म नक भवन, 9 बह द रश ह ज फर म र ग, नई ददल ल 110002 Manak Bhavan, 9 Bahadur Shah Zafar Marg, New Delhi 110002 TECHNICAL COMMITTEE: FAD 01 ADDRESSED TO: 1. All Members of Pesticides Sectional CommitteeSectional Committee, FAD 01 2. Selected members of FADC 3. All interested Dear Madam/Sir(s), द रभ ष Website: www.bis.org.in त र: म नकस स थ Phones 23230131 email: fad@bis.org.in Grams: Manaksanstha 23233375 23239402 Please find enclosed the following documents: DOCUMENT DISPATCH ADVICE Our Ref: Date FAD 01/T 22-01-2019 Sl. No. Doc. No. Title 1. FAD 01 (12482) C-1 TRICYCLAZOLE 70% WETTABLE GRANULES (WG) SPECIFICATION Kindly examine the draft Indian Standards and forward your views stating any difficulties which you are likely to experience in your business or profession, if this is finally adopted as Indian Standards. Comments if any may please be made in the format attached and mailed to the undersigned at the above address. Last date for comments: 25 FEBRUARY 2019. In case no comments are received or comments received are of editorial nature, kindly permit us to presume your approval for the above document as finalized. However, in case of comments of technical in nature are received then it may be finalized either in consultation with the Chairman, Sectional Committee or referred to the Sectional Committee for further necessary action if so desired by the Chairman, Sectional Committee. The document is also hosted on BIS website www.bis.gov.in. Thanking you, Encl: As above. Yours faithfully, -Sd/- (P Rajesh) Scientist E & Head (Food & Agri) E-mail: fad1@bis.gov.in
व य पक पचरल लन मस द प र षषत तकन क सम ततएफ ए ड 01 प रल ख प र षण स ज ञ पन स दभग ददन क एफ ए ड 01/ट 22-01-2019 1 ख द य एव क षष क ल ए क टन शक षवषय सलमतत,एफ ए ड 01क समस त सदस य 2 ख द य एव क षष षवभ ग पररषदएफए ड स क सदस य 3 र च रखन व सभ तनक य मह दय /मह दय, आपक अव कन ह त तनम नल खत मसदद स न ह : क.स. मस द स ख य ववषय 1. एफएड 01 (12482) स -1 ट र इस इक ल ज ल 70% व ट बल ग र न य ल स (डब ल ज )- ववशशष टट क पय इसप र ख क अव कन कर अपन सम मततय यह तत त ह ए भ क य द अ तत :यहमसदद भ रत य म नक क स श धन क र प म प रक लशत ह ए त इस पर अम करन म आपक व यवस य अथव क र त र म य क न इय आ सकत ह सम मततय क पय स न प र र प म अध -हस त क षर रक क भ सम मततय भ जन क ततम तत : 25-02-2019 य द क ई सम मतत प र त नहक ह त ह अथव सम मतत म क व भ ष स त ध ट ह ई त पपर त प र ख क यथ वत अ ततम र प दय य ग य द क ई सम मतत तकन क प रक तत क ह ई त षवषय सलमतत क अद यक षर क पर मशश स अथव पनक इच छ पर आग क क यशव हक क ल ए षवषय सलमतत क भ न क त द प र ख क अ ततम र प द दय य ग धन यव द, भवद य -हस त /- प रतत पपररल खत ) प र श वज ञ तनक ई एव प रम ख (ख द य एव क षष षवभ ग) ई-म :fad1@bis.gov.in
Doc No.: FAD 1 (12482) C TRICYCLAZOLE 70% WETTABLE GRANULES (WG) SPECIFICATION 1. SCOPE This standard prescribes the requirement and the methods of sampling and test for Tricyclazole 70% WG. 2. REFERENCES The standards listed below contain provisions which through reference in this text constitute provisions of this standard.at the time of publications, the editions indicated were valid. All standards are subject to revision and parties to agreements based on this standard are encouraged to investigate the possibility of applying the most recent editions of the standards listed below. IS NO Title 1070:1992 Reagent grade water (Third Addition) 6604: 1991 Code for packaging of solid pesticides (up to 500 g) (first revision) 6940:1982 Methods of test for pesticides and their formulations (First revision) 2771(Part 1):1990 Fibre board boxes-specification 8190 (Part 1):1988 Requirement for packing of pesticides: Part 1 Solid Pesticides (Second Revision) 10627:1983 Methods for sampling of pesticidal formulations 3. REQUIREMENTS 3.1 Constituents 3.1.1 The material shall consist of Tricyclazole Technical along with suitable carrier(s), stabilizers(s), and other formulant (s) 3.1.2 Tricyclazole technical employed in the formulation of this material shall conform to IS 15982: 2013. 3.2 Description: The material shall be in the form of tan to brick red colored free flowing odorless granules and shall wet readily on mixing with water providing a suspension for suitable use as spray. 3.3 The material shall also comply with the requirements given in Table 1
