Title 40

Appendix E to Subpart A of Part 82 - Article 5 Parties

40:21.0.1.1.1.1.1.24.5 : Appendix E

Appendix E to Subpart A of Part 82 - Article 5 Parties

Parties operating under Article 5 of the Montreal Protocol as of March 26, 2014 are listed below. An updated list can be located at: http://ozone.unep.org/new_site/en/parties_under_article5_para1.php.

Afghanistan, Albania, Algeria, Angola, Antigua & Barbuda, Argentina, Armenia, Bahamas, Bahrain, Bangladesh, Barbados, Belize, Benin, Bhutan, Bolivia (Plurinational State of), Bosnia and Herzegovina, Botswana, Brazil, Brunei Darussalam, Burkina Faso, Burundi, Cambodia, Cameroon, Cape Verde, Central African Republic, Chad, Chile, China, Colombia, Comoros, Congo, Congo (Democratic Republic of), Cook Islands, Cost Rica, Côte d'Ivoire, Cuba, Djibouti, Dominica, Dominican Republic, Ecuador, Egypt, El Salvador, Equatorial Guinea, Eritrea, Ethiopia, Fiji, Gabon, Gambia, Georgia, Ghana, Grenada, Guatemala, Guinea, Guinea Bissau, Guyana, Haiti, Honduras, India, Indonesia, Iran (Islamic Republic of), Iraq, Jamaica, Jordan, Kenya, Kiribati, Korea (Democratic People's Republic of), Korea (Republic of), Kuwait, Kyrgyzstan, Lao (People's Democratic Republic), Lebanon, Lesotho, Liberia, Libya, Madagascar, Malawi, Malaysia, Maldives, Mali, Marshall Islands Mauritania, Mauritius, Mexico, Micronesia (Federal States of), Moldova (Republic of), Mongolia, Montenegro, Morocco, Mozambique, Myanmar, Namibia, Nauru, Nepal, Nicaragua, Niger, Nigeria, Niue, Oman, Pakistan, Palau, Panama, Papua New Guinea, Paraguay, Peru, Philippines, Qatar, Rwanda, Saint Kitts and Nevis, Saint Lucia, Saint Vincent & the Grenadines, Samoa, Sao Tome and Principe, Saudi Arabia, Senegal, Serbia, Seychelles, Sierra Leone, Singapore, Solomon Islands, Somalia, South Africa, South Sudan*, Sri Lanka, Sudan, Suriname, Swaziland, Syrian Arab Republic, Tanzania (United Republic of), Thailand, The Former Yugoslav Republic of Macedonia, Timor-Leste, Togo, Tonga, Trinidad and Tobago, Tunisia, Turkey, Turkmenistan, Tuvalu, Uganda, United Arab Emirates, Uruguay, Vanuatu, Venezuela (Bolivarian Republic of), Viet Nam, Yemen, Zambia, Zimbabwe.

* temporarily categorized as Article 5 pending submission of ODS consumption data [79 FR 16687, Mar. 26, 2014]

Appendix E to Subpart B of Part 82 - The Standard for Automotive Refrigerant Recycling Equipment Intended for Use With Both CFC-12 and HFC-134a

40:21.0.1.1.1.2.1.8.17 : Appendix E

Appendix E to Subpart B of Part 82 - The Standard for Automotive Refrigerant Recycling Equipment Intended for Use With Both CFC-12 and HFC-134a

SAE J2211, Recommended Service Procedure for the Containment of HFC-134a, as set forth under Appendix C of this subpart, and SAE J1989, Recommended Service Procedure for the Containment of CFC-12, as set forth under Appendix A of this subpart, also apply to this Appendix E of this subpart.

SAE J1770, issued December, 1995.

Automotive Refrigerant Recycle Equipment Intended for Use With Both CFC-12 and HFC-134a Foreword

The purpose of this standard is to establish specific minimum equipment requirements for automotive refrigerant recycling equipment intended for use with both CFC-12 and HFC-134a in a common refrigerant circuit. Establishing such specifications will assure that this equipment does not cross contaminate refrigerant above specified limits when used under normal operating conditions.

1. Scope

The purpose of this standard is to establish the specific minimum equipment intended for use with both CFC-12 and HFC-134a in a common refrigerant circuit that has been directly removed from, and is intended for reuse in, mobile air-conditioning (A/C) systems. This standard does not apply to equipment used for CFC-12 and HFC-134a having a common enclosure with separate circuits for each refrigerant.

2. References

2.1 Applicable Documents - The following publications form a part of this specification to the extent specified. The latest issue of SAE publications shall apply.

2.1.1 SAE Publications - Available from SAE, 400 Commonwealth Drive, Warrendale, PA 15096-0001.

SAE J2099 - Standard of Purity for Recycled HFC-134a for Use in Mobile Air-Conditioning Systems SAE 1991 - Standard of Purity for Use in Mobile Air-Conditioning Systems SAE J2196 - Service Hoses for Automotive Air-Conditioning SAE J2197 - Service Hose Fittings for Automotive Air-Conditioning SAE J2210 - HFC-134a (R-134a) Recycling Equipment for Mobile A/C Systems SAE J1990 - Extraction and Recycling Equipment for Mobile A/C Systems

2.1.2 Compressed Gas Association (CGA) Publications - Available from CGA, 1235 Jefferson Davis Highway, Arlington, VA 22202.

