§63.626. Performance tests and compliance provisions. — Inbound Citations

(B) As an alternative to paragraph (d)(1)(ii)(A) of this section, you may establish allowable ranges for the daily averages of the pressure drop across an absorber for the purpose of assuring compliance with this subpart using the procedures described in this paragraph. You must establish the allowable ranges based on the baseline average values recorded during previous performance tests or the results of performance tests conducted specifically for the purposes of this paragraph. You must conduct all performance tests using the methods specified in § 63.626. You must certify that the control devices and processes have not been modified since the date of the performance test from which you obtained the data used to establish the allowable ranges. When a source using the methodology of this paragraph is retested, you must determine new allowable ranges of baseline average values unless the retest indicates no change in the operating parameters outside the previously established ranges.

Any affected source subject to the provisions of this subpart is exempted from any otherwise applicable new source performance standard contained in 40 CFR part 60, subpart V, subpart W, or subpart X. To be exempt, a source must have a current operating permit pursuant to title V of the Clean Air Act and the source must be in compliance with all requirements of this subpart. For each affected source, this exemption is upon the date that you demonstrate to the Administrator that the requirements of §§ 63.625 and 63.626 have been met.

(i) 1 Preparation of Sample, IBR approved for § 63.606(f), § 63.626(f).

(f) For each phosphate fertilizer process line (e.g., diammonium and/or monoammonium phosphate process line), and granular triple superphosphate process line, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (f)(1) through (3) of this section.

(2) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13 A, may be omitted.

(i) Determine the mass flow rate (Mp) of the phosphorus-bearing feed using the measurement system described in § 63.625(a).

(ii) Determine the P2O5 content (Rp) of the feed using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(A) 1 Preparation of Sample.

(B) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method A—Volumetric Method.

(C) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method B—Gravimetric Quimociac Method.

(D) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method C—Spectrophotometric Method.

(E) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(F) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(G) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method.

(f) For each phosphate fertilizer process line (e.g., diammonium and/or monoammonium phosphate process line), and granular triple superphosphate process line, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (f)(1) through (3) of this section.

(2) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13 A, may be omitted.

(i) Determine the mass flow rate (Mp) of the phosphorus-bearing feed using the measurement system described in § 63.625(a).

(ii) Determine the P2O5 content (Rp) of the feed using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(A) 1 Preparation of Sample.

(B) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method A—Volumetric Method.

(C) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method B—Gravimetric Quimociac Method.

(D) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method C—Spectrophotometric Method.

(E) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(F) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(G) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method.

(2) Calculate the equivalent P2O5 feed by determining the total mass rate in metric ton/hour of phosphorus bearing feed using the procedures specified in § 63.626(f)(3).

(f) For each phosphate fertilizer process line (e.g., diammonium and/or monoammonium phosphate process line), and granular triple superphosphate process line, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (f)(1) through (3) of this section.

(2) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13 A, may be omitted.

(i) Determine the mass flow rate (Mp) of the phosphorus-bearing feed using the measurement system described in § 63.625(a).

(ii) Determine the P2O5 content (Rp) of the feed using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(A) 1 Preparation of Sample.

(B) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method A—Volumetric Method.

(C) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method B—Gravimetric Quimociac Method.

(D) 3 Phosphorus-P2O5 or Ca3(PO4)2, Method C—Spectrophotometric Method.

(E) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(F) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(G) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method.

(1) Maintain a daily record of total equivalent P2O5 stored by multiplying the percentage P2O5 content, as determined by § 63.626(f)(3)(ii), by the total mass of granular triple superphosphate stored as specified in paragraph (b) of this section.

(v) Section XI, Methods of Analysis for Phosphoric Acid, Superphosphate, Triple Superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method, IBR approved for § 63.606(f), § 63.626(f), and (g).

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.

(g) For each granular triple superphosphate storage building, you must determine compliance with the applicable total fluorides standards specified in Tables 1 and 2 to this subpart as specified in paragraphs (g)(1) through (7) of this section.

(1) You must conduct performance tests only when the following quantities of product are being cured or stored in the facility:

(i) Total granular triple superphosphate is at least 10 percent of the building capacity, and

(ii) Fresh granular triple superphosphate is at least six percent of the total amount of granular triple superphosphate, or

(iii) If the provision in paragraph (g)(1)(ii) of this section exceeds production capabilities for fresh granular triple superphosphate, the fresh granular triple superphosphate is equal to at least 5 days maximum production.

(3) You must use Method 13A or 13B (40 CFR part 60, appendix A) to determine the total fluorides concentration (Ci) and the volumetric flow rate (Qi) of the effluent gas at each emission point. The sampling time for each run at each emission point must be at least 60 minutes. The sampling volume for each run at each emission point must be at least 0.85 dscm (30 dscf). If Method 13B is used, the fusion of the filtered material described in Section 7.3.1.2 and the distillation of suitable aliquots of containers 1 and 2, described in section 7.3.3 and 7.3.4 in Method 13A, may be omitted.

(5) Determine the amount of product (Mp) in storage using the measurement system described in § 63.625(b) and (c).

(6) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Book of Methods Used and Adopted By The Association of Florida Phosphate Chemists (incorporated by reference, see § 63.14) where applicable:

(i) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method A—Volumetric Method.

(ii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method B—Gravimetric Quimociac Method.

(iii) Section XI, Methods of Analysis For Phosphoric Acid, Superphosphate, Triple superphosphate, and Ammonium Phosphates, No. 3 Total Phosphorus-P2O5, Method C—Spectrophotometric Method, or,

(7) Determine the P2O5 content (Rp) of the product stored using, as appropriate, the following methods specified in the Official Methods of Analysis of AOAC International (incorporated by reference, see § 63.14) where applicable:

(i) AOAC Official Method 957.02 Phosphorus (Total) In Fertilizers, Preparation of Sample Solution.

(ii) AOAC Official Method 929.01 Sampling of Solid Fertilizers.

(iii) AOAC Official Method 929.02 Preparation of Fertilizer Sample.

(iv) AOAC Official Method 978.01 Phosphorus (Total) in Fertilizers, Automated Method.

(v) AOAC Official Method 969.02 Phosphorus (Total) in Fertilizers, Alkalimetric Quinolinium Molybdophosphate Method.

(vi) AOAC Official Method 962.02 Phosphorus (Total) in Fertilizers, Gravimetric Quinolinium Molybdophosphate Method.

(vii) AOAC Official Method 958.01 Phosphorus (Total) in Fertilizers, Spectrophotometric Molybdovanadophosphate Method.