Working with ACS specified products. Merck validates the»gr for Analysis«reagent range according to actual ACS standards

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Transcription:

Working with ACS specified products Merck validates the»gr for Analysis«reagent range according to actual ACS standards

Monitoring the quality of our reagents, we follow the specifications of the monographs published in Reagent Chemicals from the American Chemical Society (ACS). As our customers know, Merck has a Dr. Dietmar Oeter, Head of Quality Control at Merck Darmstadt:»Validating the range of»gr for Analysis«products were very extensive. But now we are sure to meet our customers needs.«special regard concerning quality and reliability of its products. We take an in-depth approach to the ACS specifications, comparing them with our own in-house requirements. Consequently, we verify a range of the most representative reagents. The result is no surprise: In most cases, our state-of-the-art For more information about the 9th edition of ACS source book please refer to»http://pubs.acs.org«. analytical methods verify that»gr for Analysis«grade chemicals meet or exceed the ACS requirements in the last edition of»reagent Chemicals«. 2

Most of our reagent chemicals meet the ACS specifications almost all out perform ACS Sometimes, in our opinion, the ACS specifications are limited in scope. Thus, we analyse additional parameters than required by ACS. In addition to these specifications Merck follows their own quality standards resulting from more than 300 years of experience as a global producer of lab chemicals. Other parameters not requested by ACS are tested according to the Specifications of the European based»international Organization for Standardization«(ISO). Our Validation plan for ACS reagents has been carried out according to the very strict validation instructions for pharmaceutical starting materials (e.g. according to USP and ICH Q2A Guideline for Industry, Text on Validation of Analytical Procedures (1995)). Validation plan Assay Anions* with Total Nitrogen ion chromatography (N) Comparison of methods yes yes yes Trueness yes no yes Repeatability yes yes yes Specificity yes yes yes Linearity yes yes yes Limit of determination no yes yes Limit of detection no yes yes Ruggedness yes no yes Example Sodium chloride: * Anions: Bromide (Br), Chlorate and Nitrate (as NO 3 ), Iodide (I), Phosphate (PO 4 ), Sulfate (SO 4 ). Dr. Matthias Ohm and Dr. Kerstin Reider, Quality control managers at Merck, Germany:»In our labs we are working with absolutely stateof-the-art technology.«

Chuck Wilson, Quality Control Manager at EMD Chemicals Inc., USA:»Analysts may apply alternative methods of analysis but, these methods must be validated to assure that they produce results of at least equal reliability.«we know what the ACS Reagent Committee requires Last but not least, because one of our quality control managers, Chuck Wilson, has been a member of the ACS Committee on Analytical Reagents since 1988. Chuck has been with our subsidiary in the US since 1972 and Merck is proud that he is part of the team that»wrote the book«on analytical reagents. Our analytical specialists have valid reasons for using alternative methods There are some scientifically sound reasons to use an alternative method over an ACS monograph. Some analytical methods result in precisely quantified values not only a comparison to limiting values. In order to get more meaningful and precise results, Merck applies our own in-house methods with our quality control procedures. These leading-edge technologies are, for example, anion chromatography, photometry for ammonium determination vs. wet chemical comparison to a reference solution. This is our enduring commitment to the state-of-the-art standards of service and quality. Birgit Sauerbrey, Laboratory assistant at Merck, Germany:»Merck s products are tested to meet our customer s requirements. We perform analyses on every batch so the customer receives effective analysed data every time.«

