>> Wederom: ik weet echt niet of er zoiets bestaat als 'needlepoint'. Ik zou daar helemaal niets vanaf laten hangen...
Als je puurheid classificeert aan de hand van termen als 'neeldepoint' zou een reactie waar meer onzuiverheden in zitten inderdaad in een andere klasse kunnen vallen dan een reactie die meer pure LSD bevat. Echter, het verhaal wat betreft het opmaken uit de kleur van het kristal hoe puur het is lijkt mij nogal bullshit. Deze classificatie heeft dan ook alleen zin nadat er een degelijke GC/MS analyse is uitgevoerd bijvoorbeeld. Deze oude post van Shroomery geeft kritiek op het hele classificatie verhaal aan de hand van de kristal kleuring:
First of all, I would like to point out that I am an x-ray crystallographer. My who job consists of crystallizing molecules. When I worked in organic synthesis, we used crystallization as a purification technique. When it comes to biomacromolecules, crystallization is much more difficult and you are far more likely to come across polymorphs.
It is entirely possible to have two very different looking crystals of the same substance with essentially the same purity, just as it is entirely possible to have two similar looking crystals of the same substance with very different purity. You can't tell just by looking!
However, even LSD is known to show crystal polymorphism. This means that, absolutely pure LSD tartrate exists in more than one crystal form.
Furthermore, I will say this. The idea that someone can tell crystal purity by visual inspection alone is complete and utter bullshit. I have seen substances that usually crystallize into beautiful pure white crystals precipitate as purple coloured garbage under the exact same conditions (as far as I can control for, at least). Of course, my first thought upon seeing something like that, is "Oh, my sample sucks. I may as well get rid of it." Further analyses can be very surprising. In this case, it was less than 2% impurity disrupting the crystallization process and adding the purple colour.
I have also seen beautiful crystal that give such garbage diffraction patterns that the purity must have been far below 50%, even though the crystal looked just like the pure ones that gave good diffraction data.
I suggest that you take the "needlepoint, fluff, etc." reports with more than a few grains of salt. It's complete nonsense.
>> Actieve analogen die per ongeluk kunnen ontstaan en op de blotter terecht komen, durf ik me niet over uit te spreken
Ik meen lang geleden in de Erowid LSD vault een stukje gelezen te hebben over een studie waarin gevonden werd dat resten gevonden in LSD ook een kleine psychoactiviteit vertoonde. Het ging echter maar om 1 studie... in de berg papers kan ik hem helaas niet meer snel terug vinden.
>> er zijn mensen die blotters in aluminiumfolie, in een vacuum plastic box, in de vriezer stoppen.
Ik heb dit ook altijd een beetje overdreven gevonden. Op Erowid staat een leuk artikel over een vial Sandoz LSD uit 1951:
An unopened, brown-glass vial of 1951 Sandoz LSD-25 (Delysid) was contributed to a gathering in celebration of Albert Hofmann's 100th birthday. The vial had been in the possession of a single person for the last 30+ years, stored casually, mostly in darkness. When opened, the powder was a very light brown-sugar to salmon color. One chemist described the fluffy, clumpy, sparkly crystalline powder as looking like "crushed needles". It was weighed and dissolved into four-ounce liquid doses containing between 100 and 110 micrograms each (± 10%).
Storage & Degradation
Although the vial was completely sealed, without cracks, one of the major questions was whether there would be significant loss of potency by degradation as a result of the 55 years that had passed since it was manufactured. After trying it, the predominant opinion among the more than 70 participants and observers was that there was no detectable loss in potency. This was the clearest result from the reported experiment: air-tight brown glass appears to be a very effective long-term storage method for LSD. After 55 years, stored at varying room temperatures, the LSD seemed to be fully potent.
>> Misschien zijn er wel stoffen die op (lange)termijn LSD afbreken, of omzetten zoals continuum benoemt met licht, lucht en temperatuur?
Chloride bijvoorbeeld. Nog een kleine toevoeging:
Stability of LSD in transparent containers under light was dependent on the distance between the light source and the samples, the wavelength of light, exposure time, and the intensity of light. After prolonged exposure to heat in alkaline pH conditions, 10 to 15% of the parent LSD epimerized to iso-LSD. Under acidic conditions, less than 5% of the LSD was converted to iso-LSD. It was also demonstrated that trace amounts of metal ions in buffer or urine could catalyze the decomposition of LSD and that this process can be avoided by the addition of EDTA.
