Manufacturing protocol / Bonner Biotech LLC
This document is the whole job in one place. Part Zero is the materials, held and outstanding. Part One makes the shampoo. Part Two makes the conditioning cream. They are made on different days as different batches, so each part carries its own equipment list, preparations, batch sheet, process, checks and record, and neither depends on the other having been read first. Where one part draws a comparison with the other it is commentary, never an instruction to go and look something up.
If you have not made a cosmetic batch before, these are the terms that appear in the instructions. Nothing here is jargon for its own sake. Each one means something specific that matters.
| Term | What it means |
|---|---|
| Batch | One complete make. Here it is always 2,000 g, which fills eight 8 oz bottles. |
| Phase | A named stage of the process, run at a particular temperature. Phases go in order and are not skipped or reordered. |
| Prep | Something made before starting the batch, in a separate container. The preps are listed in section 1.3 for the shampoo and 2.3 for the conditioner. |
| Deionised water | Water with the dissolved minerals removed. Sold as deionised or distilled water. Not tap water, because the calcium and magnesium in tap water interfere with the hydroxyethylcellulose, with the cationic conditioner, and with both preservative systems. |
| Slurry | A powder stirred into a liquid it does not dissolve in, so the particles end up coated and separated rather than clumped. In Part One it always means hydroxyethylcellulose powder stirred into glycerin. |
| Hydrate / swell | What hydroxyethylcellulose and Polyquaternium-10 do when they meet water: each particle takes up water and swells. It is slow, and it cannot be hurried. |
| Vortex | The dip that forms in the middle of the liquid when the stirrer is fast enough. Sifting a powder onto a moving vortex draws it in grain by grain instead of letting it sit on the surface as a lump. |
| Sift | Shake a powder through a sieve so it falls as a fine, even rain rather than a clump. A kitchen flour sifter is adequate. |
| Tare | Press the zero button on the scale with a container already on it, so the scale reads zero and then weighs only what is added next. |
| Top up to weight | Add deionised water at the end until the batch reaches exactly 2,000 g. This is always the last thing before the final pH check, because water added earlier would throw the weight out. |
| pH | How acidic the batch is, on a scale where 7 is neutral and lower numbers are more acidic. Both products are deliberately acidic. Sections 1.1 and 2.1 explain what goes wrong outside the target ranges. |
| Buffer (pH 4.0 / 7.0) | Small sachets of liquid at a known pH, used to calibrate the pH meter before every use so its readings are true. Not an ingredient. They never go in the batch. |
| Active | An ingredient included for what it does for the user rather than for how the product behaves. In Part One: d-panthenol and niacinamide. In Part Two: d-panthenol and Polyquaternium-10. |
| Surfactant | The ingredients that do the cleaning and make the foam. In the shampoo: sodium cocoyl sarcosinate and cocamidopropyl betaine. The conditioner contains none. |
| Amino acid surfactant | A surfactant built on an amino acid backbone. Sodium cocoyl sarcosinate is built on sarcosine. As a class they are the mildest commercial surfactants available and they carry among the lowest sensitisation rates, which is why the anionic in this formula is one of them. |
| Amphoteric | A surfactant carrying both a positive and a negative charge, so its overall charge depends on the pH around it. Cocamidopropyl betaine is the amphoteric here. It is present for mildness as much as for foam, for the reason given in 1.1. |
| Cationic | Positively charged. Hair carries a slight negative charge, particularly where it is damaged, so a positively charged conditioning agent is attracted to it and stays behind after rinsing. Behentrimonium methosulfate is the cationic in Part Two. |
| Emulsion | A stable mixture of oil and water that would otherwise separate. Part Two is an emulsion. Part One is not. |
| Water phase / oil phase | In an emulsion the water soluble materials are heated in one beaker and the oil soluble materials melted in another. Both reach the same temperature, then they are combined under shear. |
| Heat and hold | Holding both phases at 80 °C for 20 minutes before combining. It melts the fatty materials completely and it pasteurises the water phase. |
| Homogenise | Break the oil into droplets small enough to stay suspended, using high shear rather than gentle stirring. A stick blender does this. A paddle stirrer does not. It is done in short bursts, not one long run, because the motor will otherwise overheat and stop. |
| Gel network | The structure that forms as a cationic and a fatty alcohol crystallise together while the emulsion cools. It is what gives a conditioner its thickness and its slip. It builds over the first 24 hours, so the product on the day is thinner than the product a day later. |
| Syneresis | Water weeping out of an emulsion and pooling, usually at the bottom of the bottle. A sign the gel network did not form properly. See Appendix A.4. |
| Preservative | Stops bacteria and mould growing in the product. The two products use different preservatives on purpose, for reasons given in 1.1 and 2.1. Neither is proven by being in the formula. Appendix C covers the test that proves it. |
| Chelator | Locks up trace metal ions that would otherwise spoil the product and blunt the preservative. Sodium phytate is the chelator in the shampoo. The conditioner has none, for the reason given in 2.1. |
| INCI | The standardised international ingredient name that has to appear on the label. It is often different from the brand name the material was bought under. |
| CoA | Certificate of Analysis, the supplier document stating what is actually in the drum. Appendix B lists what each one must state. Ask for it at the point of order, not after delivery. |
| Deviation | Anything that did not go as this protocol says. Deviations are not failures, but they must be written on the batch record, because if a problem shows up later that record is how the cause is found. |
Taken from the procurement record and checked line by line against the current batch sheets. The batches column is how many 2,000 g batches the held quantity supports at the rates these formulas actually call for.
| Material | Held | Shampoo | Cream | Batches, and notes |
|---|---|---|---|---|
| Sodium cocoyl sarcosinate | 1,000 g, 30% active | 467 g | n/a | 2 batches. This is the constraint on the shampoo. It was three batches under the old three surfactant formula at 300 g. Dropping to two surfactants raised the anionic to 467 g and halved the run. Irrelevant for a 300 g trial, which needs 70 g. Reorder from Formulator Sample Shop when full batches are wanted. |
| Cocamidopropyl betaine | ~6,350 g, 30% active | 200 g | n/a | 31 batches. Ask the supplier for residual amidoamine and DMAPA in ppm, per B.1. |
| Glycerin USP | ~4,769 g | 80 g | 60 g | 59 shampoo or 79 cream. Shared between both. |
| Sodium phytate | 300 g | 3 g | n/a | 100 batches. Large surplus, because the rate fell from 6 g and it left the conditioner entirely. |
| Niacinamide | 800 g | 30 g | n/a | 26 batches. Confirm the grade and get the nicotinic acid limit in ppm on the certificate. |
| Citric acid, anhydrous | 1,000 g | ~5 g | 0 to 2 g | Effectively unlimited. Made up as the 50 percent stock in Prep 1, so 1 kg of powder yields 2 kg of stock. |
| Geogard Ultra | 226.8 g | n/a | 25 g | 9 batches. Conditioner only now, so it lasts far longer than planned. NeoDefend is the identical material if a restock is ever needed. |
| Polyquaternium-10 | 500 g | n/a | 5 g | 100 batches. Large surplus, because the rate fell from 16 g when it stopped being the sole conditioning agent. |
| d-Panthenol | ~72 g, the 60 mL bottle | 10 g | 20 g | Enough for two of each, or several trials. The 1 lb from Lotioncrafter is in 0.2 if it was never ordered. |
| Bottles, 8 oz | Held | 240 g fill | 230 g fill | 8 per batch of either. |
Plantapon LGC Sorb is no longer in either formula and does not need to be chased. It was the sole shampoo blocker in the earlier procurement record, it was sold out in every purchasable size, and it has been replaced by raising the sarcosinate and pairing it with the cocamidopropyl betaine already held.
