A FREE-FLOWING FOOD GRADE SODIUM NITRITE AND PRODUCTION METHOD THEREOF

Abstract

A free-flowing food grade sodium nitrite and production method thereof. The free flowing food grade sodium nitrite including sodium nitrate (SNI) having purity of 99.0-99.9%, wherein NaNO3 is no greater than 0.70%, wherein alkalinity as Na2CO3 is no greater than 600 ppm, wherein a chloride content is no greater than about 50 ppm, wherein a sulphate content is no greater than 50 ppm, wherein loss on drying is no greater than 0.2%, wherein a content of insoluble is no greater than 0.4%, wherein a content of a heavy metal is no greater than 10 ppm wherein a content of assay is within a range of 98.5% to 100.5%.

Claims

1. A form of a free-flowing food grade sodium nitrite comprising: sodium nitrate (SNI) having purity of 99.0-99.9%, wherein NaNO3 is no greater than 0.70%, wherein alkalinity as Na2CO3 is no greater than 600 ppm, wherein a chloride content is no greater than about 50 ppm, wherein a sulphate content is no greater than 50 ppm, wherein loss on drying is no greater than 0.2%, wherein a content of insoluble is no greater than 0.4%, wherein a content of a heavy metal is no greater than 10 ppm, wherein a content of assay is within a range of 98.5% to 100.5%.

2. The form of free-flowing food grade sodium nitrate as claimed in claim 1, wherein the heavy metal is at least Lead (pb).

3. The form of the free-flowing food grade sodium nitrite as claimed in claim 1, comprising a content of Arsenic (As) is no greater than 0.2 ppm, wherein a content of Cadmium (cd) is no greater than 1 ppm, wherein a content of Lead (pb) is no greater than 1 ppm, wherein a content of Mercury (Hg) is no greater than 0.05 ppm.

4. A method of obtaining a free-flowing food grade sodium nitrite, wherein the method comprising steps of: charging a predefined amount of water in a reactor; adding dry powder of sodium nitrite (SNI) having predefined purity in the reactor under stiffing conditions to obtain SNI liquor of mass sodium nitrite; heating the SNI liquor of mass sodium nitrite at 40-60 C. under stirring to completely dissolve the dry powder and transfer to evaporator feed tank through filters; feeding the SNI liquor of mass sodium nitrite in the evaporator to concentrate liquor to obtain slurry mass of SNI having 30 to 40% free salt concentration; filtering the slurry mass of SNI through centrifuge at a temperature within a range of 50 C.-65 C. to separate wet cake and mother liquor (ML), wherein the ML goes back to an external SNI liquor; drying the wet cake using a drying unit at a temperature within a range of 100 C.-140 C. continuously with cold zone operating at 25-60 C. to obtain dry SNI material; and coating the dry SNI material with a food grade additive in a blender to obtain free-flowing food grade sodium nitrite.

5. The method as claimed in claim 4, wherein the predefined purity of the sodium nitrite is 99.0%-99.9%.

6. The method as claimed in claim 4, wherein the SNI liquor of mass sodium nitrite is transferred to feed tank through filters in order to avoid foreign materials including black particles and other particulates to tune of 1-4 micron.

7. The method as claimed in claim 4, wherein the wet cake is having moisture content 1-12%.

8. The method as claimed in claim 4, wherein the wet cake material is dried using Vibratory Fluidized Bed Dryer (VFBD).

9. The method as claimed in claim 4, wherein the food grade additive is silica.

10. The method as claimed in claim 4, wherein the free-flowing food grade sodium nitrite is packed in bags.

11. The method as claimed in claim 4, wherein the free-flowing food grade Sodium nitrite is analyzed in view of food grade SNI specification.

Description

BRIEF DESCRIPTION OF FIGURES

[0012] The detailed description is described with reference to the accompanying Figures. In the Figures, the left-most digit(s) of a reference number identifies the Figure in which the reference number first appears. The same numbers are used throughout the drawings to refer like features and components.

[0013] FIG. 1 illustrates a method (100) for developing of free-flowing food grade Sodium nitrite (SNI), in accordance with an embodiment of the present subject matter.

[0014] FIG. 2A-2E illustrates microscopic images of the free-flowing food grade Sodium nitrate, in accordance with the Exp. no 1-5 of the present subject matter.

[0015] FIG. 3 illustrates Process Flow diagram (PFD) depicting an interaction between various components for obtaining the free-flowing food grade Sodium nitrite (SNI), in accordance with an embodiment of the present subject matter.

DETAILED DESCRIPTION

[0016] Reference throughout the specification to various embodiments, some embodiments, one embodiment, or an embodiment means that a particular feature, structure, or characteristic described in connection with the embodiment is included in at least one embodiment. Thus, appearances of the phrases in various embodiments, in some embodiments, in one embodiment, or in an embodiment in places throughout the specification are not necessarily all referring to the same embodiment. Furthermore, the particular features, structures or characteristics may be combined in any suitable manner in one or more embodiments.

[0017] The words comprising, having, containing, and including, and other forms thereof, are intended to be equivalent in meaning and be open ended in that an item or items following any one of these words is not meant to be an exhaustive listing of such item or items or meant to be limited to only the listed item or items.