CGA Pamphlet S-1.1 - Pressure Relief Device Standard

Part 1 - Cylinders for Compressed Gases

2.1.3 DOT Publications - Available from the Superintendent of Documents, U.S. Government Printing Office, Washington, D.C. 20402

2.1.4 UL Publications - Available from Underwriters Laboratories, 333 Pfingsten Road, Northbrook, IL 60062-2096.

UL 1769 - Cylinder Valves UL 1963 - Refrigerant Recovery/Recycling Equipment 3. Specification and General Description

3.1 The equipment shall be suitable for use in an automotive service garage environment and be capable of continuous operation in ambients from 10 to 49 °C.

3.2 The equipment must be certified that it meets this specification by Underwriters Laboratories Inc. (UL), or by an equivalent Nationally Recognized Testing Laboratory (NRTL).

3.3 The equipment shall have a label which states “Design Certified by (Certifying Agent) to meet SAE J1770 for recycling CFC-12 and HFC-134a using common refrigerant circuits”, in bold-type letters a minimum of 3 mm in height.

4. Equipment Requirements

4.1 General

4.1.1 The equipment shall be capable of preventing cross contamination to the level required by Section 9.2.1.G before an operation involving a different refrigerant can begin. The equipment must prevent initiation of the recovery operation if the equipment is not set up properly.

4.1.2 If an operator action is required to clear the unit prior to reconnecting for a different refrigerant, the equipment shall be provided with a means which indicates which refrigerant was last processed.

4.1.3 Means shall be provided to prevent recovery from both an CFC-12 and HFC-134a mobile air conditioning system concurrently.

4.1.4 Transfer of recycled refrigerant - Recycled refrigerant for recharging and transfer shall be taken from the liquid phase only.

4.2 Seat Leakage Test

4.2.1 Valves, including electrically operated solenoid valves, that are used to isolate CFC-12 and HFC-134a refrigerant circuits, shall have a seat leakage rate not exceeding 15 g/yr ( 1/2 oz/yr) before and after 100,000 cycles of operation. This Endurance Test shall be conducted with HFC-134a at maximum operating pressure as determined by sections 8.1 and 8.2. The Seat Leakage Test shall be performed at 1.5 times this pressure at an ambient of 24 °C.

4.3 Interlocks

4.3.1 Electrical interlock devices used to prevent cross contamination of refrigerant shall be operated for 100,000 cycles and there shall be no failure that would permit cross contamination of refrigerant. Solid state inter lock devices shall comply with the Transient Overvoltage Test and the Fast Transient (Electric Noise) Test contained in the Standard for Tests for Safety Related Controls Employing Solid-State Devices, UL 991.

4.4 Noncondensable Gases

4.4.1 The equipment shall either automatically purge noncondensables (NCGs) if the acceptable level is exceeded or incorporate a device that indicates to the operator the NCG level has been exceeded. A pressure gauge used to indicate an NCG level shall be readable in 1 psig increments. NCG removal must be part of the normal operation of the equipment and instructions must be provided to enable the task to be accomplished within 30 minutes.

4.4.2 Refrigerant loss from noncondensable gas purging, oil removal, and refrigerant clearing shall not exceed more than 5 percent by weight of the total amount of refrigerant through the equipment as detailed in Sections 8.1, 8.2, and 9.2.

4.5 Filter

4.5.1 A 15 micron filter, or other equivalent means, to remove particulates of 15 micrometers spherical diameter or greater shall be located before any manual electrically operated valves that may cause cross contamination.

4.6 Moisture and Acid

4.6.1 The equipment shall incorporate a desiccant package that must be replaced before saturated with moisture, and whose acid capacity is at least 5% by weight of the dry desiccant.

4.6.2 The equipment shall be provided with a moisture detection means that will reliably indicate when moisture in the HFC-134a exceeds 50 ppm, or in the CFC-12 exceeds 15 ppm, and requires the filter/drier replacement.

5. Operating Instructions

5.1 The equipment manufacturer must provide operating instructions, including proper attainment of vehicle system vacuum (i.e., when to stop the extraction process, and also to stop the extraction process if it is noticed that the A/C system being serviced has a leak), filter/desiccant replacement, and purging of noncondensable gases (air). The instructions shall indicate that the correct sequence of operation be followed so that the equipment can properly remove contaminates to the acceptable level. Also to be included are any other necessary maintenance procedures, source information for replacement parts and repair, and safety precautions.

5.2 The equipment must prominently display the manufacturer's name, address, the type of refrigerant (CFC-12 and HFC-134a), a service telephone number, and the part number for the replacement filter/drier. Operation manuals must cover information for complete maintenance of the equipment to assure proper operation.