Three held materials are not used in either product in this document. The caprylic/capric triglyceride, the CBG isolate and the broad-spectrum CRD were the cannabinoid premix in the shampoo. That premix has been removed and the cannabinoids move to a separate overnight scalp serum, which is where they belong. A product left on the scalp overnight gives the contact time a rinse-off never could, and an anhydrous serum needs no solubiliser at all because there is no water to hold the cannabinoids in. None of the three is wasted. They are spent on a different product, which is not specified here.
Three materials are needed and nothing else. Three further lines are listed underneath because they sat on an earlier Lotioncrafter cart that may or may not have been placed. Check the shelf and buy only what is missing.
| Material | Size | Where | What it is for, and what the size gives |
|---|---|---|---|
| BTMS-50 MB, glycol free | 16 oz | Simply Ingredients | The cationic that makes the conditioner a conditioner. 60 g per batch, so about 7 batches. Confirm the listing reads behentrimonium methosulfate and cetyl alcohol only. The common grade sold elsewhere, including Lotioncrafter and Formulator Sample Shop, carries butylene glycol as a third ingredient. |
| Cetearyl Alcohol NF | 1 lb | Lotioncrafter | The structure the cationic sits in. Without it the product is a thin gel rather than a cream. 40 g per batch, so about 11 batches. |
| Caprylhydroxamic Acid GG | 250 ml | MakingCosmetics | The shampoo preservative. Your Geogard only works below about pH 5 and the sarcosinate falls out below 5.2, so there is no pH where the preservative you own and the surfactant you own both work. 30 g per batch, so about 8 batches. |
| Material | Size | Where | Note |
|---|---|---|---|
| Hydroxyethylcellulose | 8 oz / 227 g | Lotioncrafter | 12 g per shampoo batch, 18 batches. Buy the R grade. Record the viscosity grade on arrival, because at 0.6 percent the grade decides whether the shampoo is thin or thick, and it is the one number in the formula that cannot be set without it. |
| Sodium citrate | 1 lb | Lotioncrafter | 4 g per shampoo batch, 113 batches. Buffer only. The shampoo can be made without it and will simply drift acid more readily over months. |
| d-Panthenol, 1 lb | 454 g | Lotioncrafter | Only needed once the 60 mL bottle runs out, which is after two batches of each. Not needed for trials. |
| Item | Note |
|---|---|
| Stick homogeniser | Immersion, stainless shaft. Five minutes of high shear is what forms the emulsion. A paddle stirrer will not do it. |
| Second controlled heat source | Or one water bath that takes both beakers. Both phases must reach 80 °C at the same moment. |
| Beaker, 500 mL borosilicate | For the oil phase. |
| Face shield and heat resistant gloves | For the 80 °C emulsification step. Not optional. |
Four things will ruin a shampoo batch, and the first is a reason not to make a full one yet.
Final pH must be between 5.50 and 5.80, and this window is a compromise between two real constraints rather than a preference. Below it sits the sarcosinate. Its technical literature states that below pH 5 the insoluble free acid form begins to predominate and separates out as a second phase, which implies an apparent pKa near 5 in solution and means that even at 5.5 a meaningful fraction is already present as the free acid. Above it sits the scalp and the hair. The dermatological work on shampoo pH recommends staying at or below 5.5, because higher pH raises the negative charge on the fibre, lifts the cuticle and can irritate the scalp. The two recommendations do not overlap, so the window is set as low as the surfactant will tolerate rather than as low as the hair would prefer. A reading of 5.90 is a correction and a reading of 5.10 is a reject.
The preservative no longer constrains the pH, and that is the point of it. Caprylhydroxamic acid with glyceryl caprylate is effective across pH 4 to 8, so the pH window in this product is set by the surfactants alone rather than by the preservative. It is used at 1.5 percent, which is the bottom of the manufacturer's stated 1.5 to 2.0 percent range, and it is not dosed below that on any account. The previous benzoate system was only properly active below 5.5, which put it in direct conflict with the surfactant floor and left no usable window at all. Do not substitute a benzoate or sorbate preservative back into this formula without moving the pH target down, and the surfactants will not allow that.
The first batch is a trial batch and is not for use until it has stood for four weeks. Two things can only be settled by watching a real batch. Whether the sarcosinate holds in solution at the bottom of the pH window, which fails slowly and looks perfect on the day. And whether the finished viscosity is right, which depends on the grade of hydroxyethylcellulose as much as on the 0.6 percent and is a judgement no calculation settles. Make 200 to 300 g rather than 2,000 g, fill one bottle, hold it at room temperature for four weeks and a second portion at 45 °C for one week, and inspect both against section 1.6 before committing a full batch. The fill weight check in 1.6 does not apply to a trial batch. Everything else does.
Hydroxyethylcellulose is stirred into the glycerin before it ever touches water. Tipped straight into water it forms lumps that never break down. Prep 2 in section 1.3 is that step. It also goes into plain water before anything else. Hydroxyethylcellulose can be hydrated in a surfactant solution, so this is not a chemical impossibility, but it is far slower, far more prone to lumping, and it whips air into a foaming batch that then takes hours to clear. Hydrating it first is the reliable route and there is no reason to do it any other way.
Temperature ceilings are absolute. The preservative goes in between 30 and 40 °C. Panthenol and niacinamide go in at or below 35 °C. The batch never exceeds 70 °C at any point, and it is never reheated after Phase E.
Two surfactants, and the second one is there for mildness rather than foam. An anionic and an amphoteric together form a mixed micelle that is measurably less irritating than either surfactant alone at the same total concentration. Removing the amphoteric would shorten the ingredient list and make the product harsher, which is why it is not treated as optional. Cocamidopropyl betaine is the amphoteric used here. It is mild as a molecule, it is the best foam booster of the available options, and the sensitisation record attached to it belongs to two manufacturing residues rather than to the betaine itself, which is why Appendix B sets a figure for both rather than avoiding the material. Total active surfactant is 10.0 percent, split 7.0 anionic to 3.0 amphoteric, deliberately low for a sensitive scalp. Moderate foam is designed in, and the glyceryl caprylate in the preservative will take a little more off. A rich lather is not the target and chasing one by raising the surfactant load defeats the product.