[0018] It must also be noted that, the singular forms a, an, and the include plural references unless the context clearly dictates otherwise. Although any methods similar or equivalent to those described herein can be used in the practice or testing of embodiments of the present disclosure, the exemplary methods are described. The disclosed embodiments are merely exemplary of the disclosure, which may be embodied in various forms.

[0019] In order to achieve the characteristics/properties of the free-flowing food grade SNI, the present subject matter discloses an improved process, wherein multiple process modifications are carried out based on process variables including, but not limited to, temperature adjustment, time, RPM speed of the stirrer, and adding an anticaking agent.

[0020] The improved process proposed herein resulted in obtaining the free-flowing food grade SNI with optimal values of the parameters including, but are not limited to, SNI purity, NaNO3, alkalinity as NaCO3, Chloride, Sulphate, loss on drying (LOD), max insoluble, heavy metal-sum of pb, As, cd, Pb, Hg the details of which are explained hereinafter as below.

[0021] Now referring to FIG. 1, a method (100) of obtaining a free-flowing food grade sodium nitrite is depicted, in accordance with an embodiment of the present subject matter, the method (100) comprises the following steps:

[0022] At step (101), a predefined amount of water may be charged in a reactor. In one embodiment, the water may be Potable water. Test results of the potable water is given in the below table No. 1:

TABLE-US-00001 TABLE 1 Test results of potable water Sr. Det. Method of No Test Name Unit Result Specification limit test 1 Description Clear colourless liquid containing suspended particles 2 Colour Hazen 1 Max.5 IS: 3025[part unit 4]-1983 3 Odour Agreeable Agreeable IS: 3025 [part 5]-1983 4 Taste Agreeable Agreeable IS: 3025[part- 7 & 8]-1984 5 Turbidity NTU 0 Max. 1 IS: 3025 [part 10]-1984 6 Total mg/l 114 Max. 500 IS: 3025 [part dissolved 16]-1984 solids 7 pH 7.25 6.5 to 8.5 IS: 3025 [part 11]-1983 8 Total mg/l 40.8 Max. 200 IS: 3025 [part hardness as 21]-1983 CaCO.sub.3 9 Calcium as mg/l 30.6 Max. 75 IS: 3025 [Part Ca 40]-1991 10 Chloride as mg/l 36.3 Max. 250 IS: 3025 C1 [Part-32]- 1988 11 Sulphate as mg/l 6.6 Max. 200 IS: 3025 SO4 [part-24]- 1986 12 Nitrate mg/l 2.40 Max. 45 IS: 3025[part- as 34]-1988 NO3 13 Total mg/l 51.0 Max. 200 IS: 3025 Alkalinity [part-23]- as Calcium 1983 carbonate 14 Magnesium mg/l 10.19 Max.30 IS: 3025 as Mg [Part-46]- 1994 15 Boron as B mg/l Not Max. 0.5 IS: 3025 detected [Part-57]- 2005 16 Copper mg/l Not Max. 0.05 IS: 3025 as detected [Part-42]- Cu 1992 17 Iron as Fe mg/l 0.02224 Max. 1 IS: 3025[part- 53]-2003 18 Manganese mg/l Not Max. 0.1 IS: 3025 as Mn detected [part-59]- 2006 19 Fluoride as mg/l Less than Max. 1.0 IS: 3025 [part- F 0.1 60]-2008 20 Phenolic mg/l Not Max. 0.001 IS: 3025 compound detected [part-43]- as C6H5OH 1992 21 Mercury as mg/l Not Max. 0.001 IS: 3025 [part- Hg detected 48]-1994 22 Cadmium as mg/l Not Max. 0.003 IS: 3025 Cd detected [part-41]- 1992 23 Selenium as mg/l Not Max. 0.01 IS: 3025 Se detected [Part-56]- 2003 24 Total mg/l Not Max. 0.01 IS: 3025 [part arsenic as detected 37]-1988 As 25 Barium as mg/l Not Max. 0.7 Annex F of Ba detected IS: 13428- 2003 26 Chloramines mg/l Not Max. 4.0 IS: 3025[part- as Cl2 detected 26]-1986 27 Sulphide as mg/l Less than Max. 0.05 IS: 3025 H2S 0.05 [part-29]- 1986 28 Molybdenum mg/l Not Max. 0.07 IS: 3025[part- as Mo detected 2]-2002 29 Nickel as Ni mg/l Not Max. 0.02 IS: 3025[part- detected 54]-2003 30 Silver as Ag mg/l Not Max. 0.1 Annex J of detected IS: 13428- 2003 31 Cyanide as mg/l Not Max 0.05 IS: 3025[Part- CN detected 27]-1986 32 Lead as Pb mg/l Not Max 0.01 IS: 3025 [Part- detected 47]-1994 33 Zinc as Zn mg/l Not Max. 5.0 IS: 3025 detected [Part-49]- 1994 34 Anionic mg/l Not Max. 0.2 Annex k of detergent as detected IS: 13428- MBAS 2003 35 Total mg/l Not Max. 0.05 IS: 3025 chromium detected [Part-52]- as Cr 2003 36 Mineral oil mg/l Not Max. 0.5 Clause 6 of detected IS: 3025 [part 39]-1989 infrared 37 Aluminum mg/l Not Max. 0.03 IS: 3025 [part as Al detected 55]-2003 38 Ammonia mg/l Not Max. 0.5 IS: 3025 [part (as total detected 3]-1988 ammonias N) 39 Residual mg/l Not Min. 0.2 IS: 3025 free detected [Part-26]- Chlorine as 1986 CL2 40 Polynuclear mg/l Not Max. 0.0001 APHA 6440 aromatic detected hydrocarbo ns as PAH 41 Poly mg/l Not Max. APHA 6630 chlorinated detected 0.0005 diphenyls 42 Trihalometh anes a Bromoform mg/l Not Max. 0.1 APHA 6232 detected b Dibromochl mg/l Not Max. 0.1 APHA 6232 oromethane detected c Bromodichloro- mg/l Not Max. 0.06 APHA 6232 methane detected d Chloroform mg/l Not Max. 0.2 APHA 6232 detected 43 Radioactive material a Alpha Bq/l Not Max. 0.1 IS14194 emitters detected b Beta Bq/l Not Max 1.0 IS14194 emitters detected 44 Pesticide residue i Alachlor ug/l Not Max 20 EPA 525.2 (ppb) detected ii Atrazine ug/l Not Max. 2 EPA 525.2 (ppb) detected iii Aldrin/ ug/l Not Max 0.03 EPA 508 dieldrin (ppb) detected iv -HCH ug/l Not Max 0.01 EPA 508 (ppb) detected v -HCH ug/l Not Max. 0.04 EPA 508 (ppb) detected vi Butachlor ug/l Not Max 125 EPA 525.2 (ppb) detected vii Chlorpyriphos ug/l Not Max 30 EPA 525.2 (ppb) detected viii -HCH ug/l Not Max 0.04 EPA 508 (ppb) detected ix 2,4-D ug/l Not Max 30 EPA 555 (ppb) detected (modified) x DDT ug/l Not Max 1 EPA 508 (ppb) detected a o, p, DDE ug/l Not (ppb) detected b o, p, DDD ug/l Not (ppb) detected c o, p, DDT ug/l Not (ppb) detected d p, p, DDE ug/l Not (ppb) detected e p, p, DDD ug/l Not (ppb) detected f p, p, DDT ug/l Not (ppb) detected xi Endosulfan ug/l(p Not Max. 0.4 EPA 508 pb) detected a - ug/l(p Not Endosulfan pb) detected b - ug/l(p Not Endosulfan pb) detected c Endosulfate ug/l(p Not pb) detected xii Ethion ug/l(p Not Max. 3 EPA 1657 pb) detected xiii Lindane (y- ug/l(p Not Max. 2 EPA 508 HCH) pb) detected xiv Isoproturon ug/l(p Not Max. 9 EPA 532 pb) detected xv Malathion ug/l(p Not Max. 190 EPA 8141A pb) detected xvi Methyl ug/l(p Not Max. 0.3 EPA 8141A parathion pb) detected xvii Monocrotophos ug/l(p Not Max. 1.0 EPA 8141A pb) detected xviii Phorate ug/l(p Not Max. 2 EPA 8141A pb) detected 45 E. Coli in 100 Absent Should be IS: 1622-1981 ml absent 46 Total in 100 Absent Should be IS: 1622-1981 Coliform ml absent count