6. Safety Requirements

6.1 The equipment must comply with applicable federal, state, and local requirements on equipment related to handling CFC-12 and HFC-134a material. Safety precautions or notices related to the safe operation of the equipment shall be prominently displayed on the equipment and should also state “CAUTION - SHOULD BE OPERATED BY QUALIFIED PERSONNEL”.

6.2 HFC-134a has been shown to be nonflammable at ambient temperature and atmospheric pressure. The following statement shall be in the operating manual: “Caution: HFC-134a service equipment or vehicle A/C systems should not be pressure tested or leak tested with compressed air. Some mixtures of air and HFC-134a have been shown to be combustible at elevated pressures (when contained in a pipe or tank). These mixtures may be potentially dangerous, causing injury or property damage. Additional health and safety information may be obtained from refrigerant and lubricant manufacturers.”

7. Functional Description

7.1 General

7.1.1 The equipment must be capable of ensuring recovery of the CFC-12 and HFC-134a from the system being serviced, by reducing the system to a minimum of 102 mm of mercury below atmospheric pressure (i.e., vacuum).

7.1.2 The equipment must be compatible with leak detection material that may be present in the mobile A/C system.

7.2 Shut Off Device

7.2.1 To prevent overcharge, the equipment must be equipped to protect the tank used to store the recycled refrigerant with a shutoff device and a mechanical pressure relief valve.

7.3 Storage Tanks

7.3.1 Portable refillable tanks or containers shall be supplied with this equipment and must be labeled “HFC-134a” or “CFC-12” as appropriate, meet applicable Department of Transportation (DOT) or NRTL's Standards and be adaptable to existing refrigerant service and charging equipment.

7.3.2 The cylinder valve shall comply with the Standard for Cylinder Valves, UL 1769.

7.3.3 The pressure relief device shall comply with the Pressure Relief Device Standard Part 1 - Cylinders for Compressed Gases, CGA Pamphlet S-1.1.

7.3.4 The tank assembly shall be marked to indicate the first retest date, which shall be 5 years after the date of manufacture. The marking shall indicate that retest must be performed every subsequent 5 years. The marking shall be in letters at least 6 mm high.

7.4 Overfill Protection

7.4.1 During operation, the equipment must provide overfill protection to assure that during filling or transfer, the tank or storage container cannot exceed 80% of volume at 21.1 °C of its maximum rating as defined by DOT standards, 49 CFR 173.304 and American Society of Mechanical Engineers.

7.5 Hoses and Connections

7.5.1 Separate inlet and outlet hoses with fittings and separate connections shall be provided for each refrigerant circuit.

7.5.2 All flexible hoses and fittings must meet SAE J2196 (for CFC-12) and SAE J2197 (for HFC-134a).

7.5.3 Service hoses must have shutoff devices located within 30 cm of the connection point to the system being serviced.

7.6 Lubricant Separation

7.6.1 The equipment must be able to separate the lubricant from the removed refrigerant and accurately indicate the amount of lubricant removed during the process, in 30 mL (1 fl oz) units. Refrigerant dissolves in lubricant and, as a result, increases the volume of the recovered lubricant sample. This creates the illusion that more lubricant has been recovered that actually has been. The equipment lubricant measuring system must take into account such dissolved refrigerant removed from the A/C system being serviced to prevent overcharging the vehicle system with lubricant.

(Note:

Use only new lubricant to replace the amount removed the recycling process. Used lubricant should be discarded per applicable federal, state and local requirements.)

7.6.2 The equipment must be provided with some means, such as a lockout device, which will prevent initiation of the recovery operation after switching to the other refrigerant, if the lubricant has not been drained from the oil separator.

8. Testing

8.0 Equipment shall be tested in sequence as noted in sections 8.1, 8.2 and 9.2. The filter/drier may be replaced only as noted by section 4.6.2.

8.1 CFC-12 Recycling Cycle

8.1.1 The maximum operating pressure of the equipment shall be determined when recycling CFC-12 while conducting the following tests. This pressure is needed for the Seat Leakage Test, Section 4.2.

8.1.2 The equipment must be preconditioned with 13.6 kg of the standard contaminated CFC-12 (see section 8.1.2a) at an ambient of 21 °C before starting the test cycle. Sample amounts shall be 1.13 kg with sample amounts to be repeated every 5 minutes. The sample method fixture, defined in Figure 1 to Appendix A, shall be operated at 21 °C.

8.1.2a Standard contaminated CFC-12 refrigerant shall consist of liquid CFC-12 with 100 ppm (by weight) moisture at 21 °C and 45,000 ppm (by weight) mineral oil 525 suspension viscosity nominal and 770 ppm by weight of noncondensable gases (air).

8.1.3 The high moisture contaminated sample shall consist of CFC-12 vapor with 1000 ppm (by weight) moisture.

8.1.4 The high oil contaminated sample shall consist of CFC-12 with 200,000 ppm (by weight) mineral oil 525 suspension viscosity nominal.

8.1.5 After preconditioning as stated in section 8.1.2, the test cycle is started, processing the following contaminated samples through the equipment.