Lay all of this out and confirm it before weighing anything. Once the hydroxyethylcellulose is swelling in Phase B the beaker cannot be left for 30 to 45 minutes.
| Item | Specification | Notes |
|---|---|---|
| Beaker, primary vessel | 3,000 mL borosilicate | Use the 3,000 mL, not the 2,000 mL. A 2,000 g batch of this shampoo occupies about 1,920 mL, which fills a 2 L beaker to 96 percent with no room to stir and none at all for foam. In the 3 L it sits at about two thirds. Borosilicate only, because soda lime can crack under sustained heat. |
| Hotplate / stirrer | Controlled, ±2 °C | Must take the 3 L beaker. Digital or a controlled water bath. Analogue dials do not hold temperature. |
| Overhead stirrer | Variable speed, low shear paddle | Needed for the 30 to 45 minutes of stirring while the hydroxyethylcellulose swells in Phase B. A magnetic bar will not move a thickening batch. Set the paddle about 2 cm off the base of the 3 L beaker. |
| Probe thermometer | Calibrated | Immerse in liquid, not against the wall. Do not trust the hotplate readout. |
| pH meter | Calibrated, ±0.01 | Calibrate with pH 4.0 and 7.0 buffers immediately before Phase F. |
| Digital scale | 0.1 g, capacity ≥ 3 kg | Tare before each addition. No volumetric measures for actives. |
| Small beaker | 150 to 250 mL | For the glycerin and hydroxyethylcellulose slurry, Prep 2. |
| Glass jar, sealable | 250 mL | For the citric acid stock solution, Prep 1. Label and keep. |
| 8 oz bottles | PET or HDPE, sanitised | 8 per batch. 70 percent IPA, air dried before filling. |
| Item | Notes |
|---|---|
| Nitrile gloves | Change between ingredient handling. Not latex. |
| Safety glasses | Citric acid, warm surfactants, pH adjustment. |
| Lab coat | Long sleeved. |
| Closed toe shoes | Hot liquid spill risk. |
Make both before starting Phase A. Prep 1 keeps for three months and covers many batches. Prep 2 is made fresh for this batch.
One preparation covers many batches. This batch will use somewhere between 6 and 14 g of the stock solution. Always add to pH rather than to a number.
Why this step exists. Hydroxyethylcellulose gives the shampoo its body. It does not dissolve in glycerin, the glycerin only coats it. That coating keeps the particles apart so that when they finally meet water they swell one by one instead of clumping into lumps with dry powder trapped inside. Tipped straight into water the result is lumps that never come out.
Weigh every line to 0.1 g. The citric acid and the final water top-up are approximate because they are added to a target rather than to a weight. Everything else is exact.
| Phase | Ingredient | Grams | % |
|---|---|---|---|
| A | Aqua, deionised, initial charge | 1,040 | 52.00 |
| B | Glycerin USP | 80 | 4.00 |
| B | Hydroxyethylcellulose | 12 | 0.60 |
| C | Sodium phytate | 3 | 0.15 |
| C | Sodium citrate | 4 | 0.20 |
| D | Sodium cocoyl sarcosinate, 30% active nominal | 467 | 23.35 |
| D | Cocamidopropyl betaine, 30% active | 200 | 10.00 |
| E | Caprylhydroxamic acid + glyceryl caprylate + glycerin | 30 | 1.50 |
| E | d-Panthenol | 10 | 0.50 |
| E | Niacinamide | 30 | 1.50 |
| F | Citric acid 50% stock, to pH | ~10 | ~0.50 |
| F | Aqua, top-up to weight | ~114 | ~5.70 |
| Total | 2,000 | 100.00 |
Total active surfactant is 200 g, which is 10.0 percent of the batch, split 7.0 percent anionic to 3.0 percent amphoteric. That figure assumes both surfactants are supplied at 30 percent active. Check each certificate of analysis. If a delivered active percentage differs, recalculate the weight for that line so the active contribution stays the same, and record both the supplied percentage and the corrected weight on the batch record. Do not carry a wrong weight forward because the batch sheet says 467.
Worked example, sarcosinate lot FSS55216. That lot certifies 29.4 percent active rather than 30.0. The line needs 140 g of active, so the corrected weight is 140 divided by 0.294, which is 476 g. Weigh 476 g of that lot, not 467, and write both the 29.4 percent and the 476 g on the batch record. The same calculation applies to the amphoteric line and to the BTMS-50 in Part Two.
Check the betaine certificate for its active percentage too. Cocamidopropyl betaine is normally supplied at 30 percent, which is what the 200 g assumes, but confirm it and correct the weight the same way if the lot differs. Running a nominal weight without confirming the active is how a batch ends up over or under surfactanted with no record of why.
Work straight down. Each phase names the temperature it must be run at. Confirm it on the probe before starting the phase, not after.
Nothing else goes into the beaker during this hold. The water has to be plain when the hydroxyethylcellulose meets it in the next phase.
Do not move on to Phase C until it is smooth. If there are lumps now there will be lumps in the finished bottle, and nothing later in the process removes them. Note that the finished viscosity depends as much on which grade of hydroxyethylcellulose was bought as on the 0.6 percent, so if the trial batch comes out thin, raise the level rather than assuming the process was wrong. Appendix B.1 specifies the grade.
The sodium citrate holds the pH steady on the shelf. Without it the batch drifts acid over months and moves into the range where the surfactants separate. The sodium phytate locks up trace metals, which protects the preservative and stops the batch discolouring. It is also strongly alkaline, at pH 10.7 for a 1 percent solution, and it buffers because it is a polyprotic salt. It is used at 0.15 percent rather than the 0.3 percent carried in earlier drafts, which is ample for a deionised water system and roughly halves the acid demand in Phase F. The preservative itself is no longer added here. It goes in at Phase E, because the glyceryl caprylate in it is better added cool.
Do not attempt to adjust pH in this phase. The batch is not yet at its final weight and the reading will move again once the top-up water goes in.
Panthenol is included at 0.5 percent, which is the useful level for a rinse-off product. Contact time on the scalp is around a minute, and above that level the extra simply goes down the drain. Both panthenol and niacinamide are heat sensitive and they interact, since overheated panthenol produces a breakdown product that then attacks the niacinamide. Keeping the batch cold protects both.
Viscosity continues to build slightly as the batch reaches room temperature.