Example: Validating sodium chloride [Item 1.06404] Parameter Specification ACS Specification Merck Method Merck vs. ACS Analytical method ACS Analytical method Merck Assay 99.0 % 99.5 % validated argentometric titration argentometric titration (visual indication) (potentiometer indication) ph-value (5 %, water) 5.0 9.0 5.0 8.0 follows ACS ph potentiometry ph potentiometry Water insoluble substances max. 0.005 % 0.005 % follows ACS gravimetric gravimetric Bromide (Br) max. 0.01 % 0.005 % validated anion chromatography Chlorate and Nitrate (as NO 3 ) max. 0.003 % 0.003 % validated and photometry anion chromatography Hexacyanoferrate [Fe(CN) 6 ] [no specification] 0.0001 % follows ISO Iodide (I) max. 0.002 % 0.001 % validated anion chromatography Phosphate (PO 4 ) max. 0.0005 % 0.0005 % validated colorimetry anion chromatography (direct molybdenum blue) Sulfate (SO 4 ) max. 0.004 % 0.001 % validated anion chromatography Total Nitrogen (N) max. 0.001 % 0.0005 % validated Kjeldahl Kjeldahl (comparison of limiting values) (effective) Heavy metals (as Pb) max. 0.0005 % 0.0005 % follows ACS As (Arsenic) [no specification] 0.00004 % In-house Ba (Barium) passes test passes test follows ACS Ba (Barium) [no specification] 0.001 % follows ISO Ca (Calcium) max. 0.002 % 0.002 % follows ACS flame AAS flame AAS Cu (Copper) [no specification] 0.0002 % In-house pulse polarography Fe (Iron) max. 0.0002 % 0.0001 % follows ACS K (Potassium) max. 0.005 % 0.005 % follows ACS flame AAS flame AAS Mg (Magnesium) max. 0.001 % 0.001 % follows ACS flame AAS flame AAS Ca, Mg und Me 2 O 3 -precipitate [no specification] 0.005 % In-house gravimetric method Sodium Chloride as an example shows, that a Merck product combines perfectly ACS, ISO and other important parameters. In summary you can fully rely on a Merck»GR for Analysis«graded product. 5

The»Merck GR for Analysis ACS range«: Our synonym for products of guaranteed purity Following Good Laboratory Practice (GLP) or other quality systems is now easier than before. Merck s»gr for Analysis«reagents meet ACS quality specifications ensuring the reliability, availability, convenience, packaging versatility and quality our customers need. Dr. Konrad Beckenkamp, Head of Quality Control at Merck, Germany:»Validated»GR for Analysis«products meet all requirements of demanding and critical customers.«6

ACS Products Designation Package size Cat. No.* Acetic acid (glacial) 100 % 2,5 l 1.00063.2500 Acetic anhydride 2,5 l 1.00042.2500 Acetone 2,5 l 1.00014.2500 Acetonitrile 2,5 l 1.00003.2500 Aluminium potassium sulfate dodecahydrate 1 kg 1.01047.1000 Ammonia Solution 28 30% 1 l 1.05423.1000 Ammonium acetate 1 kg 1.01116.1000 Ammonium amidosulfonate (for detection of sulfonamide in blood) 100 g 1.01220.0100 Ammonium bromide 1 kg 1.01125.1000 Ammonium carbonate 250 g 1.59504.0250 Ammonium cerium(iv) nitrate 1 kg 1.02276.1000 Ammonium chloride 1 kg 1.01145.1000 Ammonium dihydrogen phosphate 500 g 1.01126.0500 Ammonium fluoride 250 g 1.01164.0250 Ammonium heptamolybdate tetrahydrate 1 kg 1.01182.1000 di-ammonium hydrogen citrate 500 g 1.01154.0500 di-ammonium hydrogen phosphate 500 g 1.01207.0500 Ammonium iodide 250 g 1.01173.0250 Ammonium iron(iii) sulfate dodecahydrate 1 kg 1.03776.1000 Ammonium nitrate 1 kg 1.01188.1000 di-ammonium oxalate monohydrate 250 g 1.01192.0250 Ammonium peroxodisulfate 1 kg 1.01201.1000 Ammonium sulfate 1 kg 1.01217.1000 Ammonium thiocyanate 500 g 1.01213.0500 Anthrone 10 g 1.01468.0010 Aurin tricarboxylic acid ammonium salt (reagent for aluminium) 25 g 1.00128.0025 Barium acetate 500 g 1.01704.0500 Barium carbonate 1 kg 1.01714.1000 Barium chloride dihydrate 1 kg 1.01719.1000 Barium hydroxide octahydrate 500 g 1.01737.0500 Barium nitrate 500 g 1.01729.0500 Benzene 2,5 l 1.01783.2500 Benzoic acid 100 g 1.00136.0100 Boric acid 1 l 1.00165.0100 Bromine 250 g 1.01948.0250 Bromocresol green (indicator) 25 g 1.08121.0025 Bromophenol blue (indicator ph 3.0 4.6) 25 g 1.08122.0025 Bromophenol blue sodium salt (water-soluble indicator) 5 g 1.11746.0005 Bromothymol blue (indicator) 25 g 1.03026.0025 Bromthymol blue sodium salt (water-soluble indicator) 10 g 1.01895.0010 1-Butanol 2,5 l 1.01990.2500 tert-butanol 5 l 1.09629.5000 Cadmium sulfate hydrate 100 g 1.02027.0100 Calcium chloride dihydrate 1 kg 1.02382.1000 Calcium hydroxide 1 kg 1.02047.1000 * for further packsizes see the Merck Reagents Catalogue, ChemDAT the Merck Chemical Database on CD-ROM or ChemDAT -online on Internet under www.merck.de 7

