§ 80.10 Fees for certification services. (a) Fees for straight colors including lakes. The fee for the services provided by the regulations in this part in the case of each request for certification submitted in accordance with § 80.21(j)(1) and (2) shall be 25 cents per pound of the batch covered by such requests, but no such fee shall be less than $160.00. (b) Fees for repacks of certified color additives and color additives mixtures. The fees for the services provided under the regulations in this part in the case of each request for certification submitted in accordance with § 80.21(j)(3) and (4) shall be: (1) Fees for straight colors including lakes. 25 cents per pound of the batch covered but not less than $160. (2) Repacks of certified color, color additives, and color additive mixtures. (i) 100 pounds or less-$25. (ii) Over 100 pounds but not over 1,000 pounds-$25 plus 6 cents for each pound over 100 pounds. (iii) Over 1,000 pounds-$79 plus 2 cents per pound for each pound in excess of 1,000 pounds. (c) Advance deposits. Any person regularly requesting certification services may deposit funds in advance of requests as prepayment of fees required by this section. (d) Method of payment. All deposits and fees required by this section shall be paid by money order, bank draft, or certified check, drawn to the order of the Food and Drug Administration, collectable at par at Washington, D.C. All such deposits and fees shall be forwarded to the Division of Color Technology, HFF-430, Bureau of Foods, Food and Drug Administration, 200 C St. SW., Washington, D.C. 20204, whereupon after making appropriate records thereof, they will be transmitted to the Treasurer of the United States for deposit to the special account "Salaries and Expenses, Certification, Inspection, and Other Services, Food and Drug Administration." (e) Refunds from advance deposits. Whenever in the judgment of the Commissioner the ratio between fees collected (which are based upon experience and the best estimate of costs and the best estimate of earnings) and the costs of providing the service during an elapsed period of time, in the light of all circumstances and contingencies, warrants a refund from the fund collected during such period, he shall make ratable refunds to those persons to whom the services were rendered and charged, except that no refund shall be made where the computed ratable amount for the elapsed period is less than $5.00. (Sec. 706(c) and (e), 74 Stat. 402-403 (21 U.S.C. 376(c) and (e)) [42 FR 15662, Mar. 22, 1977, as amended at 47 FR 24692, June 8, 1982] Subpart B-Certification Procedures § 80.21 Request for certification. A request for certification of a batch of color additive shall: (a) Be addressed to the Commissioner of Food and Drugs. (b) Be prepared in the manner set forth in paragraph (j) of this section. (c) Be submitted in duplicate. (d) Be signed by a responsible officer of the person requesting certification of the batch. In the case of a foreign manufacturer, the request for certification must be signed by a responsible officer of such firm, and, by his agent who resides in the United States. (e) Show the name and post office address of the actual manufacturer in case such manufacturer is not the person requesting certification of the batch. (f) Be accompanied by the fee prescribed in § 80.10 unless the person has established with the Food and Drug Administration an advanced deposit to be used for prepayment of such fees. In no case shall the Commissioner consider a request for certification of a batch of color additive if the fee accompanying such request is less than that required by § 80.10 or if such fee exceeds the amount held in the advance deposit account of the manufacturer submitting such request for certification. (g) Be accompanied by the sample prescribed in § 80.22 consisting of: (1) Four ounces in the case of straight colors and lakes. (2) Two ounces in the case of repacks and mixtures. A sample accompanying a request for certification must be submitted under separate cover and should be addressed to the Color Certification Branch. (h) The name of a color additive shall be given in the following manner: (1) The name of a straight color shall be the name of the color as listed in Parts 74 and 6 of this chapter. (2) The name of a iake shall be the name derived in the manner described in Part 82 of this chapter. (3) The name of a mixture shall be the name given to such mixture by the person requesting certification. (4) The name of a repack shall be the name described in paragraph (h)(1), (2), or (3) of this section, whichever is applicable. (i) The information and samples enumerated in paragraphs (a) to (h), inclusive, of this section are the minimum required. Additional information and samples shall be submitted at the request of the Food and Drug Administration when such additional information and samples are necessary to determine compliance with the requirements of § 80.31 for the issuance of a certificate. (j) The form for submission of the application shall be one of the following, depending upon whether the color additive is a straight color, a lake, a repack of a previously certified color additive, or a color additive mixture. (1) Request for certification of a batch of straight