Run these immediately after filling, and run them again after 24 hours at room temperature. Record both sets on the batch record in 1.8.
| Check | Target | Method |
|---|---|---|
| pH | 5.5 to 5.8 | Calibrated meter at room temperature, at least 10 minutes after the last acid addition. A reading below 5.20 is a reject. Hold the batch and do not try to correct it upward. |
| Appearance | Clear to slight haze, pale straw | Against a white background in natural light. A slight haze from the glyceryl caprylate is normal. Any layer, ring at the neck or sheen on the surface is a reject. Check at 24 hours, at 7 days and at 4 weeks, because the sarcosinate sits near the bottom of its solubility range and if it is going to come out it does so on standing, not on the day. |
| Viscosity | Pourable with body, not water-thin | Record a value if a viscometer is available, otherwise a pour test against a retained standard from a passing batch. |
| Odour | Faint coconut and amino acid | Rancid, ammonia, fishy or fermented is a reject. A faint amine note suggests the panthenol was overheated in Phase E. |
| Foam | Forms within 15 seconds, moderate and creamy | 2 g on wet hands, rub vigorously. Slower to build than a conventional shampoo and that is by design. Weak or absent foam may mean the pH is out of range, so recheck it. |
| Fill weight | 240 g ± 3 g | Weigh a capped bottle and subtract the empty bottle weight. |
The batch passes when pH is in range, appearance is uniform with no second phase, odour is normal, foam forms within 15 seconds and fill weight is within tolerance. Any single out-of-range result holds the batch pending investigation. Go to Appendix A. Release for any use beyond internal trial additionally requires the preservative efficacy report described in Appendix C.
| Stage | °C | °F | Why it matters |
|---|---|---|---|
| A, pasteurisation hold | 70 | 158 | 5 minutes on plain water. It treats the water only, not the batch. |
| B, hydroxyethylcellulose | 40 | 104 | 30 to 45 minutes and it cannot be rushed. It will not swell once the surfactants are in the beaker. |
| C, phytate and citrate | 40 | 104 | Both dissolve readily at this temperature. |
| D, surfactants | 38 to 45 | 100 to 113 | Above 45 °C degrades foam structure. |
| E, preservative | 30 to 40 | 86 to 104 | Warm enough for the glyceryl caprylate to disperse, cool enough not to stress what is already in the batch. |
| E, panthenol and niacinamide | ≤ 35 | ≤ 95 | Never above 70 °C at any point in the run, and no reheating after this phase for any reason. |
| F, pH and top-up | 30 to 35 | 86 to 95 | A consistent temperature gives reproducible pH readings between batches. |
| Fill | 25 to 30 | 77 to 86 | Hot filling deforms bottles and causes condensation under the cap. |
Complete one of these for every shampoo batch and retain it for two years.
| Batch number | SHM-02-S-____ | |
| Date of manufacture | ||
| Operator | initials | |
| Raw material lot numbers | every ingredient, on the reverse if needed | |
| Surfactant active percentages as supplied | both figures, and the corrected weights | |
| Phase A hold temperature / time | target 70 °C, 5 min | |
| Phase B hydration time | target 30 to 45 min at 40 °C | |
| Temperature at Phase D | must be 38 to 45 °C | |
| Temperature at preservative addition | must be 30 to 40 °C | |
| Temperature at Phase E actives | must be ≤ 35 °C | |
| Initial pH before acid | expect 6.0 to 6.8 | |
| Citric acid stock added | g, expect 6 to 14 | |
| Final pH | must be 5.5 to 5.8 | |
| Final batch weight | 2,000 g | |
| Bottles filled | expect 8 | |
| Checks at fill, pass or hold | section 1.6 | |
| Checks at 24 hours, pass or hold | section 1.6 | |
| Appearance at 7 days and 4 weeks | no haze increase, no neck ring, no sheen | |
| Corrections made | Appendix A, corrective, total added, pH before and after | |
| Deviations and actions | anything that departed from this protocol | |
| Released by / date |
This is an emulsion and it is a different kind of make from Part One. Two beakers are heated at the same time to the same temperature and then combined under high shear. The process is unforgiving about temperature and about the order of the two phases, and forgiving about almost everything else.
What the conditioning actually comes from. Behentrimonium methosulfate is a cationic, meaning it carries a positive charge, and hair carries a slight negative charge that is strongest where the cuticle is damaged. It is therefore drawn to the parts of the hair that need it and it stays there after rinsing. As the batch cools, the behentrimonium methosulfate and the fatty alcohols crystallise together into a gel network, and that network is what gives the product both its thickness and its slip. Neither effect can be had from a thickener alone, which is why the previous gel gave wet slip and nothing after drying.
The first batch of this product is a trial batch too. Make 300 g rather than 2,000 g, fill one bottle, and hold it 24 hours, 7 days and then 4 weeks at room temperature with a second portion at 45 °C for 48 hours. Two things can only be answered by watching a real batch. Whether the gel network holds, which shows as separation or as water weeping out and is not correctable. And whether the finished viscosity actually dispenses from the bottle, which is a judgement no calculation settles. Appendix C sets this out alongside the challenge test.
Four things will ruin a conditioner batch once one is being made.
Both phases must be at 80 °C when they are combined. Not one at 80 and the other at 65. Behentrimonium methosulfate starts melting around 60 °C but is not fully incorporated until 80 °C, and cetearyl alcohol melts in the high forties. If either is not fully molten when the phases meet, the unmelted fraction sets as grit that never redisperses. Two heat sources running together, or one water bath large enough to take both beakers, is a requirement and not a convenience.
The oil phase goes into the water phase, never the other way round. Pour steadily while the homogeniser is already running. Adding the water to the oil gives an unstable emulsion that may look right on the day and separate within a week.
Cool slowly and keep stirring the whole way down. The gel network forms as the batch cools through roughly 60 °C down to 40 °C, and it needs gentle continuous movement to form evenly. An ice bath, or leaving the beaker to stand still, gives a grainy or watery product. Expect 45 to 60 minutes of cooling.
Final pH must be between 4.00 and 4.50 at 24 hours, and the 24 hour reading is the one that decides. Cationic deposition onto hair improves as pH falls, the benzoate is properly effective below 4.5 and loses reliability above 5.0, and the emulsion is stable across this range. This product keeps the benzoate system precisely because its pH window and the preservative's window agree.
Expect the batch to arrive in range on its own, and do not force it there with acid. The 25 g of preservative puts a large quantity of gluconolactone into the batch, and gluconolactone is a slow release acidifier that hydrolyses progressively to gluconic acid over the hours after it is added. Left alone this batch is likely to settle somewhere near 4.0 to 4.5 without any citric acid at all. Adding acid on the day on top of that is the most likely way to manufacture a batch that reads below 4.00 the next morning, which Appendix A.3 treats as a hold, and below 3.50 as a reject.
Polyquaternium-10 is present at 0.25 percent and is a supporting ingredient, not the conditioner. At this level it adds wet combing slip during the rinse and nothing that accumulates. It was previously the sole conditioning agent at 0.8 percent, a level that risks building up on fine or long hair over repeated washes, particularly behind a deliberately mild shampoo that will not strip it. Do not raise it above 0.3 percent.
There is deliberately no chelator in this product. Sodium phytate appears in the shampoo but not here, and its absence is a decision rather than an omission. Phytate is a strongly charged polyanion, and this batch is built around a cationic. Anionic and cationic species pair up in solution, and a benzoate or a phytate that is ion paired with a C22 quaternary is neither preserving the product nor depositing on hair. With deionised water throughout there is very little for a chelator to do here, and the risk of blunting both the preservative and the conditioning is not worth taking for it. Do not add one back.