ACS Products Designation Package size Cat. No.* Calcium nitrate tetrahydrate 500 g 1.02121.0500 Carbon disulfide 1 l 1.02214.1000 Chloramin T 250 g 1.02426.0250 Chloroform 2,5 l 1.02445.2500 Chromium(III) potassium sulfate dodecahydrate 250 g 1.01036.0250 Citric acid monohydrate 1 kg 1.00244.2500 Cobalt(II) chloride hexahydrate 250 g 1.02539.0250 Cobalt(II) nitrate hexahydrate 250 g 1.02554.0250 Copper oxide (wire about 0.65 x 6 mm for elementary analysis, surface: CuO, core: Cu 2 O) 250 g 1.02767.0250 Copper oxide (wire fine about 0.65 x 3 mm for elementary analysis) 250 g 1.02765.0250 Copper(I) chloride 250 g 1.02739.0250 Copper(II) chloride dihydrate 1 kg 1.02733.1000 Copper(II) sulfate pentahydrate 1 kg 1.02790.1000 Cupferron 100 g 1.05227.0100 Cyclohexane 2,5 l 1.09666.2500 1,2-Dichlorethane 500 ml 1.59695.0500 2,7 -Dichlorfluorescein 5 g 1.09676.0005 Dichloromethane 2,5 l 1.06050.2500 Diethyl ether 1 l 1.00921.1000 Diisopropyl ether 2,5 l 1.00867.2500 4-(Dimethylamino)benzaldehyde 100 g 1.03058.0100 N,N-Dimethylformamide 2,5 l 1.03053.2500 Dimethylglyoxime (reagent for nickel) 100 g 1.03062.0100 Dimethyl sulfoxide 1 l 1.02952.1000 1,4-Dioxan 2,5 l 1.09671.2500 Diphenylamine 100 g 1.03086.0100 1,5-Diphenylcarbazide 25 g 1.03091.0025 1,5-Diphenylcarbazone 5 g 1.03087.0005 Erichrom black T 25 g 1.03170.0025 Ethanol 2,5 l 1.00983.2500 Ethyl acetate 2,5 l 1.09623.2500 Ethyl methyl ketone 2,5 l 1.09708.2500 Ethylene glycol monomethyl ether 2,5 l 1.00859.2500 Formaldehyde solution min. 37 % (stabilized with about 10 % methanol) 1 l 1.04003.1000 Formamide 2,5 l 1.09684.2500 Formic acid 89 91 % 1 l 1.00253.1000 Formic acid 98-100 % 2,5 l 1.00264.2500 Fufural 100 g 1.04013.0100 Glycerol 2,5 l 1.04092.2500 n-hexane 2,5 l 1.04367.2500 n-hexane 2,5 l 1.04374.2500 Hydrazinium sulfate 100 g 1.04603.0100 Hydrochloric acid fuming 37% 2,5 l 1.00317.2500 Hydrofluoric acid 48% 500 ml 1.00343.0500 Hydroxylammonium chloride 250 g 1.04616.0250 Hydroxylammonium chloride (0.000001% Hg) 250 g 1.04619.0250 8