A. 13.6 kg (1.13 kg per batch) of standard contaminated CFC-12. B. 1 kg of high oil contaminated CFC-12. C. 4.5 kg (1.13 kg per batch) of standard contaminated CFC-12. D. 1 kg of high moisture contaminated CFC-12. 8.1.6 The CFC-12 is to be cleaned to the minimum purity level, as defined in SAE J1991, with the equipment operating in a stable ambient of 10, 21, and 49 °C and processing the samples as defined in section 8.1.5.

8.2 HFC-134a Recycling Cycle

8.2.1 The maximum operating pressure of the equipment shall be determined when recycling HFC-134a while conducting the following tests. This pressure is needed for the Seat Leakage Test, Section 4.2.

8.2.2 The equipment must be preconditioned by processing 13.6 kg of the standard contaminated HFC-134a (see section 8.2.2a) at an ambient of 21 °C before starting the test cycle. 1.13 kg samples are to be processed at 5 minute intervals. The text fixture shown in Figure 1 to Appendix A shall be operated at 21 °C.

8.2.2a The standard contaminated refrigerant shall consist of liquid HFC-134a with 1300 ppm (by weight) moisture (equivalent to saturation at 38°[100 °F]), 45,000 ppm (by weight) HFC-134a compatible lubricant, and 1000 ppm (by weight) of noncondensable gases (air).

8.2.2b The HFC-134a compatible lubricant referred to in section 8.2.2a shall be a polyalkylene glycol based synthetic lubricant or equivalent, which shall contain no more than 1000 ppm by weight of moisture.

8.2.3 Following the preconditioning procedure per section 8.2.2, 18.2 kg of standard contaminated HFC-134a are to be processed by the equipment at each stable ambient temperature of 10, 21, and 49 °C.

8.2.4 The HFC-134a is to be cleaned to the purity level, as defined in SAE J2099.

9. Refrigerant Cross Contamination Test

9.1 General

9.1.1 For test validation, the equipment is to be operated according to the manufacturer's instruction.

9.1.2 The equipment shall clean the contaminated CFC-12 refrigerant to the minimum purity level as defined in Appendix A, when tested in accordance with the requirements in section 8.1.

9.1.3 The equipment shall clean the contaminated HFC-134a refrigerant to the purity level defined in Appendix C, when tested in accordance with the requirements in section 8.2.

9.2 Test Cycle

9.2.1 The following method shall be used after the tests and requirements in Sections 8.1 and 8.2, respectively, are completed. Following the manufacturer's instructions, the equipment shall be cleared of HFC-134a, prior to beginning step A. The only refrigerant used for this is noted in steps A, C, and E of section 9.2.1. The test fixture shown in Figure 1 to Appendix A shall be used and the test shall be conducted at 10, 21, and 49 °C ambients.

A. A 1.13 kg standard contaminated sample of CFC-12 (see section 8.1.2a) shall be processed by the equipment. B. Follow manufacturer's instructions to clear the equipment of CFC-12 before processing HFC-134a. C. Process a 1.13 kg, standard contaminated sample of HFC-134a (see section 8.2.2a) through the equipment. D. Follow manufacturer's instructions to clear the equipment of HFC-134a before processing CFC-12. E. Process a 1.13 kg standard contaminated sample of CFC-12 (see section 8.1.2a) through the equipment. F. Follow manufacturer's instructions to clear the equipment of CFC-12. G. The amount of cross contaminated refrigerant, as determined by gas chromatography, in samples processed during steps C and E of section 9.2.1., shall not exceed 0.5 percent by weight. 10. Sample Analysis

10.1 General

10.1.1 The processed contaminated samples shall be analyzed according to the following procedure.

10.2 Quantitative Determination of Moisture

10.2.1 The recycled liquid phase sample of refrigerant shall be analyzed for moisture content via Karl Fischer coulometer titration or an equivalent method. The Karl Fischer apparatus is an instrument for precise determination of small amounts of water dissolved in liquid and/or gas samples.

10.2.2 In conducting the test, a weighed sample of 30 to 130 g is vaporized directly into the Karl Fischer anolyte. A coulometer titration is conducted and the results are calculated and displayed as parts per million moisture (weight).

10.3 Determination of Percent Lubricant

10.3.1 The amount of lubricant in the recycled sample of refrigerant/lubricant is to be determined by gravimetric analysis.

10.3.2 Following venting of noncondensable, in accordance with the manufacturer's operating instructions, the refrigerant container shall be shaken for 5 minutes prior to extracting samples for test.

10.3.3 A weighed sample of 175 to 225 g of liquid refrigerant/lubricant is allowed to evaporate at room temperature. The percent lubricant is to be calculated from the weight of the original sample and the residue remaining after the evaporation.

10.4 Noncondensable Gas

10.4.1 The amount of noncondensable gas is to be determined by gas chromatography. A sample of vaporized refrigerant liquid shall be separated and analyzed by gas chromatography. A Propak Q column at 130 °C and a hot wire detector may be used for analysis.

10.4.2 This test shall be conducted on liquid phase samples of recycled refrigerant taken from a full container as defined in 7.4 within 30 minutes following the proper venting of noncondensable gases.