Lay all of this out and confirm it before weighing anything. The two heat sources and the homogeniser are new requirements for this product and the batch cannot be made without them.
| Item | Specification | Notes |
|---|---|---|
| Beaker, water phase | 3,000 mL borosilicate | A 2,000 g batch of this cream occupies a little over 2,000 mL because the emulsion is slightly less dense than water. It will not fit a 2 L beaker at all. Borosilicate only. |
| Beaker, oil phase | 500 mL borosilicate | Holds 100 g of melted fatty material. A second beaker is mandatory, because the two phases are heated separately and combined hot. |
| Heat sources | Two, controlled, ±2 °C | Both phases must sit at 80 °C at the same moment. Two hotplates, or one water bath that takes both beakers. Heating them one after the other does not work, because the first will have cooled below its melting point before the second is ready. |
| Stick homogeniser | Immersion, high shear | Used at the moment of emulsification, in three bursts of 90 seconds rather than one continuous run, because most immersion units are not rated for continuous duty at this volume and cut out thermally partway through. An overhead paddle does not generate enough shear to form the emulsion and will give a batch that separates. The paddle is still needed for the cooling phase. |
| Overhead stirrer | Variable speed, low shear paddle | For hydrating the Polyquaternium-10 and for the 45 to 60 minutes of continuous gentle stirring while the batch cools and the gel network forms. |
| Probe thermometer | Calibrated, two if available | Two probes allow both phases to be watched at once. With one probe, move it between beakers and allow it to settle before reading. |
| pH meter | Calibrated, ±0.01 | Calibrate with pH 4.0 and 7.0 buffers immediately before Phase E. |
| Digital scale | 0.1 g, capacity ≥ 3 kg | Tare before each addition. |
| Sifter or fine sieve | Kitchen flour sifter is adequate | For adding the Polyquaternium-10 in Phase A. Sifting is the difference between a smooth cream and a gritty one. |
| Glass jar, sealable | 250 mL | For the citric acid stock solution, Prep 1. A jar made for a shampoo run serves equally here. |
| 8 oz bottles | PET or HDPE, sanitised | 8 per batch. 70 percent IPA, air dried before filling. A disc or flip cap dispenses this viscosity better than a narrow nozzle. |
| Item | Notes |
|---|---|
| Nitrile gloves | Change between ingredient handling. Not latex. |
| Face shield | Required, not optional, and worn over the safety glasses for Phase C. Molten fatty material at 80 °C meeting a running homogeniser is the most dangerous moment in either process. |
| Heat resistant gloves | For handling the oil phase beaker at 80 to 85 °C. Nitrile alone is not adequate for this. |
| Safety glasses | Throughout. Under the face shield during Phase C. |
| Lab coat | Long sleeved. This process runs hotter than the shampoo and splashes at the moment of emulsification. Keep the beaker on a stable surface at waist height and never hold it while homogenising. |
| Closed toe shoes | Hot liquid spill risk. |
Only the citric acid stock is made in advance. There is no slurry in this product. The Polyquaternium-10 is sifted directly into the water phase.
One preparation covers many batches, and a jar made for a shampoo run is equally good here. This batch will usually use none of it at all, and at most about 4 g, and only if the reading at Phase E is above 4.8. Section 2.5 explains why acid is withheld on the day.
Weigh every line to 0.1 g. The citric acid and the final water top-up are approximate because they are added to a target rather than to a weight. Everything else is exact.
| Phase | Ingredient | Grams | % |
|---|---|---|---|
| A | Aqua, deionised, initial charge | 1,600 | 80.00 |
| A | Polyquaternium-10 | 5 | 0.25 |
| A | Glycerin USP | 60 | 3.00 |
| B | Behentrimonium methosulfate + cetyl alcohol, 50% active | 60 | 3.00 |
| B | Cetearyl alcohol | 40 | 2.00 |
| D | d-Panthenol | 20 | 1.00 |
| D | Gluconolactone + sodium benzoate + calcium gluconate | 25 | 1.25 |
| E | Citric acid 50% stock, only if pH exceeds 4.8 | 0 to 4 | 0 to 0.20 |
| E | Aqua, top-up to weight | ~190 | ~9.50 |
| Total | 2,000 | 100.00 |
The ratio in Phase B is what sets the texture, and it is a ratio with a normal range. The 60 g of BTMS-50 contributes about 30 g of behentrimonium methosulfate and about 30 g of cetyl alcohol, and the separate 40 g of cetearyl alcohol brings total fatty alcohol to about 70 g. That is 3.5 percent fatty alcohol against 1.5 percent cationic, a ratio of about 2.3 to 1. Rinse-off conditioners run 2 to 1 through 3 to 1 and this sits in the lower half of that range. Running leaner on fatty alcohol than that, which an earlier draft of this formula did at 1.6 to 1, leaves more cationic than there is lipid structure to hold it, and an under-structured gel network is the direct cause of the syneresis fault in Appendix A.4.
Confirm the BTMS composition from the certificate rather than by subtraction. Most BTMS-50 sold to small formulators has the INCI behentrimonium methosulfate (and) cetyl alcohol (and) butylene glycol, with actives quoted as a range of 48 to 50 percent. The figures above assume a two component grade at 50 percent. If the grade supplied carries butylene glycol, take the cetyl alcohol percentage from the certificate and recompute the fatty alcohol total from that figure, never from 100 minus the active.
Work straight down. Phases A and B run at the same time in separate beakers and must arrive at 80 °C together.
The 20 minute hold at 80 °C does two jobs. It pasteurises the water phase, and it puts it at the temperature the oil phase needs. Note the wording. It pasteurises the water phase only, because everything added after Phase C goes in cold and carries its own bioburden, which is why the challenge test in Appendix C is what the product actually rests on.
80 °C is not a rounded up 75. Behentrimonium methosulfate begins to melt around 60 °C, but suppliers specify heating to at least 80 °C to melt and incorporate it fully, and at 75 °C a residual unmelted fraction is common even when the beaker looks clear. That fraction re-sets on cooling as permanent grit, which Appendix A.4 lists as not correctable. Look at the beaker base against the light before proceeding.
The product will look thinner at 50 °C than expected. That is correct. Most of the thickness arrives in the last 15 °C of cooling and it continues to build for 24 hours after filling.
The two brand names are the same material and are interchangeable gram for gram. It is used at 1.25 percent. The lot on file certifies 24 percent sodium benzoate, which puts the delivered benzoate at 0.30 percent of the batch, and at pH 4.3 that is roughly 0.13 percent as free benzoic acid against a commonly cited minimum of 0.05 percent. That is a real margin. Going higher was considered and rejected, because every extra gram of this material is also another gram of gluconolactone acidifying the batch overnight.
The top-up water should be at roughly batch temperature. Cold water added to a setting emulsion causes local thickening that shows as lumps.
Why there is no acid target on the day. Gluconolactone hydrolyses to gluconic acid over the hours after it is added, and that pulls the pH down by several tenths of a unit during the first day. An earlier draft of this protocol titrated to 4.3 to 4.5 at fill and expected the drift to land the batch in range. On the quantity of gluconolactone this formula carries, that approach risks manufacturing its own reject overnight. The safer instruction is the one above: read, record, fill, and let the 24 hour reading decide. If the batch reads high at 24 hours it can still be corrected then, and a correction made against a settled reading is a far better one than a correction made against a moving one.
The cream in the bottle at 24 hours is noticeably thicker than the cream that went in. Judge the finished viscosity then, never at the point of filling.
