CENTRAL MARKS DEPARTMENT II Our Ref: CMD-II/16:264 22 03 2006 Subject: Implementation of revised Indian Standard Specification for Nitric Acid Indian Standard specification for Nitric Acid as per IS 264:1976 has been revised as Nitric Acid as per IS 264:2005. In this revision, the main changes are as follows:- With a view to harmonize Indian Standard with ISO Standard, potentiometric method for chlorides, reduction and titremetry method for sulphates and spectrophotometric method for ammonium salts have been incorporated. As per provision Clause 4.6.6 of operation certification manual, a copy of revised specification was sent to MDK-3 vide CMD note ref. CMD-II/16: 264 dated 24 05 2005 and requested MDK-3 to send a draft STI of the revised version to CMD II for smooth switchover. No draft STI was received in CMD II in spite of 2 reminders. Draft STI was prepared by CMD II and sent to all MDK-3 for their comments on 03 02 06. Last date of comments was 20 02 2006. No Comments of MDK-3 was received in CMD II and incorporated. Accordingly, STI has been revised as DOC: STI/264/3, March 2006. In order to implement, revised standard and revised Scheme of Testing and Inspection, following procedure shall be adopted: For existing licensee: 1. Concerned BO to verify the manufacturing capability and availability of testing equipments as per revised specification with the licensees and obtain the declaration on CMD/PF 305 and 306. Factory testing/ independent testing depending upon nature of tests shall be carried out during routine periodic inspection at the earliest possible for all the requirements to ensure the conformity of the product to the revised standard. However, factory testing or verification of test facilities shall be invariably carried out wherever changes have occurred in the revised specification. 2. Endorsement in the licence as per revised standard shall be made after obtaining the following documents from the licensees:
a. Declaration regarding manufacturing capability and availability of testing equipment as per revised specification on CMD/PF 305 and 306. b. Acceptance of revised STI. c. Test report indicating conformity of the product to the revised specification. 3. Stoppage of marking shall be imposed in case sample fails in factory/ independent testing as per the revised version at the time of verification on the routine periodic inspection and further actions are to be taken as per Operation Certification Manual. 4. Action shall be taken as per OM 2004, if the licensee fails to submit the acceptance of STI in stipulated time. For Applicants: 5. All new applications may be recorded and processed as per revised IS 264:2005. 6. In case applicant sample is yet to be tested by Lab, necessary action may be taken immediately by BO for considering the case as per IS 264:2005 after consulting the applicant. 1. New licence granted during this period as per IS 264:1976. ROs/BOs shall ensure that new licensee shall implement the revised standard and STI within the stipulated period. REVISED STANDARD IS 264:2005 AND NEW STI DOC: STI/264/3, March 2006 WILL BE EFFECTIVE FROM 15 May 2006. Submitted for approval please. DOC: STI 264/3 (N.K. Bansal) Director (CMD-II) Joint Sc.F&H(CMD-II) DDGM
CENTRAL MARKS DEPARTMENT II Our Ref: CMD-II/16:264 17 04 2006 Subject: Implementation of revised Indian Standard Specification for Nitric Acid Indian Standard specification for Nitric Acid as per IS 264:1976 has been revised as Nitric Acid as per IS 264:2005. In this revision, the main changes are as follows:- With a view to harmonize Indian Standard with ISO Standard, potentiometric method for chlorides, reduction and titrimetry method for sulphates and spectrophotometric method for ammonium salts have been incorporated. As per provision Clause 4.6.6 of operation certification manual, a copy of revised specification was sent to MDK-3 vide CMD note ref. CMD- II/16: 264 dated 24 05 2005 and requested MDK-3 to send a draft STI of the revised version to CMD II for smooth switchover. No draft STI was received in CMD II in spite of 2 reminders. Draft STI was prepared by CMD II and sent to all MDK-3 for their comments on 03 02 06. Last date of comments was 20 02 2006. No Comments of MDK-3 was received in CMD II. Accordingly, STI has been revised as DOC: STI/264/3, March 2006. In order to implement, revised standard and revised Scheme of Testing and Inspection, following procedure shall be adopted: For existing licensee: 1. Concerned BO to verify the manufacturing capability and availability of testing equipments as per revised specification with the licensees and obtain the declaration on CMD/PF 305 and 306. Factory testing/ independent testing depending upon nature of tests shall be carried out during routine periodic inspection at the earliest possible for all the requirements to ensure the conformity of the product to the revised standard. However, factory testing or verification of test facilities shall be invariably carried out wherever changes have occurred in the revised specification. 2. Endorsement in the licence as per revised standard shall be made after obtaining the following documents from the licensees: a. Declaration regarding manufacturing capability and availability of testing equipment as per revised specification on CMD/PF 305 and 306.