[0023] At step (102), dry powder of sodium nitrite (SNI) having predefined purity may be added in the reactor under stirring conditions to obtain a SNI liquor of mass sodium nitrite. In one embodiment, the dry powder of sodium nitrate added in the reactor may be stirred at a predefined RPM and specifically designed agitator. In one embodiment, the predefined purity of the sodium nitrite is 99.0-99.9%. In one embodiment, the SNI liquor is 40-46% w/w/Min. In one exemplary embodiment, table 2 below depicts the characteristic/properties of the Sodium nitrite and water used to form the SNI liquor of mass sodium nitrite:

TABLE-US-00002 TABLE 2 characteristic/properties of the sodium nitrite and potable water No Details Quantity(gms) Purity 100% (MW) moles (MR) 1 Sodium 1140 99.1 1130 69 16.4 1.0 Nitrite (Dry Powder) 2 Potable 430 100 430 18 23.9 1.5 Water

[0024] At step (103), the SNI liquor of mass sodium nitrate may be heated at 40 C.-60 C. under stirring to completely dissolve the dry powder. The same is filtered using Whatman filter of 1-10 micron to remove the foreign particles including black particles. In case of commercial use, the filter may be a duplex cartridge filter with cartridge of 1-10 micron.

[0025] At step (104), the SNI liquor of mass sodium nitrite may be transferred to evaporator. In case of lab scale, the SNI liquor of mass sodium nitrite may be transferred to lab scale evaporator. In case of commercial, the SNI liquor of mass sodium nitrite may be transferred to a multi effect evaporator (MEE) or a simple evaporation system with any kind of crystallizer consisting of pre-heaters, calandria, Vapor liquid Separator (VLS), crystallizer, vacuum pump, condensers, salt settlers, and other heat exchangers) to obtain slurry mass of SNI having 30 to 40% free salt concentration.

[0026] At step (105), the slurry mass of SNI may be filtered through Whatman filter using Buckner funnel. In commercial batches, the filter may be a centrifuge with fine filtration basket or tub with cloth or without cloth. In one embodiment, the filtration step allows the impurities flow along with the ML and make cake to achieve the quality within the expected range at temperature within a range of 50 C.-65 C. to separate wet cake and Mother Liquor (ML). Further, the ML is kept separate in case of Lab process and in case of commercial batch, the ML goes back to an external SNI liquor of a SNI manufacturing system. The SNI manufacturing system may be external to system implemented for obtaining free flowing food grade SNI. This step makes this process unique in terms of not allowing the undesired impurities to concentrate by virtue of recycling. Further, the final product obtained by this step of filtration is free of these impurities and thereby makes the process capability robust.