Run these immediately after filling, again after 24 hours at room temperature, and again at 7 days. An emulsion fails later than a solution does, so the 7 day check is the one that matters most.
| Check | Target | Method |
|---|---|---|
| pH | 4.00 to 4.50 at 24 hours | Calibrated meter at room temperature, not at fill temperature. The 24 hour reading is the only one that decides the batch, because gluconolactone hydrolysis carries the pH down over the first day. Expect the fill reading to be several tenths higher than the 24 hour reading. Above 5.00 at 24 hours is a reject, because the preservative is no longer reliably effective there. Below 3.50 go to Appendix A.3. |
| Appearance | Uniform opaque white to off-white | Against a white background in natural light. No yellowing, no visible specks, no streaking. |
| Texture | Smooth, no grit | Rub a small amount between finger and thumb. Any grittiness means unmelted fatty material or unhydrated Polyquaternium-10. Go to Appendix A.4. |
| Viscosity | Pourable cream at 24 hours | Invert a filled bottle. It should move under its own weight within about 5 seconds. Faster than 1 second is too thin, slower than 15 seconds is too thick to dispense. |
| Separation | None at 24 hours or 7 days | Look for a clear layer at the top, an oily film, or water pooled at the base. Any of these is a reject. This is the check that catches a failed emulsion. |
| Accelerated stability | No separation after 48 hours at 45 °C | Hold one filled bottle in an oven or incubator at 45 °C for 48 hours, then cool to room temperature and inspect. A batch that separates here will separate on a shelf within months. Run this on the first batch of any new lot of BTMS-50. |
| Slip | Wet comb passes without catching | Apply to a wetted tress or a section of hair, rinse, then comb. Compare against an untreated section. The difference should be obvious and immediate. |
| Odour | Faint waxy, otherwise neutral | Rancid, sour or fermented is a reject. |
| Fill weight | 230 g ± 3 g | Weigh a capped bottle and subtract the empty bottle weight. |
The batch passes when pH is in range, the cream is uniform and free of grit, nothing has separated at 24 hours or 7 days, slip is demonstrable and fill weight is within tolerance. Any single out-of-range result holds the batch pending investigation. Go to Appendix A. Release for any use beyond internal trial additionally requires the preservative efficacy report described in Appendix C.
| Stage | °C | °F | Why it matters |
|---|---|---|---|
| A, Polyquaternium-10 | 40 | 104 | Warm enough to hydrate in 20 minutes, cool enough to control the vortex while sifting. |
| A, water phase hold | 80 | 176 | 20 minutes. Pasteurises the water phase and matches the oil phase. |
| B, oil phase | 80 to 85 | 176 to 185 | Must be completely clear. Suppliers specify at least 80 °C. Unmelted behentrimonium methosulfate sets as permanent grit. |
| C, emulsification | 80 | 176 | Both phases at the same temperature at the moment they meet. Below 78 °C on either side, stop and reheat. |
| C, cool down | 80 to 40 | 176 to 104 | 45 to 60 minutes with continuous gentle stirring. The gel network forms below about 60 °C and cannot be hurried. |
| D, panthenol and preservative | ≤ 40 | ≤ 104 | No reheating after this phase for any reason. |
| E, pH reading and top-up | 35 to 40 | 95 to 104 | Read warm and record the temperature. Top-up water at roughly batch temperature, or local thickening shows as lumps. |
| Fill | 35 to 40 | 95 to 104 | Filled warm on purpose. Below 30 °C it is too thick to transfer cleanly. |
Complete one of these for every conditioner batch and retain it for two years.
| Batch number | SHM-02-C-____ | |
| Date of manufacture | ||
| Operator | initials | |
| Raw material lot numbers | every ingredient, on the reverse if needed | |
| BTMS-50 composition as supplied | active, cetyl and any glycol, plus corrected weight | |
| Polyquaternium-10 hydration time | target 20 min at 40 °C | |
| Water phase temperature at combine | must be 78 to 85 °C | |
| Oil phase temperature at combine | must be 78 to 85 °C | |
| Oil phase fully clear before combine | yes or no, and action if no | |
| Homogenisation | three bursts of 90 seconds | |
| Cool down time, 80 to 40 °C | target 45 to 60 min | |
| Temperature at Phase D | must be ≤ 40 °C | |
| pH before any acid | expect 4.2 to 5.0 | |
| Citric acid stock added | g, expect 0 unless pH exceeded 4.8 | |
| pH at fill, with temperature | record only, not a gate | |
| Final batch weight | 2,000 g | |
| Fill temperature | must be 35 to 40 °C | |
| Bottles filled at 230 g | expect 8 | |
| Checks at fill, pass or hold | section 2.6 | |
| pH at 24 hours, room temperature | must be 4.00 to 4.50, this is the gate | |
| Checks at 24 hours, pass or hold | section 2.6 | |
| Checks at 7 days, pass or hold | section 2.6 | |
| Accelerated stability, 48 h at 45 °C | first batch of any new BTMS lot | |
| Corrections made | Appendix A, corrective, total added, pH before and after | |
| Deviations and actions | anything that departed from this protocol | |
| Released by / date |
A batch cannot be titrated while a corrective is being weighed out from powder. Make both of these in advance and keep them on the bench next to the pH meter. Between them they move the pH in either direction using nothing that is not already in one of the two formulas.
Why sodium citrate and not an alkali. It is the conjugate base of the citric acid already in the batch, so correcting with it moves the pH along a buffer pair that is already there rather than introducing new chemistry. It is also gradual, which makes it very hard to overshoot. Sodium hydroxide would be the industrial answer and it is the wrong tool at this scale, because it creates local zones of very high pH as it disperses, and in a batch containing panthenol and a preservative that is a real risk. Do not use sodium bicarbonate, because it will react with the citric acid, release carbon dioxide, and foam a surfactant batch out of the beaker.
Target is 5.50 to 5.80. Find the reading in the first column and work across. The bands are written to two decimal places and are contiguous, because the meter reads to two decimal places and a reading of 5.85 must land somewhere.
| Reading | Verdict | Action |
|---|---|---|
| Below 5.20 | Reject | The sodium cocoyl sarcosinate is at or past its solubility limit and the insoluble free acid form predominates. The amphoteric is unaffected and is not the problem. The batch may look clear today and will separate over weeks. Do not correct upward and do not fill. Hold, record the deviation, and dispose. Investigate the acid addition step before the next run. |
| 5.20 to 5.49 | Correctable, hold | Add sodium citrate 20 percent solution in 1 g steps, stirring and waiting 30 seconds between readings, until the reading reaches 5.50 to 5.80. Record the total added. The batch is saleable only if the total sodium citrate solution added is under 15 g and the 24 hour appearance check passes with no haze increase and no second phase. |
| 5.50 to 5.80 | In range | Proceed to top-up and fill. |
| 5.81 to 6.30 | Correct down | Continue adding citric acid 50 percent stock in 0.5 g steps. This is the normal position mid-titration and is not a deviation unless it occurs after the final top-up. |
| Above 6.30 after acid | Investigate | Either the citric acid stock is weaker than it should be, most likely past its 3 month life, or the sodium citrate was over-weighed in Phase C. Make fresh stock, verify the Phase C weight against the batch sheet, and record the finding before continuing. |
Target is 4.00 to 4.50, read at room temperature at 24 hours rather than at fill. Every row below is an action taken after the batch has been filled and stood, because under this protocol no acid is added on the day. The bands are contiguous to two decimal places.