10.4.3 The samples shall be shaken for at least 15 minutes prior to testing while at a temperature of 24 °C ±2.8 °C.

10.5 Refrigerant Cross Contamination

10.5.1 The amount of cross contamination of CFC-12 in HFC-134a or HFC-134a in CFC-12 shall not exceed 0.5 percent by weight as determined by gas chromatography. A sample of vaporized refrigerant liquid shall be separated and analyzed by gas chromatography. A 1% SP-1000 on Carbopack B (60/80 mesh) column may be used for the analysis.

[62 FR 68053, Dec. 30, 1997]

Appendix E to Subpart F of Part 82 - Test Procedure for Leaks From Containers Holding Two Pounds or Less of Refrigerant for Use in an MVAC

40:21.0.1.1.1.6.1.15.27 : Appendix E

Appendix E to Subpart F of Part 82 - Test Procedure for Leaks From Containers Holding Two Pounds or Less of Refrigerant for Use in an MVAC

This appendix is based on the California Air Resources Board (CARB) standard TP-503: Test Procedure for Leaks from Small Cans of Automotive Refrigerant, as amended on January 5, 2010; and CARB standard BP-A1: Balance Protocol for Gravimetric Determination of Sample Weights using a Precision Balance, as amended January 5, 2010.

Section 1. Applicability

This test procedure is used by manufacturers of containers holding two pounds or less of refrigerant for use in a motor vehicle air conditioner (MVAC) to determine the leakage rate of small containers of automotive refrigerant that are subject to the requirements of 40 CFR part 82, subpart F. Specifically, this test procedure will specify the equipment, procedures, and calculations to determine if a container holding two pounds or less of refrigerant for use in an MVAC complies with the leakage rate specified in § 82.154(c)(2)(ii). All terms in this appendix will follow the definitions in § 82.152 unless otherwise defined in this appendix.

All containers holding two pounds or less of refrigerant for use in an MVAC must comply with other applicable codes and regulations such as local, state, or Federal safety codes and regulations.

This test procedure involves the use of materials under pressure and operations and should only be used by or under the supervision of those familiar and experienced in the use of such materials and operations. Appropriate safety precautions should be observed at all times while performing this test procedure.

Section 2. Principle and Summary of Test Procedure

This procedure is used to determine the leakage rate of containers holding two pounds or less of refrigerant for use in an MVAC (small cans). Testing will involve subjecting both full and partially empty cans in both upright and inverted positions at two temperatures: 73 °F and 130 °F.

Thirty small cans are tested under each condition for a total of 240 small cans tested. Small cans are brought to temperature stability, weighed, then stored for 30 days under specified conditions of temperature, orientation, and state of fill, then re-weighed. Leakage rate (grams/year) is estimated by (weight loss in grams) x 365/(days duration). The leakage rate is then compared to a standard of 3.00 grams/year to determine if a given small can complies with the leakage rate specified in § 82.154(c)(2)(ii).

Section 3. Biases and Interferences

3.1 Contaminants on the operator's hands can affect the weight of the small can and the ability of the small can to absorb moisture. To avoid contamination of the small can, the balance operator should wear gloves while handling the small cans.

3.2 Weight determinations can be interfered with by moisture condensing on the small can and by thermal currents generated by temperature differences between the small can and the room temperature. The small cans cool during discharge and could cause condensation. For these reasons, small cans must be equilibrated to balance room temperature for at least four hours before weighing.

3.3 Variations in the temperature, pressure, and humidity of the ambient air will cause variations in the buoyancy of the small can. These variations should typically be less than 25 mg for a small can. If the small can is not leaking at all, then the uncorrected weight changes will be within the range of 0 ± 25 mg, which is about ten percent of the 247 mg loss expected after thirty days for a can leaking at 3 g/yr. In that case buoyancy corrections can be omitted. If the absolute value of the uncorrected weight change exceeds 25 mg, then all calculations must be made using weights corrected for buoyancy based on the temperature, pressure, and humidity of the weighing room.

3.4 Some electronic balances are sensitive to the effects of small static charges. The small can should be placed directly on the balance pan, ensuring metal to metal contact. If the balance pan is not grounded, the small can and balance pan should be statically discharged before weighing.

Section 4. Sensitivity and Range

The mass of a full small can could range from roughly 50 g to 1000 g depending on the container capacity. A top loading balance, capable of a maximum weight measurement of not less than 1,000 g and having a minimum readability of 0.001 g, reproducibility and linearity of ± 0.002 g, must be used to perform mass measurements.

Section 5. Equipment

5.1 A top loading balance that meets the requirements of Section 4 above.

5.2 A NIST traceable working standard mass for balance calibration. A NIST traceable working standard mass for a balance linearity check. A reference mass to serve as a “blank” small can.

5.3 An enclosure capable of controlling the internal air temperature from 73 °F ± 5 °F, and an enclosure capable of controlling the internal air temperature to 130 °F ± 5 °F.

5.4 A temperature instrument capable of measuring the internal temperature of the temperature conditioning enclosures and the balance room with a sensitivity of ± 2 °F.

5.5 A barometric pressure instrument capable of measuring atmospheric pressure at the location of the balance to within ± 0.02 inches of mercury.