3.3.1 When determined by the method prescribed in Annex A, the observed Tricyclazole content, percent (m/m) of any of the samples shall not differ from the declared nominal value by more than the percent tolerance limits indicated below: Nominal Value Tolerance Limit Percent Percent Up to 9 +10-5 Above 9 and below 50 ±5 50 and above +5-3 Table I Requirements for Tricyclazole 70% WG (Clause 3.3) Sr Characterstic Requirement Method of Test Ref to No Annex Clause No of IS 6940 (1) (2) (3) (4) (5) i) Tricyclazole Content, Nominal value as declared on the container ( see 3.3.1) A --- ---------- Percent by Mass ii) Material Passing thro 98.0 ------- 11.1 45µ IS Sieve, Percent By mass, Min iii) Suspensibility,Percent 70.0 ---------- 11.2 By Mass, Min iv) Wettability in Seconds, Max. 120 --------- 11.4 v) Attrition Resistance, 90.0 B ---- ------- % by mass (Min) vi) Moisture Content (Max) 2.0 ------------- 4.1 vii) ph (1 % w/v aq. Solution) 6.0 to 8.0 C -- ---------- viii) Persistent foam (ml) after 60 D -- ----------- one minute ix) Dust Content (mg) (Max) 30 E -- ----------- 4. PACKING 4.1 The material shall be packed in trilaminated pouch with material of construction of 12 microns PET/9 microns Al foil/75-85 microns Poly, which shall be packed in secondary
pack of duplex board / 3 ply E fluted carton conforming to IS 2771(Part.1)1990. This carton shall be further packed in 5 ply corrugated fibre board box as a transport pack conforming to IS 2171 (Part. 1) 1990 The capacity of the pouches shall be 60gm, 120gm, 240gm and 480 gm. These shall be properly heat sealed to make these leak proof and pilfer proof. The packaging shall also conform to the general requirements as given in IS: 8190 (Part I): 1988, Indian Standard requirement for Packing of Solid Pesticides (2 nd Revision) and amendments thereof, if any. 5. MARKING 5.1 The containers shall be securely closed and the following information shall be marked legibly and indelibly on each container in addition to any other information as is necessary under the Insecticides act 1968 and rules framed there under (a) (b) (c) (d) (e) (f) (g) Name of the material Name of the manufacturer Date of manufacture Batch number Net mass of the contents Tricyclazole content, percent (m/m); and A cautionary notice worded as in the Insecticides Act, 1968 & Rules. 6.0 SAMPLING 6.1 When freshly manufactured material is offered for inspection, representative samples shall be drawn according to IS 10627: 1983 and tested within 90 days of its manufacture. When the material is offered for inspection after 90 days according to IS 10627: 1983. However, the criteria for conformity of the material when tested shall be the limits of tolerances, as applicable over the declared nominal value and given under 3.3.1 of this standard. 7.0 TESTS 7.1 Tests shall be carried out by the appropriate methods referred to in 3.3 and col 4 and 5 of Table 1. 7.2 Quality of reagents Unless specified otherwise, pure chemicals and distilled water (IS: 1070 1992) shall be employed in tests. NOTE Pure chemicals shall mean chemicals that do not contain impurities, which affect the results of analysis.
