可提升硫排放数据可靠性与可比性，支持炼油厂硫回收装置优化运行、减排管理和环境合规审查。

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美国环保署 EPA Method 15A-炼油厂硫回收装置总减少硫排放量的测定 2017

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