Determination of heavy metal in crude drug

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Determination of heavy metal in crude drug

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ANALYSIS OF CRUDE DRUG:

ANALYSIS OF CRUDE DRUG Prepared by:- Maunang Patel Guided by:- Aarti Zanwar

DETERMINATION OF HEAVY METAL:

DETERMINATION OF HEAVY METAL

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Heavy metal eg….. Antimony Arsenic Barium Beryllium Cadmium Lead Mercury Osmium Thallium Vanadium Radioactive metals Aluminium

LIMIT TEST FOR ARSENIC The amount of arsenic in the medicinal plant is estimated by the matching the depth of color with that of a std. stain.:

LIMIT TEST FOR ARSENIC The amount of arsenic in the medicinal plant is estimated by the matching the depth of color with that of a std. stain.

Preparation of the sample by acid digestion:

Preparation of the sample by acid digestion Heat gently cool

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Heat again cool

Apparatus :

Apparatus A : approximately 60 ml generator bottle with 40 ml indicating line. B : glass tube with 6.5 mm inner diameter C and D : a ground joint glass tube with 6.5 mm inner diameter and 18 mm outer diameter at the joint. Inner joint and the outer joint forms a concentric circle. E : rubber stopper F : narrow part of the glass tube B. Glass wool is inserted up to this part. G : rubber board H : clamp

Method :

Method Moisten some cotton wool with lead acetate (80 g/l) TS, allow to dry and lightly pack in to the tube which fits in to the wide mouth bottle to not less than 25 mm from the top. Between the flat surface of the tube place piece of mercuric bromide paper AsR that is large enough to cover their opening (15 mm × 15 mm) The Merc. Bromide paper AsR can be fitted by any other means provided that… The whole of the gas passes through the paper The portion of the paper in contact with the gas is circle 6.5 mm in diameter The paper is protected from the sunlight during the test

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Allow the reaction to proceed for 40 minute

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The most suitable temprature for carrying out the test is generally about 40’C but evolution of the gas may change with the different batch of granulated Zinc. The reaction may be accelerated by placing the apparatus on a warm surface . Care being taken to ensure that the Merc. Bromide paper AsR remains dry throughout. Between successive test the tube must be washed with HCL acid (250 g/l) AsTS. Rinsed with water and dry.

Preparation of standard stains:

Preparation of standard stains Add 10 mL of std. HCL acid (250 g/L) AsTS and 1 mL of dilute arsenic AsTS to 50 mL of water. The resulting solution when treated as describe in the general test yields a stain on mercuric bromide paper AsR referred to as the standard stain (10 µg of As)

LIMIT TEST FOR CADMIUM AND LEAD:

LIMIT TEST FOR CADMIUM AND LEAD The method of determination of left to the analyst. Nevertheless the determination must be consistent and sensitive enough to allow comparison with a reference material.

Apparatus :

Apparatus The equipment consists of a digestion vessel, consisting of a vitreous silica crucible having height 62 mm diameter 50 mm and capacity 75 mL with a vitreous silica cover. Material used are Digestion mixture:- 2 parts by weight of nitric acid (1000g/L) TS and 1 weight of perchloric acid (1170g/L) Reference material:- olive leaves (olea euroaea) and hay powder Clean with nitric acid (100g/L) TS the digestion vessel and all over equipment to be used for the determination rinse thoroughly several times with water and dry out at 120’C.

Preparation of sample:

Preparation of sample Put cover without exerting pressure

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Every sample should be tested in parallel with a blank.

Method :

Method The content of lead and cadmium may be determined by inverse volumetry or by atomic absorption spectroscopy. metal ADI Arsenic 0.0015mg/kg lead 10mg/kg Cadmium 0.3mg/kg

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