ANNEX A [Clause 3.3.1 and table 1, Sr. No. (ii)] DETERMINATION OF TRICYCLAZOLE CONTENT A-0 GENERAL: Two methods namely, High Performance Liquid Chromatography (HPLC) or Gas Liquid Chromatography (GLC) may be used for determination of Tricyclazole Content. However, either HPLC or GLC shall be the referee methods. A-1 Gas Liquid Chromatography (GLC) Method A-1.1 Principle Determination of Tricyclazole content in a WG sample, by using a Gas chromatograph (GLC) with Flame Ionisation Detector (FID) using an internal standard technique. A-1.2. Apparatus A-1.2.1 A Gas chromatograph (GLC) equipped with FID and chromatography software/ Printerplotter cum Integrator A-1.2.2 Analytical balance A-1.2.3 Microlitre syringe 10 μl capacity A-1.2.4 Ultrasonic bath A-1.2.5 Standard Volumetric glassware A-1.3. Chromatographic conditions The following are the suggested analytical conditions for the determination of Tricyclazole content in WG samples. These conditions may be varied, if necessary, provided the standardization is done: Instrument:- A Gas chromatograph (GLC) equipped with FID and chromatography software/printerplotter cum Integrator Stationary Phase:- 5% SE-30 (or equivalent) on Chromosorb-WHP(100/120 mesh), 6 x 2.0 mm ID Glass Temperature: Column oven : 250 C (Isothermal) Injector : 260 C Detector : 270 C Gas flow rates: Nitrogen (carrier): 30 ml / min. Hydrogen : 30 ml / min. Air : 300 ml / min. A-1.4 Reagents
A-1.4.1 Acetonitrile HPLC grade A-1.4.2 Internal Standard Di Octyl phthalate AR grade A-1.4.3 Tricyclazole Reference standard of known purity. A-1.5 Procedure A-1.5.1 Preparation of Internal Standard: Weigh out accurately about 2.5 g of Di-Octyl Phthalate into a 100mL volumetric flask. Dissolve and homogenize in Acetonitrile, by swirling. Make up to the mark with Acetonitrile. A-1.5.2 Preparation of Standard Solution: Weigh out accurately about 0.25-0.30 g of Tricyclazole reference standard of known purity, in duplicate, into a 25 ml volumetric flask. Add 5 ml of the internal standard solution (A-1.4.1) and homogenize the content by swirling. Make up to the mark with Acetonitrile. Mark these flasks as C1 & C2. A-1.5.3 Preparation of Formulation Sample Solution: Weigh out accurately about the WG sample quantity equivalent to contain Tricyclazole tech., in duplicate, into a 25 ml volumetric flask. Add 5mL of internal standard solution (A-1.4.1) to the sample, followed by 10-15 ml of Acetonitrile. Sonnicate this solution for about 5 minutes and allow it to attain room temperature. Make up to the mark with Acetonitrile. Stopper the flask and shake well. Mark these flasks as S1 & S2. Filter the sample solution through Whatman no. 1 (or equivalent) paper to get clear solution prior to injection on to GC column. A-1.6 Estimation A-1.6.1 Inject 1 µl of Tricyclazole standard solution into the gas chromatograph, using a microliter syringe (10 µl), until area of Tricyclazole and Internal standard in replicate injections matches within ±2%. Inject WG sample solutions and note down the peak areas of both. Inject the standard and sample solution in following sequence and then compute the percentage purity of Tricyclazole in WG sample using the formula given in A-1.8. A-1.6.2 Sequence of injection to be followed C1, C2, S1A, S1B, C2, C1, S2A, S2B, C2 A-1.7 Retention Time (guideline values): Tricyclazole 3.5 min. Di-Octyl phthalate 8.0 min. Total Run Time 12 min. A-1.8 Calculation;- From chromatograms note the peak areas of Tricyclazole and Internal standard. Calculate the percent of Tricyclazole content in the sample as follows:
Tricyclazole content, = M 1 x A 2 x A 3 x P (Percent m/m) ---------------------- M 2 x A 1 x A 4 Where, M 1 = Mass in g of standard Tricyclazole in standard solution, M 2 = Mass in g of sample taken for test, A 1 = Area of Tricyclazole peak in the chromatogram of standard Solution, A 2 = Area of Tricyclazole peak in the chromatogram of sample solution, A 3 = Area of internal standard peak in the chromatogram of Standard solution, A 4 = Area of internal standard peak in the chromatogram of Sample solution, P = Percent purity of Tricyclazole reference standard TYPICAL GC CHROMATOGRAM DOP Peak Tricyclazole Peak