ACS Products Designation Package size Cat. No.* 8-Hydroxyquinoline 250 g 1.07098.0250 Imidazole (buffer substance) 250 g 1.04716.0250 Iodic acid 100 g 1.00357.0100 Iodine (resublimed) 500 g 1.04761.0500 Iron(II) sulfate heptahydrate 1 kg 1.03965.1000 Iron(III) chloride hexahydrate 1 kg 1.03943.1000 Iron(III) nitrate nonahydrate 1 kg 1.03883.1000 Isoamyl alcohol 2,5 l 1.00979.2500 Isobutanol 1 l 1.00984.1000 Isobutyl methyl ketone (for extraction analysis) 2,5 l 1.06146.2500 Isooctane 2,5 l 1.04727.2500 Lead(II) acetate trihydrate 1 kg 1.07375.1000 Lead(II) carbonate 250 g 1.07381.0250 Lead(II) hydroxide acetate (anhydrous, for the analysis of sugar acc. to Horne) 1 kg 1.07414.1000 Lead(II) nitrate 1 kg 1.07398.1000 Lithium carbonate 250 g 1.05680.0250 Lithium chloride 250 g 1.05679.0250 Lithium sulfate monohydrate 250 g 1.05694.0250 Magnesium acetate tetrahydrate 1 kg 1.05819.1000 Magnesium chloride hexahydrate 1 kg 1.05833.1000 Magnesium nitrate hexahydrate 500 g 1.05853.0500 Magnesium oxide 500 g 1.05866.0500 Magnesium sulfate heptahydrate 1 kg 1.05886.1000 Manganese(II) chloride tetrahydrate 1 kg 1.05927.1000 Manganese(II) sulfate monohydrate (spray-dried) 250 g 1.05941.0250 Mercury(II) acetate 250 g 1.04410.0250 Mercury(II) bromide 50 g 1.04421.0050 Mercury(II) chloride 250 g 1.04419.0250 Mercury(II) iodide (red) 250 g 1.04428.0250 Mercury(II) nitrate monohydrate 50 g 1.04439.0050 Mercury(II) sulfate 250 g 1.04480.0250 Methanol 2,5 l 1.06009.2500 Methyl orange (C.I.13025, indicator) 25 g 1.01322.0025 Methyl red (C.I. 13020, indicator) 25 g 1.06076.0025 Molybdatophosphoric acid hydrate 100 g 1.00532.0100 Murexide (ammonium purpurate, metal indicator) 25 g 1.06161.0025 Ninhydrin 100 g 1.06762.0100 Nitric acid fuming 100 % 1 l 1.00455.1000 Nitric acid 69% 2.5 l 1.01799.2500 Oxalic acid dihydrate 1 kg 1.00495.1000 Perchloric acid 60 % 2,5 l 1.00518.2500 Perchloric acid 70 72 % 2,5 l 1.00519.2500 Perchloric acid 70 % (max. 0,000005% Hg) 1 l 1.00514.1000 Petroleum benzine (boiling range 40 60 C) 2,5 l 1.01775.2500 Phenol 1 kg 1.00206.1000 Phenol red (indicator) 25 g 1.07241.0025 Phenol red sodium salt (indicator) 5 g 1.11748.0005 9

ACS Products Designation Package size Cat. No.* Phenolphthalein (indicator) 25 g 1.07233.0025 Ortho-Phosphoric acid 85% 1 l 1.00573.1000 di-phosphorus pentoxide 500 g 1.00570.0500 Potassium bromate 250 g 1.04912.0250 Potassium bromide 500 g 1.04905.0500 Potassium carbonate 1 kg 1.04928.1000 Potassium chloride 500 g 1.04933.0500 Potassium chromate 1 kg 1.04952.1000 Potassium cyanide 1 kg 1.04967.1000 Potassium dichromate 500 g 1.04864.0500 Potassium dichromate (max. 0.000001% Hg) 500 g 1.04865.0500 Potassium dihydrogen phosphate 1 kg 1.04877.1000 Potassium disulfate (Potassium pyrosulfate) 1 kg 1.05107.1000 Potassium hexacyanoferrate(ii) trihydrate 500 g 1.04984.0500 Potassium hexacyanoferrate(iii) 1 kg 1.04973.1000 Potassium hydroxide pellets (max. 0.002% Na) 1 kg 1.05021.1000 Potassium hydroxide pellets (max. 0.05% Na) 1 kg 1.05029.1000 Potassium iodate 500 g 1.05051.0500 di-potassium oxalate monohydrate 1 kg 1.05073.1000 Potassium perchlorate 1 kg 1.05076.1000 Potassium permanganate 1 kg 1.05082.1000 Potassium permanganate (max. 0.000005% Hg) 1 kg 1.05084.1000 Potassium peroxodisulfate 250 g 1.05092.0250 Potassium sodium tartrate tetrahydrate 1 kg 1.08087.1000 Potassium sulfate 1 kg 1.05153.1000 Potassium thiocyanate 1 kg 1.05125.1000 1-Propanol 1 l 1.00997.1000 2-Propanol 2,5 l 1.09634.2500 Pyridine 2,5 l 1.09728.2500 Pyrogallol (1,2,3-trihydroxybenzene) 50 g 1.00612.0050 Silica gel with moisture indicator (blue gel, 0,2-1 mm, desiccant) 1 kg 1.01908.1000 Silica gel with moisture indicator (blue gel, 1 3 mm, desiccant) 1 kg 1.01925.1000 Silver diethyldithiocarbamate (reagent for arsenic and antimony) 5 g 1.01515.0005 Silver sulfate 100 g 1.01509.0100 Sodium acetate (anhydrous) 1 kg 1.06268.1000 Sodium acetate trihydrate (indifferent to potassium permanganate) 1 kg 1.06267.1000 Sodium carbonate (anhydrous) 1 kg 1.06393.1000 Sodium chloride 1 kg 1.06404.1000 tri-sodium citrate dihydrate 1 kg 1.06448.1000 Sodium dichromate dihydrate 1 kg 1.06336.1000 Sodium diethyldithiocarbamate trihydrate (reagent for copper) 100 g 1.06689.0100 Sodium dihydrogen phosphate monohydrate 1 kg 1.06346.1000 tetra-sodium diphosphate decahydrate 500 g 1.06591.0500 Sodium disulfite (sodium metabisulfite) 1 kg 1.06528.1000 10