[0027] At step (106), the wet cake may be dried using a drying unit at temperature 100 C.-140 C. continuously with cold zone operating at 25 C.-60 C. to obtain dry SNI material. In one embodiment, Loss on drying (LOD) may be below 0.2%. Further, in commercial case, wet cake material may be dried using VFBD dryer.

[0028] At step (107), the dry SNI material may be coated with a food grade additive in a blender to obtain free-flowing food grade sodium nitrite. In one embodiment, the food grade additive is silica. In commercial case, the blender is ribbon blender and in case of laboratory, small kind of blender is used. Further, in commercial case, the free-flowing food grade sodium nitrite may be packed in bags.

[0029] Further, the free-flowing food grade SNI may be analyzed in view of food grade SNI specification.

[0030] Now referring to Table 3, the specification of the free-flowing food grade sodium nitrite, is depicted. In one embodiment, the free-flowing food grade sodium nitrite may comprise 99.0-99.9% SNI purity, max 0.70% NaNO3, max 600 ppm alkalinity as NaCO3, max 50 ppm Chloride, max 50 ppm Sulphate, max 0.2% loss on drying, max 0.40% insoluble, max 10 ppm heavy metal-sum of pb, max 0.2 ppm As, max 1 ppm cd, max 1 ppm Pb, max 0.05 ppm Hg, 98.5% to 100.5% assay.

TABLE-US-00003 TABLE 3 specification of the free-flowing food grade sodium nitrite Sr. No Details Characteristics/properties 1 SNI - Purity % 99.0-99.9% 2 SNI-Appearance White or slightly yellowish crystalline powder 3 NaNo3% 0.70% Max 4 Alkalinity as Na2CO3 (ppm) 600 ppm Max 5 Chloride (ppm) 50 ppm Max 6 Sulphate (ppm) 50 ppm Max 7 Loss on drying % 0.2% Max 8 Insoluble 0.40% Max 9 Heavy Metal-Sum as Pb 10 ppm Max 10 As 0.2 ppm Max 11 Cd 1 ppm Max 12 Pb 1 ppm Max 13 Hg 0.05 ppm Max 14 SiO2 (Anticaking agent) 0.25-0.35% 15 Assay 98.5% to 100.5%

[0031] Now referring to Table 4 below, input and analysis parameters of few lots is depicted. Input parameter such as Quantity and analysis parameters such as sodium nitrite, Sodium nitrate, Alkalinity as Na2CO3 and chloride of plant SNI D-5 dry for lot No 1-5 are represented in the table 3.

TABLE-US-00004 TABLE 4 Input and analysis parameter of Lot no 1-5 Sr. Plant SNI Lot No. Lot No. Lot No. Lot No. Lot No. No D-5 dry Unit 1 2 3 4 5 1 Quantity Kg 20 10 4 10 4 Analysis 2 Sodium % 99.33 99.19 99.4 99.2 99.4 nitrite 3 Sodium 0.49 0.6 0.5 0.4 0.39 nitrate 4 Alkalinity as Ppm 283 333 922 1008 880 Na2CO3 5 Chloride Ppm 15 47.5 67 53 27

[0032] Now referring to Table 5, input and analysis parameters of few experiments are depicted. Input parameters such as SNI, potable water, distilled water, SNI wet cake, SNI dry, % recovery and analysis parameters such as sodium nitrate, Alkalinity as Na2CO3 and chloride of SNI for Exp no 1-5 are represented in Table 5.

TABLE-US-00005 TABLE 5 input and analysis parameters of Exp 1-5 Sr. Exp Exp Exp Exp Exp No Input Unit No. 1 No. 2 No. 3 No. 4 No. 5 1 SNI Gm 1140 1140 1140 1140 1140 2 Potable Gm 460 460 460 460 460 water 3 Distilled 0 0 0 0 0 water 4 SNI wet Gm 710 695 692 691 687 cake 5 SNI dry Gm 700 685 678 684 676 6 % recovery 61.4 60.1 59.5 60 59.3 Analysis 7 Sodium % 99.6 99.5 99.25 99.46 99.46 nitrite 8 Sodium % 0.49 0.6 0.5 0.4 0.39 Nitrate 9 Alkalinity Ppm 110 101 113 488 194 as Na2CO3 10 Chloride Ppm 30 15 13 16 13

[0033] Now referring to table 6, analysis parameters of SNI coating for Exp 1-5 are depicted. Based upon the analysis of parameters values obtained in Exp. No 1, Exp No. 2, Exp. No 3, Exp. No 4, and Exp No 5 represented in below table 6, it is observed that values of NaNO2 (Dry basis), NaNO3, Na2CO3, sulphate, chloride, LOD, insoluble are as per the desired specification of free-flowing food grade SNI.