- Li Z., McNally A. J., Wang H., Salamone S. J. (October 1998). "Stability study of LSD under various storage conditions". J. Anal. Toxicol. 22 (6): 520–5. PMID 9788528.
Op deze pagina (Rhodium Archive - LSD by Michael Valentine Smith) staat een overzicht met synthese methodes, hierop staan tevens de yields vermeld bij iedere methode en stappen om van iso-LSD naar LSD te gaan:
The following methods all proceed from lysergic acid (I). Methods 1, 2, 4, and 6 give less than 20% iso-LSD in the product but methods 2, 5, and 9 seem to have the highest total yield (about 80%) of LSD plus iso-LSD. Since unreacted lysergic acid can be recovered and run through the synthesis again, and iso-LSD isomerized to LSD as described here, it is probably best to use the simplest methods. These comparative yields come mostly from the reference to method 9.
Wat betreft de zoutvorm schijnt de meest voorkomende vorm LSD tartrate te zijn:
The simplest form of LSD is called the "free base" which means that it is just the LSD molecule itself with no stabilizing salt. The LSD sold on blotter or in other forms on the street is often 'attached' to a salt. One of the most common forms is LSD tartrate, or an LSD molecule with tartaric acid acting to make it a salt.
Hofmann experimented with a 0.5% aqueous LSD tartrate solution, orally administrating a 250 ug dose.
Since that time, LSD (as both the freebase and tartrate) has been illegally distributed for use in many physical forms
- Hallucinogens: A Forensic Drug Handbook
Tablets and pieces of blotter normally contain between 20 and 200 ug of LSD tartrate.
- Handbook of Forensic Drug Analysis
>> En ik weet niet precies hoe ze LSD testen bij het testcentrum
Zie dissertation van T.M Bruntvan het Trimbos DIMS: Chapter 2: The Drug Information and Monitoring System (DIMS) in the Netherlands: implementation, results and international comparison
Qualitative and quantitative analyses of the drugs samples that have been sent to the DIMS Bureau were performed in the laboratory of the Delta Psychiatric Hospital (Deltalab, Poortugaal, The Netherlands), which specializes in analyzing drug samples. A set of robust analytical methods was used to identify known and unknown components, to quantify and classify them. After crushing and homogenizing the sample, three separate analytical techniques were used.
First, thin layer chromatography (Toxilab®A) was performed for identification.
Subsequently, the quantification of the main components (e.g. amphetamine, metamphetamine, 3,4-methylene-dioxyamphetamine (MDA), 3,4-methylene-dioxyethylamphetamine (MDEA), N-methyl-a-(1,3-benzodixol-5-yl)-2-butamine (MBDB), caffeine, cocaine and heroin) was performed with gas chromatography - nitrogen- phosphorous detection (GC-NPD).
In case of any discrepancies, or trace amounts requiring quantification, a gas chromatography-mass spectrometry (GC-MS) method was introduced as the tiebreaker. This generally needed to be done in approximately 10% of the samples. GC-MS (Varian Saturn 4D, Varian Medical Systems, Houten, The Netherlands) conditions were similar to GC- NPD and substances were identified full scan (EI) with the NIST-library. GC-MS was also used for quantification of certain uncommon substances (e.g. γ-hydroxybutyrate (GHB), γ-butyrolactone (GBL), para- methoxyamphetamine (PMA), para-methoxymethamphetamine (PMMA), ephedrine, ketamine and lysergic acid diethylamide (LSD)). In exceptional cases, identification was performed using advanced GC-MS and nuclear magnetic resonance (NMR) spectroscopy structural analysis (e.g. 2,5- dimethoxy-4-bromophenethylamine (2C- , 2,5-dimethoxy-4- bromoamphetamine (DOB) and 4-methylthioamphetamine (4-MTA)).