b. Acceptance of revised STI. c. Test report indicating conformity of the product to the revised specification. 3. Stoppage of marking shall be imposed in case sample fails in factory/ independent testing as per the revised version at the time of verification on the routine periodic inspection and further actions are to be taken as per Operating Certification Manual 2004. 4. Action shall be taken as per OM 2004, if the licensee fails to submit the acceptance of STI in stipulated time. For Applicants: 5. All new applications may be recorded and processed as per revised IS 264:2005. 6. In case applicant sample is yet to be tested by Lab, necessary action may be taken immediately by BO for considering the case as per IS 264:2005 after consulting the applicant. 7. New licence granted during this period as per IS 264:1976. ROs/BOs shall ensure that new licensee shall implement the revised standard and STI within the stipulated period. REVISED STANDARD IS 264:2005 AND NEW STI DOC: STI/264/3, March 2006 WILL BE EFFECTIVE FROM 15 May 2006. DOC: STI 264/3 action. downloaded. All RO s/bo s are requested to take appropriate necessary STI is already available on BIS internet site and can be (CMD-II) Sc.F&H(CMD-II) Joint (N.K. Bansal) Director Circulated to all RO sbo s, CMD-I Cc: CHD - with a request to gazette it w.e.f. 15 May 2006.
SCHEME OF TESTING AND INSPECTION FOR CERTIFICATION OF NITRIC ACID ACCORDING TO IS: 264-2005 (Third Revision) 1. Laboratory - A laboratory shall be maintained which shall be suitably equipped and staffed to carry out the different tests in accordance with the methods given in the Indian standards. 2. Test Records - All records of analysis and tests shall be kept in suitable forms approved by the Bureau of Indian Standards (BIS). 2.1 Copies of any records that may be required by BIS shall be made available at any time on request. 2.2 Quality Control - It is recommended that, as far as possible, Statistical Quality Control (SQC) methods may be used for controlling the quality of the product as envisaged in this Scheme[See IS 397(Part 1):2003, IS 397 (Part 2):2003 and IS 397 (Part 3):2003]. 2.2.1 All instruments/equipments are required to be brought under calibration control, as per frequency to be decided depending upon the usage. 2.3 In addition, effort should be made to gradually introduce a Quality Management System in accordance with IS/ISO 9001:2000. 3. Standard Mark The Standard Mark(s) as given in Column (1) of the first Schedule of the licence shall be marked/stenciled on each container provided always that the material in each container to which this mark is applied conforms to every requirement of the specification. 4. Marking - In addition, the following information shall be given on each container and also the package in red letters not less then 25 mm high showing: a) Name of the manufacturer and recognized trade Mark, if any: b) Name of the material; c) Grade of the material; d) Net mass of the material; e) Batch number or identification in code or otherwise to enable the date and batch of manufacture to be traced back to factory records; and f) The following minimum cautionary notice, prominently displaced. CORROSIVE, HANDLE WITH CARE g) Licence No. (CM/L ----------------------) 4.1 The data of chemical analysis with respect to the requirements prescribed in Col. 6 of Table 1 to IS 264:2005 shall also be shown on the containers
of the analytical reagent grade of the material. 4.1.1 The packages shall be labeled as shown in Fig. 15 of IS: 1260 (Part 1). 5.0 Packing The acid shall be packed in such container as agreed to between the purchaser & the supplier and subject to the relevant provisions of Red Tariff No. 18 of 1960 issued by Indian Railway Conference Association with any alterations or additions made there after Nitric Acid of chemically pure and/analytical Reagent grade shall be supplied in glass bottles or glass carboys fitted with tight fitting Teflon Washers (of thickness 0.2 mm) and stoppered with HDPF or other suitable stopper. The use of HDPF or other suitable caps over the stopper is recommended. 5.1 When Nitric Acid is supplied in screw-stoppered stone bottles or glass carboys, the containers shall be fitted with leak-tight stoppers and, if required by the purchaser, provided with asbestos washers. The stoppers shall be further sealed by putty from china clay or a mixture of sulphur and sand. 5.2 The bottles or jars shall be packed in suitable pent top packing cases. The bottles may also be placed in expanded polystyrene as expanded polyethylene containers and finally in corrugated fiber board boxes. They shall be placed in an upright position on one layer of sand or ashes free from cinders and the empty surrounding space shall also be filled with the same material to prevent movement carboys shall be packed in suitable iron hampers or wooden crates, the interspace being sufficiently stuffed with whiting kieselghur or other non-combustible absorbent material. 6. Levels of Control - The analysis and tests, as indicated in Table 1 and at the levels of control specified therein, shall be carried out on the whole production of the factory covered by this scheme and appropriate records and charts maintained in accordance with Para 2 above. All the production which conforms to the Indian Standard and covered by this licence shall be marked with the Standard Mark. 6.1 Control Unit The total quantity of the acid of a particular grade produced during the day and thoroughly homogenized shall be considered as a control unit. 6.1.1 A sample drawn from each control unit of acid manufactured shall be taken and shall satisfy the requirements of the specification for the relevant grade. If the sample fails in any one or more requirements of the specification for the relevant grade the entire quantity of the acid represented by the control unit shall be rejected. The acid could, however, be reprocessed and the defect rectified. Such reprocessed material when tested again shall conform to all the requirements of the specification for the relevant grade before it is considered fit for marking.