5.6 A relative humidity measuring instrument capable of measuring the relative humidity (RH) at the location of the balance with a sensitivity of ± 2 percent RH.

5.7 A hose with appropriate fitting for dispensing refrigerant from the small can to a recovery machine.

5.8 A refrigerant recovery machine to collect the discharged refrigerant from small cans being tested.

Section 6. Calibration Procedures

6.1 Calibrations are applied to the balance and to the support equipment such as temperature, humidity, and pressure monitoring equipment. Procedures for calibration are not spelled out here. General calibration principals for the support equipment and the balance are described in Section 11, Quality Assurance/Quality Control. Detailed calibration procedures for measurements made using the balance are contained in Attachment A: “Balance Protocol for Gravimetric Determination of Sample Weights using a Precision Balance.”

Section 7. Small Can Preparation

7.1 Receive a batch of 240 small cans of one design to be tested. These may include several SKUs from different manufacturers if the container and valve combination are the same.

7.2 Clean small cans with Alkanox solution or equivalent and dry with a lint free towel.

7.3 Confirm that the sample ID sticker on the small can matches the sample ID on the chain of custody forms.

7.4 Select a reference mass similar to the weight of a full small can. If multiple sets of similar sized small cans are being tested, only one reference mass is needed; it can be used with all sets. Store the reference mass in the balance area.

7.5 Evacuate the contents of one half of the small cans (120 cans) into the refrigerant recovery machine using normal DIY dispensing procedures until each small can is approximately half full.

7.6 Select a reference mass similar to the weight of the half-full small can. If multiple sets of similar size small cans are being tested, only one reference mass is needed; it can be used with all sets. Store the reference mass in the balance area.

Section 8. Small Can Weighing

Weighing cans on the balance is done in accordance with Attachment A to this appendix. Attachment A describes how to conduct weight determinations including appropriate calibration and QC data. This section, “Small Can Weighing,” describes the overall process, not the details of how to use the balance.

Initial Weights

8.1 Put on gloves. Check the small cans for contamination.

8.2 Place the 240 small cans into a location where they can equilibrate to balance room temperature. Record the small can test IDs and the equilibration start time on the Small Can Test Data Forms available on EPA's Web site in sets of thirty, one form for each of the eight test conditions.

8.3 Let cans equilibrate for at least four hours.

8.4 Weigh the set of 240 small cans and the reference weights using Attachment A and log the results to the Balance Weighing Log Form available on EPA's Web site.

8.5 Transfer data from the Balance Weighing Log Form to the Small Can Test Data Form in sets of 30, one set for each of the eight conditions to be tested.

Thirty-Day Soak

8.6 Place each set of 30 small cans into the appropriate orientation and temperature for soaking:

30 full small cans - 73 °F, upright 30 full small cans - 73 °F, inverted 30 full small cans - 130 °F, upright 30 full small cans - 130 °F, inverted 30 half-full small cans - 73 °F, upright 30 half-full small cans - 73 °F, inverted 30 half-full small cans - 130 °F, upright 30 half-full small cans - 130 °F, inverted

8.7 Soak the small cans for 30 days undisturbed.

Final Weighing

8.8 Place the 240 small cans into a location where they can equilibrate to balance room temperature.

8.9 Let the small cans equilibrate for at least four hours.

8.10 Weigh the set of 240 small cans, the reference weights, and any additional sets of small cans using Attachment A.

8.11 Transfer data from the Balance Weighing Log Form to the corresponding Small Can Test Data Forms.

Section 9. Calculations Corrections for Buoyancy

The calculations in this section are described in terms of “weight.” Mass is a property of the small can, whereas weight is a force due to the effects of buoyancy and gravity. Procedures for correcting the effect of buoyancy are given in Attachment B of this appendix. Ignoring buoyancy, i.e., using weight data uncorrected for buoyancy effects, is acceptable for a thirty day test if the absolute magnitude of the weight change is less than 25 mg. If the uncorrected weight change exceeds 25 mg for any small can, then correct all small can weights for buoyancy using the procedures in Attachment B before performing the calculations described below.

Calculation of Leak Rate

The emission rate in grams/day for each small can is calculated by subtracting the final weight from the initial weight and then dividing the weight difference by the time difference measured in days to the nearest hour (nearest 1/24 of a day). The emission rate in g/day is multiplied by 365 to determine emission rate in grams/yr. If the annual emission rate for any small can exceeds the entire small can contents, then the annual emission rate for that small can is adjusted to equal the entire small can contents/year (e.g., about 350 g/yr for a 12 ounce small can). The annual emission rate for the purpose of the test is calculated by averaging the 240 individual adjusted annual emission rates and rounding to two decimal places. The cans fail the test if the adjusted annual emission rate averaged over 240 cans is greater than 3.00 g/yr. The calculations are described below.