Deze paper bied mooie overzichten en additionele informatie over de technieken inclusief flow-charts voor analyse: Trans European Drug Information (TEDI) - Guidelines for Drug Checking Methodology. Voor additionele informatie over GC/MS zie pagina 13 t/m 16, hieronder een aantal quotes uit dit stukje:
Gas Chromatography/Mass Spectrometry (GC/MS)
The description of this method comes from the experience of the Drug and Information Monitoring System (DIMS), located at the Trimbos-Institute in the Netherlands. This procedure is validated according to the principles described in ISO 15189.
The Drug and Information Monitoring System (DIMS) was established in 1992 to prevent serious health problems that could arise as a consequence of the consumption of illicit drugs. To this aim, drugs are chemically analyzed by a sub-contracted laboratory which, until 2009, was the Deltalab Laboratory in Rotterdam. From then on this service has been provided by the DSM Resolve Laboratory in Geleen, The Netherlands.
DSM Resolve analyses a fixed amount of drug specimens with a yearly budget. All extra analyses and as- sociated costs are billed separately. The service contract includes: weekly chemical analyses, reporting back to DIMS, feedback, and all material costs associated with the analyses. The agreement also stipu- lates that intellectual ownership of the drug data belongs to DIMS and that nothing concerning this data may be reported without prior consultation. The laboratory applies proprietary analytical methods.
The time elapsed between injection and elution is called the "retention time" (RT). RT helps to differentiate between compounds. However, RT is not always a reliable parameter to determine the unique identity of a compound. If two drug samples do not have overlapping RTs those samples are different substances. Identi- cal RTs for two drug samples do not, however, exclude the possibility that they are in fact different sub- stances. Potentially thousands of chemicals have the same RT, peak shape, and detector response. Consequentially, it is essential to couple GC to mass spectrometry (MS), collectively termed GC-MS.
MS identifies substances by impacting molecules with high energy electrons, this results in their fragmentation into ions with different masses and electric charge (other forms of ionization are also possible, this one is the most common and known as electronic impact). Ions are accelerated through a magnetic field; differences in mass and electric charge determine their speed and the time to reach the detector. The proportion between ions of different masses for a given compound defines its mass spectrum, which is unique for the compound concerned. The intensity of ions is proportional to the amount of a given compound present in the sample. Therefore, the mass spectrum combined with the RT allows the indisputable qualitative identification of compounds while intensity of fragments of ions at this RT allows its quantitation. Mass spectra observed in a given sample are typically compared with computerized (or printed) libraries of reference for the identification of compounds. Mass spectra for psychoactive substances and other drugs are available to the laboratory through relevant chemical and toxicological libraries, either through contacts with forensic institutes or through international connections with the EMCDDA and the Early Warning System.
Summary of analytical characteristics:
Benefits: combining GC with MS is ideal, making qualitative and quantitative determination possible.
Results are highly accurate and small amounts of drugs are needed for analysis. Through the use of an
adequate library of mass spectra it is possible to identify the substances in a sample.
The costs of the technique for the association: the contract with the laboratory is for a maximum of 100 samples per week, this includes LC-DAD quantification of 10 frequent substances and GC-MS of all substances. Special requested analyses and quantifications of unknown or rare substances are excluded.
For a quantity of 100 drug samples, the cost is 31 € per sample. The extra requested analyses cost 82 € per sample. This low price for each sample is linked with the high number of samples analyzed for the laboratory. In other conditions, the price would be higher.
Reliability of results: it is a highly reliable and reproducible method, which has been previously well
described and documented by many groups (forensic, SAMHSA, NIDA, DEA, etc.). It is the golden
Nog een interessant stukje uit het Hallucinogens: A Forensic Drug Handbook wat betreft het leggen van blotters:
However, haphazard dipping, per se, is not the most common way of applying LSD/solvent to paper. Such ungoverned dipping has two drawbacks: first, valueable LSD solution is lost from paper when too much liquid is applied since it often drips off, and second, there is a real possibility of an accidental overdose for the person manipulating the paper. Most large-scale blotting operations attempt to "calibrate" the paper they are using. This is accomplished through experimentation in order to determine how much solution is required to wet the paper up to the edges through the phenomenon of capillary action. The paper is then "laid" out in the orientation in which it will be dried. Next the "calibrated" amount of LSD solution is applied. Often a large syringe or pippette, with or without a hose on the end to direct the liquid stream, is used to both measure the solution and apply the "calibrated" amount.