| Reading | Verdict | Action |
|---|---|---|
| Below 3.50 | Reject | Too acidic for the emulsion to hold reliably and harsh on the scalp. Correcting back up from here needs enough sodium citrate to shift the electrolyte balance and destabilise the gel network. Hold and dispose. |
| 3.50 to 3.99 | Correctable, hold | Add sodium citrate 20 percent solution in 0.5 g steps until 4.00 to 4.50 is reached. Saleable only if the total added is under 8 g and no separation appears at 24 hours and 7 days. Emulsions tolerate added electrolyte less well than solutions do, so the allowance here is tighter than in A.2. |
| 4.00 to 4.50 | In range | Release subject to the other checks in 2.6. No action. |
| 4.51 to 5.00 | Correct down, hold | The batch has settled higher than expected, which means the gluconolactone hydrolysed less than usual. Return the bottles to the beaker, warm gently to 35 °C with stirring, add citric acid 50 percent stock in 0.5 g steps to reach 4.00 to 4.50, then refill. Record as a deviation and re-run the 24 hour check from the new fill. |
| Above 5.00 at release | Reject | The preservative is not reliably effective above 5.0 and the product cannot be relied on to stay clean for its shelf life. Do not release, whatever the other checks say. |
These faults have no equivalent in Part One. An emulsion can be made wrong in ways that only show up after it has stood, which is why the 24 hour and 7 day checks are not optional.
| What is seen | Cause | Action |
|---|---|---|
| Gritty between the fingers | Oil phase was not fully molten at combine, or the Polyquaternium-10 was dropped in rather than sifted. | Not correctable. The unmelted fraction will not redisperse by reheating, because it re-sets on cooling in the same state. Reject. Next batch, hold the oil phase until it is completely clear and sift the Polyquaternium-10 onto a moving vortex. |
| Too thin, will not build overnight | Insufficient shear at emulsification, or fatty alcohol under-weighed, or cooled too fast. | Recoverable once. Reheat the whole batch to 70 °C with stirring, homogenise 5 minutes, then cool slowly with continuous stirring as in Phase C. Re-add nothing. Record as a deviation and re-run every check. If it is still thin after a second 24 hours, reject. |
| Clear or oily layer on top at 24 h or 7 d | The emulsion did not form. Usually the phases were at different temperatures, or the water was added to the oil. | Not correctable. Reject. This is the fault the accelerated stability check is designed to catch before eight bottles are committed. |
| Water pooled at the base, syneresis | Gel network formed incompletely, almost always from cooling too fast or stirring stopping partway down. | Not correctable. Reject. Next batch, extend the cool down to the full 60 minutes and do not leave the beaker unattended. |
| Too thick to pour from the bottle | Cetearyl alcohol over-weighed, or an unusually high cetyl fraction in the BTMS lot. | Not a reject. The product is functional and simply awkward to dispense. Use it. On the next batch reduce the cetearyl alcohol to 30 g, which is the lowest that still holds the fatty alcohol to cationic ratio at 2 to 1, and record the change against the BTMS lot number. |
| Yellowing over days | Trace metal contamination, usually iron from tap water or an unsuitable vessel. | Not correctable. Reject. Confirm deionised water was used throughout and that no steel utensil entered the batch. |
| Material | INCI | Specification | Certificate must state |
|---|---|---|---|
| Deionised water | Aqua | Deionised or distilled, not tap | Conductivity where supplied commercially. Record the source on the batch record. |
| Glycerin | Glycerin | USP or Ph. Eur., vegetable origin | Assay and origin. |
| Hydroxyethylcellulose | Hydroxyethylcellulose | Cosmetic grade | Viscosity grade, as a specification and not a record-only field. Grades range from roughly 75 to 5,000 centipoise at the same nominal concentration, so at 0.6 percent the same weight of a different grade gives anything from water to a firm gel. Specify a high viscosity grade in the region of 3,400 to 5,000 centipoise at 1 percent and buy the same grade every time. This system cannot be salt-thickened as a rescue, because hydroxyethylcellulose is non-ionic. |
| Sodium phytate | Sodium Phytate | White powder or crystals, not a solution. Shampoo only | pH of a 1 percent solution, calcium content, sulfate content and a microbial panel. Lot FSS55599 on file certifies pH 10.7, calcium and sulfate each at or below 0.01 percent, total count and yeast and mould each below 100 CFU/g and zero Gram negative bacteria. The form matters, because the batch sheet weights assume the solid. A solution grade would need recalculating for its stated active. |
| Sodium citrate | Sodium Citrate | USP or food grade | Assay. |
| Citric acid | Citric Acid | Anhydrous, USP or food grade | Assay. Anhydrous, not monohydrate, or the stock solution strength is wrong. |
| Sodium cocoyl sarcosinate | Sodium Cocoyl Sarcosinate | 30 percent active liquid | Active percentage, sodium chloride content and pH of a 10 percent solution. Also written confirmation that no nitrosating agent is used in manufacture or present in the supply chain, which is the standing condition on the safe use of sarcosinates. Lot FSS55216 on file certifies 29.4 percent active, 0.1 percent sodium chloride and pH 7.6, and requires remixing before weighing because it sediments on standing. |
| Cocamidopropyl betaine | Cocamidopropyl Betaine | 30 percent active liquid, high purity grade | Active percentage, sodium chloride content, and residual amidoamine and residual DMAPA each stated as a figure in ppm. The residual figures are the point of this row. The sensitisation record attached to this material belongs to those two manufacturing impurities and not to the betaine, so a lot with low residuals is a mild, well understood surfactant and a lot with unstated residuals is an unknown. Reject any lot where amidoamine exceeds 10 ppm or where either figure is absent from the certificate. |
| Preservative, shampoo | Caprylhydroxamic Acid (and) Glyceryl Caprylate (and) Glycerin | As supplied, used at 1.5 percent | Composition and active percentages. Effective across pH 4 to 8, which is why it is in Part One. The manufacturer states a use range of 1.5 to 2.0 percent, so 1.5 is the floor and not a nominal figure to be trimmed. |
| Preservative, conditioner | Gluconolactone (and) Sodium Benzoate (and) Calcium Gluconate | As supplied, used at 1.25 percent | Sodium benzoate percentage, gluconolactone percentage, calcium gluconate percentage and water content. Sold as Geogard Ultra or NeoDefend, the same material under two names, interchangeable gram for gram. The calcium gluconate third component must appear on the label INCI and is often omitted from secondary literature. Lot FSS54476 on file states 76 percent gluconolactone, 24 percent sodium benzoate and 0.2 percent water against specification ranges of 70 to 80 and 22 to 28, and does not quantify the calcium gluconate. Those figures are the lot result rather than a full composition, so require the calcium gluconate figure on the next certificate. |
| d-Panthenol | Panthenol | D isomer, 98 percent or better | Assay and isomer confirmation. The racemic DL form has roughly half the activity at the same weight. |
| Niacinamide | Niacinamide | USP | Assay and nicotinic acid content. Nicotinic acid is the flushing impurity and the degradation product, so a low figure on arrival gives more shelf life before it matters. |
| BTMS-50 | Behentrimonium Methosulfate (and) Cetyl Alcohol, glycol free grade preferred | Active percentage per certificate | Every component with its percentage, not just the active. Most grades sold to small formulators are behentrimonium methosulfate (and) cetyl alcohol (and) butylene glycol with actives quoted as 48 to 50 percent, and the glycol adds an ingredient this formula does not need. Whichever grade is supplied, take the cetyl alcohol figure from the certificate and never from 100 minus the active. A lot running high on cetyl gives a thicker cream at the same weight, which is the cause listed against that fault in A.4. |
| Cetearyl alcohol | Cetearyl Alcohol | Cosmetic grade, C16 and C18 | C16 to C18 ratio and melting range. |
| Polyquaternium-10 | Polyquaternium-10 | Cosmetic grade | Viscosity grade and nitrogen content. |
| Bottles | n/a | 8 oz PET or HDPE with disc or flip cap | Food or cosmetic contact grade confirmation. |
A batch is not started until every material going into it has a certificate on file carrying the figures named in B.1. Three are held. The remainder are outstanding and are listed here so the gap is visible rather than discovered at the bench.