TABLE-US-00006 TABLE 6 analysis parameters of SNI coating for Exp 1-5 Specification SNI coating of free-flowing Analysis food grade Exp Exp Exp Exp Exp No parameters SNI No. 1 No. 2 No. 3 No. 4 No. 5 1 NaNO2 (Dry 99.0% Min 99.15 99.08 99.1 99.05 99.03 basis) (%) 2 NaNO3 (%) 0.70% Max 0.16 0.032 0.0327 0.0325 0.15 3 Na2CO3 600 ppm Max 110 101 113 488 194 (ppm) 4 Sulphate 50 ppm Max 32 38 26 25 40.3 (ppm) 5 Chloride 50 ppm Max 30 15 13 16 13 (ppm) 6 LOD (%) 0.2% Max 0.2 0.18 0.19 0.12 0.2 7 Insoluble (%) 0.40% Max 0.29 0.32 0.4 0.35 0.31

[0034] Further, the parametric values such as tap density, untap density, ratio of tap/untap, angle of repose, sieve analysis of SNI coating of the table 6 are observed to be advantageous in obtaining free flowing food grade properties to SNI. Referring to FIGS. 2A-2E microscopic images of the free-flowing Sodium nitrate in accordance with Exp. no 1-5 are illustrated.

[0035] The brief experimental method followed is as per below:

[0036] The SNI technical grade having purity 99-0 to 99.9% is taken from the plant with defined lot. Its initial analysis is as per Table 5. This is dissolved in potable water and evaporated in a laboratory scale evaporator. The slurry is filtered, and the product is dried in specific conditions with addition of food grade additive (such as silica) and the product is analyzed and the results are as per Table 6.

[0037] Test-1: Purity Testing Method of Sodium Nitrite

[0038] In one embodiment, a purity of Sodium nitrite in Table 1 was tested using a following method:

[0039] An amount of 3.16 gm KMnO.sub.4 was dissolved in 100 ml D M water. The solution of KMnO.sub.4 were then digested over a hot plate for one hour. The KMnO.sub.4 solution was cooled filtered through Grade 4 sintered glass funnel without applying vacuum for 24 hours. After 24 hours KMnO.sub.4 solution was diluted 1000 ml by demineralized water (DM) water. The solution was standardized same for exact normality of 0.1N. An accurately about 1.0 gm dry sodium nitrite test sample (2.0 to 3.0 gm for liquid) was taken and diluted to 250 ml volumetric flask by Dist. water. A 20 ml of 0.1 N KMnO.sub.4 were taken in solutions in 250 ml beaker and 5 ml of concentrated H.sub.2SO.sub.4 in 50 ml Dist. Water were added. The temperature was maintained to about 40 C. and titration was performed by NaNO.sub.2 solution from Burette, keeping the tip of the burette under the surface of KMnO.sub.4 solution with continuous stirring. NaNO.sub.2 solution were added very slowly. The end point was observed as pink to colourless, and the Burette reading (BR) was noted to obtain results in the Table. 1.

[0040] % of sodium nitrite in the dry of sodium nitrite test sample was calculated as below:

[00001]$\%w/w=\frac{\mathrm{Normality}\mathrm{of}\mathrm{KMnO}434.510025020}{\mathrm{Gram}\mathrm{sample}1000B.R.}$

[0041] Test-2: Loss on Drying (LOD) of Sodium Nitrite

[0042] In one embodiment, an amount of loss on drying of all forms Sodium nitrite in Table 1 was tested using a Mettler Toledo Halogen Moisture Analyzer Model-HG-53 and by following method:

[0043] Following protocol was followed to test the LOD: Start the instrument, pre-heat the empty aluminium pan (foil) at temp+/100 C. for five minutes. Then take the quantity mansion in bellow table. Set the temperature & time as mentioned in below table. Press Start key and observe the final reading directly as % loss on drying.

TABLE-US-00007 Sample Time Sample quantity Temp C. +/ 2 C. Minutes NaNO.sub.2 samples 5 gm 110 10 of Table 1

[0044] Test-3: Alkalinity by Content of Na2CO3 Impurity in the Forms of SNI

[0045] In one embodiment, an alkalinity content of all forms Sodium nitrite in Table 1 was tested using a following method: [0046] (a) Reagents used: 0.1 N H.sub.2SO.sub.4 Solution; 0.1 N H.sub.2SO.sub.4 is prepared by mixing 2.82 ml. of pure Sulphuric acid in water and dilute to 1000 ml by distilled water, standardize it. [0047] (b) 0.1% w/v Phenolphthalein indicator solution: Dissolve 0.1 gm of Phenolphthalein powder in 80 ml of 95% methanol and finally dilute to 100 ml with distilled water.

[0048] Protocol Followed:

[0049] Weigh accurately nearest to 25 gm of sample and transfer it to 250 ml conical flask. Add 50 ml of distilled water and boil it for five minutes, cool it, and add 4 to 5 drops of Phenolphthalein Indicator. Titrate against 0.1 N Sulphuric acid till pink colour to colourless end point. Note the burette reading (BR).