6.2 On the basis of tests and analysis results, the decision regarding conformity or otherwise, of a control unit to a given requirement shall be made. 6.3 Routine analysis of the nitric acid, technical grade going into the manufacture of the pure and analytical reagent grades of acid, shall be made on each consignment received into the factory and appropriate records shall be maintained. 6.4 In respect of all other clauses of the specification the factory will maintain appropriate controls and checks to ensure that product conforms to the various requirement of the specification. 7. Rejection - A separate record shall be maintained giving information relating to the rejection of the production which do not conform to the specification and the method of their disposal. Such material, if packed in containers, shall in no case be stored together with that conforming to the specification. 8. Samples - The licensee shall supply, free of charge, the sample or samples required in accordance with the Bureau of Indian Standards (Certification) Regulations from his factory or god owns. BIS shall pay for the samples taken by it from the open market. 9. Replacement- Whenever a complaint is received soon after the goods with the Standard Mark have been purchased and used, and if there is adequate evidence that the goods have not been misused, defective goods or their components shall be replaced or repaired free of cost by the licensee in case the complaint is proved to be genuine and the warranty period (where applicable) has not expired. The final authority to judge conformity of the product to the Indian Standard shall be with BIS. The firm should have own complaint investigation system as per IS 15400. 9.1.1 In the event of any damages caused by the goods bearing the Standard Mark, or claim being filed by the consumer against BIS Standard Mark and not conforming to the relevant Indian Standard, entire liability arising out of such non conforming product shall be of licensee and BIS shall not in any way be responsible in such cases. 10. Stop Marking - The marking of the product shall be stopped under intimation to BIS, if at any time, there is some difficulty in maintaining the conformity of the product to the specification, or the testing equipment goes out of order. The marking may be resumed as soon as the defects are removed under intimation to BIS.
The marking of the product shall be stopped immediately if directed to do so by BIS for any reason. The marking may then be resumed only after permission by BIS. The information regarding resumption of marking shall also be sent to BIS. 11. Production Data The licensee shall send to BIS, as per the enclosed Performa to the authenticated by a Chartered Accountant or by the manufacturer by giving an affidavit/undertaking, a statement of the quantity produced, marked and exported by him and the trade value thereof at the end of each operative year of the licence.
Clause 4.1 Description TEST DETAILS Requirements IS: 264-2005 NITRIC ACID Table 1 LEVELS OF CONTROL (Para 6 of the Scheme of Testing and Inspection) Test Method Clause Reference IS 264:2005 Visual 4.1.1 & 4.1.2 LEVEL OF CONTROL No. of Lot size Samples One sample Each control unit REMARKS Samples shall be drawn from storage container after homogenizing the contents. A day s production of acidof one grade shall constitute a control unit. 4.2 & Table 1 Total acidity (as NHO3) Annex A do-- - Residue on ignition Annex B Chlorides (as Cl) Annex C Sulphates (as H 2 SO4) Annex D Heavy metals (as Pb) Annex E Nitrous acid (as HNO 2 ) Arsenic (as As) Iodine Iron (as Fe) Manganese (as Mn) Annex F Annex G Annex H Annex J Annex K Not applicable in case of technical and analytical reagent grades, Not applicable in case of technical, Nitration and explosive grades. Not applicable in case of technical, chemically pure and analytical reagent grades. Not applicable in case of technical, Nitration and explosive and chemically pure grades. Not applicable in case of technical, Nitration and explosives and chemically pure grades.
IS: 264-2005 NITRIC ACID Table 1 LEVELS OF CONTROL (Para 6 of the Scheme of Testing and Inspection) Clause 4.2 & Table 1 TEST DETAILS Requirement Test Method s Clause Reference Phosphate (as Annex L IS 264:2005 PO4) Silicate (as SiO2) Ammonium salts (as NH3) Annex L Annex M LEVEL OF CONTROL No. of Lot size Samples One sample Each control unit REMARKS Not applicable in case of technical, Nitration and explosive and chemically pure grades. Not applicable in case of Nitration and Explosives, Chemically pure and analytical reagent grades.
IS: 264-2005 NITRIC ACID FORM II RECORD OF RAW MATERIAL (Para 5 of the Scheme of Testing and Inspection) DOC: STI 264/3 Sl. No. Date Source of supply Quantity of acid received K Quantity used Kg. Balance in stock Kg. Result of Analysis Remarks IS: 264-2005 NITRIC ACID FORM III RECORD OF RAW MATERIAL NOT CONFORMING TO THE SPECIFICATION (Para 7 of the Scheme of Testing and Inspection) Sl No. Date of manufacture and Batch number Quantity of material Kg. Method of Disposal Remarks