A-2 High Performance Liquid Chromatography (HPLC) Method A-2.1 Principle: Tricyclazole content in WG samples is determined by high performance liquid chromatography (HPLC) technique using an internal standard method. A-2.2 Apparatus: High Performance Liquid Chromatograph - Equipped with a constant flow (Isocratic) pump, HPLC column heater compartment, sample injector capable of injecting 20 microliter aliquots, UV detector (231nm wavelength), and a Chromatography software/printer-plotter cum integrator. Analytical Balance (Least count 0.1mg). Microliter Syringe - 50 l Filtration apparatus with 0.45µm membrane filters. Standard Volumetric glassware A-2.3 Chromatographic conditions: The suggested HPLC operative parameters are as follows, but can be changed if necessary, provided standardization is done: Column: Purospher RP-18, 250mm x 4.6mm, 5 m, stainless steel or equivalent Mobile Phase: Acetonitrile: Water (50:50, v/v), ph of water = 2.85, adjusted with aqueous o- Flow rate: Injection vol.: 20 l phosphoric acid solution (10%). 0.85 ml / min. UV Detector wavelength: 231 nm A-2.4. Reagents: A-2.4.1 Acetonitrile HPLC grade A-2.4.2 Water, HPLC grade A-2.4.3 Methanol, HPLC grade A-2.4.4 Acetophenone (internal standard) AR grade of known purity A-2.4.5 Tricyclazole reference standard of known purity A-2.4.6 o-phosphoric acid HPLC grade, 85% A-2.5 Preparation: A-2.5.1 Preparation of mobile phase: Adjust the ph of HPLC grade water to about 2.85 with 10% o-phosphoric acid solution in water. Add filtered water (ph-2.85) to filtered acetonitrile in equal proportion (50:50 by volume) in a volumetric flask/reservoir bottle. Sonicate for 15min, and allow mobile phase solution to attain room temperature.
A-2.5.2 Preparation of an internal standard solution: Weigh out accurately about 1.5g of Acetophenone into a 100mL volumetric flask. Dissolve in Acetonitrile and then make up to volume with the same. Sonicate the solution for about 5 minutes and allow it to attain room temperature. A-2.5.3 Standard solution preparation: Weigh out accurately about 50 mg of Tricyclazole reference standard of known purity, in duplicate, into a 100mL volumetric flask. Add 50mL Methanol, sonicate for 5min to dissolve the material. Pipette out 5 ml of internal standard solution into the volumetric flask. Mix by swirling and then make up the volume with Methanol. Pipette out 1mL of diluted solution in a 100mL volumetric flask and dilute up to the mark with the mobile phase. Mark the flasks as C1 and C2. A-2.5.4 Sample solution preparation: Prior to weighing, the sample should be homogenized using a clean pestle and mortar. Then weigh out accurately about sample, in duplicate, equivalent to contain 50mg of Tricyclazole into a 100mL volumetric flask. Add 50mL Methanol, sonicate for 5min to dissolve Tricyclazole. Pipette out 5 ml of internal standard solution into the volumetric flask. Mix by swirling and then make up the volume with Methanol. Filter through 0.45µm membrane filter. Pipette out 1mL of diluted solution in a 100mL volumetric flask and dilute up to the mark with the mobile phase. Mark the flasks as S1 and S2. A-2.6 Estimation: A-2.6.1 Equilibrate the column with mobile phase for about 45 minutes before commencement of analysis. After a stable baseline is obtained, inject the standard solution on to HPLC column, until area of Tricyclazole and Internal standard in replicate injections matches within ±2%. Inject the standard and sample solution in following sequence and then compute the percentage purity of Tricyclazole in WG sample using the formula given in A-2.8 A-2.6.2 Sequence of injection to be followed C1, C2, S1A, S1B, C2, C1, S2A, S2B, C2 A-2.7 Retention Time (indicative values) Tricyclazole : ~ 4.8 min. Acetophenone : ~ 8.4 min. (Internal Standard) Total run time : ~ 10.0 min. From the chromatograms of the standard solution and sample solution measure the peak areas of the active ingredient and the internal standard and calculate the percentage of the active ingredient as given in the calculation. A-2.8 Calculation: M 1 x A 3 x A 2 x P Tricyclazole content, % m/m = -----------------------
M2 x A4 x A1 Where, M1 = Mass, in g, of standard Tricyclazole in standard solution. M2 = Mass, in g, of sample taken for the test; A1 = Area of Tricyclazole peak in the chromatograph of the standard solution A2 = Area of Tricyclazole peak in the chromatograph of the sample solution A3 = Area of internal std. peak in the chromatograph of the standard solution A4 = Area of internal std. peak in the chromatograph of the sample solution; and P = Percent purity of Tricyclazole reference standard Typical HPLC Chromatogram Tricyclazole Peak Acetophenon e Peak
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