[0050] % Of content of Na2CO3 impurity in the forms of SNI in the dry of sodium nitrite test sample was calculated as below:

[00002]$\%w/w\mathrm{alkalinity}\mathrm{as}\mathrm{sodium}\mathrm{carbonate}-\frac{BR2\mathrm{Normality}\mathrm{of}H2\mathrm{SO}453100}{\mathrm{Gram}\mathrm{sample}1000}$

[0051] Test-4: Impurity Content of Chloride as Cl

[0052] In one embodiment, a chloride content of all forms Sodium nitrite in Table 1 was tested using a following method:

[0053] Reagents Used: [0054] (a) Nitric acid pure (70% w/w) [0055] (b) Standard Silver Nitrate solution0.1 N: Dissolve 17 gm Silver Nitrate pure in DM water and dilute to 1000 ml in volumetric flask and standardise it. [0056] (c) Nitrobenzene pure [0057] (d) Standard Ammonium thiocyanate solution0.1 N: Dissolve of 7.6 gm Ammonium thiocyanate pure in 400 ml of DM water and dilute to 1000 ml in volumetric flask and standardize it. [0058] (e) Ferric Ammonium Sulphate indicator saturated solution: Dissolve Ferric Ammonium Sulphate pure in DM water up to saturated solution.

[0059] Protocol Followed:

[0060] Weigh accurately nearest to 10 gm of sample (Suitable quantity) in 250 ml conical flask. Add about suitable quantity of Nitric acid depending as product to be analysis till removal of Nitrous gas. Add 10 ml of 0.1 N Silver Nitrate solutions. Add 5.0 ml Nitrobenzene and shake vigorously. Titrate it against 0.1 N Ammonium Thiocyanate solutions, using 1 ml Ferric Ammonium Sulphate indicator solution. Note the burette reading (BR). End point will be faint brown in colour.

[0061] % Of content of Chloride (Cl) impurity in the forms of SNI in the dry of sodium nitrite test sample was calculated as below:

[00003]$\%w/w\mathrm{alkalinity}\mathrm{as}\mathrm{Chloride}\mathrm{as}CI=\frac{35.5\left[\left(N\mathrm{of}\mathrm{AgNO}310\right)-\left(BRN\mathrm{of}\mathrm{NH}4\mathrm{SCN}\right)\right]100}{\mathrm{Gram}\mathrm{sample}1000}$

[0062] Test-5: Impurity Content of Heavy Metal as Pb

[0063] In one embodiment, an impurity content of heavy metal Pb of all forms Sodium nitrite in Table 1 was tested using a following method:

[0064] Reagents Used: [0065] (a) Concentrated Hydrochloric acid pure (30% w/w) [0066] (b) Nitric Acid pure (70% w/w) [0067] (c) Standard lead solution (1 ml=0.01 mg): Dissolve 1.600 gm Lead Nitrate pure in water and 1 ml of concentrated Nitric acid and make the volume up to 1000 ml mark by D M water. Transfer exactly 10 ml of this solution to a 1000 ml volumetric flask, again dilute with D M water and make up the volume to 1000 ml mark. 1 ml of this solution is equivalent to 0.01 mg of Lead (Pb) [0068] (d) 6% w/v Dilute Acetic acid solution: Take 6 ml, acetic acid and dilute it to 100 ml by D M water in volumetric flask. [0069] (e) Hydrogen Sulphide solution: Prepare fresh solution using concentrated Hydrochloric acid and Iron pyrites (Ferrous Sulphide).

[0070] Protocol Followed:

[0071] Take 10 gm sample (Suitable quantity) in glass dish add 25 ml D M water, dissolve it, add 25 ml concentrated hydrochloric acid and evaporate to dryness on water-bath until the odor of hydrochloric acid is no longer perceptible. Dissolve the residue in 30 ml DM water; transfer it to 100 ml Nessler cylinder. If solution is dark/black, then solution pass through activated carbon (Charcoal powder) & collect the clear colorless solution. In this clear color solution, add 2 ml dil. Acetic acid & pass H2S gas for 1 minutes & dilute 50 ml mark See the dark colour and compare it with standard colour of Lead.

[0072] Standard Lead Colour: Take 10 ml, 20 ml & 50 ml of 1 ml=0.01 mg Lead standard solution in different 100 ml Nessler cylinders, add 2 ml dilute acetic acid, add 10 ml Hydrogen Sulfide solution, or pass H2S gas dilute to 50 ml mark. See the dark colour and compare with above dark colour of sample solution. If sample colour is less than the std colour then sample is passing.

[0073] % Of content of Lead as Pb impurity in the forms of SNI in the dry of sodium nitrite test sample was calculated as below:

[00004]$\mathrm{Lead}\mathrm{as}\mathrm{Pb}w/w\mathrm{ppm}=\frac{BR0.011000}{\mathrm{gm}\mathrm{sample}}$

[0074] Now referring to FIG. 3, process flow diagram (PFD) depicting an interaction between various components for obtaining a free-flowing food grade sodium nitrite is illustrated, in accordance with an embodiment of the present subject matter.