Loss rate for each small can

Eidaily = (Wifinal − Wiinitial)/(Difinal − Diinitial) g/day Eiannual = 365 × Eidaily g/year Eiadjusted = Minimum of (Eiadjusted, Ci/year) g/yr Where, Ei = emission rate Wifinal = weight of can i after soaking (grams) Wiinitial = weight of can I before soaking (grams) Difinal = date/time of final weight measurements (days) Diinitial = date/time of initial weight measurements (days) Ci = original factory mass of refrigerant in can i

Note: Date/Times are measured in days. Microsoft Excel stores dates and times in days, and the calculations can be made directly in Excel. If calculations are made manually, calculate serial days to the nearest hour for each date and time as follows:

D = Julday + Hour/24 Where, Julday = serial day of the year: Jan 1 = 1, Jan 31 = 31, Feb 1 = 32, etc. Hour = hour of day using 24-hour clock, 0 to 23

Calculate the average loss rate for the 240 small cans as follows:

Emean = [Sum (Eadjustedi), i = 1 to 240]/240 Section 10. Recordkeeping

During small can weighing, record the small can weights and date/times on the Balance Weighing Log Form. After each weighing session, transfer the measured weights and date/times from the Balance Weighing Log Form to the Small Can Test Data Form.

At the end of the test, complete the calculations described in Section 9, Calculations, and record the results on the Small Can Test Data Form.

Section 11. Quality Assurance/Quality Control

11.1 All temperature, pressure, and humidity instruments should be calibrated annually against NIST traceable laboratory standards. The main purpose of the NIST traceable calibration is to establish the absolute accuracy of the device. The instruments should also be checked periodically such as weekly, monthly, or quarterly against intermediate standards or against independent instruments. For example, a thermocouple can be checked weekly against a wall thermometer. A barometer or pressure gauge can be checked weekly by adjusting to sea level and comparing with local airport data. The main purpose of the frequent checks is to verify that the device has not failed in some way. This is especially important for electronic devices such as a digital thermometer, but even a liquid filled thermometer can develop a problem such as a bubble.

11.2 The balance should be serviced and calibrated annually by an independent balance service company or agency using NIST traceable reference masses. Servicing verifies accuracy and linearity, and the maintenance performed helps ensure that a malfunction does not develop.

11.3 The balance must also be calibrated and its linearity checked with working standards before and after each weighing session, or before and after each group of 24 small cans if more than 24 small cans are weighed in a session. Procedures for calibrating and using the balance, as well as recording balance data, are described in the accompanying balance weighing protocol. These procedures include zero checks, calibration checks, and reference mass checks. Procedures for calculating quality control data from those checks are described in Attachment A.

11.4 The small cans are cleaned then handled using gloves to prevent contamination. All equilibration and soaking must be done in a dust free area.

Section 12. Balance Protocol for Gravimetric Determination of Sample Weights Using a Precision Balance

12.1 Scope and application

This Protocol summarizes a set of procedures and tolerances for weighing objects in the range of 0 to 1,000 g with a resolution of 0.001 g. This protocol only addresses balance operations, it does not address project requirements for equilibration, sample hold time limits, sample collection etc.

12.2 Summary of method

The balance is zeroed and calibrated using procedures defined herein. Object weight determinations are conducted along with control object weight determinations, zero checks, calibration checks, sensitivity checks, and replicate weightings in a defined sequence designed to control and quantitatively characterize precision and accuracy.

12.3 Definitions

N/A.

12.4 Interferences

Object weights can be affected by temperature and relative humidity of their environment, air currents, static electricity, gain and loss of water vapor, gain or loss of and loss of volatile compounds directly from the sample or from contaminants such as finger prints, marker ink, and adhesive tape.

Contamination, transfer of material to or from the samples, is controlled by conducting operations inside a clean area dedicated to the purpose and having a filtered laminar air flow where possible; by wearing gloves while handling all samples and related balance equipment; by using forceps to handle small objects, and by keeping the balance and all related equipment inside the clean area.

Air currents are controlled by conducting weighing operations inside a closed chamber or glove box and by allowing the substrates to reach temperature and relative humidity equilibrium. The chamber is maintained at 40 percent relative humidity and 25 °C by a continuous humidity and temperature control system. The temperature and RH conditions are recorded at least once per weighing sessions. Equilibration times for samples that are particularly sensitive to humidity or to loss of semi-volatiles species are specified by project requirements.

Static electric charges on the walls of the balance and the weighed objects, including samples, controls, and calibration weights, can significantly affect balance readings. Static is avoided by the operator ground himself and test objects as described in the balance manual.

12.5 Personnel health and safety

N/A

12.6 Equipment and supplies

• Filtered, temperature and humidity controlled weighing chamber.

• Precision Balance

• Plastic forceps

• Nylon fabric gloves.

• Working calibration weights: ANSI Class 2, 1000g and 500 g

• Working sensitivity weight: 50 mg

• Reference objects: references are one or more objects that are typical of the objects to be weighed during a project, but that are stored permanently inside the balance glove box. Reference objects are labeled Test1, Test2, Test3, etc.

12.7 Reagents and standard

N/A

12.8 Sample collection, preservation, and storage

N/A. See relevant project requirements and SOPs.

12.9 Quality control

Data quality is controlled by specifying frequencies and tolerances for Zero, Calibration, Linearity, and Sensitivity checks. If checks do not meet tolerance criteria, then samples must be re-weighed. In addition, the procedures specify frequencies for Control Object Checks.