color additive. Quantity used (in pounds) § 80.31 Obtained from Certification. (a) If the Commissioner determines, after such investigations as he considers to be necessary, that: (1) A request submitted in accordance with § 80.21 appears to contain no untrue statement of a material fact; (2) Such color additive conforms to the specifications and any other conditions set forth therefor in Parts 81 and 82 of this chapter. (3) The batch covered by such request otherwise appears to comply with the regulations in this chapter, the Commissioner shall issue to the person who submitted such request a certificate showing the lot number assigned to such batch and that such batch, subject to the terms, conditions, and restrictions prescribed by Part 74, 81, and 82 of this chapter, is a certified batch. (b) If the Commissioner determines, after such investigation as he considers to be necessary, that a request submitted in accordance with § 80.21, or the batch of color additive covered by such request, does not comply with the requirements prescribed by paragraph (a) of this section for the issuance of a certificate, the Commissioner shall refuse to certify such batch and shall give notice thereof to the person who submitted such request, stating his reasons for refusal. Any person who contests such refusal shall have an opportunity for a regulatory hearing before the Food and Drug Administration pursuant to Part 16 of this chapter. § 80.32 Limitations of certificates. (a) If a certificate is obtained through fraud or misrepresentation of a material fact, such certificate shall not be effective, and a color additive from the batch on which such certificate was issued shall be considered to be from a batch that has not been certified in accordance with the regulations in this part. Whenever, the Commissioner learns that any certificate has been obtained through fraud or material misrepresentation, he shall notify the holder of the certificate that it is of no effect. When the dye solution is at room temperature, transfer the solution to a 1000 mL separatory funnel. Rinse the beaker three times with 50 mL portions of H2O, transferring each rinse to the 1000 mL funnel. Add 150 mL of ether to the funnel, stopper and shake for 10 seconds, then invert funnel and open stopcock to remove gas buildup. Shake the funnel for one minute, opening the stopcock a few times while the funnel is inverted to remove gas buildup. (Use this shake procedure throughout method.) Allow the funnel to stand until the layers have separated. Transfer the bottom (aqueous) layer to a 500 mL separatory funnel, add 100 mL of ether, stopper and shake for one minute. When the layers have separated, drain off the bottom layer into a waste beaker. Pour the ether layer in the 500 mL separatory funnel into the 1000 mL separatory funnel. Rinse the 500 mL sep. funnel with 100 mL H2O, then transfer it to the 1000 mL sep. funnel, stopper and shake for one minute. When the layers have separated, drain off the bottom aqueous layer into the waste beaker. Rinse the 500 mL funnel at least three times (total) and repeat the 100 mL water washes until no color is present in the aqueous layer. Discard the bottom aqueous layer to the waste beaker after each separation. Shake the ether layer twice more with 100 mL portions of H2O, discarding the bottom aqueous layer after each separation. Remove the unsulfonated subsidiary color from the ether by shaking the ether layer for one minute with 20 mL of 2% (w/w) NaOH. Appropriately label a 100 mL beaker. After the layers separate, drain the aqueous alkaline layer into the beaker and save for the determination of 3-hydroxy-4[(4-methylphenyl) azol-2-naphthalenecar boxylic acid, sodium salt. If there is any color left in the ether, shake for one minute with another 20 mL portion of 2% (w/w) NaOH. After the layers have separated, drain off the aqueous alkaline layer into the 100 mL beaker. If color remains in the ether layer, repeat the above step for a total of three washes of the ether with 2% (w/w) NaOH. Note: Three washes is usually sufficient to remove the unsulfonated subsidiary. With the stopper removed, gently swirl the ether layer in the sep. funnel twice to separate the remaining aqueous base. Drain this into the 100 mL beaker. Appropriately label a 250 mL beaker. Pour the ether layer into the beaker. Allow the ether to evaporate to near dryness. Cool to room temperature. Add ca 8 mL ethanol (95%). Swirl beaker to mix contents. Quantitatively transfer to a 25 mL graduate using ethanol (95%) rinses. Add ethanol (95%) to bring volume to 15 mL. SPECTROPHOTOMETRIC ANALYSIS Spectrophotometer Parameters: Cell length: 1 cm (Note: Reference and (1) Record the visible spectrum of a blank. Fill the reference cell with distilled water and the sample cell with ethanol (95%). (2) Rinse the sample cell with 2-3 mL of the ether soluble material (in ethanol solution); then fill the cell. Record the visible spectrum of the ether soluble material. (3) Compare the spectra obtained to the spectra attached. The attached spectra represents 150% of the absorbance at each wavelength for similarly analyzed D&C Red No. 6 Lot AA5169. The spectra of the current sample must not exceed the attached spectra at any wavelength in order to pass test. |