[0075] In one embodiment, the dry powder of SNI is poured into a SNI powder hopper (302). The SNI powder hopper (302) is configured to add dry powder of SNI having 99.0-99.9% purity in the under stirring conditions in the reactor such as dissolution tank (301). The reactor comprises the predefined amount of the charged water. Further, SNI liquor of mass sodium nitrite may be heated at 40 C.-60 C. under stirring to completely dissolve the dry powder. The SNI liquor of mass sodium nitrite may be transferred to storage tank (304) through filters (303) in order to avoid any kind of foreign materials like black particles and other particulates to the tune of 1-4 micron. The SNI liquor of mass sodium nitrite is fed to MEE to concentrate liquor to obtain slurry mass of SNI having 30 to 40% free salt concentration. The slurry mass of SNI is filtered through centrifuge at the temperature within the range of 50 C.-65 C. to separate wet cake and mother liquor (ML), wherein filtration allows the impurities flow along with the ML. The ML is collected in the ML tank (308). The ML goes to an external SNI liquor of a SNI manufacturing system. Further, the wet cake is dried using VFBD (315) at a temperature within the range of 100 C.-140 C. continuously with cold zone operating at 25 C.-60 C. to obtain dry SNI material. More specifically, dried SNI material is transferred to the cyclone tank (312) for centrifuge separation to separate undersized particles. The undersized particles are transferred into an undersized product hopper (318). The dry SNI material is coated with a food grade additive in the blender (316) to obtain free-flowing food grade sodium nitrite. The free-flowing food grade SNI is collected in the product hopper (317).

[0076] In one embodiment, sample of free-flowing Food grade Sodium Nitrate is examined using European Pharmacopeia 7.0 (EP 7.0).

[0077] Test 1Identification

[0078] In one embodiment, identification of Sodium nitrite was tested using a following method: [0079] Step 1: Dilute 2.5 gms sample to small qty. of distilled water (or CO2 free water), make up to 50 mls of solution A (hereafter referred as Solution S1). [0080] Step 2: Dilute 1 ml of solution A to 25 ml with water to prepare Solution B. [0081] Step 3: Add 0.1 ml of the solution B into 1 ml of sulphonic acid solution, wherein sulphonic acid solution is prepared by mixing 0.5 g of sulphanilic acid, 30 ml of glacial acetic acid and 120 ml of water; heating with stirring until dissolved and further allowed to cool and filter. [0082] Step 4: Allow to stand for 2-3 min. [0083] Step 5: 1 ml of b-naphthol solution R and 1 ml of dilute sodium hydroxide solution.

[0084] An intense red colour developed which is indicative of the sample passing of the test.

[0085] Test 2: Appearance of Solution

[0086] It is observed that solution S1 is clear.

[0087] Test 3: Acidity or Alkalinity

[0088] In one embodiment, acidity or alkalinity of the free-flowing SNI was tested using following method:

[0089] Add 0.05 ml of phenol red solution into 10 ml of solution S1. Add 0.1 ml of 0.01 M sodium hydroxide. The solution is red.

[0090] Add 0.3 ml of 0.01 M hydrochloric acid. The solution is yellow and the test for acidity and alkalinity is passed.

[0091] Test 4: Chloride

[0092] In one embodiment, an amount of Chloride in the free-flowing SNI was tested using following method:

[0093] Dissolve 3 g sample in distilled water. Continuously add 10 ml of Nitric acid and evaporate to dryness. Dissolve the residue in 10 ml of distilled water R, neutralize with sodium hydroxide solution and dilute to 30 ml with distilled water which is solution S2 [0094] Step 1: Dilute 10 ml of solution S2 to 15 ml with water. The solution complies with the limit test for chlorides. [0095] Step 2: Add 1 ml of dilute nitric acid R into 15 ml of the prescribed solution of step 1. [0096] Step 3: Pour the mixture as a single addition into test tube containing 1 ml of silver nitrate solution R2. [0097] Step 4: Prepare a standard in the same manner using 10 ml of chloride standard solution (5 ppm) R and 5 ml of water R. [0098] Step 5: Examine the tubes laterally against a black background.

[0099] Result of this test indicates an amount of Chloride is less than 50 ppm in free-flow SNI. This result complies with the standard specification of sulphate in food grade SNI which is maximum 50 ppm.

[0100] Test 5: Sulphates

[0101] In one embodiment, amount of sulphates in the free-flowing SNI was tested using following method: [0102] Step 1: Dilute 7.5 ml of solution S2 to 15 ml with distilled water R. The solution complies with the limit test for sulphates. [0103] Step 2: Add 3 ml of a 250 g/l sodium of barium chloride R to 4.5 ml of sulphate standard solution (10 ppm SO.sub.4) R1. Shake and allow to stand for 1 min. [0104] Step 3: Add 15 ml of the solution to 2.5 ml of this solution and 0.5 ml of acetic acid R. [0105] Step 4: Prepare a standard in the same manner using 15 ml of sulphate standard solution (10 ppm SO.sub.4) R instead of the solution to be examined. [0106] Step 5: After 5 min, any opalescence in the test solution is not more intense than that in the standard.

[0107] Result of this test indicates an amount of sulphate is less than 100 ppm in free-flow SNI. This result complies with the standard specification of sulphate in food grade SNI which is maximum 200 ppm.

[0108] Test 6: Heavy Metals (pb)

[0109] In one embodiment, amount of heavy metals (pb) in the free-flowing SNI was tested using following method: [0110] Step 1: Dissolve 1 g in 6 mL of 3 N hydrochloric acid and evaporate on a steam bath to dryness. [0111] Step 2: Reduce the residue to a course powder and continue heating on the steam bath until the odour of hydrochloric acid no longer is perceptible. [0112] Step 3: Dissolve the residue in 23 ml of water and add 2 mL of 1N acetic acid: compare with std. 10 ppm solution with above process.

[0113] Result of this test indicates the amount of heavy metal is less than 1 ppm in the free-flow SNI. The result complies with the standard specification of heavy metals (pb) in food grade SNI which is maximum 20 mg/kg.