| Material | Status | What the certificate gives, or what is still needed |
|---|---|---|
| Sodium cocoyl sarcosinate | On file | Lot FSS55216, manufactured 20 July 2026, retest 20 July 2027. Active 29.4 percent, sodium chloride 0.1 percent, pH 7.6 at 10 percent. Apply the corrected weight worked in section 1.4. |
| Geogard Ultra | On file | Lot FSS54476, manufactured 10 June 2026, retest 10 June 2027. Gluconolactone 76 percent, sodium benzoate 24 percent, water 0.2 percent. INCI carries a calcium gluconate third component. |
| Cocamidopropyl betaine | Held, figures outstanding | The material is in stock. What is missing is the residual amidoamine and DMAPA figures in ppm, which is one email to the supplier. Not a blocker for a trial batch. It is a blocker for selling the product on a hypoallergenic claim, because that claim rests on this number rather than on an assumption. |
| BTMS-50 | Not yet ordered | Request at the point of order. Active percentage and cetyl alcohol fraction. |
| Cetearyl alcohol | Not yet ordered | Request at the point of order. C16 to C18 ratio and melting range. |
| Caprylhydroxamic acid blend | Not yet ordered | Request at the point of order. Composition and active percentages. |
| Sodium phytate | On file | Lot FSS55599, manufactured 18 August 2026, retest 18 August 2027. Supplied as a white powder. pH 10.7 at 1 percent, calcium and sulfate each at or below 0.01 percent, and a full microbial panel passing. The low calcium figure matters, because calcium competes for the chelation this material is in the formula to provide. |
| Remaining materials | Outstanding | Glycerin, hydroxyethylcellulose, sodium citrate, citric acid, d-panthenol, niacinamide, Polyquaternium-10. Standard assay certificates, per B.1. |
Nothing on this list now blocks a batch. Removing the cannabinoids from the shampoo took the one genuinely blocking certificate out of the product, because that was the certificate underwriting the legal THC content per container. What remains are ordinary incoming quality records, and a missing one delays a release rather than stopping a make. The residual amidoamine and DMAPA figures for the betaine are the exception in one narrow sense: not a blocker for making a batch, but a blocker for making a hypoallergenic claim about it.
Both products are water based, both have a water activity close to 1, and both are preserved with organic acid systems rather than with a broad spectrum synthetic. Neither can be assumed to be adequately preserved on the strength of the formula alone. A challenge test is what turns that assumption into evidence.
Do not release either product beyond internal trial use without a passing challenge test in hand. Use ISO 11930 or USP 51, run on the finished product, made to this protocol, in its final packaging. Treat the conditioner as the more likely of the two to fail, and treat that as a real possibility rather than a formality. Its preservative works through undissociated benzoic acid, and a benzoate ion paired with a C22 quaternary is not doing that job. If it fails, the answer is a cationic compatible preservative rather than more of the same one. This is the single most consequential test on either formula, and it is the one that protects the person using the product rather than the appearance of the batch.
The test is run once per formulation rather than once per batch. It must be repeated whenever any of the following changes: the preservative or its level, the pH target, any surfactant in Part One, the cationic or fatty alcohol in Part Two, the packaging, or the water source. Retain the report against the product file for the life of the formulation.
| Test | When | Purpose |
|---|---|---|
| Challenge test, ISO 11930 or USP 51 | Once per formulation, before any release | Proves the preservative system holds against bacterial, yeast and mould challenge for the shelf life. |
| Trial batch, 200 to 300 g | Both products, before the first full batch of either | Held four weeks at room temperature and one week at 45 °C, then inspected against the release checks. For the shampoo this is what answers the sarcosinate solubility question in section 1.1 and settles the finished viscosity. For the conditioner it answers whether the viscosity dispenses from the bottle and whether the gel network holds. |
| Accelerated stability, 48 h at 45 °C | Conditioner, first batch of each new BTMS lot | Catches an emulsion that will separate on a shelf within months. |
| Micro count on finished batch | Periodically, and on any batch with a deviation | Total viable count and absence of specified organisms. Confirms the process is clean, as distinct from confirming the preservative works. |
The term hypoallergenic has no legal definition in the United States. The Food and Drug Administration attempted to define and regulate it in the 1970s and the rule was struck down, so the word may be used but it carries no agreed standard and no automatic support. What gives it substance is the specific, documented evidence behind it.
Four things support the positioning on these formulas, and three of them are already in place. The products carry no added fragrance, no essential oil and no colourant, which removes the largest single category of cosmetic contact allergens. Both preservative systems are among the lower sensitisers available. The shampoo's anionic is amino acid derived, which is the mildest commercial surfactant class, and it is paired with an amphoteric rather than used alone, so the mixed micelle makes the system gentler than the sum of its parts. The one surfactant with a documented sensitisation record, cocamidopropyl betaine, is controlled by the residual specification in Appendix B rather than by assumption, because the risk in that material sits in two manufacturing impurities that a certificate can put a number against.
The fourth is a human repeat insult patch test on the finished product, typically 50 to 200 subjects, which is the evidence a retailer or a practitioner will ask for. It is not required for personal or internal use and it is not a substitute for the challenge test in C.1, which addresses a different risk entirely. It becomes necessary at the point the positioning is used in trade.
One honest limit on the claim. No formula containing surfactants is free of sensitisation potential, and a product that cleans hair cannot be. What this specification does is remove the avoidable allergens, characterise the unavoidable ones, and put a number on the residuals that carry the risk. That is a defensible position. A claim that the products contain no allergens is not, and should not appear on any label or in any material.