Data quality is quantitatively characterized using Zero Check, Calibration Check, and Control Check data. These data are summarized monthly in statistics and QC charts.

12.10 Calibration and standardization

The absolute accuracy of the balance is established by calibration against an ANSI Class 2, stainless steel working weight: 1000.000 g ± 0.0025 g. Linearity is established checking the midpoint against an ANSI Class 2 stainless steel working weight: 500.000 ± 0.0012 g. Sensitivity is established using and ANSI Class 2 stainless steel or aluminum working weight: 50 mg. Precision is checked by periodically checking zero, calibration, and reference object weights.

12.11 Procedure

12.11.1 Overview of Weighing Sequence

Weighing a series of substrates consists of performing the following procedures in sequence, while observing the procedures for handling and the procedures for reading the balance:

1. Initial Adjustment 2. Weigh eight samples 3. Zero Check 4. Weigh eight samples 5. Zero Check 6. Weigh eight samples 7. Calibration Check 8. Return to step 2. 9. If less than 24 cans are weighed, perform a final Calibration Check at the end of weighing.

This sequence is interrupted and samples are reweighed if QC check tolerances are not met. Each of these procedures along with procedures for handling and reading the balance are described below. The QC tolerances referred to in these procedures are listed in Table 1.

12.11.2 Handling

1. Never touch samples, weights, balance pans, etc. with bare hands. Wear powder free gloves to handle the weights, controls, and samples.

12.11.3 Reading the Balance

1. Close the door. Wait for the balance stabilization light to come on, and note the reading.

2. Watch the balance reading for 30 sec (use a clock). If the reading has not changed by more than 0.001 g from the reading noted in step 1, then record the reading observed at the end of the 30 sec period.

3. If the reading has drifted more than 0.001 g note the new balance reading and go to step 2.

4. If the balance reading is flickering back and forth between two consecutive values choose the value that is displayed more often than the other.

5. If the balance reading is flickering equally back and forth between two consecutive values choose the higher value.

12.11.4 Initial Adjustment

1. Empty the sample pan Close the door. Select Range 1000 g 2. Wait for a stable reading 3. Record the reading with QC code IZC (initial zero check) 4. Press the Tare button 5. Record the reading in the logbook with QC code IZA (initial zero adjust) 6. Place the 1,000 g working calibration weight on the balance pan 7. Wait for a stable reading. 8. Record the reading with QC code ICC (initial cal check) 9. Press the Calibrate button 10. Record the reading with QC code ICA (initial cal adjust) 11. Remove the calibration weight. 12. Wait for a stable reading. 13. Record the reading with QC code IZC. 14. If the zero reading exceeds ± 0.002 g, go to step 4. 15. Place the 500 g calibration weight on the balance pan 16. After a stable reading, record the reading with QC code C500. Do not adjust the balance. 17. Add the 0.050 g weight to 500 g weight on the balance pan. 18. After a stable reading, record the reading with QC code C0.05. Do not adjust the balance. 19. Weigh reference object TEST1, record reading with QC code T1. 20. Weigh the reference object TEST2, TEST3, etc. that is similar in weight to the samples that you will be weighing. Record with QC code T2, T3, etc.

12.11.5 Zero Check

1. Empty the sample pan. Close the door. 2. Wait for a stable reading 3. Record the reading with QC code ZC 4. If the ZC reading is less than or equal to the zero adjustment tolerance shown in Table 1, return to weighing and do not adjust the zero. If the ZC reading exceeded the zero adjustment tolerance, proceed with steps 5 through 7. 5. Press the Tare button 6. Record the reading in the logbook with QC code ZA. 7. If the ZC reading exceeded the zero re-weigh tolerance, change the QC code recorded in step 3 from ZC to FZC. Then enter a QC code of FZ into the QC code column of all samples weights obtained after the last valid zero check. Re- weigh all of those samples, recording new data in new rows of the logbook.

12.11.6 Calibration Check

1. First, follow procedures for Zero Check. If the ZC was within tolerance, tare the balance anyway (i.e., follow steps 5 and 6 of the Zero Check method) 2. Place the 1,000 g working calibration weight on the sample pan, wait for a stable reading. 3. Record the reading with QC code C1000 4. If the C1000 reading is less than or equal to the calibration adjustment tolerances, skip steps 5 through 8 and proceed to step 9. Do not adjust the calibration. 5. If the C100 reading exceeded the calibration adjust tolerance, press the Calibrate button. 6. Record the reading in the logbook with QC code CA 7. Perform a Zero Check (follow the Zero Check method) 8. If the C1000 reading exceeded the calibration re-weigh tolerance, change the code recorded in step 3 from C1000 to FC1000. Enter FC into the QC column for all sample weights obtained after the last valid calibration check. Re-weigh all of those samples, recording new data in new rows of the logbook.

12.11.7 Replicate Weighing Check

1. This protocol does not include reweigh samples to obtain replicates. The projects for which this protocol is intended already include procedures multiple weightings of each sample.