[0114] Test 7: Loss on Drying

[0115] In one embodiment, Loss on drying in the free-flowing SNI was tested using following method:

[0116] Food grade SNI is dried over silica gel for 4 hours. It loses not more than 1% of its weight i. e. 0.066.

[0117] Test 8: Assay

[0118] In one embodiment, assay in the free-flowing SNI was tested using following method: [0119] Step 1: Dissolve 0.400 g in 100.0 ml of water R. [0120] Step 2: Introduce 20.0 ml of the solution into a conical flask containing 30.0 ml of 0.1 M cerium sulphate, while stirring continuously and keeping the tip of the pipette below the surface of the liquid. [0121] Step 3: Immediately stop the flask and allow to stand for 2 min. [0122] Step 4: Add 10 ml of 200 g/l solution of potassium iodide R and 2 ml of starch solution R.

[0123] While stiffing continuously, titrate with 0.1 M Sodium Thiosulphate until the blue colour disappears. Carry out a blank titration. 1 ml of 0.1 M Cerium Sulphate is equivalent to 3.45 mg of NaNO.sub.2.

[0124] Result of this test indicates the amount of assay is 99.16% (Dry basis) in the free-flow SNI. The result complies with the standard specification of assay in food grade SNI which is 98.5% to 100.5% (dried substance).

[0125] In another embodiment, sample of free-flowing Food grade Sodium Nitrate is examined using USP-29.

[0126] Test 1Identification

[0127] In one embodiment, identification of Sodium nitrite was tested using a following method: [0128] Step 1: Dilute 2.5 gms sample of distilled water, make up to 50 mls of solution A. [0129] Step 2: Dilute 1 ml of solution A to 25 ml with water to prepare solution B. [0130] Step 3: Add 0.1 ml of the solution B 1 ml of sulphonic acid solution. Sulphanilic Acid Solution is prepared by mixing 0.5 g of sulphanilic acid, 30 ml of glacial acetic acid and 120 ml of water and heat with stirring until dissolved and allowed to cool and filter. [0131] Step 4: Allow to stand for 2-3 min. [0132] Step 5: Add 1 ml of b-naphthol solution R and 1 ml of dilute sodium hydroxide solution R.

[0133] An intense red colour is developed which is indicative of the sample passing of the test.

[0134] Test 2: Loss on Drying

[0135] In one embodiment, Loss on drying in the free-flowing SNI was tested using following method:

[0136] Food grade SNI is dried over silica gel for 4 hours. It loses not more than 0.25% of its weight i. e. 0.083.

[0137] Test 3: Heavy Metals (pb) [0138] Step 1: Dissolve 1 g in 6 mL of 3 N hydrochloric acid and evaporate on a steam bath to dryness. [0139] Step 2: Reduce the residue to a course powder and continue heating on the steam bath until the odor of hydrochloric acid no longer is perceptible. [0140] Step 3: Dissolve the residue in 23 mL of water and add 2 mL of 1 N acetic acid: Compare with std. 10 ppm solution with above process.

[0141] Result of this test indicates the amount of heavy metal is less than 0.0001 in the free-flow SNI. The result complies with the standard specification of heavy metal in food grade SNI which is maximum 0.0020%.

[0142] Test 4: Assay [0143] Step 1: Dissolve about 1 g of Sodium Nitrite, accurately weighed, in water to make 100.0 mls. [0144] Step 2: Pipette 10 mL of the Sodium Nitrite solution into a mixture of 50.0 mL of 0.1 N potassium permanganate VS, 100 mL of water, and 5 mL of sulfuric acid. When adding the Sodium Nitrite solution, immerse the tip of the pipette beneath the surface of the permanganate mixture. [0145] Step 3: Warm the liquid to 40, allow it to stand for 5 minutes, and add 25.0 mL of 0.1 N oxalic acid VS. [0146] Step 4: Heat the mixture to about 80, and titrate with 0.1 N potassium permanganate VS. Each mL of 0.1 N potassium permanganate is equivalent to 3.450 mg of NaNO2.

[0147] Result of this test indicates the amount of assay is 99.03% (Dry basis) in the free-flow SNI. The result complies with the standard specification of assay in food grade SNI which is 97% to 101% (dried substance).

[0148] In accordance with embodiments of the present disclosure, a method for obtaining of free-flowing food grade sodium nitrite described above may have following advantages including but not limited to: [0149] The moisture content of the free-flowing food grade sodium nitrite may not be greater than 0.2%. [0150] The store shelf life of the free-flowing food grade SNI may be improved.

[0151] Various modifications to the embodiment will be readily apparent to those skilled in the art and the generic principles herein may be applied to other embodiments. However, one of ordinary skill in the art will readily recognize that the present disclosure is not intended to be limited to the embodiments illustrated but is to be accorded the widest scope consistent with the principles and features described herein.

[0152] The embodiments, examples and alternatives of the preceding paragraphs, the description, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments unless such features are incompatible.

[0153] The foregoing description shall be interpreted as illustrative and not in any limiting sense. A person of ordinary skill in the art would understand that certain modifications could come within the scope of this disclosure. The embodiments, examples and alternatives of the preceding paragraphs or the description and drawings, including any of their various aspects or respective individual features, may be taken independently or in any combination. Features described in connection with one embodiment are applicable to all embodiments, unless such features are incompatible.