ACS Products Designation Package size Cat. No.* Sodium fluoride 1 kg 1.06449.1000 Sodium formate 500 g 1.06443.0500 Sodium hexanitrocobaltate(iii) (sodium cobalt(iii) nitrite) 100 g 1.02521.0100 Sodium hydrogen carbonate 1 kg 1.06329.1000 di-sodium hydrogen phosphate (anhydrous) 2,5 kg 1.06586.2500 di-sodium hydrogen phosphate heptahydrate 1 kg 1.06575.1000 Sodium hydroxide (pellets) (max. 0.02% K) 1 kg 1.06469.1000 Sodium hydroxide (pellets) (max. 0.0002% K) 1 kg 1.06495.1000 Sodium metaperiodate 250 g 1.06597.0250 Sodium nitrate 1 kg 1.06537.1000 Sodium nitrite 500 g 1.06549.0500 Sodium nitroprusside dihydrate (disodium pentacyanonitrosyl ferrate(ii) dihydrate) 1 kg 1.06541.1000 Sodium peroxide 500 g 1.06563.0500 tri-sodium phosphate dodecahydrate 1 kg 1.06578.1000 Sodium sulfate (anhydrous) 1 kg 1.06649.1000 Sodium sulfate (anhydrous, coarse granules 0.63 2.0 mm) 1 kg 1.06637.1000 Sodium sulfate decahydrate 1 kg 1.06648.1000 Sodium sulfite (anhydrous) 1 kg 1.06657.1000 di-sodium tetraborate decahydrate 1 kg 1.06308.1000 Sodium tetraphenyl borate 1 kg 1.06669.1000 Sodium thiosulfate pentahydrate 1 kg 1.06516.1000 Strontium chloride hexahydrate 1 kg 1.07865.1000 Sulfanilic acid 100 g 1.00686.0100 Sulfuric acid 95 98 % 2,5 l 1.00732.2500 L(+)-Tartaric acid 1 kg 1.00804.1000 Tetrahydrofuran 2,5 l 1.09731.2500 Thiourea 250 g 1.07979.0250 Thymol blue (indicator) 25 g 1.08176.0025 Thymol blue sodium salt (water-soluble indicator) 5 g 1.11749.0005 Thymolphthalein (indicator) 25 g 1.08175.0025 Tin(II) chloride dihydrate 1 kg 1.07815.1000 Titriplex II (ethylenedinitrilotetraacetic acid) 1 kg 1.08417.1000 Titriplex III (ethylenedinitrilotetraacetic acid, disodium salt dihydrate) 1 kg 1.08418.1000 Toluene 2,5 l 1.08325.2500 Trichloroacetic acid 1 kg 1.00807.1000 Trichloroethylene 2,5 l 1.11872.2500 1,1,2-Trichlorotrifluoroethane 2,5 l 1.08440.2500 Tris(hydroxymethyl)aminomethane (buffer substance) 500 g 1.08382.0500 Urea 1 kg 1.08487.1000 Xylene 2,5 l 1.08681.2500 Xylenol orange tetrasodium salt (metal (pm) indicator) 5 g 1.08677.0005 Zinc chloride 1 kg 1.08816.1000 Zinc oxide 1 kg 1.08849.1000 Zinc sulfate heptahydrate 1 kg 1.08883.1000 11

We provide information and advice to our customers to the best of our knowledge and ability, but without obligation or liability. Existing laws and regulations are to be observed in all cases by our customers. This also applies in respect to any rights of third parties. Our information and advice do not relieve our customers of their own responsibility for checking the suitability of our products for the envisaged purpose. W. 281128 Release date: October 2005 Merck KGaA 64271 Darmstadt, Germany Fax 0049 (0) 61 51 72-60 80 E-mail: inorganics@merck.de www.merck.de